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Principles of Plant Design

Assignment: Design a single process unit plant to produce any product. Carefully explain
the sub units below: Introduction given justification of the design, flow sheet and layout,
mass and energy transfer (evemn if it is a physical process), mechanical design,
equipment selection, piping of material input and output, Risk analyses and
instrumentation and cost of setting up the plant.

Unit 1: Introduction: Chemical engineering design


Unit 2: Process design principles
Unit 3: Flow sheets/ Plant layout
Unit 4: Mass and Heat transfers
Unit 5: Equipment Selection
Unit 8: Mechanical design of equipment
Unit 10: Piping and Instrumentation
Unit 11: Costing and project evaluation

Week 1: Introduction: Chemical engineering design


Q 1. What quality parameters will you recommend to someone
wanting to purchase/produce a given product.
INTRODUCTION
Growth of chemical industry is determined by the extent of modernization of
the chemical technology. Increased productivity, better quality products and
reduced overhead cost are the major parameters used in assessing a
progressive technology. These parameters can be improved by:
1. Expansion of production system or the productivity of the chemical
technological systems;
2. Intensification of the production efficiency;
3. Reducing electricity consumption and maximum utilization of heat of
chemical reactions;
4. Reducing the production stages and conversion to closed circuit
system;
5. Transition from batch to continuous process and
6. Automation of the production processes.
Productivity P can be defined as the quantity of product Q obtained or utilized
raw material per unit time.

Q
(kg / hr )................................................................................................4
t

Productivity can also be measured in terms of volume Qv as

Qv 3
(m / hr )......... ...................................................................................5
t

Increased quantity of raw material per reaction volume enhances economy of product unit
cost. Increased reactors geometrical dimension and productivity reduces the amount of
working capital by enhancing the heat utilization efficiency, utility coefficient of raw
material and the human resources. As a result of these economic advantages, for quite a
long time, intensification of production was directed at increasing the volume of reactors.
However, increased reactors volume is accompanied by corresponding technological
problems particularly hydraulic instability, non-uniform temperature and concentration

distribution. These problems have limited the scope of application of volume increase as
a means of intensification of technological process.

At present greater emphasis is placed on increasing the efficiency of the


reactors. Efficiency can be defined as the productivity per unit volume v
(m3) or area (m2) of the reactor.

P Q
............................................................................................6
v tv

Qv
..........................................................................................................7
tv

P Q
...................................................................................................8
s ts

or

or

High efficiency can be achieved by:


1. Better design and construction of machines / reactors and
2. Modernization of technological processes.
Efficiency is proportional to the rate of reaction Therefore by studying the
kinetics of technological processes, the act of designing, construction of
reactors / machine and choice of technological regime can be improved upon.
In most recent reactors or modernized ones, intensification of chemical
processes is achieved by better mixing of the reacting components. Increased
efficiency should not be accompanied with corresponding electricity
consumption. Decreased electricity consumption per unit product can be
achieved by:
1.
2.

Reducing the draught resistance in the system;


Reducing the extent of mixing, though this could affect the process
kinetics;
3.
Maximum utilization of heat of chemical reaction for mixing of raw
materials and steam production.
The third point is considered as the most effective means of reducing energy
loss in industry. In most reactors with exothermic reactions, heat exchangers
are installed to optimize reaction kinetics and increase the efficiency of heat
utilization.
Reducing the production stages and transition to closed circuit system will
reduce expenditure on fixed capital and cost of production. Transition to
closed circuit system enhances the conversion from batch to continuous

process. In the batch process materials are loaded into the reactor, where
they undergo a series of physico-chemical transformations and then
discharged after the required retention time. The units operations are labour
intensive and may not be easily mechanized. Automation of batch process is
very difficult to achieve due to the ever-changing technological parameters
(temperature, pressure / concentration, residence time, etc.). In continuous
process, loading of raw materials and discharging of the final product are
continuous and systematized. The technological processes are synchronized
with other secondary and transporting operations. At any given point in the
reactor, the temperature, pressure, concentration, etc. are constant. Hence it
is easy to observe the working regime, mechanize the loading and
discharging operations. Automation can be easily introduced. Better quality
products may be produced and utilization of heat from chemical reaction
better organized.
Mechanization of labour intensive operation and its automation is the most
prospective means of increasing efficiency. Mechanization is the substitution
of human labour with machines. Mechanization enhances productivity by
increasing the level of machines participation while reducing that of man.
Automation can be described as the exclusion of man from the production
processes by automatic mechanisms. Automation is a higher form of
mechanization. It greatly increases productivity and quality of product. In
chemical industry, the common parameters easily automated are
temperature, concentration, flow rate, etc.
Mans ability to obtain a 100% efficient process is still hampered by our
limited knowledge in materials behavior, plant layout techniques and the
consequent influence on plant operability, positioning and number of
compressors, heaters, the desired products etc.
Process design organizes the sequence of bringing together the required
physical and chemical operations. It involves defining the flowsheet,
operation conditions obtained from the material and energy balance,
specifications and materials of construction of the equipment, plant layout,
technical and economic feasibility of the project etc. The degree of
thoroughness of a process design depends on the complexity of the project.
For some only a preliminary design will suffice. Others may require a detailed
design to establish the technical and economic feasibility and safety of the
project.
Practically all engineering process designs involve these basic components:
transport reaction transport. The first transport involves the initial raw
materials or semi finished products from their sources to the reaction zone or
reactors. The second transport is for the removal of the finished products

from the reaction zone to the packaging zone or warehouses. In each of these
stages the focus is cost reduction.
Process equipment can be propriety or custom designed. Propriety equipment
are designed by the manufacturer based on the end user specifications like
pumps, cooling towers, compressors, dryers, mixers, valves, furnaces, etc.
Custom design of a part/unit of equipment is required to complete the
standardization. In specifying for these equipment, only characteristics that
define the process operating conditions are necessary. It is however advisable
to use the standard manufacturer specification form in making any order for
propriety equipment.
Propriety equipment are available off the shelf Custom-designed equipment
may sometime be requested to meet specific characteristics like safety, extra
large or miniature sizes etc. Both the propriety and custom designed
equipment are expected to comply with approved standards and codes from
government agencies, insurance and professional engineering bodies.
Standards and codes have been developed are being improved upon to meet
present
realities
to
ensure
safe
and
economic
design,
construction/fabrication, testing and maintenance of engineering equipment
and structures. Manufacturers and even contractors can develop their
specific standards and codes to ensure high product quality and efficiency of
production, handling and maintenance of processes. Although most standards
and codes are not legalized by the Act, they are respected by stakeholders
since they are seen as compendium of best experiences in their areas.
Modeling
Q 2. What is the role of modeling in the design of a process
technology?
Modeling means the study of a process or reactor through the physical or
mathematical equations or model; that is a simplified system that allows for
direct monitoring and control of phenomena in the process. Models are
prognoses tools for evaluation of chemico- technological processes and
working regime of industrial reactors.
System analysis may be considered in the following stages:

1. Conceptualization and analysis of the object to determine its individual elements


and their relationship. Establish the hierarchical structure and selection of the
desired elements based on the design objects. It is important to effectively
describe a system characteristic design theory and thus evolve the required model
methodology. The conceptual stage actually begins with the descriptive model. It
splits the entire process into units that can be further split into smaller units for

ease of understanding the process phenomena. Entities which are related by


principle and law are grouped into the same unit or sub unit. The extent of
splitting is determined by the researcher experience and knowledge. Particle size
can be considered in the macro, micro, molecular, element, atomic, nano, etc.
depending on the type of system and available mathematical expression of the
process phenomena. Reduction of the particle size significantly complicates the
surface physicochemical processes (see section 2.2 decarbonization model).
Existing mathematical model may not effectively describe the changing surface
phenomena with continuous size reduction.
2. Formulation of the element concepts or idea as mathematical models based on the
identified scientific laws and experimental data. The established mathematical
model can then be used to develop those for the input and output parameters.
3. Mathematical modeling and simulation of the process. The developed software
based on the developed model formula can be used not only in investigate the
process but to make prognoses of the effects of parametric excitations on the
overall technological process. Experimental verification of model portrays the
theoretical level of understanding of the investigated phenomena; neglecting the
adopted assumptions.
4. Identifying physical and mathematical models elements consist of identifying the
independent variables and process state.
The first step in physical and mathematical modeling is to find out the
mathematical functional relation between rate of reaction u or rate constant k
or product output and other technological parameters. The rate of chemical
reaction is mainly dependent on the concentration of the reactants and
products C1, C2, C3; coefficients of effective diffusivity of components D 1, D2,
D3; temperature in the reaction medium T and pressure P; extent of mixing of
reactants (phases) this is dependent on the relative velocity of the phases
wg, wl, ws; catalyst activeness Ac; density of reactants g, l, s; viscosity
coefficient dynamic or kinematic ; surface tension ; geometrical
characteristics of the reactor, height H, diameter D, etc.

u f (C , C , C ...D D , D ..T , P, w , w , w ...A , , , , , H , D)..23


1 2 3 1, 2 3
g l s C g l s
Kinetic characteristics are also dependent on the heat transfer conditions in
the reactor and should be considered during modeling. The deduced optimum
parameters should guarantee minimum cost of production at minimum utility
coefficient of raw materials, energy, fuel and other economic parameters.
There are various modeling techniques, some of which are considered below.

In designing, it is important to have information about the reaction chemical


kinetic and desired capacity of production and then decide if the process
should be continuous or batch and on method of charging and discharging.
Experiments are organized particularly for processes whose mechanism are
poorly understood or lack sufficient data for the researcher to work with and
develop the kinetics. All experimental rates are an embodiment of kinetics
and mass transfer phenomena. When technical grade or synthetic
compounds are involved the derived rates can be a near representation of
the global rate for the reaction as secondary reactions are almost eliminated.
In reacting raw materials, it is not correct to refer to the obtained rate as a
representative of the desired reaction; since there were lots of secondary
reactions also occurring. For reacting natural raw materials experiments are
performed to serve as a guide.
The choice of reactor is influenced by the fact that apart from chemical and
physical processes (diffusion of reactants and products), the production and
distribution of heat also takes place during the production process.
The method of technological calculations and choice of parameters differs
with processes, depending on the type of reactor used. Classifications of
reactors are primarily based on factors influencing the kinetics. Such factors
include the hydrodynamic conditions and temperature regime. Reactors
operating at extreme hydrodynamic regime are classified into ideal plug flow
and well mixed and those at isothermal condition into adiabatic or
polythermal. Such idealized classification helps in eliminating secondary
influences during consideration of the reaction kinetics.
Industrial reactors are far more complex than the ideal ones. Calculations of
industrial reactors parameters are based on experimental data. The ideal
model only serves as reference when determining the basic technological
parameters and reactors dimension. Investigation of reactor characteristics
is performed by mathematical representation of the processes, that is
investigation of changes in T, C, and P. Modeling can be performed for an
infinite elementary size or the complete reactor using the material and
energy balances.

Week 2: Process design principles


DESIGN AS CHEMICAL TECHNOLOGICAL SYSTEM
Q3. A product is as good as the collective quality of the systems
involved. Briefly discuss this statement?

A system is a combination of various subsystems or units. The thorough


knowledge of the fundamental sciences of any complex inter connected and
inter dependent reacting system and its intra connections and intra reactions
with others will greatly enhance the quality of the design to be developed.
The development of any original product therefore starts from the
understanding of the art of the science of the phenomena that brought it into
existence. Each sub system is investigated on its own to determine its
hierarchy, functions and the intra reactions with the other members of the
system. Consequently, one of the major principles of system design is the
analyses and syntheses of the reacting sub systems and their overall
hierarchical relationship.
It is very important to know the main objective/properties of any product to
be designed. The extent to which the quality of the desired product is
achieved in a furnace for example is dependent on physico-chemical
properties of the raw materials, the prevailing internal atmospheric condition
and the chemical composition of the refractory materials etc. If only a
physical change in composition is desired then the possibility of chemical
reaction of the raw materials or its mineralization must be eliminated. When
chemical transformation of the raw materials is desired then the prevailing
technological conditions should ensure their maximum rate of reaction.
Thermal treatment in furnace is also influenced by the prevailing physical and
chemical atmospheric condition in the camera. The atmospheric condition is
determined by the firing regime, composition of the fuel, types and condition
of burners, etc.
Heat treatment directed at physical transformation of the material often
involves not only heat transfer but maybe complicated by mass transfer. The
loss of moisture mass transfer during the initial drying time significantly
dictates the heat transfer mechanism and developed heating regime for a
product. In a heating process like heating, cooling, condensation and
evaporation only the first two is exclusively heat transfer. The others involve
both heat and mass transfer.
In the process of heating or cooling, a material may experience change in its
aggregate structure due to evaporating, condensing, melting or crystallizing.
In these cases, the heat is now distributed not in one phase but into two
phases. In designing for processes undergoing phase change the initial
convective transfer criteria equation, have to be modified by introducing
corrective coefficient to account for the new phase.
The quality of any design is therefore greatly depends on the available
knowledge and experience of the designer.

Introduction to the Principles of Chemical Processes have been extensively


develop in my book Odigure J. O. (2013) Introduction to Principle of Chemical

Processes. ISBN 987-2-639-51749-1 Scholar Press. Germany. 304p.

Week 3: Flow sheets/ Plant layout


CHEMICO-TECHNOLOGICAL SYSTEMS
Q4. All Chemico-technological systems obey simple principles of
layout. What are these principles?
Production processes consist of inter-related technological devices or
aggregates used in the conversion of raw materials to the final product. In
some cases, the optimum working parameters of each unit could vary
significantly. For example, the production of Portland cement consists of
series of stages:
1. Preparation of raw materials using the crusher, grinding mills, dryers,
homogenisation systems, etc.
2. Sintering or burning of the raw materials in rotary kiln at temperature
of about 1400oC.
3. Cooling or quenching of cement clinker to about 100 oC, using the
rotary or planetary or grate cooler.
4. Production of Portland cement by grinding cement clinker and gypsum
sometimes with other mineral additives in grinding mills.
5. Packaging and distribution.
The flow of materials in each stage shows deviation from the approximated
plug flow to mixed, during preparation of materials and a combination of both
regimes during sintering and production of the Portland cement.
Consequently the optimum function of the overall process cannot be
considered as an additive function of the optimum parameters of each unit,
though each element is a contributor to the overall functionality of the
process. Therefore, it is necessary not only to study each element of the
technological process, but the entire chemico-technological process (Figure
1).

Preparation of rawChemical
materialsreaction or Preparation
conversion of the final product

Figure 1 Chemico-technological systems

Chemico-technological system consists of inter-related technological


aggregates functioning as a unit and in which defined technological operation
is performed - such as preparation of raw materials, chemical reaction or
conversion of the raw materials and preparation of the final product
(extraction, purification, aesthetic preparation, etc.). Chemical industry can
be considered as an individual system or subsystems interacting with one
another according to the hierarchical structure presented in Figure 2. In the
first level are the technological processes such as mechanical, hydro
mechanical, thermal, extraction, chemical reactions, etc. The second level
consists of complex chemico-technological processes of the various
departments. The third level is made up of complex chemico-technological
system, production of the desired or intermediate product. Fourth level
consists of chemical industry in general.

Each technological operation takes place in an individual device, that is, an


element of the chemico-technological system. When designing chemicotechnological process or system, only properties of each element that
interacts with another should be considered. The overall condition of any
element depends on the technical parameters and technological regime of
the chemico- technological system.

IV. Chemical Industry


III. Production of the desired and intermediate product
II. Chemico-technological system at various departments

I. Initial aggregates/ raw materials departments

Figure 2 Hierarchical Structure of Chemical Industry.


Technical parameter embodies the geometrical characteristics of the element
- volume, diameter, height, etc. The technological regime considers the
influence of combination of the elements internal parameters on the rate of
technological process and quality of the product. Such internal parameters
include
concentration,
temperature,
pressure,
catalyst
activeness,
hydrodynamic flow, etc. These parameters determine the functionality of
chemico-technological system. The functionality or efficiency of the system

can be measured using the quantity and quality of the product, working and
fixed capital investment, energy requirement, etc.
A diagram showing the sequential arrangement of aggregates in a process is
known as the technological scheme. Technological scheme of a chemicotechnological process can be divided into open and closed circuits. In the
open circuit system, the reacting components or at least one of the
components goes through the reactor only once. For processes with
insignificant extent of reaction two or more similar reactors are connected in
series. Example of open circuit system is the adsorption of SO 3 during the
production of H2SO4 at atmospheric pressure. Open circuit system is used for
both irreversible and reversible processes with high product output. For
processes with product output between 4 and 20% (synthesis of alcohol,
ammonia, etc.) and reactions containing insignificant amount of impurities,
the closed circuit is more economically feasible.
In the closed circuit, system reacting mixture or one of the phase is returned
to the reactor at least once, until the expected extent of reaction is attained.
Examples of closed circuit production processes include synthesis of
ammonia, alcohol, fuel gas, etc. It is also used in grinding where the extent of
reaction after each cycle is insignificant. Therefore the reacting mixture is
repeatedly returned to the reactor after partial or complete extraction of the
product, until the expected extent of conversion is attained. At each stage
fresh raw material, equal to that expended is added. Since in the reaction
process only the main components are involved, leaving the inert compounds
or impurities in the circulating mixture, it is necessary to remove part (purge)
of the reacting mixture after each cycle to reduce the concentration of the
impurities. The economic and ecological advantages of closed circuit system
are numerous. It helps to reduce the amount of carcinogenic substances
released to the environment.
In some heterogeneous processes, a combination of open and closed circuits
might be preferred. In the initial stage one of the reacting phases is
processed using the closed or open circuit. While in the final stage the other
open or closed circuit systems might be preferred. An example can be found
in the production of cement where grinding of raw mix is organised using the
closed, while sintering is by the open circuit systems. The combined system is
also used in the purification of flue and industrial gases. Technological
scheme of a chemico-technological system shows the type and method of
elements, bonds and sequence of technological operation. Each element
(machines, aggregates, etc.) is represented by accepted symbols and their
communication links (piping) shown with the help of arrows (Figure 3).
Technological scheme may also include information on the raw materials and
technological parameters. It is the result of researches into the production

process. It is visual, easy to understand, but does not give a complete


information about the production.

Raw material
Crusher

De-dusting
device

Conveyor
Classifier
Mill
Weighing
Machine

Gypsum

Storage

Rotary furnace

Elevator

Heat source

Figure 3 Technological scheme of gypsum production.


STRUCTURAL SCHEME OF CHEMICO-TECHNOLOGICAL SYSTEM
In this system the elements are represented in form of blocks with inlets and
outlets (Figure 4). It is a visual presentation of the technological links
between the blocks, showing the direction of materials and energy flow. It can

be used as a base for mathematical modelling of the chemico-technological


system.
1

Figure 4 Structural scheme of cement production.


1 Crusher, 2 mill/dryer, 3 homogeniser, 4 rotary kiln, 5 cooler, 6
mill, 7 classifier.
TECHNOLOGICAL OPERATORS OF CHEMICO-TECHNOLOGICAL SYSTEM
These are elements in the system where the initial physical properties or
parameters of the incoming materials and energy are converted into the
desired final product as a result of physico-mechanical and chemical
transformations. The physical parameters include temperature, density,
viscosity, etc. Changes in these parameters may be as a result of chemical
reaction, mass transfer, separation/extraction, mixing, heating, etc. processes
taking place in the elements.
Technological operators are divided into the main and auxiliary. The main
operators are used for chemical reactions, mass transfer, separation, mixing,
etc. (Figure 5). Auxiliary technological operators are used for heating/cooling,
compression or expansion, in order to change the aggregates state, (via
condensation, evaporation, dissolution, etc.). Auxiliary operators are used to
influence mainly the energy requirement and phase condition of the system
(Figure 5).
Main operators

Mass transfer

Chemical
Reaction

Classification

Auxiliary operators

Compression and
expansion

Conversion of
aggregate state

Heating or
cooling

Mixing

Figure 5 Technological operators

Technological operators in technological scheme give the concise information about the
interrelation of elements and physico-chemical processes (Figure 6).
VA

VC

Vf
VD

VB
Preparation of raw
Chemical reaction
materials
materials
Figure 6 Technological operators scheme

Mixing of

Plant Layout
Q5 How will you from the details contained in the plant layout
determine the required space for a production process?
The choice of site is influenced by many factors. In this project it is
assumed that the plant will be located at a site that will ensure easy
availability of cassava tubers. Political consideration is ignored in this
project. However it is expected that all administrative standards/laws
enforced by the Local, State and Federal Governments will be met. It is
expected that the factory will have basic utilities water, electricity,
access roads, etc.
The basic input data for the space requirement were obtained from the
design

calculations

and

techno-economic

considerations.

The

constructionability and expliotationability of the plant should also fully


considered. These include size and configuration of space allocation,
geotechnical and geology of soil, environmental factors, allowance for
future expansion, possibility of corporation (Odigure 1998) with other
plants, etc (Table 19).

Basic technical properties of the designed and selected equipment


1
2

Peeling unit

Manual

Productivity

16,000kg/day

Washing unit
Washing basins
Number

Dimension

3x4m

Bucket lifting system


Capacity

150kg

Figure 19 Spaces allocation for the major equipment


S/No

Unit

1
2
3
4
5
6
7
8
9
10
11
Subtotal

Raw materials unit


Peeling unit
Washing Unit
Grating unit
Detoxification unit
Dewatering unit
Rotary disintegrator/classifier
Drying unit
Milling/classifier unit
Bagging unit
Storage unit

Space allocated, m
Length
Width
10
10
5
5
5
5
2
2
6
10
3
3
1.5
1
9
3
2
2
3
3
10
10
56.5
10
11.3
2
66.8
12

Safety and utility factor of 20%


Total

Hammer mill/grater
Diameter of shaft

600mm

Length of mill

400mm

Velocity of bits

1250rev/min

Dimension of mill

Length

0.45m

Width

0.65

Height

1.10m

Productivity

2000kg/hr

Electric motor power

10kW

Detoxification tank
Number of tanks

Volume/Mass

22m3/(7000kg/tank)

Length

5.6m

Bottom diameter

2.4m

Height

1.3m

Number of blades

Shaft diameter

95mm

Electric motor power

6kW

Water jacket
Height

1m

Total area

9.63m3

Mass flow rate

1x10-3kg/s

Design space between jacket and tank 50mm


5

Cylindrical conical helical conveyor centrifuge


Feed inlet diameter

50mm

Speed

2000rev/min

Through put

Liquid

300l/hr

Solid

1000kg/hr

Bowl diameter

700mm

Length

1.4m

Electric power

5kW

Rotary disintegrator/classifier
Length
Diameter

1.0m
0.4m

Electric motor
7

5kW

Dryer
Length

7.7m

Diameter

1.6m

Heat exchanger

Outer pipe diameter

200mm

Inner pipe diameter

50mm

Number of pipes

Electric motor power

5.6kW

Productivity

928.8kg/hr

Hammer mill-cyclone classifier


Diameter of mill shaft

800mm

Velocity of bits

40m/s

Height of mill-separator

2.1m

Productivity

2000kg/hr

Electric power

5kW

Cut particle diameter


9

<180m

Collector
Main cyclone: height

2m

Diameter

500mm

Feed inlet

125x250mm

Outlet

250mm

Flour outlet

125mm

The 3 battery cyclone


Electric power
10

Half the main cyclone


5kW

Packaging unit
Storage tank
Capacity

4000kg

Number

Packaging equipment
Productivity

10000kg/day

The plant layout is as presented in Figure 12


70m
7
8

4
5

Side View

12m

Top View

Figure 12 Plant layout of the cassava processing plant


Key: 1 Washing basin, 2 Hammer mill, 3 Detoxification tank, 4
Centrifuge filter, 5 Rotary classifier, 6 Dryer, 7 Hammer mill
Cyclone classifier, 8 Cyclone collector.

DESIGN OF CHEMICAL INDUSTRY AND MODELLING OF CHEMICOTECHNOLOGICAL PROCESSES


Industrial machines/processes are designed using:

Experience gained from existing ones. This is commonly refrred to as reverse


engineering. This often involves physical modeling of the process.
Laboratory experimental data obtained using basic scientific laws and principles.
Conceptual mathematical models derived using descriptive models of the process
principles and laws.

In designing new factory, it is necessary to perform technical and technoeconomical evaluations to ascertain the viability of the project. Various
engineering specialists in chemical, mechanical, electrical, civil structure,
are involved in the designing process.
The initial parameters required may include:
1.

4.
5.
6.
7.
8.

Location of factory.
2.
The capacity.
3.
Type of products.
Type and quantity of raw materials.
Technology of production.
Technological regime.
Type of reactors and secondary machines.
Process control. Etc.
Optimization of these parameters is necessary to ensure maximum
productivity, not only for the individual processes, but also of the entire plant.
For example the chemical preparedness of Al 2O3, Fe2O3, SiO2 and CaO in
cement raw mix increases with higher fineness and homogeneity. However,
increased fineness and homogeneity means higher cost of grinding, and dedusting operations and consequently increased cost of production. Therefore
optimum fineness and homogeneity should be determined considering the
cost of grinding, homogenization and de-dusting operations.
The process of designing is performed in two basic phases: the initial or
conceptual and the detailed design. Quality management should form an
integral part of the various stages of engineering design. This will enhance
not only successful attainment of set goals, but maximization of available
resources.
Q6. Discuss the three stages of a plant design.
CONCEPTUAL DESIGN STAGE
Quality management of engineering design starts with "raw material" or
information gathering and control. The engineering portion of quality
management plan addresses the design activities that occur during the
conceptual design stage. The main feature of design work is the technological
calculations. This should be performed for various process routes before the

choice of technology is made. The technological route (schematic diagram)


shows the details of the chemico-technological processes and the position of
each device, apparatus, reactors, communication network and the processes
in general. The main technical characteristics should be shown in the
technical drawings. These activities form the bases for the project cost
estimation and consequently, the approval or disapproval of project funding.
At this stage the quality management plan is to provide the design team with
tools / documents that clearly state the requirements, quality expectations
and ensure completeness of input data. In addition the quality management
plan should enhance recognition of poorly defined units so that appropriate
risk management measures can be considered.
Poorly defined scope-of-work results in design related rework. This normally
manifests itself during detailed design stage. It results in schedule slippage,
cost overruns and rework. On the average, design rework account for about
12% of total installed cost, with design deviations accounting for about 80%
of it.
The scope of work should clearly define the project objectives. Such
objectives include plant capacity, product quality, project schedule and cost,
use of new technology, safety, maintainability, project expansionability, start
up, running cost, etc.
The basic data required during the conceptual design stage include:
a.

Detailed material and energy balance;

b.

Operating and design conditions for the various units and devices;

c.

Construction materials, pipes and electrical fittings' specifications;

d.

Appropriate selection of materials and equipment;

e.

Feasibility report including guideline on pre-investment cost for future


expansion;

f.

Thorough evaluation of existing Federal, State and Local Governments


regulatory and permitting requirements;

g.

Site considerations: electrical power supply and distribution, real


estate allowance, specifications for plant, soil condition, local building
codes, existing utility systems, etc.;

h.

Environmental requirements;

i.

Safety, constructability and technology. These are the three issues that
must be treated together during the conceptual design stage. The
quality management plan must allow for the consideration of options

of
various
disciplines

construction-structure,
operations,
maintenance, research and development, safety, industrial hygiene,
contracting, etc.
j.

Procurement. A detailed procurement plan showing the strategies and


preferred suppliers should be prepared during the conceptual design
stage. This will reduce uncertainties and quality problems particularly
for the major electrical equipment, the control systems and fabricated
mechanical parts.

Data gathering can be very difficult to achieve due to market influences and
competitive nature of business operations. However, an alternative to
incomplete data availability is to perform some thorough economic analysis.
This will ascertain the feasibility of each design unit - raw materials'
qualities / quantities, plan schedules, budgeting, procurement, construction,
etc.

Week 4: Mass and Heat transfers


DETAILED DESIGN STAGE
The detailed design stage is the next after the conceptual design. It focuses
on problems associated with communications and change management.
Communication management problems include: not informing all participants
of changes in the conceptual plan, not understanding project objectives, not
understanding the market force, etc. Often, very few design errors result from
technical incompetence. Therefore, the detailed design phase should focus on
procedural matters associated with documentation, dissemination and
monitoring of information. It should also provide feedback information and
initiate corrective actions where necessary. Change management is the
process of resisting or avoiding change on the conceptual design plan and
ensuring that the inevitable change is communicated and implemented on
time observing all procedures.

After the choice of process route and direction of materials and products flow, the
materials (mass) and energy balance are calculated. From these data, the technical and
technological parameters of the reactors (size, capacity, residence time, etc.) are
calculated. Mathematical modelling of the processes and reactors are also performed at
this stage. The reactors construction materials should be determined considering the
corrosiveness of the medium, working temperature, pressure, service life, etc. From the
overall capacity of the factory, the number of reactors and other devices are calculated.
During the technological calculation, the hydrodynamic, heat and mass transfer and

chemical kinetics data are evaluated to find the optimum technological regime and
consequently choice of required equipment. Mass and energy balance are calculated
during design of new factory or analyses of old ones. Examples will be considered later.
MATERIAL BALANCE
Q7. What is the principal reason for a plant material and energy
balance?
According to the law of conservation of mass, mass can not be destroyed or
created during chemical reactions. That is the mass of reactant(s) must be
equal to that of the product(s). Material balance is calculated from the main
chemical reaction, taking into consideration all the secondary reactions and
impurities.
For the continuous process, material balance is calculated for a given period
of time. That is the feedstock to the reactor at a given time is equal to the
output. The total mass of material in a reactor is constant. The quantity of
material should be calculated independently for the solid, liquid and gas.

M s M l M g M s1 M l1 M g1 ..................................................9
where Ms, Ml and Mg mass of feedstock; Ms1, Ml1 and Mg1 mass of output
(product).
In most production processes the reactants could exist in one or two
phase(s), thus simplifying the equation 9. In designing, the productivity of a
plant (factory) is usually given and consequently the quantity of raw
materials required can be calculated. The ratio of the quantity of the raw
materials required to produce a unit mass of the product is referred to as the
utility coefficient. It expresses the amount of raw material required to
produce a unit mass (kg, ton, mole) of the product. In calculating the material
balance, it is necessary to:
1.

Formulate and solve the mathematical equations (expression) that will


represent the operating technological parameters in relation to the
materials input.

2.

Calculate the product output.

3.

Investigate the chemical kinetic of the reacting compounds.

In some cases as a result of phase transition, the quantity of feedstock in a


given phase may not be equal to that of the product. For a gaseous phase
reactant, the material balance can be represented as in equation 10.

M g M g 1 M g M gd ..................................10
where Mg1 is the resultant increase in reactant mass, M gd resultant increase
as a result of mass transfer (adsorption, absorption, condensation, etc.).
For example, in plug flow reactor at stationary state, the material balance of
reactant A, per unit time can be represented as in equation 11.

M Ao M A f M A .............................................................................11
where MAo - feedstock (input) of reactant A, MAf output of A, MA quantity of
A involved in chemical reaction. In the differential form, the material balance
for a stationary state system can be expressed through the flow rate, w, per
height or length H, of the reactor, or change in concentration M A or rate of
change of A due to chemical reaction or mass transfer in gas phase u A.

w(

C A
) u A .............................................................................................12
H

where w(CA/H) transfer of reactant A per unit height, that is the difference
in mass of A entering an infinite elementary volume of reactor and that
leaving it. This is equal to M Ao MAf. In non-stationary regime where the
feedstock is more than that used

C A
C
w( A ) u A .............................................................................................13
t1
H
where CA/t1 rate of increase of reactant A in an infinite elementary
volume, t1 time required for the increase.

ENERGY BALANCE
According to the law of energy conservation, the total energy in a closed
system is constant. In chemico-technological processes the law of
conservation of mass is the bases on which energy balance is computed; the
total amount of energy released to a system must be equal to that expended.
Heat balance is calculated using the material balance and heat of physical
and chemical changes occurring in the reactor, taking to account the external
heat sources and losses through products removal and the reactors wall.
The energy balance computation can be represented as

Qs Ql Q g Q p Qr Qin Qs ' Ql ' Q g ' Q p ' Qr ' Qin' .....................14


where Qs, Ql, Qg initial heat content of the solid, liquid and gaseous feeds
respectively; Qs, Ql, Qg heat content of their products; Q r, Qr exo- and
endothermic heat of reaction; Qin external heat source, Qin heat lost to
the surrounding. Qs, Ql, Qg values are generally calculated as

Q McT ...........................................................................................................15
where M mass (kg) or mass flow rate (kg/s), c specific heat capacity (J/
(mol.K) and T (K) temperature.

For gases the specific heat capacity at constant pressure and a given temperature T can be
determined using

C p a o a1T a 2T 2 ............................................................................................16
The coefficients ao, a1 and a2 are known values and can be got from chemical
handbooks.
For mixtures, the specific heat capacity c m can be calculated applying the
additive law. For example, in an n component mixture with c 1, c2, c3cn, the

cm

m1c1 m2 c 2 m3 c3 .......mn c n
................................................................17
m1 m2 m3 .........mn

For solids, except for those shown below, the elements atomic heat content is the same
and is approximately equal to 27J/(mol.K), while the molecular heat content is the sum of
their atomic heat content.

Elements

Si

CP, J/(mol.K)

14.4

13.9

7.5

14.6

20.9

20.2

22.6

16.28

The heat content of the liquids may also include the latent heat of fusion and
in case of gases heat of vaporization. Heat released during physical
changes; crystallization, condensation, adsorption, etc. should also be
computed during heat balance.

Q p m1 r1 m2 r2 m3 r3 ............................................................................18
where m1, m2, , m3 . heat of phase transition. It is also necessary to
compute the heat adsorbed as a result of desorption of gases, vaporization,
fusion, etc. Heat of exothermic and endothermic reactions should be
calculated form the chemical equation for each of the processes.

A B D H .........................................................................................19
The total heat is the sum of each individual reaction.
Qin heat released to the chemical reactor should be calculated from the heat
lost by the heat carrier (steam, air, water, etc.).

Qin mc(Tin T f )......................................................................................20


Qin mr......................................................................................................21
It can also be calculated using the heat transfer formula

Qin k t F (To T f )t....................................................................................22


where kt coefficient of heat transfer, F heat transfer surface area, T o
mean temperature of heat carrier, Tf mean temperature of the material in
the reactor, r heat of vaporization, t time. Using the heat transfer formula,
the quantity of heat lost to the surrounding can be calculated.

Assignment
Q8. Design a very simple technological process of your choice.
Carefully mimic the example below.
To be submitted by the 10th Week

Example

BAKING OF PASTRIES
Introduction
The major ingredient used for baking of cake is flour. Others include water, egg, sugar,
colour, baking soda, etc. depending on what you want. The procedure and a simple recipe
could be 500g of flour poured into a bowl together with 250g butter, 250g sugar, 125g of
egg, 50g baking soda, 25g of water, 10g nut and 2g flavor (Total weight of 1212g). The
weighed out materials are mixed manually or mechanically in a mixer for 30 minutes to
form a consistent paste. The paste is now put in a pan of a desired shape and transferred
to an oven with temperature of 120-150oC. The residence time in the oven is 90 minutes.
The cake from the oven is cooled to ambient temperature.
Assumptions

There are no chemical reactions involved in the process except for organic

fermentation and the consequent release of gases.


No experimental data were used; the objective is to show how design
could be conceptualized from everyday activities like cooking.

Schematic Diagram
The schematic diagram gives a pictorial description of the materials flow and
transformation at the unit operations in the process. For beginners it is recommended to
always indicate the operating conditions (temperature, concentration or pressure, mass,
etc.) in each unit diagram. Ability to identify all possible technological secondary and
primary technological products will help in the development of the material and energy
balances. From the description of the process:
ii Identify the possible physical or chemical reactions taking place. For each
reaction, schematically draw the reacting processes or units indicating the
inputs and outputs streams.
iii Identify the nature of the input stream and decide if you require a mixer or a
separator or a compressor, etc.

iv Identify if output stream will need a separator or a mixer or the quantity is


more than is required for the next unit.
v Identify if you need a back feed stream for excess output.
The final schematic diagram is further evaluated during the detailed analyses of the
design cost, safety, environment, etc.

Oil
Flour
Butter
Water
Baking Soda

Mixer

Oven
at 120oC

Product at 30oC

Paste at 30oC

Technological loss
Water (Steam)

Low volatile

Figure 1 Schematic Diagram of Cake Baking


Material Balance
According to the law of conservation of mass; matter cannot be destroyed or created
during chemical process.
Mass Input = Mass Output + Accumulation
This implies that the mass of the feed must be equal to the mass of the product (cake)
which is the primary product, accumulation in the mixer, water loss as steam during
heating in the oven and possibly low volatile compounds contained in the feed.
Table 1 Material balance in the Mixer
Materials

In, g

Percentage

Flour

500

41.25

Butter

250

20.62

Out, g

Percentage

Sugar

250

20.62

Egg

125

10.31

Baking soda

45

3.71

Water

25

2.06

Nuts

10

0.82

Flavor

0.17

Oil

0.41

Paste

1200

99.01

Technological loss

12

0.99

1212

100

Total

1212

99.98

Table 2 Material Balance in the Oven


Materials

In, g

Percentage

Out, g

Percentage

Paste

1200

100

1150

95.83

Steam

40

3.33

Oil

0.58

Burning (Browning of the surface)

0.25

1200

99.99

Total

1200

100

Experimental values were not used in developing the material balance. Results obtained
from the material balance help in computing the mass of the materials in the reaction
zone for the duration of the residence time. For a batch process as in baking of cake, the
calculated mass can be converted to volume to enable us estimated the volume of space
to be occupied by the paste. It is important to note that the adopted technological regime
is dependent on the mass/volume of material to be processed. The bigger the mass the
more energy is required for the mixing, the bigger the size of the mixer, the toughness of
the material of construction, etc.

Energy Balance
According to the law of conservation of energy, the total energy in a closed system is
constant. In any process, the law of conservation of mass is the basis on which energy
balance is computed. The total energy introduced or released to a system must be equal to
that expended. In endothermic process, energy is supplied to the system to initiate the
reaction. In exothermic the system will generate the required energy.
Mixing
In this process, the reactions taking place is more of gel formation of the flour particles.
Work done is by mechanical mixing whether by hand or transmission via a shaft can be
calculated using Nusselt criteria equation. The quality of mixing is strongly determined
by the medium temperature, kinematic viscosity of the feed and the frequency of rotation
of the shaft.
Nu f =0.87

0.62
m

Pr

1 /3
f

f
w

0.14

( )

Knowing the Criteria equations,

m =

d2 f
D
Nuf =
v

the d and D of the blade and

mixer are determined.


Where d diameter of the mixing blade, m; f frequency of the shaft rotation, rev/min.;
v kinematic viscosity, m2/s; D diameter of mixer, m; - dynamic viscosity of the
paste, kg/(m.s); - coefficient of heat transfer, kJ/(m.s.oC); - coefficient of thermal
conductivity, kJ/(m.s.oC). The equation is true for mixer with diameter of not more than
300mm.
Oven
Heat supplied to the system is to cook the paste. The essence of computing the energy
balance is to determine the energy demand by the system and the type of oven design
required.

Heat supplied to the system or Heat received Oven


Q1 Heat required to fire the Oven to the required temperature of 120oC. The heat is
obtained by burning cooking gas.
Q1 = GgcgTg
Where G - quantity of gas required; c - specific heat capacity of the gas and T operating
temperature of the oven.
Q2 Initial heat content of air in the oven = macaTa
Q3 Initial heat content of the paste - mpcpTp
Heat utilization or lost
Q4 - Heat lost to the paste to the cooking temperature = mcccTc
Q5 Heat lost to water at 100oC = mwcwTw
Q6 Heat lost to water converted to steam = mw1cw1Tw1 + mw1L
Q7 Heat lost to oil mocoTo
Q8 Heat lost to the surrounding. This taken as a fraction of that supplied = 10% of Q 1 =
0.1 GgcgT
Heat received = Heat lost
Q1 + Q2 + Q3 = Q4 + Q5 + Q6 + Q7 + Q8
GgcgTg + macaTa + mpcpTp = mcccTc + mwcwTw + mw1cw1Tw1 + mw1L + mocoTo + 0.1 GgcgT
Q1 = {(mcccTc + mwcwTw + mw1cw1Tw1 + mw1L + mocoTo) (macaTa + mpcpTp)}/0.9
This is the quantity of heat released during burning of the fuel source or required for the
baking process. If we know the heat capacity of the source of fuel, the quantity of heat
released by burning a specific unit (volume or mass) of the source we can easily calculate
the quantity of fuel purchased.

For example, Qs for natural gas, 35615kJ/nm3. Therefore, the quantity of gas required for
the process will be Q1/35615nm3.
The computed values should be tabulated and presented as in Table 3.
Table 3 Heat balance in the Oven
Heat supplied

Value, kJ

Heat utilized

Kj

Burning of Fuel

Q1

Heat lost to the paste to Q4= mcccTc


the cooking temperature

Initial

heat Q2= macaTa

content of air in

Heat lost to water at Q5= mwcwTw


100oC

the oven
Initial

heat Q3 = mpcpTp

content of the

Heat

lost

to

water Q6= mw1cw1Tw1 + mw1L

converted to steam

paste
Heat lost oil
Heat

lost

Q7 = mocoTo
to

the Q8= 10% of Q1 = 0.1

surrounding. This taken GgcgT


as a fraction of that
supplied
Total

Mechanical Design
Mixer

b=R
h
D
Figure 2 Schematic diagram of a horizontal blade mixer
The criteria equations enable us to find the diameters of the blades and mixer. The
starting power for a shaft horizontal blade mixer can be calculated
2 z T 1 27 2 z F b 3
z
Ng=
=
=60. 108 F b D 3 n3
102
64.2 .102

Where N power required at start up, kW, z number of blade pair; mechanical
efficiency of the motor; velocity, m/s; D diameter (Figure ), m; n frequency, rev/s;
T1 life force require to move the mass at rest =
T1=

G 3o F b 2o
=
2g
2

Fb surface area of the blade in contact with the mass, m2;

Fb =b h sin

Where b blade length = R = radius, m; h blade height, m; angle of blade in the


direction of flow.
There are other types of mixers depending on the position and nature of the blades. There
are vertical, tunnel, propeller and pneumatic mixers.

Oven
The question was how would the next generation of oven look like?

The quantity of heat lost to the surrounding speaks of the heat retention efficiency of the
process. The objective is to reduce the loss during the design through better materials
selection.
The oven has a double layer with a middle air space
Qloss = Q8 = kFT
K is the coefficient of heat transfer, w/m2.oC
k=

1
1 1
+ +
1 2

Where 1 is the heat transfer coefficient of the inner stainless steel plate, w/m2.oC. It is
approximately determined as
1 = 9.3 + 0.058Tw = 9.3 + 0.058x120 = 16.26w/m2.oC; where Tw is the inner wall
temperature.
= air insulator thickness assumed to be 5mm
= coefficient of thermal conductivity of air, = 0.024 w/m2.oC
2 = 9.3 + 0.058Tw = 9.3 + 0.058x30 = 11.04w/m2.oC; where Tw is the outer wall
temperature.
K = 0.447 w/m2.oC
T = 120 - 30 = 90 oC
Q8 = 0.447x90F
From the energy balance the value of Q8 could be computed and then F, the heat transfer
surface area could be calculated. Let us assume that the Q8 = 45W
Then the heat loss surface area F = 45/(0.447x90) = 1,11m2

An oven has 6 sides. Let us assume that heat is evenly supplied to the working area from
3 sides. Each side will then be = 1.11/3 = 0.37m 2. For square shaped the length and the
breadth = 0.61m.
The beauty of design is determined by the ability to define the aesthetics of your product.
In determining the aesthetics, it is important to consider the following factors.

The movement or dynamics of the material,


The physical or chemical state of the products,
The reaction atmosphere; is it reducing or oxidizing, atmospheric, low or

high pressure,
The points of charging and discharging of materials and energy (flue gases

or effluent), and
The dynamics or pattern of heat transfer, etc.

It is important to ensure uniform heat supply to materials fired. The calculated heat
transfer area is not the same as the final volume of the working zone. The working zone
volume is determined by that of the material or cake depending on which has the greater
volume.
For reactors in continuous flow system, the F is equivalent to the zone of desired primary
and secondary reactions. The materials are placed on mobile bed. The volume of material
in this zone at any given time is determined by its flow rate and the residence time. In the
given example of cake, the paste cuts are placed on the mobile bed moving at constant
velocity; calculated using the residence time of reaction or baking time.
For cylindrical shaped mobile oven the heat transfer surface area F = circumference x
length of the reaction zone F = 2 rL. F = 2 rL.
For box shaped mobile oven F = Length x Breadth

The heat transfer surface area, F is part of the working volume space. F location should
ensure effective heat contact with the material. The F either is at a single point in the
oven or distributed horizontally and vertically to different points/area along the oven.
Unlike fixed bed or batch oven, the materials and energy flow could be in co or counter
current direction. T is therefore calculated using the log mean value.
Q = kFT
Where k overall heat transfer coefficient, kW/m2.oC
F heat transfer surface area, m2.
T mean temperature at ambient temperature of 30oC.
k is a function of the oven construction material stainless steel sheet. For ease of
comparison, the same materials of construction will be selected as in the batch.
Consequently, the k value remains the same.
At kiln outlet temperature of 70oC

120 30 70 30
2.3 lg

Q
K T

120 30
70 30

45
0.447 x61.72

Check: Tw = 30 +

50
0.81

= 1.63m2

k
T

30 + (0.447x61.72)/16.26 = 31.7oC.
At kiln outlet temperature of 60oC

= 61.72oC

T = 54.67oC.
F = 1.84m2.
Check: Tw = 31.5oC.

At kiln outlet temperature of 80oC


T = 68.13oC.
F = 1.48m2.
Check: Tw = 31.87oC.

ToutletoC

ToC

F,m2

TwoC

60

54.67

1.84

31.5

70

61.72

1.63

31.7

80

68.13

1.48

31.9

One striking observation is that the Tw remain practically at the same level. It shows that
the initial material of construction used for the batch process is more than adequate for
the continuous process. Increase in the quantity of heat lost with the outgoing gases
results in decrease in the heat transfer surface area. In other words, we can choose to pay
more for energy during the operation of the plant and spend less now on capital cost for
materials. The calculated F for the batch is smaller. The higher F value for continuous is
due to the required cooling zone area. Let us assume that a tunnel oven will be use with a
circumference of radius equal to the length of the stationary cubic oven earlier designed.
F = Dxlength
1.84 = 3.142x0.61xL; L = 0.96m.

For rectangle F = width x height; 1.84 = 0.61h; or h = 3.02m


Unlike the batch, continuous oven F value is made up of the pre heating, reaction and
cooling zones; the lower the outlet temperature of the outgoing material the higher the F
value.

Figure 3 Proposed Cubic shape heat


0.61m

transfer surface area (stationary regime)

0.61m

0.61m

Heat transfer area


0.96m

Figure 4 Proposed tunnel shaped Oven with heat transfer area in the tunnel wall and
mobile bed material.

Heat transfer area

3.02m

0.61m
Figure 5 Proposed box shaped Oven with heat transfer area embedded in the mobile bed
carrying the materials
The calculated F is part of the reaction volume calculated from the material balance. For
fixed bed or stationary regime, the calculated heat transfer area is embedded in the
volume is to ensure uniform distribution of heat to the materials (Figure 3).

The major advantage of Figure 4; the proposed tunnel shaped Oven with immobile heat
transfer area in the tunnel wall and mobile bed material, over Figure 3 is the possibility of
heat retention within and mechanization of the charging and discharging areas.
In Figure 5, both the material and the heat sources are mobile. In dynamic or mobile
regime, the nature of the materials, the reactions regime, etc. determined the material and
heat flow pattern (co or counter current flow). In baking, to allow for gradual evaporation
of water a counter current flow pattern is used. The volume of material in the heat
transfer area is regulated by the velocity of the mobile bed; which is determined by the
time required for evaporation of water (drying), secondary and primary reactions.

Ancillary Equipment
These are equipment required to support optimum production process. For example, the
heat required for the process comes from burning of natural gas in a furnace. The
temperature generated could be higher than that expected in the reaction zone. The
burning chamber might be some distance from the reactor. It follows that you need to
store the natural gas, burn it in a chamber, and then mix with air and finally pipe to the
reactor. The process will therefore require a pressurized storage tank, a compressor, a
specialized burner. Simple put you will need a heat-generating unit as part of the
production unit. These equipment capacity, power rating, productivity, etc. are selected
based on the design calculations.
References
1. Odigure J. O. (2013) Introduction to Principle of Chemical Processes.
ISBN 987-2-639-51749-1 Scholar Press. Germany. 304p.
2. Odigure J. O. (2013) Modeling and Simulation of Chemical Reacting
Systems and Environment. ISBN 987-2-639-51769-2 Scholar Press.
Germany. 287p.
3. Odigure J. O. (2013) Introduction to Design for Small and Medium
Chemical Processes. ISBN 978-3-639-70619-2 Scholar Press.
Germany. 267p
4. Perry R.H. and D.W. Green Perrys Chemical Engineers Handbook, 7th
edition, McGraw-Hill Book Co., New York, 1997.

5. Plant Design and Economics for Chemical Engineers (1991). 4 th Ed.


McGraw-Hill Inc. NY. Ed. B. J. Chark and J. M. Morriss.
6. Sinnott R. K. (1994). Chemical Engineering Design. Pergamon Press
LTD, London.
7. Smith, J.M. (1981): Chemical Engineering Kinetics. 3rd Edition, McGrawHill international book Company. PP 6-661.

Week 5 and 6: Selection and Choice of Equipment

REACTORS FOR HOMOGENEOUS PROCESSES


Q9. All reactors are constructed to ensure maximum exposed
surface area of the reactants. How is this reflected in the
design of reactors for homogenous processes G-L, G-S. G-L?

Construction of reactors for homogeneous processes is simpler and


easily automated than those of the heterogeneous, due to easy mixing
of reactants. Industrial reactors operate between ideal plug flow and
well mixed. The driving force in real reactors is smaller than that in the
ideal plug flow. Therefore, the extent of mixing or intensity is
dependent on the time necessary to ensure transition from diffusion to
kinetic controlled regime and thereafter further mixing will reduce the
rate of reaction. In exceptional cases, intensification of mixing might be
necessary to reduce local self-heating, increase heat transfer between
the reacting mixture and heat transfer surfaces, etc. Constructions of
reactors depend on the nature of the medium (gas, liquid, vapour),
technological parameters, properties of reactants, etc.
Practically in all reactors, mixing leads to fall in process driving force
and consequently the overall rate of reaction. Therefore, in converting
ideal well mixed to real or industrial reactors, it is necessary to
introduce corrective coefficients and limit conditions. Such corrective
coefficients are determined experimentally. Mixing significantly affects
the rate of reaction along the reactors height or length and to a lesser
extent in the direction of flow. The well-mixed equations are more
suitable for the calculation of design characteristics, if the extent of
mixing greatly affects the process driving force. For liquid phase
homogeneous reaction, intensification of mixing greatly influences the
rate of reaction as a result of enhanced homogenisation and heat
transfer processes.

Gaseous homogeneous processes are better conducted in a capacity-type reactor (Figure


4.2).
CH4 + Cl2 CCl4 + CHCl3
CH4 + O2 CO + H2O
H2 + Cl2 2HCl
Reactant

Product
Figure 4.2 Capacity-type reactor
Reactions such as listed below could be conducted in capacity type or
tubular reactors (Figure 4.3).
2C3H8
2CH4

C2H4 + C3H6 + CH4 + H2


C2H2 + 3H2

CH4 C

+ 2H2

CnH2n+2

C2H4 + Cn-2H2n-2

ClCH2 -CH2Cl

CH3CHCl + Cl.

RH + SO2 + Cl2

R-SO2Cl + HCl

Mixing of gases is performed by simple devices such as nozzle,


injector, centrifuge, cascade mixers, etc.

Commonly used gaseous

homogeneous phase reactors include:


I.

Capacity type reactor with injection of gases and vapour. It is


used in the synthesis of HCl (Figure 4.2)

II.

Capacity type reactor with centrifugal mixing of gaseous


mixture.

This is an approximated well-mixed isothermal

reactor.
III.

Tubular reactor with heat exchanger.

It is an approximated

plug flow with polythermal temperature regime (Figure 4.3)


Reactant

Coolant

Coolant

Product
Figure 4.3 Tubular reactor with heat exchanger

IV.

The tube in tube reactor with the heat carrier or absorber


going through the intertubular space. It operates as plug flow
polythermal reactor and is used for highly exothermic
reactions (Figure 4.4)
Coolant out
Reactant
Product

Coolant in
Figure 4.4

Tube-in-tube reactor

For liquid phase homogeneous processes, reactors with mechanical and pneumatic mixers
are used. Increased efficiency is achieved by increasing the residence time of material in
the reactor via increasing the effective length of the reaction compartment, utilizing cocurrent flow of materials and column reactors. Liquid phase reactors are equipped with
heat exchangers for heating or cooling of the reactants. Mixing can be by mechanical or
pneumatic methods. Examples include the stirred reactor with propeller mixer (Figure
4.5), pneumatic mixer (Figure 4.6) and spray-injector (Figure 4.7).
Air
Reactant
Shaft

Reactant

Product

Product

Figure 4.5 Stirred reactor with


Stirred reactor with

Figure

propeller mixer

pneumatic mixer.
L

Flue gas

G
Product

4.6

Figure 4.7 Stirred reactor with spray-injector mixer.

REACTORS FOR G-L SYSTEMS


Reactors used in G L heterogeneous systems consist of reaction volume where physical
processes - mass transfer processes such as physical absorption and desorption,
evaporation, distillation, heat transfer and chemical processes, can take place. The G L
heterogeneous processes include production of soda, mineral acids, organic syntheses,
etc. Reactors commonly used are presented in Table 4.1. All the reactors have
approximated plug flow or well-mixed regime. In this system reactors
design/construction are determined by the technology of increasing the contact surface
area of either the gas or liquid phases.
Packed bed reactors are commonly used in absorption, desorption processes during
production of mineral acids and organic syntheses. Bubble type reactors may have one or
more caps per grid depending on the properties of the gas or liquid, expected efficiency
or selectivity. In each grid the gas contained in the bubbles is mixed with the liquid. Cross
flow of the gas and liquid is observed in the grids surfaces, while along the reactors
height the flow pattern is counter current flow pattern (Figure 4.9). Bubble type reactors
are widely used in the chemical industry; in the production of soda, fractional distillation
of crude oil, organic syntheses, concentration (evaporation) of acids, etc. They are more
difficult to construct than the packed beds.
Capacity type reactors with liquid sprayinjector device are used. Increased surface area
is achieved by dispersion of the liquid phase using mechanical or pneumatic sprayer.
Capacity type reactor is used in the production of H2SO4, purification processes, etc.
(Figure 4.10).
In the film type reactor (Figure 4.11), air at a velocity of 0.7 to 3.5m/s is passed bottom
up through the grid. At the chosen velocity, if the frictional force between the gas and the
liquid is balanced by the weight of the liquid, a fluidised layer of very mobile bubble will
be formed.

Table 4.1 Reactors for heterogeneous Gas-Liquid processes


Type of
reactor

Schematic presentation

Packed bed
and tubular

Mixing regime,
flow pattern and
processes

Characteristics

Plug flow, counter


or co-current.
Adsorption,
desorption,
purification of
gases

Low efficiency, low


energy
consumption for
gases but high for
liquid. Simple to
construct, reliable,
easy to control and
stable in operation.

G Plug flow for


gases, well mixed
for liquid. Cross
flow on grid and
counter current
along reactor
height. Same
processes as in
packed bed.

Average efficiency.
High energy
consumption and
selectivity, reliable
and stable in
operation.

Plug flow for


gases, well mixed
for liquid. Cross
flow on grid and
counter current
along reactor
height. Same
processes as in
packed bed.

High efficiency and


energy
consumption. Easy
to control. High
selectivity in
multiple column.

Plug flow, counter


or co-current.
Adsorption,
pyrolysis and
polymerisation.

Low efficiency.
Simple to construct.
Easy to control and
regulate.

G
L

L
G

L
L

Fluidized
liquid layer

G
L

a. With
grids
b. Bubble
cap

L
Fluidized
liquid bed

G
L
L

Fluidized
column

L
G

Tubular
Tube in
Tube

Coolant
G
L

G
L
Coolant
Spraying of
the liquid
phase

a.
Capacitytype

Ideal plug flow,


counter or cocurrent.
Adsorption,
desorption,
purification of
gases,
polymerisation

G
G

b. Cyclone
scrubber
G

Low efficiency.
High energy
consumption, small
hydraulic
resistance. Not
stable in operation.

L
G

Cap
Upper
flow
pipe

Gas
Gas
L
Figure 4.9 Construction of bubble reactors
At a higher air velocity, the film layers will be destroyed and the liquid carried away with
the outgoing gas in form of capsules. Film reactors are commonly used in the purification
of flue gases.
G

L
L

L
L
G

Figure 4.10 Capacity-type reactor

Figure 4.11 Film reactor

with sprayer

(Fluidized liquid bed)

REACTORS FOR G S SYSTEMS


Some of the commonly used reactors in G S system is schematically presented in
Figure 4.16. Most non-catalyzed heterogeneous reactions take place at high temperature
in reactors usually referred to as furnace or kiln. The required heat is derived from
burning of fuel or heat of exothermic reaction or conversion of electrical energy to heat.
Most industrial reactors are built to satisfy the following conditions:
a.

Maximum heat transfer from the heat carrier to the materials (reactants).

b.

Maximum coefficient of heat utilization minimum heat loss via utilization of


heat regeneration techniques.

c.

High productivity.

d.

Maximum product output and high quality of product.

e.

Simple and reliable construction.

f.

Operational stability.

g.

High degree of mechanisation and automation of process.

Industrial furnaces are classified using the following criteria:


1. The source of heat energy. 2. Method of heating. 3. Technological applications. 4.
Principle of construction etc.

1.

Source of heat energy. Furnace are classified into


i. Fuel furnace using solid, liquid and gaseous fuel.
ii.

Electric furnace in which the source of heat is electrical energy

iii.

Furnace in which the required temperature is attained by heat of


exothermic reaction.

2.

Method of heating
a. Directly heated furnace. These are subdivided into furnaces in which the heat
energy is:
1.

In contact with the materials as in cement kiln, alumina calcinator, and


electric arc.

2.

Released directly on the material, the burning of the material takes place
inside the furnace, as is the case in shaft furnace.

3.

Transferred via radiation from the hot solid bodies via a medium to the
reactants as in tunnel furnace, annealing furnace, etc.

C. Rotary kiln
S

d. Column roaster

G S
S

G
S
G

S
G

S
G

S
G

S, L
G
G
a.
Shaft furnace

S
G
b

G
G

S
S
S

G
e. Belt conveyor
G
f. Fluidized bed
Figure 4.16 Schematic presentations of reactors for G S system.
b. Indirectly heated furnace. The heat energy is transferred through the wall or solid
medium between the heat source and the materials. Examples include the coke
oven with external heater, muffle, tubular, crucible and retort furnace.

The principle of heat transfer is similar to that of mass transfer. The methods of
intensification presently used in the industries to enhance heat transfer processes are
similar to those of mass transfer considered in chapter 2. The overall heat transfer
equation for directly heated fuel fired furnace, with the heat transferred by heat carrier
can be in the simplified form represented as

Q FT ................................4.67
where Q quantity of heat transferred per unit time, T mean temperature difference
between the material and the heat carrier, F material surface area, - coefficient of heat
released, depends on the relative rate of mixing the heat carrier and material, their
density, viscosity, the coefficient of heat transfer, heat capacity, form and condition of
particles; surface, furnace construction, etc.
The mass and heat transfer rates can be intensified by:
a.

Increasing the heat transfer surface via grinding and mixing.

b.

Increasing the temperature driving force via counter current flow of material
and heat carrier.

c.

Increasing the extent/coefficient of heat released via utilization of radiation


heat from the furnace.

d.

Intensification of turbulence of the heat carrier.

e.

Increasing the coefficient if heat conduction, etc.

For directly heated furnace

Q KFT ................................4.68
where K coefficient of heat transfer. In the general form

1
.................................4.69
1
1


1
2

1 coefficient of heat released from the heat carrier to the wall separating it from the
material, 2 coefficient of heat released from the wall to the material, - wall thickness,
- wall heat conductivity.
Like the directly heated furnace, increase in the value of T for indirectly heated furnace
can be achieved by.
i. Increasing the temperature of the heat carrier.

ii.

Increasing the conductivity coefficient of the dividing wall via better selection of
the construction material.

iii.

Utilizing counter current flow of material and heat carrier.


Increase in heat transfer surface for indirectly heated furnace is achieved by increasing
the overall length of the reaction volume via introduction of fins or baffles. The heat
transfer coefficient can be increased also by reducing the wall thickness or increasing its
conductivity coefficient via better selection of material. The coefficient of heat released is
often determined during induced convection heat transfer condition using empirical
criteria equation such as the Nusselt criteria.

Nu A. Re m Pr n G

p
.4.70

where Nu al/ the Nusselt criteria, Re = wl/ the Reynold number, Pr = /a the Prandlt
criteria, G = L1/L2 geometrical simplex characterising the influence of geometrical
parameters on a. L1/L2 dimension of heat transfer surface(dimension of the reactor, heat
exchanger tubes, packings, etc.). - coefficient of temperature conductivity, w velocity
of gas or liquid relative to the heat transfer surface, - kinematic viscosity, a - /Cp coefficient of temperature conductivity, Cp specific heat capacity at constant pressure,
- density of the gas or liquid. The coefficients A and exponents m, n, p are determined
experimentally and are available in chemical handbooks.
3.

Technological application. Furnaces are classified into:


a.

Dryer, used to reduce the moisture content of material.

b.

Heater used in heating material. No physical change in aggregate


condition should be observed. Examples include thermal treatment of
metal and glass.

c.

Furnace used in melting material at high temperature such as electric


furnace.

d.

Sintering furnace used for burning of mineral raw materials such as


ceramic, cement, lime, etc.

e.
4.

Furnace for pyrolysis used for thermal treatment of fuel in vacuum.

Principle of construction. The design of reactors for G S system is based on:


a.

Kinetic equation, based on the reaction rate at the solid particle surface.

b.

Hydrodynamic regime of the two phases.

c.

Distribution of the particle sizes in the raw meal.

d.

Temperature distribution.

e.

Expected productivity, etc.

In general furnaces are constructed to enhance mixing or increased contact surface area
(Table 4.6).

Table 4.6 Classification of furnace using principle of construction and operation


Type/Name of
furnace

Type of process

Shaft
Blast.

Smelting of iron, copper, lead and nickel ore.

Calcinator.

Dissociation of carbonante.

Furnace for low


carbonisation.
Gas generator.

Hydrodynamic
and heat regime
Approximated
plug flow
pattern.
Polythermal

Low temperature carbonisation of coal and


tuff.
Gasification of solid fuel

Burning of
powdery material
introduced by
spraying/injection
.

Burning of iron pyrite concentrate and metals


ore

Dryer

Drying of material

Fluidized
Roaster

Burning of non-metals, limestone, etc.

Low temperature

Carbonization of coal, tuff, semi coke, etc.

Same as shaft

Approximated
well mixed.
Isothermal

Carbonisation
Regenerator

Burning of carbonaceous material from


catalyst surface.

Dryer

Drying of granules.

Gas generator

Gasification of solid fuel.

Cracking

Dissociation of high molecular fuel.

Rotary

Same as shaft

Cement kiln

Production of cement.

Sintering

Sintering of aluminate and silicate during the


production of alumina and silicate materials.
Dissociation of hydrated Na2CO3, CaCO3, etc.

Calcinator

Reduction of sulphates

Production of
Na2S, BaS, etc.

Drying of ore, minerals, salts, etc.

Dryer
Tunnel

Same as rotary

Roaster

Production of refractory, ceramic, etc.

Pyrolysis

Low temperature carbonisation of shale,


pyrolysis of wood, etc.

Smelting

Smelting of sulphur ore

Dryer

Drying of ceramic products

Chamber
For firing of
ceramic product

Firing of refractory and ceramic products.

For firing of glass


product

Firing of glass.

Ring or annular
Muffle

Rotor

Approximated
ideal plug flow.
Polythermal

Burning of brick and ceramic products.


Production of HCl and Na2SO4, transition of
yellow phosphorous to red, etc.
Dissociation of magnesium salts,
carbonisation, drying of wood, etc.
Gasification of solid fuel.

Low temperature
gasification
Dryer

Drying of ceramic, refractory, salt, etc.

Bath
Annealing

Smelting of steel (open-health), Cu, Pd, Ni,


etc. glass

Converter,
crucible, pot

Smelting of steel, Cu, etc.

Cyclone
Sintering

Burning of ferrous and non-ferrous

Flaring

Burning of fuel

Various regime

Approximated
well mixed.
Isothermal

Tubular
Pyrolysis

Ideal plug flow


Rectification of crude oil, etc.

Electric
Arc: Indirect
heating

Smelting and refining of non-ferrous metal


and alloy

Direct heating

Smelting of high quality steel, production of


ferroalloys, electrocracking of hydrocarbon.

Various regime

Resistance:
Indirect heating
Direct heating
Combined
heating method
Induction

Nitration of carbon, calcium, silicon and


silicon glass.
Production of artificial graphite, CS, CN.
Production of carbide, sublimation of
phosphorus, separation of metals from ores
and concentrates, electrolysis of molten
solutions, production of electrocorundum and
refractory.
Smelting of metals and alloys, silicon glass.

Q10. All reactors are constructed to ensure maximum exposed


surface area of the reactants. How is this reflected in the
design of reactors for heterogeneous processes S-L, L-L, S-S?

REACTORS FOR L S SYSTEMS


Most L-S processes take place in diffusion-controlled region, therefore in their reactors
design, various techniques directed at increasing the contact surface area and intensity of
mixing are applied. In the majority of these reactors the solvent is passed through
suspended or fluidised solid particle layer for thoroughly mixed (Table 4.7).

Table 4.7 Reactors for liquid solid system


Type of Schematic presentation
contact
reactor
Filter bed
S
L
L
of solid
S
adsorbent

S
S

Characteristic

Well mixed, cross


flow, co-current (at
the nucleus).
Adsorption, ion
exchange
processes.

High intensity,
moderate energy
consumption.
Simple to
construct. It could
be periodic but it
is easy to control

Well mixed, co or
counter current.
Mixing, extraction,
polymerisation,
leaching processes

High productivity
but high energy
consumption. Easy
to control, not
always reliable
and difficult to
maintain.

S
L

Fluidized
b ed
a. Normal
b.
Fountain

Mixing regime
Flow pattern and
example
Plug flow, counter
current.
Adsorption, ion
exchange, leaching
processes

Low intensity and


energy
consumption.
Simple to
construct and
control. Reliable.
Periodic or
continuous. Can
attain high
selectivity

L
L

L
S
S
L
L

With
mixer
a.
Mechanic
al

L
S

Product
b.
Pneumatic

Air Air
L, S

Well-mixed, cocurrent. Mixing,


extraction,
polymerisation,
leaching processes

Average
productivity,
periodic, simple to
construct and
reliable

Plug flow cocurrent.


Dissociation

Low productivity.
High energy
consumption.
Difficult to
construct.

Plug flow, cocurrent.


Dissociation,
leaching,
transportation

Low productivity,
high energy
consumption.
Difficult to
construct,
continuous
operation.

Product
c. Mixing
in column

Product
d. Screw
L, S

Product

Multiple
with
possible
combinati
on of
mixing
devices

L
Counter current.
High productivity,
Adsorption, ion
capital intensive,
exchange, leaching continuous
operation

L
L
L

Reactors with filter bed may be cylindrical in shape with the grids placed at the lower
part in the reaction zone. On the grids are porous solid granules or particles of the
adsorbent. The liquid is filtered through this layer of solid material. The internal surface
area of the solid material is determined by its porosity. Reaction in filter bed is limited by
internal diffusion. The rate and the direction of the liquid flow depend on the height of
the filter bed and granules sizes. In most cases the liquid stream flows top down. Filter
bed reactors are used in adsorption, ion exchange, leaching processes, etc.
Multiple filter bed reactors are widely used in leaching and ion exchange processes. The
depleted solution is removed at the last reactor along the liquid flow direction as fresh
ones are poured into the first. The used solid reactant is discharged at interval and fresh
ones introduced. Reactors with continuous regime in which the solid solute particles are
suspended in the liquid phase are also used in the adsorption and ion exchange processes.
These reactors are very effective when the difference in densities of the liquid solvent and
the solid solute is high, the later having large surface area.
For system with insignificant difference in densities and small size granules, the fountain
reactors are more feasible (Table 4.7b). Fountain reactors are used for polydispersed solid
materials and where the use of grid is not advisable due to the aggressiveness of the
medium. Velocity of flow in fountain reactor (cm/s) far exceed that of suspended or
fluidised bed (mm/s), consequently the former is more efficient. One of the construction
peculiarity of the fountain reactor is that the diameter of the lower part of the reactor da
(Table 4.7b), must be smaller than that of the communication tube dT (da dT) to ensure
the formation of a stable fountain. At the same time the fluid velocity wf must be lower
than that necessary to suspended the particles wp to avoid the removal of the later from
the reaction zone.
During ion exchange process in fountain reactor, the liquid is passed through the reactor
from the bottom up until the solute (ionate) is saturated with the cation of the non-ferrous
metal in the solvent. Regeneration of the solid is performed in the same sequence using
the regenerating solvent to obtain a concentrate of the non-ferrous metal solution.
REACTORS WITH MECHANICAL AND PNEUMATIC MIXING DEVICES
The impeller-anchor or agitator mixers are commonly used for L-S processes such as
extraction, dissolution, leaching, polymerisation, and organic and inorganic syntheses.
For liquid with average viscosity the impeller-agitator could be used, while the anchorimpellers are more appropriate for high viscosity systems (Figure 4.21). The anchor
impeller can withstand intensive mechanical loading and has low hydrodynamic
resistance. The outer part of the impeller should be quite close to the reactors wall to
avoid the formation of crust on its surface.
Screw mixer (conveyor) consists of a rotating shaft on which are welded spirally metallic
or plastic blades. Materials are fed into the mixer via the loading zone and discharged at
the other end. Reactors with screw mixer may be equipped with heat exchangers to
regulate the rate of chemical reactions (Table 4.7e).

SOLID SOLID, LIQUID LIQUID AND MULTIPLE PHASE SYSTEMS


Caking, baking, sintering, clinkering and vitrification are processes involving SS
materials during burning. In this book, sintering will be commonly used to represent
these processes. Sintering is the production of porous solid products from finely ground
solid materials at high temperature. Sintering often occurs in presence of insignificant
amount of liquid component. During heating of solid mix, reactions occur between the
solid components or the solid and gaseous components or solid and liquid components
produced during complete or partial melting of the solid components or their intermediate
products. Sintering is commonly used in metallurgy, silicate industries, etc.
Technological processes involving two or more liquid components include extraction,
emulsification and demulsification. Extraction is the selective removal of a desired
component in a liquid mixture using a solvent in which it is very soluble. Extraction is
more feasible as a separation technique when it is impossible or difficult to use
distillation or fractional distillation techniques due to insignificant difference in boiling
points of the liquid mixture components.
Emulsification (immiscible liquid) production of emulsion. This is the dispersion of one
liquid in another in form of fine capsules. Demulsification is the reverse of emulsification
process. These processes are used in the production of paints, pigments and various high
molecular polymers. Demulsification is used in the petroleum industry during dewatering of crude oil. Reactors for heterogeneous (immiscible) liquids are equipped with
various kinds of mixing devices and heat exchangers. Heterogeneous liquidliquid
(immiscible) process is organised using the batch or continuous regime with well-mixed
flow pattern of the fluid in the reactor. Their reaction kinetic is the same as that of
homogeneous system.

Reactant
Mixer
Gaseous product
Steam

Steam

Water

Water

Product
Figure 4.21 Reactor with anchor-impeller.
Packed bed or column reactors with counter current flow pattern (more viscous flowing
up down, while the lighter fluid down up) are used for liquid extraction processes. In
most chemico-technological processes more than two phases are involved. Examples
include the production of steel involving the solid, liquid and gaseous phases. The rate of
multiple phase system is determined by that of the slowest reaction involving any of the
phases.
REACTORS FOR CATALYZED REACTIONS
Q11-12. What is unique in the design of reactors for catalytic process. Will you
recommend a fluidized bed reactor for catalytic processes.
Reactors for heterogeneous phase catalysis especially the contact reactors must:

Be operated on a continuous regime.

Possess high production intensity.

Guarantee an optimum regime especially operating temperature.

Ensure minimal hydraulic resistance

Simple to construct.

Homogeneous phase catalyzed reactions are easily conducted in contact reactors like the
capacity-type, column and tubular reactors, heat exchanger, etc. For example dehydration
of acetic acid in vapour state using triethylphosphate (gas) as catalyst is conducted in
tubular reactor. The heat required for the reaction is supplied by the flue gases circulating
in the inter tubular space. Liquid phase catalyzed reactions are conducted in reactors
equipped with mixing devices.
Construction of reactors for catalyzed processes depends on the phases of the catalyst and
reactants. Heterogeneous catalyzed reactions can occur in the gaseous phase using solid
or liquid catalyst. Most industrial catalyzed processes occur in the gaseous phase on solid
catalyst.
Catalyzed reactions are classified into isothermal, adiabatic and polythermal, depending
on the temperature regime. Using the extent of mixing, catalyzed reactions are classified
into:
1. Ideal plug flow, well mixed and partially mixed.
2. Suspended or fluidized catalyst layer.

3. Mobile catalyst stream flowing between the reaction compartment and the
regenerator.
REACTORS WITH FILTER BED CATALYST
The catalyst is placed on stationary column or inside the tube. The reactant is passed
through the catalyst layer, in a regime close to ideal plug flow. The higher the
height/depth of the catalyst layer the lesser its activeness and probability of the gases
mixing along the reactors length/height. Catalyst used in filter bed can be in form of
different size particles/grain/tablet/granule of 4 5mm in cross section; smaller size
particles increase the hydraulic resistance of the system and are easily sintered during
firing. The quantity of catalyst on the bed and number of column and their positioning are
dependent on the catalyst activeness, condition of heat transfer and type of reaction. The
higher the activeness, rate of reaction and equilibrium product output the smaller the
quantity of the required contact mass.
The method of heating or choice of heat exchanger determines the construction of filter
bed contact reactor. In endothermic reactions, it is easy to regulate heat supplied to the
catalyst bed. More difficult to control is the temperature regime in reversible exothermic
reactions as it is necessary to regulate the heat supplied to or removed from the reaction
zones.
Filter bed catalyst reactors have the following disadvantages:

Porous catalyst grains are poor heat conductors. This makes it very difficult to
guarantee uniform distribution of heat/temperature along the reactors height.
The only available method of heat transfer process is to place the heat
exchanger inside the catalyst layer. Even this method should be applied
carefully as the catalyst can easily be deactivated due to drastic fall in
temperature around the heat exchanger (attributable to the poor conductive
properties of porous catalyst grains).

Poor conducting properties of the porous catalyst filter bed makes it difficult
to regulate and maintain optimum temperature regime. For example in
exothermic reactions, with increasing contact time the mass temperature
increases steadily (Figure 69, 70). This deactivates the contact mass and
reduces the productivity.

Only grains of 4 6mm in cross section are recommended as smaller ones


greatly increases the hydraulic resistance in the reactor.

Continuous utilization of catalyst at high temperature in filter bed will lead to


its smelting. This increases the hydraulic resistance, distorts the distribution of
gases and reduces the catalyst activeness.

Catalyst in contact reactors is not easily regenerated. This considerably


increases the cost of production, as the catalyst has to be replaced on
deactivation.

FILTER BED REACTORS WITH HEAT EXCHANGERS


They are easy to construct. The temperature regime is regulated by changing the
composition or temperature of the initial reactant. These reactors are used for reversible
exothermic reactions using a thin layer of very active catalyst (Figures 5.6 and 5.7).
Reactant
Reactant

Inlet

Water
(Heat carrier)

.
.

Water
Product
Refractory lining
Product
Figure 5.6 Filter bed catalyst reactor
Containing very active catalyst.

Figure 5.7 Filter bed catalyst


reactor for processes with low
heat of reaction.

The quantity of catalyst used is determined by its activeness. For catalyst with low
activeness the height of the catalyst layer could be in metres. In exothermic processes the
temperature of the reacting gases on the catalyst surface increases proportionally with the
extent of reaction x.
Filter bed catalyst reactors are usually fitted with heat exchangers to maintain optimum
operating temperature. There are various ways of regulating heat of reaction
(temperature) in the catalyst bed. The heat supply and removal techniques used during
construction of reactors are similar for both exothermic and endothermic reactions. The
reactors are classified into the following groups.

Contact reactors with periodic supply and removal of heat.

Contact reactors with external heat exchangers.

Contact reactors with internal heat exchangers.

These are sub divided depending on the position of the heat exchanger into
a. Reactors with heat exchanger between two reactors.
b. Heat exchanger is placed between the reactants layer in the column
*

Contact reactors with combination of two or more heat exchanger techniques.

CONTACT REACTORS WITH PERIODIC SUPPLY OR REMOVAL OF HEAT


These reactors are mainly used for endothermic catalyzed reactions. The reaction
chamber is lined with refractory material. The reactant and the heat carrier is alternately
passed into the chamber. The heat carrier transfers it heat to the catalyst and refractory
lining, heating the catalyst to the activation temperature (Ta). The refractory lining also
serves as heat accumulator; releasing the heat as the chambers temperature drops. After
heating the reactant is then released to the chamber. This type of reactor is used in
dehydrogenation of hydrocarbon, catalyzed cracking of hydrocarbon and other
endothermic processes where the regeneration of the catalyst might not be necessary. It is
very inefficient in operation.
CONTACT REACTORS WITH EXTERNAL HEAT EXCHANGERS
Heat exchange between the reactant and the heat carrier takes place in the external heat
exchangers arranged in series (Figure 5.9). This is to maintain optimum operating
temperature in the reactor or column. Figure 5.9 is an example of reactors with
intermediate (external) heat exchangers. It is used for reversible exothermic reactions.
The initial reacting mixture is heated in the inter tubular space of the heat exchangers (c,
b and a) using heat of exothermic reactions or heat contained in the outgoing products to
the required activation temperature. The reacting mixture is then sent to the contact
reactors 1, 2 and 3 after heating in the intra tubular space of the heat exchangers (a, b and
c).
Contact reactors
1

Heat exchangers
a

c
Reactant

Product
Figure 5.9 Schematic diagram of multiple reactors with external heat exchangers
The product output in each contact column 1, 2 and 3 decreases with the contact time
(x1 > x2 > x3, Figure 5.10). Consequently the reaction heat effect and the quantity of
heat removed after each column in the exchangers decreases. Therefore the quantity of
catalyst in each column 1, 2 and 3 increases steadily the further it is from the inlet; this
increase the contact time between the reactant and the catalyst. However the extent of
reaction steadily decreases according to the law of active mass. Cooling of the reacting
mixture in the exchangers a, b and c are indicated on Figure 5.10 by the horizontal lines
a, b and c.
CONTACT REACTORS WITH HEAT EXCHANGERS PLACED IN THE
COLUMN
In these reactors the heat exchangers are embedded inside the reaction chamber (Figure
5.11). Heating or cooling of the reacting mixture takes place in the column using the heat
carrier or coolant passing through the tubular space of the exchanger. The heat exchanger
is positioned above the grid and between the columns. The height of the catalyst bed in
each column decreases upward as the extent of reaction and consequently the heat
released decrease downward.
Processes in this contact reactor can also be represented as in Figure 5.11. In the columns,
reactions take place in adiabatic condition using the heat of reaction as heat source.
Cooling of the reacting mixture is made possible using the coolant flowing in the
exchanger or fresh reactants in counter current flow to reaction products.

Catalyst layer
Heat exchanger
Catalyst layer
Reactant

Product

Figure 5.11 Contact reactor with the heat exchanger embedded in the reaction chamber

TUBULAR CONTACT REACTORS


This reactor can be used for exothermic and endothermic processes. The reactions take
place in polythermal condition inside the tubes (filled with the catalyst) in the reaction
chamber. The heat lost is partially compensated from external heat supply. For
endothermic reaction hot heat carrier is first passed through the catalyst. The reacting
mixture in counter current flow to the heat carrier is heated to the activating temperature.
The heat content of the product can be used in preliminary heating of the fresh reactant or
utilized in boiler (Figure 5.12).
Reactant

Heat carrier

Heat carrier

Product
Figure 5.12 Tubular contact reactor
Tubular contact reactors are sometimes built in form of tubular heat exchangers placed
inside a container (Figure 5.12) or as furnace with the tubes containing the catalyst
positioned inside. Example of endothermic process conducted in tubular contact reactor
includes dehydrogenation of butane. For exothermic reactions the heat carrier is passed
either through the catalyst tubes or between the tubes. The heat transfer process is
between the catalyst and the cold, fresh reacting mixture.
Various heat transfer techniques are now used in the construction of contact reactors. For
example in tubular column-contact reactor, the catalyst could be positioned in columns
and tubes arranged above the grid. Reactors with combined heat transfer techniques
operate very close to the optimum temperature regime and are preferred to the fluidized
bed reactors.
CONTACT REACTORS WITH FLUIDIZED OR SUSPENDED CATALYST
LAYER (FLUIDIZED BED REACTORS)
Fluidized bed has many advantages compared to filter contact catalyst bed. Catalyst
grains of 0.1 2mm in diameter can be used and it has better heat conductivity thus
minimizing possibility of smelting. The particles are suspended by the gaseous or liquid
reactant passed through the grid bottom-up at a velocity enough to move the particles and

the entire catalyst mass from stationary to fluidized state (critical velocity). In suspension,
the catalyst grains can move in all direction thus enhancing diffusion of reactants
molecules into its pores. The hydrodynamic regime in the fluidized catalyst bed is close
to well mixed with isothermal temperature regime.
The schematic diagram of contact reactor with fluidized catalyst layer for exothermic
processes is presented in Figure 5.13. The reactor may have more than one grid or
column evenly distributed along the reaction chamber. The reactant is passed bottom up
while the product is collected from the upper segment. In most design the upper segment
is larger in diameter than the lower.
Product

Fluidized
catalyzed bed

Heat
carrier

Reactant
Figure 5.13 Multiple column fluidized bed reactor
This difference in diameter helps to reduce the velocity of the outgoing product/mixture
and thus enhance the sedimentation of the catalyst particles. The heat of reaction is
removed by the heat exchangers positioned in the reaction chambers; above each column.
As the catalyst particles are not in permanent contact with the exchangers surface, the
disadvantages associated with contact reactors are minimized and the heat transfer is
high. In construction, heat exchangers used in fluidized/suspended catalyst bed are much
simpler than those of filter bed; does not require complex internal and external
intermediate exchangers and are smaller in surface area.
Heat is easily transferred by convection in fluidized bed as a result of the continuous
movement of the contact mass. Consequently it is easy to maintain the required
temperature (isothermal) in the reaction chamber. The coefficient of heat transfer in it is
greater than that of the filter. Therefore the probability of catalyst deactivation due to
intensive heat removal or overheating as a result of high initial reactant concentration is
minimal. The above factor also eliminates the necessity of preheating the initial reactant
to the activation temperature Ta as it can be easily heated; compliment of the high heat
conductivity of the system. In the first (lower) column the temperature is maintained by

regulating the heat content of the initial reactant. Heat exchanger may not be necessary in
this column.
Contact reactor with fluidized bed has high productivity due to:

The small catalyst particle sizes. This enhances complete utilization of the
internal surface area and

Easy maintenance of temperature regime.

The main disadvantages of fluidized bed when compared to the filter bed are:

It has very small driving force due to the effective mixing of the reactant. The
decrease in driving force is proportional to the extent of reaction. Utilization
of multiple columns minimizes this effect and makes it possible to operate at
close to optimum temperature.

Wearing of catalyst grains surfaces especially the edges. Only high


mechanical strength particles with high resistivity to attrition should be used
in fluidized bed reactors.

Catalyst used in fluidized bed can be regenerated continuously or discharged depending


on the technology. Continuous regeneration of catalyst in contact reactor is widely
practised in hydrogenation, dehydrogenation of paraffin, cracking processes, etc.
Q13. Heat exchange is a very important component in a reactor design. In all the
reactors considered for the homogenous and heterogeneous processes how was heat
transfer considered?
REACTORS WITH MOBILE CATALYST
These reactors are widely used in steam cracking of petroleum products and other
processes requiring continuous circulation of the catalyst between the reactor an
regenerator (Figure 5.15). Two types of contact reactors with mobile catalyst are widely
used:
1.
Small catalyst grains are suspended
by gas stream, and
2.

Large size grains made to move


down a shaft in co-ordinated co or counter current flow to the reactant.
Product
Regenerator
Mobile fluidized

catalyst bed

Regenerated catalyst
returned

Reactant
Heat
carrier
Figure 5.15 Schematic diagram of contact reactor with mobile catalyst
In the former the velocity of the gas flow is very high and the particles are removed from
the reaction chamber. The catalyst is then separated from the gaseous mixture in cyclone
and sent to the regenerator, where in fluidized condition the hydrocarbon deposit on its
surface is burnt off. The regenerated hot catalyst along with the gaseous reactant is
returned to the reaction chamber. The major disadvantage of mobile catalyst contact
reactor is the incomplete separation of the catalyst from the gas stream. A lot of attention
is given to purification process thus increasing the cost of production.

Week 8: Mechanical design of equipment: storage tanks, heat exchangers


Week 9: Mechanical design of equipment: Pressure vessels, columns
Mechanical design of equipment is the first stage of physical expression of the concept as
a product. There is no universal technique in developing a mechanical design.
However there are some basic steps that are fully established. Mechanical
design will often start with stating the basic assumption or conditions to be
eliminated or achieved.

The use of all information on the physics, chemistry and the basics sciences in resolving
the effects of expected forces or reactions to determine the outward physical
manifestation of a product. The extent an equilibrium is achieved will determine the cost,
functionability, survivability, reliability, constructability or manufacturability of
the equipment.
A mechanical design can be aided with the use of software tools to create
elegant outward geometrical forms. It is important that selection of any
software must be based on understanding of the theorems of the equipment
to be designed.

Equipment design can be started based on the expected outward and


ergonomic appearance. Such product may be more attractive and perhaps
more user-friendly.
Mechanical design could be initiated from:

DESIGNING FROM KNOWN SCIENTIFIC PRINCIPLES


CONTACT REACTOR DESIGN
The choice of design technique is determined by the given technological conditions and
parameters and client objectives. In the example below the volume of catalyst, the heat
transfer surface area guaranteeing maximum process rate and expected extent of reaction
will be calculated. The features to be considered in choosing a reactor for a given process
include the reactor type, extent of reaction and expected productivity, the technoeconomic index, that is the quantity of metal expended per unit product, cost of
production, extent of energy conservation, availability and economic catalyst, etc.
CONTACT REACTOR WITH FILTER BED CATALYST LAYER FOR
EXOTHERMIC REACTION
Q14. Briefly discuss the various stages of designing for a contact reactor with filter bed
catalyst layer.
The following major steps might be considered during the design process.
1.

It is necessary to construct an approximated x = f(T) diagram (Figure 5.14),


especially when considering the possible use of multiple column reactor. The
equilibrium xeq T curve should be constructed using values from standard
chemical hand books. For cases where the equilibrium constants are given, the x eq
should be calculated using eq. 43, 44 chapter 2. For simple reaction such as A + B

xeq
= 2C, without volume change

k eq
k eq 2
.

For some reactions coefficients accounting for volume change are introduced to
the ideal equation. In the absence of textbook xeq, equilibrium constant values for
various temperatures can be calculated using eq. 53 57 in chapter 2. The

optimum temperature curve is derived from experimental data or calculated using

T
eq
T
op
2.3RT
eq E mq
1
lg
mq
E
Where T temperature, K, R gas constant, 8.31kJ/(mol.K), m coefficient
representing the stoichiometry of the major component when 1M of the desired
product is produced., q heat of reaction, kJ/mol, E activation energy, kJ/mol.
Optimum temperature may be calculated using the extent of reaction.
2.

The material balance for the entire reactor or when necessary for each column is
calculated according to chapter one and the x = f(T) diagram. From the material
balance the gas volumetric flow rate V, m3/s and extent of reaction are calculated.

3.

Contact time t, is calculated using the process rate eq. 94 108, chapter 2 and or
for kinetic controlled ideal plug flow reactor eq. 17 23 chapter 3. For first order

t
reaction

1
1
In
k 1 x

The value x is given or determined using the x T diagram, k is determined from


experimental data or mathematical modeling. The influence of temperature on
reaction rate is determined using the Arrehenius equation. The time t is the contact
time between the gas and the catalyst. In most cases this calculation is very
difficult to solve analytically, therefore graphical integration or iteration methods
are widely used.
4.

Having calculated V and t, the volume of the contact mass m3 is calculated,

v Vt
.
The assumed contact time wf, hr-1 or s-1

V
w
a v

The loading coefficient = 1.3 2.5. It is obtained from practical experience. The
loading coefficient varies with the type of reaction, catalyst used and position of
the reactor or column. also considers the influence of internal and external
diffusions, expected change in catalyst activeness with time and decrease in
process driving force due to mixing. Therefore in practice the assumed contact
time wa do differ from t.
5.

The heat balance should be calculated varying the heat exchanger surface area and
temperature until the optimum technological regime is attained.

6.

The cross-sectional volume of the reactor F is calculated using

V
w
a

wa assumed contact time in the layer. The actual contact time wf must ensure
adequate mass and heat transfer between the catalyst and gas, and guarantee
satisfactory hydraulic condition.

w w
f
a
where - porosity of the catalyst layer. It is equal to the ratio of the free grain
volume to the overall volume of the layer.
7.

Height of the catalyst layer H

F
4V

A D 2 w
a

8. Hydraulic resistance

P P P P ....
c
g
l

where Pc hydraulic resistance due to the catalyst layer, Pg


resistance due to the grid, Pl local resistance at the inlet and
outlet points.
Resistance along the piping should also be considered where
necessary. The resistance at each layer can be calculated.
Standard equations could be obtained from textbooks. For
example

s
P
c
3

w2
g f
H
2g

where - coefficient of friction between the gas and the catalyst

grains. For granulated contact mass

3.7 Re 0.35

, where Re

Reynold number, s external surface area of the grains per 1m3


catalyst, m2/m3, - porosity, - gas density, kg/m3, wf - actual gas
velocity, m2/s.
These calculated values x, Top, t, v, V, heat balance F, wa, wf, P, etc.
are subject to construction and economic factors and could be
changed. Consequently, design calculations may be repeated until
the required values are obtained.
9.

On the bases of the design calculation, the technological flow-chart


is developed. Equipment design as conducted above should be
presented in form of technical drawing.

DESIGNING FROM MATHEMATICAL MODELS


Q15. What is the first step in model design of a process?
Modeling means the study of a process or reactor through the physical
or mathematical equations or model; that is a simplified system that
allows for direct monitoring and control of phenomena in the process.

Models are prognoses tools for evaluation of chemico- technological


processes and working regime of industrial reactors.
System analysis may be considered in the following stages:
1

2
3

Conceptualization and analysis of the object to determine its individual elements


and their relationship. Establish the hierarchical structure and selection of the
desired elements based on the design objects. It is important to effectively
describe a system characteristic design theory and thus evolve the required model
methodology. The conceptual stage actually begins with the descriptive model. It
splits the entire process into units that can be further split into smaller units for
ease of understanding the process phenomena. Entities which are related by
principle and law are grouped into the same unit or sub unit. The extent of
splitting is determined by the researcher experience and knowledge. Particle size
can be considered in the macro, micro, molecular, element, atomic, nano, etc.
depending on the type of system and available mathematical expression of the
process phenomena. Reduction of the particle size significantly complicates the
surface physicochemical processes (see section 2.2 decarbonization model).
Existing mathematical model may not effectively describe the changing surface
phenomena with continuous size reduction.
Formulation of the element concepts or idea as mathematical models based on the
identified scientific laws and experimental data. The established mathematical
model can then be used to develop those for the input and output parameters.
Mathematical modeling and simulation of the process. The developed software
based on the developed model formula can be used not only in investigate the
process but to make prognoses of the effects of parametric excitations on the
overall technological process. Experimental verification of model portrays the
theoretical level of understanding of the investigated phenomena; neglecting the
adopted assumptions.
Identifying physical and mathematical models elements consist of identifying the
independent variables and process state.

The first step in physical and mathematical modeling is to find out the
mathematical functional relation between rate of reaction u or rate
constant k or product output and other technological parameters. The
rate of chemical reaction is mainly dependent on the concentration of
the reactants and products C1, C2, C3; coefficients of effective diffusivity
of components D1, D2, D3; temperature in the reaction medium T and
pressure P; extent of mixing of reactants (phases) this is dependent
on the relative velocity of the phases wg, wl, ws; catalyst activeness Ac;
density of reactants g, l, s; viscosity coefficient dynamic or
kinematic ; surface tension ; geometrical characteristics of the
reactor, height H, diameter D, etc.

u f (C , C , C ...D D , D ..T , P, w , w , w ...A , , , , , H , D)..23


1 2 3 1, 2 3
g l s C g l s

Kinetic characteristics are also dependent on the heat transfer


conditions in the reactor and should be considered during modeling.
The deduced optimum parameters should guarantee minimum cost of
production at minimum utility coefficient of raw materials, energy, fuel
and other economic parameters.

DESIGNING FROM EXPERIMENTAL DATA


Q16. Designing from experimental data is quite different from
designing from theoretical analysis of a process. Which is
better?
In designing, it is important to have information about the reaction
chemical kinetic and desired capacity of production and then decide if
the process should be continuous or batch and on method of charging
and discharging.
Experiments are organized particularly for process whose mechanism
are poorly understood or lack sufficient data for the researcher to work
with and develop the kinetics. All experimental rates are an
embodiment of kinetics and mass transfer phenomena. When technical
grade or synthetic compounds are involved the derived rates can be a
near representation of the global rate for the reaction as secondary
reactions are almost eliminated. In reacting raw materials, it is not
correct to refer to the obtained rate as a representative of the desired
reaction; since there were lots of secondary reactions also occurring.
For reacting natural raw materials experiments are performed to serve
as a guide.
The choice of reactor is influenced by the fact that apart from chemical
and physical processes (diffusion of reactants and products), the
production and distribution of heat also takes place during the
production process.
The method of technological calculations and choice of parameters
differs with processes, depending on the type of reactor used.
Classifications of reactors are primarily based on factors influencing
the kinetics. Such factors include the hydrodynamic conditions and
temperature regime. Reactors operating at extreme hydrodynamic
regime are classified into ideal plug flow and well mixed and those at
isothermal condition into adiabatic or polythermal. Such idealized
classification helps in eliminating secondary influences during
consideration of the reaction kinetics.
Industrial reactors are far more complex than the ideal ones.
Calculations of industrial reactors parameters are based on

experimental data. The ideal model only serves as reference when


determining the basic technological parameters and reactors
dimension. Investigation of reactor characteristics is performed by
mathematical representation of the processes, that is investigation of
changes in T, C, and P. Modeling can be performed for an infinite
elementary size or the complete reactor using the material and energy
balances.

Q17 Example of design from experimental data. Will you recommend a theoretical
approach to this experimental method?
DESIGN OF ESSENTIAL OIL PILOT PLANT
Odigure J. O., Okonkwo E. M., Williams I. S. et.al. J. Scientific & Industrial Research.
India, vol. 65, Nov. 2006, pp. 912-915. ( In collaboration with National Research Institute
for Chemical Technology Zaria and Raw Materials Research and Development Council,
Abuja)
EXECUTIVE SUMMARY
The numerous economic incentives of the Federal Government of Nigeria aimed at
facilitating rapid industrial growth of the nation, are added advantages to investors in the
ESSENTIAL OILS production sector. There is an overwhelming need and market for the
product. Essential oils are indispensable in any perfume, beverages, cosmetics, soap,
foods, and pharmaceuticals industries.
They are found in various parts of plants such as the fruits, flowers, leaves, seeds, stems,
barks, woods, roots, or the whole plant. Essential oils bearing plants are readily available
in all geographical zones of our country. Various technology have been developed for
essential oils production, however the technology of steam distillation or better put, the
use of steam as heat carrier have gained wide application.

To a large extent the development of the essential oil sector in the country has been very
slow either due to lack of proper technological know-how or non-availability of local
processing equipment. Therefore the major objective of this design is to develop a cost
effective, environmentally friendly process that takes into consideration the technological
development of our economy and market structure.
A packed bed steam extraction tank still equipped with a condensing unit has been
designed. The expected productivity is (0.864x4x200) = 691.2m3 per year. Analysis of the
designed process shows that it is suitable for local cottage industry.
PROCESS DESIGN
INTRODUCTION
Essential oils are sometimes called volatile Oils or Ethereal Oils; the term essential is
derived from essence and has no connotation of need. Essential Oils are mostly
volatile in steam and generally are mixture of a variety of chemical low carbon
hydrocarbon compounds, together with their oxygenated derivatives such as alcohols,
esters, aldehyde, ketones, ether and acids. They are found in various parts of plants such
as the fruits, flowers, leaves, seeds, stems, barks, woods, roots, or the whole plant.
Essential oils are indispensable in any perfume, beverages, cosmetics, soap, foods, and
pharmaceuticals industries. Presently, almost all the essential oils used in the country are
imported and the demand for the products is increasing rapidly with serious consequence
on the meager foreign reserve.
Essential oils bearing plants are readily available in all geographical zones of our country
most especially the Eucalyptus. It grows well in area threatened by desertification and
therefore its massive cultivation will tremendously help in solving the ugly problem.
However lack of proper know-how and processing equipment has frustrated local
production.

Various technology have been developed for essential oils production, however the
technology of steam distillation or better put, the use of steam as heat carrier have
gained wide application. This will be adopted in this project.
Essential oils to a large extent are practically insoluble in water and reasonable stable to
action of heat. Unfortunately most parameters required for proper design are not readily
available. Consequently, it was essential to experimentally determine them.
Comprehensive experiments on characterization of the technological parameters and
crude obtained were performed in laboratory condition. The results are presented below.
PROJECT OBJECTIVE
The main objective is conceptualize, design, construct and test run a pilot plant for the
production of 8.64x10-1m3/hr or 2.4x10-7m3/s (864l/hr or 0.738kg/hr) of essential oils
from locally sourced plants using Eucalyptus leaves as a case study with steam as the
carrier medium. It is expected that the fabricated pilot plant will be simple and cheap to
enhance the local development of essential oils cottage industries in the country.
EXPERIMENTAL RESULTS
The results of various experiments aimed at finding optimum technological condition for
the production of essential oil from Eucalyptus leaves are presented Figures 1 14.

Fig. 15 Comparativ e analy sis of steam leav e ratios


8

Steam-leaves, ml/g (200g leaves)


Steam-leaves, ml/g (400g leaves)
Steam-leaves, ml/g (600g leaves)
Steam-leaves, ml/g (200g leaves)
Steam-leaves, ml/g (400g leaves)
Steam-leaves, ml/g (600g leaves)

Steam-leaves, ml/g (200g leaves)


Steam-leaves, ml/g (400g leaves)
Steam-leaves, ml/g (600g leaves)
Steam leav e ratio, ml/g

Steam-leaves, ml/g (200g leaves)

Steam-leaves, ml/g (400g leaves)


Steam-leaves, ml/g (600g leaves)
Steam-leaves, ml/g (200g leaves)
Steam-leaves, ml/g (400g leaves)
Steam-leaves, ml/g (600g leaves)

Steam-leaves, ml/g (200g leaves)


Steam-leaves, ml/g (400g leaves)
Steam-leaves, ml/g (600g leaves)
Steam-leaves, ml/g (200g leaves)

Steam-leaves, ml/g (400g leaves)


Steam-leaves, ml/g (600g leaves)

0
10

20

30

40

50

Time, min

60

70

80

90

Fig 16 Comparativ e Oil-leav e ratio


4

oil-leaves ratio x10-2ml/g (200g


leaves)
oil-leaves ratio x10-2ml/g (400g
leaves)
3.5

oil-leaves ratio x10-2ml/g (600g


leaves)
oil-leaves ratio x10-2ml/g (200g
leaves)
oil-leaves ratio x10-2ml/g (400g
leaves)

oil-leaves ratio x10-2ml/g (600g


leaves)
oil-leaves ratio x10-2ml/g (200g
leaves)
oil-leaves ratio x10-2ml/g (400g
leaves)

2.5

oil-leaves ratio x10-2ml/g (600g


leaves)

Oil-leav e ratio x 10-2ml/g

oil-leaves ratio x10-2ml/g (200g


leaves)

oil-leaves ratio x10-2ml/g (400g


leaves)
oil-leaves ratio x10-2ml/g (600g
leaves)
oil-leaves ratio x10-2ml/g (200g
leaves)

1.5

oil-leaves ratio x10-2ml/g (400g


leaves)
oil-leaves ratio x10-2ml/g (600g
leaves)
oil-leaves ratio x10-2ml/g (200g
leaves)

oil-leaves ratio x10-2ml/g (400g


leaves)
oil-leaves ratio x10-2ml/g (600g
leaves)

0.5

oil-leaves ratio x10-2ml/g (200g


leaves)
oil-leaves ratio x10-2ml/g (400g
leaves)

0
10

20

30

40

50

60

70

80

90

oil-leaves ratio x10-2ml/g (600g


leaves)

Time, min

In all the Figures 1 14 there are time lags. This is the period the introduced steam is
utilized to heat up the reactor and the content. The period is dependent on the rate of
steam supply and leaves weight. It is generally between 16 21min. for moderate heating

and 12 18min for fast. However fast heating may not yield greater oil. The moderate
heating regime seems to give the best oil production with maximum oil output of 3.0x10 2

ml/g. Calculations of the gradient of Fig. 5 and 6 revealed the steam utilization (steam

required to transport the oil) and oil production rates are 9.33x10 -4ml/s and 9.42x10-6 ml/s.
per gram leave. This gives a steam : oil ratio of 100:1. Analysis shows that the rate at
which steam passes through the leaves bed may deviate from linear relationship to curve
depending on the loading capacity.
Comparative analyses of the figures are presented in Figures 15 and 16. They clearly
confirm the chosen steam oil ratio. They showed that maximum oil could be obtained at
an optimum steam leave ratio. High steam supply does not necessarily enhance the rate
of oil removal from the system. The Figures also show that maximum oil removal is
independent on the heating regime. It is a function of the steam flow rate and leaves
packing density.
Process technology
Several process technologies for the development of essential oils have been developed.
In all cases the action of heat and moisture is used to breakdown the cell tissues of plant
and liberate the essential oil.
In this project the steam distillation technique has been adopted because of the efficiency.
In this technology steam obtained via distillation of water is passed through packed bed
of plant materials. The emerging steam-oil vapour mixture is led to the condenser for
condensation. The condensate is collected and allowed to separate into water and oil
layer. The crude oils is collected and dewatered before storage.
The process technology therefore consists of the tank still or reactor, the condenser and
separator (Figure 17). The steam required for the process shall be obtained for a steam
generator or water distillation equipment.

Oil
Steam/
Tank still
(At steady state)oil
Condenser

Separator

Water

Steam
Oil
Tank still
Leaves(At unsteady state)

Spent leaves

Steam
Condensate
Figure 17 Schematic diagrams for the production of essential Oils.
DESIGN CONDITIONS
The technological conditions used for the design are to a large extent determined
experimentally. They are summarized as follow:
Optimum steam:Oil ratio per gram leave

9.33x10-4:9.42x10-6 (ml/s)

Optimum steam supply rate per gram leave

9.33x10-4ml/s

Residence time after first water oil mixture drops

50-60min.
853.8kg/m3

Density of essential oil


Density of steam oil mixture

853.96kg/m3

Viscosity of steam oil mixture

6.92x10-4Ns/m2

Heat capacity of mixture c

4.0kJ/kg.oC

Thermal conductivity of mixture kf

0.69W/moC
995kg/m3

Density of steam
Viscosity of water w

8.0x10-4Ns/m2
25oC

Cooling water inlet temperature


Cooling water outlet temperature

50oC

Condensate temperature

40oC

Steam temperature

100oC

Operating pressure

atmospheric

Productivity

8.64x10-4m3/hr

Density of leave

1800 kg/m3

Operating bulk density

310 kg/m3

MATERIAL BALANCE
Based on the defined process productivity the material balance was performed starting
from the separating unit.
Separator unit
The material balance over the separator is as presented in Figure 18
Oil 2.4x10-7m3/s
Or 2.05x10-4kg/s
Water oil mixture
Separator

2.424x10-5m3/s
or 0.020705kg/s

Water 2.4x10-5m3/s
or 0.0205kg/s

Figure 18 The separating unit material balance


Condenser Unit
The material balance over the condenser unit is as presented in Figure19.
The values for the coolant are as obtained during the condenser design calculations (To
be presented later).
TANK STILL
PACKED BED
According to the experimental results, the process in the packed bed consists of two
stages. The first is the induction period in which the material is heated to the steam
temperature. This is the unsteady state. The second stage or the steady state condition is
the period the oil now deposited on the leaves surfaces is transferred by the moving steam
to the condenser.

5.8x10-6m3/s Coolant out


0.057kg/s
Steam oil mixture
2.424x10-5m3/s
or 0.020705kg/s

Water oil mixture


2.424x10-5m3/s
or 0.020705kg/s
Condense
r

5.8x10-6m3/s Coolant in
0.057kg/s
Figure 19 Condenser unit material balance
From the experimental results the maximum mass of oil that can be removed from the
leaves per gram is 3x10-2ml/s. At a production rate of 2.4x10-4m3/s or 0.864m3/hr per
batch cycle of maximum 1hr.
The quantity of leaves required therefore can be determined as
1kg leaves will give a maximum of 3.0x10-2m3 crude oil
x leaves will be required to produce 0,864m3 oil
x

0.864
3.0 x10 2

= 28.8kg leaves

The quantity of steam required = mass flow rate of the steam x induction time
Experimentally the maximum induction period is 21min. however 25min will be
considered for this project. 0.0205x25x60 = 30.75kg
Theoretically the condensate flow rate is the same as the steam. Allowing for film
condensate on the leaves surfaces of 10%, the condensate flow rate is assumed as
0.01845kg/s
For the unsteady state, the material balance is represented below (Figure.20)

Condensate 0.00205kg/s

Oil 2.05x10-4kg/s (2.4x10-7m2/s)

Tank still

At unsteady state

Leaves

Spent leaves (28.787kg/hr)

28.8kg/hr

Steam
Condensate
-5 3
2.4x10 m /s
30.75kg
0.0205kg/s
0.01845kg/s
Figure 20 Material balance at unsteady state

At steady state a steam-oil mixture is formed with the outgoing steam (Figure 21).
Steam-oil mixture
2.424x10-5m3/s (0.020705kg/s)

Tank still

(At steady state)

Steam
2.4x10-5m3/s
0.0205kg/s
Figure 21 Material balance at steady state
The material balance of the packed bed indicated that the mass of leaves required for the
production is 28.8kg. The density of the fresh leaves is about 1800kg/m3. The observed
bulk density for the optimum sample was 310kg/m3
Therefore the volume of the packed bed using the bulk density V = 28.8/310 =0.093m3.
For a cylindrical shaped vessel
V = 0.093 = 0.785D2H
For this design a height to diameter ratio H:D =1.3 was chosen.
Therefore V = 0.093 = 0.785D2(1.3D) = 1.021D3

D = 0.45m
H = 0.585m
ENERGY BALANCE
At unsteady state the packed leaves bed could be likened to plug flow system in which
the fluid (steam) at 100oC flows into it, loses the heat to the bed (Figure 22). The heat
lose by the steam will continue until a steady state is reached at which the temperature of
the bed is equal to that of the team

Condensate 0.00205kg/s

Leaves
28.8kg/hr

Oil 2.05x10-4kg/s (2.4x10-7m2/s)

Tank still

At unsteady state

Steam
2.4x10-5m3/s
0.0205kg/s

Spent leaves (28.787kg/hr)

Condensate
30.75kg
0.01845kg/s

Figure 22 Heat balance at unsteady state


The condensation of steam on the leaves surfaces is a complicated heat transfer processes
it involves three fluid flowing phases: the vapour, condensate and oil. At steady steam
supply rate in a given reactor of height H, the induction period is dependent on the steamleaves ratio or packing density.
The steam gives up it heat content and condenses on the leaves surface. No temperature
drop is expected. The heat supplied to the system Qsupplied
Qin = msL
Where ms mass flow rate of steam 0.0205kg/s, L latent heat of vaporization of water
22600kJ/kg.K.
Qsupplied = 0.0205x 22600= 463.3kJ/s

At a steam transfer efficiency of 90%, it is expected that additional 46.33kJ/s will be


required from the steam generator to the tank still chamber.
STEAM GENERATOR CAPACITY AND ENERGY UTILIZATION
The required process heat = 463.3 + 46.33 = 509.63kJ/s
Comparatively the required mass or volume for various heat sources can be computed
from the known available heat content. From Perry, based on their increasing hydrogen
content the following fuel sources could be classified into
Coke < coal < wood < fuel oil < natural gas < bagasse < hydrogen
The available heat content in some sources and their densities are presented in Table 17.
Table 17 Calculated required quantities of various energy sources
Heat source
Light oils

Available heat
38.2MJ/m3

Density, kg/m3
1.006

Required quantity,
1.3 x10-5m3/s or 0.013l/s

Natural gas

37.3MJ/m3

876

1.4 x10-5m3/s or 0.014l/s

Coke

21.1MJ/kg

1280

2.4 x10-5kg/s

Lignite (wood)

23.2MJ/kg

720

2.2 x10-5kg/s

Coal

30.2MJ/kg

800

1.7 x10-5kg/s

Comparatively it is better to use fuel sources with high heat content. However choice of
fuel source is mainly determined by availability and cost. This varies with locations.
Heat received by the tank still and the contents
The condensing steam loses it heat and is removed from the system at 100oC.
Heat adsorbed by the system Qrecieved = heat content of the oil, Spent leaves, condensate
removed from the reactor with marginally fall in temperature , condensate on leaves
surface, heat of vaporization of condensate and construction material Qoil + Qsl + Qc +
Qcls Qcv + Qcm respectively.
Heat acquired by oil
Qoil = moilcToil
where moil 2.05x10-4kg/s, c = 2.6x10-3 J/kg.K, Toil - 100-25 = 75o.
Qoil = 4.0x10-3kJ/s

Heat acquired by spent leaves


Qsl = msl.c. Tsl
where msl - 28.787kg/hr or 0.0079964kg/s, c to half that of wood = 0.9414kJ/kg.K, T sl
100-25 = 75oC.
Qsl = 0.565kJ/s
Heat lost with outgoing condensate
Qc = mccT = 0.01845x4200x (100-96) = 309.96/s
Heat acquired by condensate on leaves surface to heat it up to 100oC
Qcls = mcls.c. Tcls
where mcls - 0.00205kg/s, cp of water 4200kJ/kg.K, Tcls = 4.0oC.
Qcls = 34.44kJ/s
Heat acquired by condensate on leaves surface to vapourize it.
Qc = mclsvL
where L latent heat of vaporization.
Qc = 0.00205x22600 = 46.33kJ/s
Heat transfer loses via leakages from various connections = 5% of total heat supplied. =
20.85kJ/s
Qreceived - 412.17kJ/s
Qcm = kFTcm

k = 205.9W/m.K, F surface area of the reactor, T cm - mean

temperature difference
At equilibrium
Qsupplied = Qrecieved + KFTcm
kFTcm = 463.3 412.17 = 51.13kJ/s
DESIGN OF THE TANK STILL
Qcm = 4.83kJ/s = KFTcm
Where K is the overall heat transfer coefficient. It is a function of the tank still
construction material aluminum and insulator (fiber with binder and baked)
K = 1/(/ + 1/1) =
Where - insulator thickness 20mm, - heat transfer coefficient of insulator 5.5 kW/mK,
- heat transfer coefficient of aluminum 0.2059 kW/mK

K = 1/(0.005/5.5 + 1/ 275.9x10-3) = 1/(0.00364 + 3.63) = 0.275W/mK


Tcm = 100 25 = 75oC
Therefore F = 51.13/(0.275x75) = 2.48m2
2.48m2 = DH
where D diameter of the tank still; this will be taken as 0.45m as earlier calculated from
the material balance, H the overall height of the tank, m.
An inner holding casing shall be provided to ensure easy transfer of heat and removal of
spent material. This shall be constructed from the same material as the outer conducting
aluminum alloy casing. An allowance of 0.005m between the two casings shall be
provided.
Therefore casing diameter

= 0.44m

Flat sheet bar width

= 0.010mm
= 45o

Bar spacing width


Nos of vertical bars

= 360/45

Total bar length

=8

= 8x.585

= 4.68m

Bracing support material length (see diagram) =


circumference x5

= 6.9m

Base material (using grid method)

= 3.52m

Total material length

= 15.1m

The total area of the inner holding casing = 0.01x15.1 = 0.151m2.


Therefore L = (2.48 - 0.151)/(3.142x0.45) = 1.65m
The calculated height of the packed bed was 0.585m. The difference (1.65 0.585) =
1.065m

PRESSURE DROP ACROSS THE PACKED BED


The pressure drop across the packed bed is dependent on the packing density of the
leaves. As observed experimentally, an optimum steam leaves ratio is necessary for the
process. According to Perry 1984 the pressure drop across a packed bed of a single
incompressible fluid through an incompressible bed of solid particles could be correlated

by the formula. The bed was considered as fairly incompressible based on experimental
observations. However corrective coefficient will be introduced to account for possible
compression of the leaves bed.
P = [2mG2L(1 - )3-n]/[Dpgcs3-n3]
where P pressure drop, Pa,
L depth of packed bed, m = 0.585m
gc dimensionless constant
Dp average particle diameter, defined as the diameter of a sphere of the same volume as
the particle. Average volume of a leaf branch 1.5x10 -3m3. Volume of a sphere =
4r3/3. Dp = 0.142m
- voidage (fractional free volume) = Volume of leaves/ volume of bed zone = (mass of
leaves/leaves density)/ volume of bed zone = (28.8/1800)/0.093 = 0.170
n exponent, a function of the modified Reynolds number N Re. NRe = DpG/ =
0.142x0.0205/8x10-4 = 3.64. From the Chart n = 1.
s shape factor of the solid, defined as the quotient of the area of a sphere equivalent to
the volume of the particle divided by the actual surface of the particle
= 1.5x10-3/0.785x0.1422 = 0.9375
G fluid mass velocity based on empty chamber cross section. 0.0205kg/s.
- fluid density, - 995 kg/m3
m

frictional factor, a function of NRe. = 100/3.64 = 27.48


Therefore P = [2x23.48x0.02052x0.585(1-0.17)2] /
[0.142xgcx995x0.93752x0.173]
= 0.0079866/0.61gc = 0.01309/gc

The observed insignificant pressure drop is expected considering that the process takes
place at atmospheric condition.
Using the velocity-head concept and approximate velocity drop can be obtained
P = h 50(v2/2gc)
0.01309gc = 50(v2/2gc)
5.236x10-4 = v2
v = 0.02288kg/s - mass velocity

This implies that the actual mass velocity of steam from the generator to the tank still
should be maximum 0.205 + 0.02288 = 0.0538kg/s
CONDENSER DESIGN
Essential oils are generally corrosive and is therefore assigned to the tube side.
Heat capacity of the steam-essential oil mixture = 4000.0kJ/kg.oC.
Heat load Q = mmcT = 0.020705x 4000x(100-40) = 4970kJ/s
Heat capacity of water = 4.2kJ/kg oC
Cooling water mass flow rate Gw = Q/cT = 4970/(4200x(50-25) = 0.047kg/s
The mean log temperature change
T = [(100-40) (50-25)]/In[(100-40)/(50-25)] = 40oC.
Calculate the dimensionless temperature ratio for a one pass and two tubes passes.
R = (100 40)/(50 25) = 2.4
S = (50 25)/(100 40) = 0.33
From the temperature correlation factor graph Ft = 0.85
Therefore Tm = 0.85x40 = 34oC.
From the correlation Table of hot fluid versus cold fluid the overall heat transfer
coefficient U was taken as 300W/m2.oC.
Therefore the provisional area Ap = 4970/(300x34) = 0.49m2
From standard a 16mm internal diameter (d i), 20mm outer diameter (do) and 0.55m tube
length (L) made from aluminum was chosen.
Allowing for welding L was taken as 0.51m.
Area of 1 tube
A = circumference x L = 2.0x10-2 x0.51 = 0.032m2
Number of tubes Nt = Ap/A = 0.49/0.032 = 15.29
The estimated shell diameter Dh = do(Nt/k1)0.453
Where k1 constant = 0.215 using a square pitch tubes arrangement
Dh = 0.02(15/0.215)0.453 =137mm
A bundle clearance of 13mm will be allowed
Therefore the shell diameter ds = 137 + 13 = 150mm

Tube side coefficient (coolant)


Mean water temperature t = (50+25)/2 = 38oC
Tube cross sectional area = 0.785x162 = 201mm2
Tubes per pass 15/2 = 8
Total flow area ATw = 8x201x10-6 = 1.6x10-3m2
Water mass velocity Gs = Gw/ ATw = 0.047/1.6x10-3 = 29.22kg/s.m2
Density of water = 995kg/m3
Viscosity of water w 8x10-4Ns/m2
Water linear velocity u = 29.22/995 = 0.029m/s
Heat transfer coefficient hi
hi = {4200(1.35 + 0.02t)x u0.8}/di0.2
{4200(1.35 + 0.02x38)x0.0290.8}/160.2 = 4200x 2.11x0.059/1.74 = 299.85W/m2 oC
Re = Gsxde/ = 29.22x16x10-3/8x10-4 = 584.4
Shell side coefficient
Choice of baffle spacing IB = ds/5 = 150/5 = 30mm
Square tube pitch Pt = 1.25do = 1.25x20 = 25mm
Cross flow area As = [(Pt do)/ Pt]dsIB] =
[(25 -20)/25]x150x30x10-6 = 9.0x10-4 m2
Mass velocity Gs1 = 0.0207/9.0x10-4 = 23.0kg/s.m2
Equivalent diameter de = 1.27/do(Pt2 0.785do2) =
1.27/20(252 -0.785x202) = 19.75mm
Linear velocity u1 = Gs1/ = 23/853.8 = 0.027m/s
Where - density of steam oil mixture
Mean shell temperature (100 + 50)/2 = 75oC
Viscosity = 6.92x10-4Ns/m2
Heat capacity c = 4kJ/kg oC
Thermal conductivity = 0.69W/m oC
Re = 23x19.75x10-3/0.69 = 658.33
Pr = cp/kf = 4x10-3x6.92x10-4 /0.69 = 4.01

From the chart at a 15% baffle cut jh = 2.5x10-2


Taken into account viscosity correction, the heat transfer coefficient hs can be calculated
from the Nusselt equation
Nu = hsde/kf = jhRePr0.33[(/w)0.14]
hs = [(0.69/19.75x10-3)x2.5x10-2x658.33x4.010.33](6.92/8)0.14 =
= 34.94x0.025x658.33x1.58x0.98 = 890.41
Estimation of wall temperature
Mean temperature difference = 75 38 = 37oC
Mean temperature difference across the oil film = (U/hs)T =
(300/890.41)x37 = 12.47oC.
Mean wall temperature 75 12.47 = 62.53oC
The overall heat transfer coefficient is calculated as , W/m2 oC
1/U = 1/hs + 1/hod + [doIn(do/di)]/2kw + (do/di)x1/hid + (do/di)/1/hI
where hid and hod are the inside and outside fluid film coefficient, W/m2 oC = 6000,
kw thermal conductivity of the tube wall material (aluminum alloy) 205.9W/m2 oC.
1/U = 1/890.41 + 1/6000 + [20x10-3 In(20/16)]/2x205.9 + 20/16 x 1/6000 + 20/16 x
1/299.85 = 0.001123+ 0.0001667 + 0.00001084 + 0.0002083 + 0.004169 =
0.0056778
U = 176.12 W/m2 oC
This is below the assumed value of 300W/m2 oC. It shows the low heat load of the
condenser and consequently the potential for process expansion.
At Tube side
From the chart at Re = 584.4
jf = 0.2x10-1
P = [8jf(L/di)(/w)0.14 + 2.5]ut2/2
(8x0.02x(0.55/0.016) x 0.98 + 2.5)995x 0.0292 /2 = 2.2N/m2
At shell side
From the chart at Re = 658.33
jf = 0.2x10-1
P = [8jf(ds /de)(L/IB)us2/2

8x0.02x (150/19.75) x (0.51/30x10-3) x853.8x0.0272/2 = 6.43N/m2.


The obtained pressure drops in the condenser show that the baffle pitch is adequate
PIPING DESIGN
Pipe sizing was performed in accordance with Darcy Rational relation for compressible
vapors and gases.
Flow rate of the steam at steady state Q is 0.0207kg/s or 2.42x10-5m3/s or 0.004ft3/min
Using the standard nominal pipe and schedule 40, a 1.5in pipe of internal diameter on the
schedule was selected.
Therefore the Re = 50.6Q/dw = 50.6x0.004/1.61x 0.8 = 0.157
This is equivalent to a laminar regime
From the Chart the friction factor was calculated as: = 64/Re = 64/0.157 407.6
The length of the straight pipe was assumed as 1.5m based on the expected distance
between the tank still and condenser.
Therefore the pressure head drop for the straight pipe h was calculated as follows:
H = LQ2/2g = 407.6x1.5x(2.42x10-5)2/[(1.61x0.0254)x2x9.8] = 4.46x10-7m
A long radius screwed 90o elbow was selected to link the tank still and the condenser.
From the chart at 1.61in, the resistance coefficient K was 0.46
Pressure head lose due to elbow he = kQ2/2g = [407.6x(2.42x10-5)2]/2x9.8 = 1.37x10-11m
Total head loses (frictional loses) = 4.46x10-7 + 1.37x10-11 = 4.46x10-7
The pressure lose is quite insignificant. This means that the pipe sizes 1.5m long and
41mm internal diameter and outer diameter 48mm are adequate.
SEPARATOR UNIT
Separation of the steam oil mixture is due to the immiscibility of condensed steam and
oil. The oil and water layer are allowed to accumulate in the vessel, to be drawn off
periodically. The collection vessel is made from glass with separate outlet valve for the
two components.
It is expected that separation will take place every hour.

Therefore the volume of the vessel = 2.424x10-5 x 3600 = 0.08726m3/hr


Allowing 20% extra volume for safety, the actual operating volume = 0.1047m 3.
Knowing that V = 0.785D2xh
Taking the internal vessel diameter as 0.4m. The vessel height h = 0.65m.
The oil is about 1% of the total volume 0.00087m3.
The expected oil height h at a base diameter of 0.4m; h = 0.00087/(0.785x0.4 2) =
0.00087/0.1256 = 0.0069m or 6.9cm. Discharge of the separated water and oil will be
conducted by a opening gate valve installed at the lower part of the collection vessel. The
operation will be observed visually through a transparent ruler installed on collected.
The mechanical drawings of the process line showing the tank still and condenser are
presented in Figures 23 and 24. Figure 23 envisages the utilization of a steam generator
and steam gate valve to ensure the steady flow of steam into the still tank. Figure 24
however is more suitable for situation where the steady supply of steam might not be
feasible. The steam is generated directly from the water bank located at the lower part of
the tank still.

Tank still unit


450

Condenser unit
1500

48

1650

585
A

B
750
550
170

550
Steam from generator

170

A-A
Total length = 15100x10

20, 16 tubes
of bars at 45o

-B
Figure 23 Mechanical drawings of the process line with steam supplied from a generator
(Scale 1 in to 375mm)

Tank still unit


450

Condenser unit
1500

48

585
1650

750
550

- -------------------

170

A-A
A_A
Total length = 15100x10

20, 16 tubes

B-B
Figure 24 Mechanical drawings of the process line with direct heating of water in the still
tank (Scale 1 in to 375mm)

ELECTRICAL DESIGN/INSTRUMENTATION
The main aim of process instrumentation and automation is to ensure process stability at
optimum technological condition, high productivity at minimum energy utilization and

process safety. The functional schematic diagram of the design process is presented in
Figure 25.
THE TANK STILL
Analysis of the proposed production technology shows that for efficient operation of this
unit the automation process must guarantee the designed temperature and steam flow rate
regimes. Temperature and flow rate (pressure gauge) sensors are installed before and after
the packed bed. The automation involves regulation of the steam flow rate and
stabilization of the temperature regime. The steam flow rate is monitored either manually
or with the aid of digital pressure gauge. The signal is sent to the control board from
where secondary signal is sent to the regulatory mechanism to allow more or reduce the
flow from the steam generator. The same procedure is applied for the temperature sensor
(digital thermometer or visual observation). A signal from the control board is sent to the
regulatory mechanism to maintain the required steam temperature.
THE CONDENSER
F
The regulated parameters
are the temperature of the coolant. Increase in the temperature

of the outlet water mean increased temperature of the crude condensate. The installed
temperature gauge will send signal to the control board Tfor increase in the coolant flow
rate. The functioning of the condenser, tank still and steam generator is synchronized.
TE

When the tank still is open no steam will be sent to it and water to the condenser will
stop. The devices will stop functioning.
T

PE

TI

PQI

TR

Pf

TI

PQI

TR

TI

PE

TR

PQI

Figure 25 Functional schematic Process Instrumentation and Control


Key: T temperature, P pressure, F flow rate, E electrical signal, I indicator, H
manual control, Q quantity, R registration, f ratio.

Figure 26 An Essential Oil Production Plant fabricated using the above design (National
Research Institute for Chemical Technology, Zaria, Nigeria

REFERENCES
1

Practical manual on Essential Oils Industry. Produced by the Thailand Institute of


Scientific and Technological Research with collaboration from the Central
Institute of Medicinal and Aromatic Plants, Lucknow, India, for the UNIDO,
Vienna, Austria.

Ludwig, E. E. (1995). Applied Process Design for Chemical and Petrochemical


Plants. Vol. 1, 3rd Ed. Gulf pub. Co. Houston, Taxas.

Odigure J. O. (1995). General Chemical Engineering Technology. Jodigs and


Associates, Minna. 299p

Sinnott R. K. (1994). Chemical Engineering Design. Pergamon Press LTD,


London.

Perry R.H. and D.W. Green Perrys Chemical Engineers Handbook, 7th edition,
McGraw-Hill Book Co., New York, 1997

Week 11: ECONOMY OF PRODUCTION AND RISK


Q19 Cost is a very important aspect of any design product. Why?
Cost of production of a given product is a measure of the competiveness of a
manufacturer for a given societal accepted quality. In our global market arena
effective cost and quality management will define the existence of any nation
economic survival. Cost is a function of the operation, fixed capital costs
relative to the product output. The fixed capital is calculated as the
depreciation cost of the investment and bank interest on the working capital.
The operation cost is a function of the cost of the raw materials, labour, and
maintenance, overheads like administrative cost, sales, research and
development. Increasing investment on the fixed capital cost in form of
automation may lead to fall in operation cost. However it is very important to
remember that increased investment in automation may result to
unemployment.
Many books on economic analyses and cost of process equipment are
available but, it is important to note that the direct application of the
calculated cost often do not reflect the prevailing market realities in most
developing countries. It is therefore important that the calculated costs are
subjected to reinterpretation considering the local capital, labour, utilities
availability, security cost.
SAFETY CONSIDERATIONS
The safety of any design is the outward expression of its quality. It is a
judgment on the state of societal acceptance. It is the embodiment of the
quality of the analyses and syntheses of the various stages of the design. It in
an indicator that all the elements of uncertainty and probability of error
embedded in the conceptual, detailed and fabrication design stages are
insignificant. These errors are contained in the physical data used,
assumptions made on correlations of units and materials behavior,
approximations of design calculations, change in operating conditions and
environment, etc. Safety consideration starts from the very point of
conceptualization of a project. The extent to which safety is applied should be
determined by the prevailing government regulations and cost. Adequate

safety can be ensured by allowing the inadequacy


compensated for, by a higher more efficient one.

of

equipment

RISK ANALYSIS AND ENVIRONMENTAL CONSIDERATIONS


Q20. Risk analysis starts from preliminary stage of design. Why?

Any project requires a rational approach in assessing the suitability to


the environment and acceptability to man. Risk is the probability of
occurrence of a hazardous event. It is the possibility of the plant
transiting from normal to abnormal operating regime. The plants
impact on the environment should be studied from the conceptual
stage of design.
A plant or system is design for normal operation. For automated
system, any slight deviation of the process parameters is quickly
corrected by the control mechanism. However, they do malfunction
because of age, climatic condition, maintenance, inexperienced, etc.
These could make their reading unreliable. Therefore, human
intervention could be necessary to adjust the system to the set
parameters by calculating the materials and energy balances, initiate
long-term corrective measures, etc. to return the system to normal.
Operators intervention might not be necessary for computed
controlled systems designed for abnormal situation because the
adjustments are performed automatically.

Risk analysis is performed at the various stages of a process plant. Risk


could be technical, social, economic, etc. Risk analyses are performed
at the conceptual design, detail design, construction, commissioning
and operation stages. There are various risk analyses techniques
available to assess the suitability and acceptability of a process plant.
They include the Check list, Hazard Operability Study (HAZOP), the
Fault Tree, Event Tree, Dow Fire and Explosion Index, Explosion and
Toxicity Index, Instantaneous Fractional Annual Loss, Cause
Consequence Analysis, Pinch Analysis, etc.

Early risk analysis at the conceptual design stage helps to identify


possible technical, economic and social consequences of establishing
the plant. At this stage, it is important:

To identify potential failure causes


Assess and quantify the consequences of the potential failure
Estimate the probability of the event occurrence
Carefully examine the design to eliminate the possibility of the event
occurrence.

The risk analyses are normally considered for each unit individually. It
could following the following methodology; starts from the

Design concept;
Systematic design appraisal and review of the conceptual and then the
detailed technical drawings, feasibility and environmental impact
assessment reports,
List of top hazard at the various subunits and units using any risk analysis
technique to establish,
Estimate the probability of occurrence of the top event/hazard
Assess the viability of the design units using:
a The existing rules and regulations,
b Operating standards and codes, and
c Documented historical records of possible event occurrence.
Feed back the obtain results for design improvement and optimization of
the process.
Evaluation and reliability of the units and system;
Assess the overall technical, economic and social safety of the plant.

The subunits or units that fall below or equal to the accept probability
of occurrence are accepted as having passed. In case of the units with
probabilities higher than the set standard there will be need to re
design the process or introduce mitigating features like temperature
control sensors, pressure release valves, level gauges, etc. The
survivability of the plant is based on the total probability of the units
and extent of accidental event harmful consequences. Survivability is
about predicting the impact of any accidental event on the operating
personnel or community or environment and is often quantified in
terms of the economic implication.
All industrial processes are potential environmental sources of pollution
as they by their activities release pollutants to the atmosphere; hence

the need to give attention to possible environmental problems during


the design and operation of chemical process plants. Elimination of
potential accidental pollutants release can be achieved through proper
understanding of the process chemistry, control of the process
parameters, closed circuit production, etc.
Pollution is preventable. It is a necessity because of the human factors
and materials cost implications. Pollution prevention strategy could
evolve through the following steps:

Definition of the problems


Developing
some
conceptual
pollution
prevention
strategies and
Performing a cost/benefit analyses to find the best
alternative.

Definition of the problem start with understanding the process


operation, the production technology and engineering design; relative
to the technical, social, and economic. This will enhance early
identification of the possible emission causes and sources. It is
important to know where, when, how, and why these emissions and
wastes are generated. The prevention should focus on mitigating the
causes and release of the pollutants to the environment. Emission and
waste are results of faulty process chemistry (materials and energy
balances, reaction kinetics, etc.), technological processes design and
poor human organization practices. In developing the conceptual
pollution prevention strategies, it is necessary to address the
fundamental causes, rather than the symptoms of the emissions and
wastes. For example, odorous emission from poultry house is
associated with compounds of ammonium and sulphides present in the
excreta. Fresh excreta emit lesser odorous gases. Immediate
evacuation of fresh excreta and proper ventilation will lead to less
odorous environment. This will mean hard work. The long-term
strategy will be to convert the compounds to less odorous ones.
Pollution prevention strategies include:

Engineering design-based pollution prevention, in the following areas like


storage and handling of materials, process equipment, process control and
instrumentation, recycling and recovery equipment
Process chemistry and technology-based strategies for the raw materials
and unit operations,

Operations-based pollution prevention strategies for inventory


management, housekeeping practices, operating practices, and cleaning
procedures
Maintenance-based strategies, like enforcing existing preventive
maintenance programmes and proactive preventive maintenance
strategies.

ECONOMIC ANALYSIS

EQUIPMENT COST ESTIMATES


Calculation of equipment cost estimates are based on standard procedure for determining
cost. Estimates were based on the cost of the original equipment as at 1991 with
appropriate allowances for inflation, insurance and transportation (Plant Design and
Economics, 1991). The estimated costs of the equipment are presented in Table 8.
Table 8 Bill of Quantity of some major equipment
Equipment

1
2
3

4
5
6
7

Geomet Unit
ry,
M2

Rotary
dryer,
indirect heating
26.7
Metering machine
Cyclone
heat
exchangers
7.56
2.25
1.42
0.62
Bucket elevator
25m
Screw conveyor
< 10m
Pipes, m
0.365
0.44
0.351
Rotary kiln
57

8
9

Gear motor, kW
Rotary pump
motor
10 Rotary cooler
11 Gear motor, kW
12 Rotary pump
motor
13 Dust collector

Refractory(+
0.02m
insulator),
kg

Productiv Material
ity
Of construction
x103
kg/hr

1
1

Insulator

64.8
25.2

1
1
1
1
1
1
5.54
0.5
14.3
1

2354.9
2246.1
1412.3
1026.3
73.9
73.9

28041

1
1

+
68.7

25.2
10
70.1

4910

25.2
15

Unit
Cost,
$x103

Asbestos, low alloy


iron wall.
20
35

Total
Cost,
$x103

20
35

Asbestos, Fireclay, 50
low alloy iron wall. 35
28
30
6
Asbestos, Fireclay, 8
low alloy iron wall. 15
15
15
Asbestos, Fireclay,
low alloy iron wall. 40
8
6

50
35
28
30
6
8
83.1
7.5
214.5

Asbestos, Fireclay, 60
low alloy iron wall.
12

60

40
8
6

12

+
69

From
cooler:
cyclone
Venturi scrubber
Hydroclone
Exhaust pipe
Pump + gear motor,
kW
14 From Rotary dryer
Cyclone
Pump + gear motor,
kW
15 Tractor shovel
16 Tank trailer

0.785
0.049
0.785
13.36

6
6
6
1

30

0.785

10

30
192
16m3

1
1
1

45600
45600
45600
121600

4
4
3
33

24
24
18
33

76000

40

105HP

6
75
35.7

6
75
35.7

Total cost

910.8

Cost estimate of major equipment.


The total estimated cost as at 1990 amounted to $910800.
Allowing for 20% inflation over a 14-year period and 35% for shipment and insurance
to Nigeria, the grand total estimate for equipment = $1,411,740.00
The ratio factors for estimating fixed capital investment items based on the above
estimated delivery equipment cost were used to estimate other parameters (Table 9).
Table 9 Estimated cost of fixed capital investment
Fixed Items
1
Purchased equipment delivered, including
fabrication locally of some process machinery
2
Purchased equipment installation (45%).
3
Instrumentation and process control equipment
(11%)
4
Installation (9%)
5
Piping, excluding those in the process plant (5%)
6
Electrical (10%)
7
Building (25%)
8
Service facilities (40%)
9
Land 6%
Total direct plant cost
Engineering and supervision (15%)
Contractors fee (5%)
Contingency (10%)
Fixed Capital Investment (FCI)
Estimation of Annual Product cost.

Cost, $x103
1411.74
635.28
155.29
127.10
70.59
141.17
352.94
564.70
84.70
3543.51
531.53
177.18
354.35
4606.57

The cost of material was estimated based on anticipated Government incentives


industrial structure and prevailing average market price of the finished product. The
following were considered in fixing the cost of raw material limestone.
Social services 15% of the average current market price of lime $39/T.
Right of exploitation 7%.
Therefore raw material cost will consist of 23% of the average current market price of
lime $39/T.
Total annual production material cost = 0.23x7x3600x24x300x39/1000 = $1627516.80
Cost of Energy per day
Average fuel/gas consumption per kg = 4132kJ/kg
1m3 of natural gas will give 36515kJ
Therefore 4132kJ will require 8.619m3
Annual natural gas requirement = Production output 181440x8.619 =
1563885.79m3
Fuel gas
Annual fuel consumption
1563885.79
Cost of gas
$0.3/m3
Cost of fuel
$469165.73
Allowing for independent market sources of 51% above NNPC official price
The cost of fuel is taken as
= $709200.00
Electricity
Annual consumption 144x24x300 = 1036800
Cost 0.05/kW.hr
$51840.00
Total raw material cost
$2388556.80
Operating Labour Cost
The plant production capacity is estimated at 604.8T per day. The manning of the various
units have been estimated generously despite the estimated automation of process
control (Table 10)
Table 10 Operating Labour Cost.
Position

Grade level Number


HATISS
required

Qualification

Experience, Annual
years
Salary ($)

General
manager

14

B.Eng

12

9000

Production
manger

12

B.Eng Chem.
Engr.

7000

Accountant

12

B.Sc

7000

Cashier

08

HND

7000

Technologis
t

09

B.Eng

12000

OND in
Mech./Electrical
Engr.

18000

Labourer

02

20

NA

40000

Security

10

Ex service

Drivers

03

10
TOTAL

Trade test

Technician

20000
3

30000
150000

Estimation of Variable Cost.


The variable cost includes:
(i)
Raw material cost per year = $2388556.80
(ii)
Cost of maintenance = 8% of fixed capital
Refractory material cost. = 30% of material
Miscellaneous material = 10% of material
Maintenance cost = 8% of FC
= 0.08 x $4606570 = $368525.6
Cost of miscellaneous = 0.1 x $2388556.80 = 238855.7
Refractory = 0.3x2388556.8 = 716567.04
Total variable cost = $1323948.34.
Estimation of Utility Cost.
These include electricity for lightening, electric motors for pumps and energy for
control panel other than those used in the production process.
Utility cost (UC)
= 5% of total variable cost
= 0.05 x $1323948.34
= $66197.4
Fixed Cost (to be included in production cost)
These include the following:
(i)
Maintenance cost
(ii)
Operating Labour cost
(iii)
Plant Over head = 50% of operating labour cost

= $368525.6
= $150000.00.
= 75000.000

(iv)
Capital charges = 15% fixed capital
(v)
Insurance = 1% fixed capital cost
(vi)
Land Tax rates = 2% fixed capital cost
TOTAL FIXED COST

= $690985.5
= $460657.00
= $921314.00
= $2666482.1

Direct Production Cost (DPC)


= Total variable cost + Total fixed cost + utilities
= 1323948.34 + 2666482.1 + 66197.4 =
= $4056627.74
Annual production rate (APR)
= 7x3600x24x300 = 181440T
Production cost (PC) =

APC/APR
= (4056627.84)/( 181440T / year) = $22.36 per ton.

Selling Price.
This is a function of total production cost demand and market forces. The
distribution price of $35.00 per ton would be recommended as the initial price.
Annual product sales (APS)
= $35 x 181440 = $6350400.00
Annual profit before tax = APS APC
= $6,350,400.00 4,056,627.74 = $2293772.26
Profit after tax (40%) = 0.6x2293772.26 = $1376263.36.
Depreciation
Determining the depreciation rate by the straight line method was adopted:
d =

(V Vs) / n
Where d = Annual depreciation $ / year
V = Original value of the property at start of service life period, complete
installed and ready for use.
Vs = Salvage value of property at end of service life.
n = service life period.
Let Vs after 10 years be taken as 15% of FCI = $690985.5
Annual depreciation per year
= ($4606570 - 690985.5)/ 10Years = $391558.45

Pay Back Period (PBP)

This is the minimum length of time required to recover the original capital
investment inform of cash flow based on the total income minus all cost except
depreciation.
PBP

=
(Fixed capital investment) / (Average profit / year +
depreciation / yr)
=
4606570 /($1376263.36 + $391558.45/ year )
=
2.61 years.

Rate of Return on Investment


=
=

Annual profit x 100 / TCI


(1376263.36 x 100) / 4606570.00

29.88%

Average

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