CHAPTER 1

INTRODUCTION
1.1 HISTROY In the year 1882, Pentaerythritol was discovered by product of the reaction hydroxide and impure formaldehyde. The name Pentaerythritol which was assigned to this compound was derived from erithritol to indicate the presence of 4 - hydroxyl groups and the prefix Penta to show that there are 5 carbon atoms in the molecules. Pentaerythritol is a white crystalline compound. The high melting point, slight solubility in water and the ready reactivity of its 4 hydroxide groups have been attributed to the compact symmetric structure of the molecules. It is an optically inactive compound, resembling cane sugar in appearance and has a sweet taste characteristic of polyols. Pentaerithritol is nonhygroscopic and stable in air and sublimes slowly on heating. It is moderately soluble in cold water, quite soluble in hot water, and has only limited solubility in organic liquids. It is used in paints, varnishes industry and the production of resins. Pentaerithritol is increasingly used in resins manufacturing mainly because of its desirable characteristics and price stability. 1.2 APPLICATION OF PENTAERITHRITOL It is used to manufacture of Paints & Varnishes. It is used to manufacture of Pentaerithritol Nitrate (P.E.T.N). It is used to manufacture of Plasticizers & Lubricants. Pentaerithritol combination with metal salts used as heat stabilizers. Acrolin prepared from Pentarithritol used for electrical insulation,surface coating films and fibers

CHAPTER 2

AIM AND SCOPE

The objective of the project work is to study the manufacture of Pentaerithritol for 600 tons per annum. To solve the material balance and energy balance for the process To design the reactor and vacuum tray dryer involved in the process To study the plant layout, safety, health and environment aspects To estimate the cost and payback period of the process The scope of the project is to select the method for the manufacturing of pentaerithritol for the following features mentioned below Less energy consumption. High purity. High yield / conversion. Recovery of by product as sodiumformate.

CHAPTER 3 PROCESS DESCRIPTION AND DESIGN

3.1. METHODS OF PRODUCTION 3.1.1 Using soda ash as condensing agent Raw Materials Required a) Formaldehyde b) Ca (OH) 2 solution c) Acetaldehyde d) Soda ash

3.1.2 Using Sodium hydroxide as condensing agent Raw materials required a) Formaldehyde b) Formic acid c) Acetaldehyde d) Sodium hydroxide 3.1.3 Slection of method: Using NaOH as condensing agent

4 HCHO + CH3CHO + NaoH

(CH2OH) 4 C + HCOONa
Pentaerithritol

Justification of Process Selection Yield 85-90% Less energy consumption Easy removal Recovery of by product as sodiumformate High yield / conversion

3.1.4 Process description A solution of formadehyde (30%) is added to NaOH solution. The temperature is maintained at 30oC by suitable agitation. liquid acetaldehyde (99%) is added slowly added under the surface of formaldehyde alkali solution. External cooling is required to maintain the reaction temperature around 20-30 oC the mole ratio of formaldehyde to acetaldehyde 5:1.A ratio of 1:1.5 mole hydroxide ion per mole of acetaldehyde appears to the optimum amount of condensing agent. The crude reaction mixture is then transferred to neutralization reactor. Formic acid is added here to reduce the Ph of the solution to 7.8-8.0 & to remove sodium ions present as Sodiumformate.The solution is then evaporated to a specific gravity of 1.270.ITt is then chilled to crystallize Pentaerithritol and resulting slurry is centrifuged & dried to obtain crystalline Pentaerithritol as final product. The mother liquor goes to recovery system to recover Sodiumformate by evaporative crystallization followed by centrifuging & drying to obtain crystalline Sodiumfomate as by product.

3.1.5 Chemical Properties of Pentaerithritol 1) Molecular Formula 2) Molecular Weight 3) Boiling Point 4) Melting Point 5) Density 6) CAS No. -

(CH2OH)4C
136.15 276C AT 760 mm of Hg 262C 1.1318gm/cc 115-77-5

3.1.6 Physical Properties of Pentaerithritol Pentaerithritol are crystalline solids. Those solids are soluble in water. Solubility decreases with increase in molecular weight. Their solubility and melting points show alternation or oscillation from one member to the near. It is moderately soluble in cold water, quite soluble in hot water, and has only limited solubility in organic liquids. It is an optically inactive compound, resembling cane sugar in appearance and has a sweet taste characteristic of polyols. Pentaerithritol is nonhygroscopic and stable in air and sublimes slowly on heating.

3.1.7 Process flow diagram 5

TO VACCUM

HCHO NaOH CH3CHO REACTOR NEUTRALISER

HCOOH

EVAPORATOR

C.W OUT

CW IN

HOLDIN G TANK

TO VACCUM

AIR OUT

VACUM CRSTALLI SER HOLDI NG TANK

P.E.T CRYSTAL

DRIER
CENTRIFUGE

HOT AIR IN

HCOONa + water

Figure 3.1: Process flow diagram (Manufacturing of pentaerithritol)

3.1.7 Process flow diagram

TO VACUM

VACCUM CRSTALLISER

TO ATM CENTRIFUGE

DRIER

DRIED HCOONa

CENTRIFUGE ML(P.E.T)

MOTHER LIQUOUR

HOT AIR IN

Figure 3.2: Process flow diagram (Recovery of sodiumformate)

3.2 MATERIAL BALANCE

3.2.1 Material balance for P.E.T and sodiumformate manufacturing: BASIS: 600 tons/annum 7

2000 kg/day of Pentaerithritol REACTION: 4 HCHO + CH3CHO + NaoH (4 x 30) 44 40 (CH2OH) 4C + HCOONa 136.15 68

3.2.2 Material balance around Reactor: Reactor input CH3CHO required = = = For 85% conversion = = = CH3CHO purity(99%) HCHO required = = = = = Mole ratio CH3CHO: HCHO= = kgmoleCH3CHO/kgmole (CH2OH) 4C x kg P.E.T (44/136.15) / 2000kg of P.E.T 646.34 kg/day CH3CHO kg required / 0.85 646.34 / 0.85 765 kg/day 765 / 0.99 757.5 kg /day (CH3CHOkg/kgmoleCH3CHO) x kgmoleHCHO (757.5 / 44) x 30 2065 kg/day 1: 4.55 (CH3CHOkg/kgmoleCH3CHO) 4.55 x (757.5 X 44) x 30 2350 kg/days 2350/0.37 6350 kg/day (CH3CHOkg/kgmoleCH3CHO) x kgmole NaOH (757.5 / 44) x 40 688.4 kg 1 : 1.52 kg CH3CHO x kgmoleNaOH x 1.52 (757.5) x 40 x 1.52 1050 kg 1050 / 50 2100 kg/day 8 x

kgmoleHCHOx4.55 = = HCHO purity (37%) = = NaoH required = = = Mole ratio CH3CHO:NaOH = = = = NaOH purity(50%) = = Reactor output:

P.E.T produced

(CH3CHOkg/kgmoleCH3CHO)xkgmoleP.E.T (757.5/44) x136.5 2341.23 kg/day (CH3CHOkg/kgmoleCH3CHO) x kgmoleHCOONa (757.5 /44) x 68 1170.0 kg/day

= HCOONa produced = = =

Material balance around reactor:

Component

Input (kg/day)

Output (kg/day) 284.70 361.60 2341.23 1700.00 5057.50 9125.00

CH3CHO HCHO NaoH (CH2OH) 4C HCOONa H2O TOTAL

757.50 2350.00 1050.00 5057.50 9125.00

3.2.3 Material balance around Neutralizer: NaOH + HCOOH 40 46 HCOONa + H2O 68 18

Neutralizer input NaOH Unconverted = 316.6kg (kgmoleHCHO/kgmoleNaOH) x 316.6 (46/40) x 316.6 415.84 kg 9

HCHO required for neutralization = = =

HCHO purity (34.6%)

= =

415.84 / 0.346 1200 kg/day

Neutralizer output: HCOONa produced = (kgmoleHCOONa/kgmoleNaOH) x 316.6 +1170kg = = H2O produced = = = = = Material balance around Neutralizer: 613.94 kg + 1170 kg 1783.94 kg/day kgmoleH2O/kgmoleNaOH x 316.6 (18 / 40) x 361.6 946.88 kg 5057.5 +946.88 6005.5 kg/day

Material

Input (kg/day)

Output (kg/day) 2341.23 1783.94 **** 284.67 **** 6005.50 10415.00 balance around

P.E.T HCOONa NaOH HCHO HCOOH H2O TOTAL 3.2.4 Material Evaporator Data required: Out going slurry: Component H2O P.E.T HCOONa TOTAL

2341.23 1170.00 361.60 284.70 1200.00 5057.50 10415.00

Specific gravity 1.0 1.396 1.8 *****

Weight(kg) (x) 2341.23 1783.94 4125.17 + x

Volume(lt) (x) 1677.10 991.08 2668.18+ x

10

Specific gravity of out going slurry (Weight / volume) of out going slurry (4125.17 + x) / (2668.18 + x) H2O along with out going slurry (x) H2O evaporated Material balance around Evaporator Material

= = = = = =

1.27 1.27 1.27 2727.94 kg/day 6005.16 2727.94 3277.22 kg/day

Input (kg/day)

Output (kg/day) 2341.23 1783.94 **** 284.67 3272.22 2727.94 10415.00

P.E.T HCOONa HCHO HCHO(evaporated) H2O(evaporated) H2O(along slurry) TOTAL

2341.23 1783.94 284.67 **** **** 6005.50 10415.00

3.2.5 Material balance around Vacuum crystallizer: Assume -14.8% loss in solution P.E.T as crystal = 2341.23 x 0.148

= = = Material balance around Vacuum crystallizer MATERIAL INPUT 11

341.23 kg/day 2341.23 341.23 1194. kg/day

OUTPUT

(kg/day) P.E.T 2341.23

(kg/day) ****

Material OUTPUT 1873.94 HCOONa(in solution) INPUT 1783.94 (kg/day) P.E.T( In solution) (kg/day) **** P.E.T P.E.T(As crystal) H 2O H 2O H2O(to TOTAL 347.23

1194.0 **** 1194.0 1994.00 127.8 6.0 2727.94 2727.94 ***** 6583.11 121.8 6583.11

3.2.6 Material balance around Centrifuge: Assume moisture accompanying with crystal Hence moisture with crystal 0.09 x = = = 9.0 % x / (x+1194) 127.28 kg

Material balance around Centrifuge

12

atm) TOTAL 2121.8 2121.8

3.2.7 Material balance around Dryer:

Material

INPUT (kg/day)

OUTPUT (kg/day) ***** 1783.94 2600.66 347.23 1994.00 127.28

P.E.T HCOONa (in solution) H2O( in solution) P.E.T(As soluble) P.E.T (in wet cake) H2O (in wet cake)

1994.00 1783.94 2727.94 347.23 ***** *****

TOTAL 6853.11 6853.11 P.E.T PRODUCED 2000 kg/day

Centrifuge mother liquor containing HCOONa + Water is sent to Evaporative vacuum crystallizer for HCOONa recovery 13

3.2.8 Material balance around Evaporative vacuum crystallizer: Data required: Out going slurry: Component H2O P.E.T HCOONa TOTAL Specific gravity 1.0 1.396 1.8 ***** Weight(kg/day) (x) 347.23 1783.94 2131.17 + (x) = = = = = = 1.37 1.37 1.37 1185.0 kg / day 2600.66 1185.0 1415.66kg/day Volume(lt) (x) 248.73 991.08 1239.81 + (x)

Specific gravity of out going slurry (Weight / volume) of out going slurry (2131.17 + x) /(1239.81 + x) H2O along with out going slurry (x) H2O evaporated

Material balance around Evaporative vacuum crystallizer

COMPONENT

INPUT (kg/day)

OUTPUT (kg/day) 347.23 1783.94

P.E.T HCOONa H2O H2O evaporated TOTAL

347.23 1783.94 2600.00 ***** 4731.83

1415.66 4731.83

3.2.9 Material balance around Centrifuge: Assume moisture accompanying with crystal Hence moisture with crystal 0.04 x = = = 4.0 % x / (x+1783.94) 71.1 kg

14

COMPONENT

INPUT (kg/day)

OUTPUT (kg/day) ***** 89.94 1113.9 347.23 1694.00 71.00 6853.11

HCOONa HCOONa (in ML) H2O(in ML) P.E.T(in ML) HCOONa (in wet cake) H2O (in wet cake) TOTAL

1783.94 ***** 1185.00 347.23 ***** ***** 6853.11

3.2.10 Material balance around Dryer:

COMPONENT

INPUT (kg/day)

OUTPUT (kg/day) 1694.00 6.00

HCOONa H2O

1694.00 71.00

HCOONa PRODUCED 1700 kg/day 65.0 H2O(to atm) ***** TOTAL 1765.00 1765.00

3.3 ENERGY BALANCE

3.3.1 Energyrgy balance around Reactor: Mass of Acetadehyde(M CH3CHO) Mass of Sodium hydroxide (MNaoH) Mass of Formaldehyde (M HCHO) Mass of Sodiumformate(M HCOONa) Mass of P.E.T(MP.E.T) 15 = = = = = 757.50 kg 1050.00 kg 2350..00 1170.00 kg 2341.23 kg

Feed inlet temperature Product outlet temperature Reaction temperature Reference temperature

= = = =

25C 30C 80C 25C

Energy balance equation Heat input + (MP.E.T x heat of reaction) =Heat output+Heat load on Reactor Cooling jacket Heat input Feed temperature = reference temperature So, heat input = 25C =0

Table 3.1 Heat Values of Components

COMPONENT

REACTANT HCHO NaOH CH3CHO

PRODUCT HCOONa P.E.T

Specific heat capacity (Kcal/gm C)

o

0.526

0.540

0.312

0.269

0.386

16

Heat of formation (kcal/gmole) -60.57 -72.01

-142.53

-226.0

-100.0

Heat of reactionat 25 oC

HF product - HF reactant (-326.65) - (-275.11)

= Enthalpy at 25 oC

- 51.49 Kcal/gm mole

(-51.49x 2341.231000)/136.15

-886396.56 Kcal/day m.Cp.dt

HF reactant

((2350 x 0.526)+(1050x0.54)+ (757.5x0.312)(298-303)

-10199.1 Kcal/day m.Cp.dt

HF product

(2341.23 x 0.386) + (1170 x 0.269) x 5

6092.2 Kcal/day

HF product+HF reactant+ heat of reaction at 25 oC -101991.1 + 6092.2 - 886396.56 17

-890503.46Kcal/day

Heat loss by radiation 10% = -89050.35Kcal/day

Heat to be removed (Q) = 890503.46 - 89050.35

801453.117Kcal/day

Heat removed = Heat generated = Q = (mCpdt)Water Q = m*1*(303-293)

= Mass of H2O required ( m ) =

801453.11 Kcal/day

801453.11 / 10

80145.31 kg/day

3.3.2 Energyrgy balance around Holding Tank: Here the reactor outlet mass is heated up to 90oC before feeding to evaporator.

Temperature of the holding tank = 90 oC mCpdt

Heat to be supplied

(2341.23 x 0.386 +1783.94 x 0.269 + 6005.16 x 1+ 284.67x .576) x (90-30)

453154.75 kcal/day

Heat loss due to radiation =

10% 18

Haet required

= = = =

Heat supplied (10%)x453154.75 1.1*453154.75 498470.2338kcal/day

Heat loss by radiation

= =

498470.23-453154.75 45315.47kcal/day

Steam required @ 2.1125 atm Ms = = Heat loss by condensation = = Heat to be supplied by steam = = (525.64-121.27) x 948.3 383471.19kcal/day 498470.23/525. 948.3kg/day 121.27x948.3 115000 kcal/day

19

3.3.3 Energy balance around dryer: Amount of P.E.T to be dsried Water to be removed = = 1994 kg/day 121.28kg/day

Sensible heat required to heat material from 25 oC -100 oC =mCpdt

(1994\x (100-75) x (0.386+ 121.80) x (100-75) x 1

66822.3 Kcal /day

Heat required for vaporization of 121.28 kg of water

121.28 x 540

65491.2 Kcal/day

Hence total heat required

66822.3+65491.2

132313.50kcal/day

Assuming 10% heat loss due to radiation

Hence heat required

1.1 x 132313.50

145544.85 kcal/day

Steam required

145544.85/525.64

276.88kg/day

20

3.3.4 Energy balance around Evaporator: BASIS: P.E.T-2000kg/ day. Data required for calculation: As per evaporator material balance, Feed Vapour Product Feed enters at Steam table data Steam,2 atm,121oC (HS) Condensate,1 atm,105oC(HC) = = 645.26 Kcal/kg 105.60 Kcal/kg = = = = 10415.00 kg/day 3561.89kg/day 6853.11kg/day 90oC

Table 5.1 Heat Values of Components REACTANT HCHO Specific heat capacity (Kcal/gm C)
o

PRODUCT CH3CHO HCOONa P.E.T

NaOH

0.526

0.540

0.312

0.269

0.386

Heat of formation (kcal/gmole) -60.57 -72.01

-142.53

-226.0

-100.0

General heat balance equation for evaporator

F.HF + S(HS-HC)

E.HE + PHP 21

Feed (F) Enthalpy of feed

= = =

10451 kg/day (mCpdt) feed (2341.23x0.396) + (1783.94x0.269) + (6005.5x1) x 90

F. HF Vapour (E)
o

= = = = C = = =

679708.08 kcal/day 28321.17 kcal/hr 3561.89 kg/day Water vapor evaporated x Enthalpy at 100

3561.89 kg/day x 644.22 kcal/kg 2294640.776 kcal/day 95610.03 kcal/day 6853.11kg/day (mCpdt) product (2341 x 0.368) + (2727.94 x1) + (1783.94 x 0.269) x 90

Product (P)

Enthalpy of product (HP)

= =

= =

411152.4kcal/day 17131.39kcal/day

Substituting the above values in equation -1 Mass of steam(S) Steam economy = = 3717.20kg/day (kg water evaporated) / (kg of steam required) = = (3561.89/3717.2)x10 0.95

22

3.4 EQUIPMENT DESIGN 3.4.1 Design of vacuum tray drier

23

Figure 3.1: Design of vacuum tray drier

BASIS : 48 Tray capacity Shell : Length of the shell Breadth of the shell Area of the shell Area of the shell Tray: Length of the tray Breadth of the tray Area of the tray Total number of tray L b = = = = 0.8m 0.4m Lx B 48 number L b = = = = 1.7m 0.91m Lx B 1.547 m2

Area of the tray Total area of the tray

= = =

0.32m 48 x 0.32 15.36 m2

Shelves: Length of the shelves Breadth of the shelves L b = = = = Area of the shelves Total area of the tray Overall surface area of the drier = = = = 1.2m 0.8m Lx B 16 0.96m 16 x 0.96 (1.547+15.6+15.36) 32.27m2

24

3.4.2 Design of Evaporator Circulation and heat transfer in this type of evaporator is strongly affected by the liquid level as indicated by an external gauge, which is only about half way of the tube. Slight reduction in level below the optimum results in incomplete wetting of the tube walls with a consequent increase in tendency to foul and causes rapid reduction in capacity. When this type of evaporator is used with a liquid that can deposit scale, it is customary to operate with the liquid level appreciably higher than the optimum level which is above the top tube sheet. Advantages of Short Tube Vertical Evaporator: High heat transfer coefficient Low head Easy mechanical descaling Mild scaling solution can be used for mechanical cleaning as the tubes are short and large in diameter. Crystalline products can be removed using the agitatorProcedure followed in design of evaporator assembly (ref: Unit operation of chemical engineering Mc Cabe) Q Q Q U = = = = U.A dt 1316857.14 1316857.143 x 0.252 = 331848 Btu/hr 160 Btu/hr.ft2. oF Ref: Unit operation of chemical JM Coulson & JF RICHARDSON PAGE-520 T Hence A = = 45oF (331848) / 45 X 160) = 46.09 ft2

For Sheet Diameter: 25

C/S Area of one tube

= = =

/4) d2) (3.14/4) x (2.2)2x48 182.463 in 2

From Mc Cabe, 30% of A is the area of downcomer = = ( /4) d2 Hence, d Length and Number of tubes: In standard short tube evaporators the length varies from 4 to 8 ft and the diameter is around 2 to 4 inches, In this case, the length is assumed as 4 ft and diameter as 2 inches. Outer area of each tube = = Number of tubes required = = Hence we can take 22 to 24 tubes. d0l 3.14 X (2.12/12) X4 = 2.1ft2 46.09/2.1 22.2 tubes = = 182.463 x 0.3 54.4 in2 54.4 in2 8 inches

A staggered arrangement is used as it permits higher tube accommodation, for a given distance between the tubes. From the approximate calculations, the shell inside diameter is taken as 21.2 inches. Thickness of Shell = = (P.d) / (2.f.E) + Corrosion Allowance (30 X 21.2) (2X0.8 X 3312.5) + 0.08 26

= Hence Outer Diameter = =

0.2 inches maximum 21.2 + 0.2 + 0.2 21.6 inches

Length of the evaporator is proportioned with respect to the length of tubes. Design of evaporator and its accessories: The standard evaporator consists of a vertical cylinder with calendria cross which the heat exchange takes place. The cylindrical body terminates at the top in a save all , the objective of which is to separate the liquid d roplets which maybe entrained with vapour from the soilution. Previously the evaporator body was fabricated with cast iron; however more recently fabrication using steel plate is becoming more common. Height of the Vessel: The space above the tubular calendris represents the greater part of the volume taken up by the equipment. The objective is to diminish the risk of entrainment droplets of solution projected by boiling. Various MOC used as follows:

Part Shell Tubes Brass,

Old Steel Bronze Cast Iron

Modern Mild Steel Mild Steel

Special Stainless Steel -

The height of the cylindrical portion above the steel plates is 1.5 to 2 times the length of the tube. Calendria: It is the continuation of the shell or body of the evaporator. It is often fixed to the shell. The bore of the holes provided in the tube plate is about 1/32 inch greater

27

than the outer diameter of the tubes. Vertical baffles are often placed in the calendria with the object of compelling the steam to follow a certain path. Center Wall (Downcomer): The calendria is generally designed with a wide tube or center wall. Solution which has been projected over the top tube plate is returned to the bottom by the downcomer. This center well is often used to collect the concentrated solution in order to transfer it from vessel to other. Air source for condenser: Air introduced into the condensers comes from various sources such as air contained in the heating system, air introduced in the cold rejection water, air entering by leakage.

Specification sheet of evaporator Number Required Type 1 Short tube, vertical calendria type evaporator Normal Capacity Working Pressure Critical Dimension 328.25 l/hr 2 atm Overall height = 220 inch

28

Inside diameter of Shell = 21.2 inch Inside diameter of tube = 2 inch Thickness of shell = 0.2 inch Thickness of tube = 0.1 inch Diameter of downcomer = 3 inch Length of tube = 48 inch Number of tubes = 22 to 24 Material of construction Baffles Nozzles or jet stream Cost Stainless steel As per requirement As steam inlet to increase velocity Rs.6,00,000 (Approx)

CHAPTER 4

COST ESTIMATION,PLANT LATOUT,MATERIAL SAFETY 29

4.1 COST ESTIMATION

4.1.1 Estimation of Direct and Indirect cost:

Marshall and Shift index in 1992 for equipments is 943.1 Cost estimation based on the equipment Cost of the reactor Cost of the Neutraliser Cost of the Holding tank Cost of Crystallizer Cost of pump Cost of the Dryer Cost of the Centrifuge Total cost of the equipment = = = = = = = = Rs 1.7 x 106 Rs 0.62x106 Rs 1.1x106 Rs 0.71x106 Rs 0.25x106 Rs 0.25x106 Rs 0.32x106 Rs 4.3x106.

4.1.2 Estimation of total direct cost:

Purchased equipment cost ( E ) Purchased equipment installation (39% of E)

= = =

Rs 4.3x106 4.3x106x 0.39 Rs 1.677x106 = 4.3x106x0.28 Rs 1.204x106 4.3x106x0.31 Rs 1.333x106

Instrumentation (installed cost), 28%E = Piping installed, 31%E =

Electrical installation, 10%E

4.3x106x0.1 Rs 0.43x106 4.3x106x0.1

Yard improvement, 10%E

30

Rs 0.43x106 4.3x106x0.55 Rs 2.365x106 4.3x106x0.06 Rs 0.258x106 Rs 11.997x106

Service facility, 55%E

Land, 6%E

Total direct cost (D)

4.1.3 Estimation of total indirect cost: Rs 1.376x106

1. Engg and supervision ( 32% E )

2. Construction + contractor fees (25% direct costs) = 11.997x106x0.25 Rs 2.99925 x106 Rs 4.37525x106 Rs 16.37225x106 (4.37525+0.1x11.997x106) Rs 5.57495x106

Therefore total indirect cost (I)

DIRECT AND INDIRECT COST (TOTAL)

Contingence (10%D+I)

Fixed capital investment (FCI) Contingence + D + I 31 = Rs 21.9472x106

Working Capital: (10-20% of Fixed-capital investment)

Consider the Working Capital

15% of Fixed-capital investment

i.e., Working capital = 15% of 21.9472*106

0.15 21.9472x106 Rs 3.29208x106

Total Capital Investment (TCI):

Total capital investment

Fixed capital investment + Working capital Rs 25.23925x106 Rs 25.23925x106

i.e., Total capital investment

4.1.4 Estimation of Total Production cost:

Manufacturing Cost

Direct production cost + Fixed charges +

Plant overhead cost.

4.1.5 Fixed charges:

(10-20% total product cost)

32

i. Depreciation: (depends on life period, salvage value and method of calculationabout 13% of FCI for machinery and equipment and 2-3% for Building Value for Buildings) Consider depreciation = 13% of FCI for machinery and equipment and 3% for Building Value for Buildings) Rs. 2.85313106

i.e., Depreciation

ii. Local Taxes: (1-4% of fixed capital investment) Consider the local taxes = 3% of fixed capital investment 0.0321.9472*106 Rs. 0.6584106

i.e. Local Taxes

iii. Insurances: (0.4-1% of fixed capital investment) Consider the Insurance = 0.7% of fixed capital investment 0.007s Rs 21.9472*106 Rs. 0.15363106

i.e. Insurance

iv. Rent: (8-12% of value of rented land and buildings)

Consider rent

10% of value of rented land and buildings Rs. 0.13023x106 Rs. 3.79539106 33

Rent

Thus, Fixed Charges

4.1.6 Direct production cost:

(about 60% of total product cost)

Now we have Fixed charges

10-20% of total product charges

Consider the Fixed charges

15% of total product cost

Total product charge

fixed charges/15% 3. 79539106/15% 3. 79539106/0.15

Total product charge (TPC)

Rs. 25.3026106

i. Raw Materials: (10-50% of total product cost) Consider the cost of raw materials = 25% of total product cost 25% of 25.3026106 Rs. 6.32565106

Raw material cost

ii. Operating Labour (OL): (10-20% of total product cost)

Consider the cost of operating labour

12% of total product cost 12% of 25.3026106 Rs 3.0363106

Operating labour cost

iii. Direct Supervisory and Clerical Labour (DS & CL): (10-25% of OL) 34

Consider the cost for Direct supervisory and clerical labour Direct supervisory and clerical labour cost = 12% of 3.0363 Rs. 0.364357106 = 12% of OL

iv. Utilities: (10-20% of total product cost) Consider the cost of Utilities t Utilities cost = 12% of 25.3026106 Rs. 0.12 25.3026106 Rs. 3.036312106 = 12% of total product cos

v. Maintenance and repairs (M & R): (2-10% of fixed capital investment) Consider the maintenance and repair cost = 5% of fixed capital investment Rs. 0.0525.23925*106 Rs. 1.26196106

i.e. Maintenance and repair cost

vi. Operating Supplies: (10-20% of M & R or 0.5-1% of FCI)

Consider the cost of Operating supplies =

15% of M & R 15% of 1.26196106 Rs. 0.18929106

Operating supplies cost

35

vii. Laboratory Charges: (10-20% of OL) Consider the Laboratory charges = 15% of OL 15% of 3.0363106

Laboratory charges

Rs. 0.45544106

viii. Patent and Royalties: (0-6% of total product cost) Consider the cost of Patent and royalties st = 4% of 25.3026106 Rs. 1.0121106 Rs. 15.68141106 = 4% of total product co

Patent and Royalties cost

Thus, Direct Production Cost

4.1.7 Plant over head cost:

(50-70% of Operating labour, supervision, and maintenance or 5-15% of total product cost); includes for the following: general plant upkeep and overhead, payroll overhead, packaging, medical services, safety and protection, restaurants, recreation, salvage, laboratories, and storage facilities. Consider the plant overhead cost = 60% of OL, DS & CL, and M & R 60% of ((3.0363106) + (0.364357106) + (1.26196106) Rs. 2.79765106 36

Plant overhead cost

Plant overhead cost

Thus, Manufacture cost

Direct production cost + Fixed charges + Plant overhead costs.

Manufacture cost

15.68141106 + 3.79539106 + 2.79765106 Rs 22.27445106

II. General Expenses

Administrative costs + distribution and selling costs + Research and development costs

Administrative costs :( 2-6% of total product cost)

Consider the Administrative costs Administrative costs

= =

5% of total product cost Rs. 1.26513106

Distribution and Selling costs: (2-20% of total product cost); Includes costs for sales offices, salesmen, shipping, and advertising. Consider the Distribution and selling costs Distribution and selling costs Distribution and Selling costs = = = 15% of total product cost 15% of 25.3026106 Rs. 3.75453106

Research and Development costs: (about 5% of total product cost)

Consider the Research and development costs = 5% of total product cost 5% of 25.3026106 Rs. 1.26513106 37

Research and Development costs

Financing (interest): (0-10% of total capital investment) Consider interest = 5% of total capital investment 5% of 25.23925x106 Rs. 1.26196106

i.e. interest

Interest

Thus, General Expenses

(3.75453+1.26515+1.26195) x106 Rs 6.29163x106

III. Total Product cost

Manufacture cost + General Expenses

Total product cost

22.27445106+ 6.29163x106 Rs 28.55608 x106

= Gross Earnings/Income: Wholesale Selling Price of P.E.T per ton Hence Wholesale Selling Price of P.E.T per ton. = =

$ 650

650 46

Rs. 29900

Total Income product manufactured

Selling price Quantity of

29900 (2 T/day) (300 days/year) Rs. 17.94 106

Total Income 38

Gross income

Total Income Total Product Cost Rs 17.94106 28.556106 Rs10.62106

Gross Income Let the Tax rate be 45% (common)

Taxes

45% of Gross income 45% of 10.62106 Rs. 4.61106 Gross income Taxes Gross income (1- Tax rate) (10.62106) (4.62106) Rs. 6.01106

Taxes

Net Profit

= =

Net profit

= 4.1.8 Rate of return:

Rate of return

(Net profit100)/Total Capital Investment (6.01106100)/ (25.23925106)

Rate of Return

Rate of Return

23.99%

4.1.9 Payback period:

Payback period

= = =

(Total capital investment+total product cost) /net profit (25.239 x 106+28.556x106 )/ 6.01x106 4.3954 years 39

4.2 INSTRUMENTATION The primary objective of a designer when specifying instrumentation and control. Safe plant operation To keep the process variable within known safe operating limits To detect dangerous situations as they develop and to provide alarms automatic shutdown systems To provide interlocks to prevent dangerous operating procedures To achieves the desired product output To maintain the product composition within the specified quality standards.

Process may be controlled more precisely to give more uniform and higher quality products by the application of automatic co troll often leading to higher profit automatic is also beneficial in certain remote, hazardous or routine operations For manual control, an operator periodically measures the temperature .if it is below the desired value, the operator increases the steam flow by opening the valve slightly for automatic control ,a temperature sensitive device is used to produce a signal (electrical , pneumatic etc.) propositional to the measured temperature . This signal is fed to a controller, which compares it with a preset desired values or set point . If a difference exists, the controller changes the opening of the steam control valve to correct the temperature.

4.2.1 Control valve: The control valve contains a pneumatic device that moves the valve stem as the pressure on a spring loaded diaphragm changes .the stem positions a plug in the orifice of the valve body. as the pressure increases ,the plug moves downward and restricts the flow of fluid through the valve. The valve may also be constructed to have air to- open action. Most commercial valves move from fully open to fully closed as the valve top pressure changes from 3to 15psi. In general the flow rate of fluid through the valve depends upon the upstream and downstream fluid pressure and the size of the opening through the valve

4.2.2 Controler: 40

The control hardware is required to control the temperature of a stream leaving the heat exchanger. In general a controller contains Transducers (temperature to current ) Controller-recorder (current to current) Converter(current to pressure) Pressure valve (pressure to flow rate) Thermocouple is used to measure the temperature, the signal from the thermocouple is sent to the transducer, which produces an output in the of 4-20mA, which is a linear function of the input. The output of the transducer enters the controller where it is compared to the set point to produce an error signal. The controller converts the error to an output in the range of 3-16 psig which is a linear function of the input. Finally, the output of the converter is sent to the top of the control valve, which adjusts the flow of cooling water to the heat exchanger. Electricity is needed for the transducer, controller and converter. A source of 20psig air is needed for the converter. In a well-tuned control system, the response of the temperature will oscillate around the set point before coming to a steady state. 4.2.3 Instrment In Batch Reactor: Pressure gauge, Temperature indicator, Steam control valves, Cooling water control valves, Radar level indicator, Differential pressure level indicator, Pressure transmitter, Orifice plate,

41

4.3 PLANT LOCATION AND LAYOUT 4.3.1 Plant Layout and Site Selection: The following are the three necessary for the general plant layout The starting point or location or reference A kinetic diagram or directional factor A statement of the special requirement for various product ,raw material ,by product storage facilities and for processing department From known calculated or estimated space requirement for individual equipment. It is possible to obtain proper allocation of equipment and overall dimensions of the building Process Plant Piping The American national standard institute (ANSI) and the American petroleum institute (API) have established dimensional standard for the most widely used piping components they list these standard of the American society for testing material (ASTM) and American welding society(AWS).The consideration to be evaluated when selecting pipe material are: Possible exposure to fire respect to loss of strength, degradation Ability of thermal insulation Susceptibility of the pipe to brittle failure Susceptibility of piping material to crevice corrosion The Susceptibility of packing ,seal gasket as well as compatibility with the fluid handled The refrigerating effect sudden loss of pressure as volatile fluid in determining the lowest expected service temperature

42

The organization which generate standards of major importance to chemical process industries in United States are tested American national standard institute (ANSI) American society of mechanical engineers(ASME) American society for testing material (ASTM) International organization for testing material (ISO) The economic consideration and efficient operation of a process unit depend on how well plant and equipment specified on the process flow sheet is laid out .the major factors to be considered are Economic consideration construction and operating cost Damage to persons and property in case of fire explosion and toxic release Future expansion Modular construction In preparing the layout, one has to satisfy various regulation acts which are in force in the area where the plant is located. The main considerations are Factories act The explosives act Excise rules Health rules The boiler act

4.3.2 Plant Layout

43

Figure 4.1 Plant Layout

4.4 MATERIAL HANDLNG AND SAFETY Safety is one of the important aspect in any chemical industry. To run the process effectively, safety rules and regulations has to be followed. the guide lines are provided by the government and the industries has to implement them. Here we present about the safety guidelines adopted in ammonia plant 44

In any industry, whether it is a small or large scale industry, safety must be emphasized .there is a safety department to look after the safety procedures inside the industry 4.4.1 Kinds of Safety: Careful precautions are given to the workers upon their work The safety officer looks after the loading and unloading operating operations inside the plant There is an emergency control center for meeting in the emergency period There are assembly points inside the plant for the assembling of the workers during the emergency period. Mock drills are conducted in every 3months and they check with their availabilities The management is conducting seminars for the workers once in a month on the related areas such as safety, occupational health hazard, first aid, etc. PPEs of all kind are provided to the workers Fresh air line and showers are provided Medical center is established for emergency situations

4.4.2 Safety Equipment: Personal safety Equipment safety Material safety Personal Safety is for personnel proteciton Respiratory Non respiratory 45

Respiratory is used for to ovid inhalation of chemical Air supplying respiratory Air purifying respiratory Other safety protection is mentioned below. Helmet Safety shoe Gloves Apron Goggles, etc .

Equipment Safety is to safe operation. Some of the safety feature adopted in process is listed below. Rupture disc Pressure safety valve Set points Alarm Emergency shut off Trips Material Safety Set points Controls to temperature, pressure, ph, etc Standard operating procedure Material safety data sheet

4.4.3 Fire Fighting Equipment: Mechanical form DCP etc, Hydrant Single headed fire hydrant Double headed fire hydrant Fire water monitor fire escape hydrant Foam trally With water monitor 46

4.4.4 Safety in Batch Reactor: Rupture disk pressure safety valve alarm system tripping system set points Interlocks & control A rupture disc or bursting disc is a pressure relief device that protects a vessels or system from over pressurization. Rupture discs have a one-time use thin foil that fails at a predetermined pressure, either positive or vacuum. Rupture discs provide fast response to an increase in system pressure but once the membrane has failed it will not reseal.The equipment must be protected against being subjected to an internal vacuum (i.e., low pressure) that is lower than the equipment can withstand. Vacuum relief valves are used to open at a predetermined low pressure limit and to admit air or an inert gas in to equipment so as control the amount of vacuum.

If the chemical is drawn from the tank additional nitrogen pressure is fed to the tank by the blanketing regulator system. In case, if the nitrogen is not available from the source, then the tank may go under negative pressure and vacuum is created in the tank. due to this the tank may collapse. to avoid such accidents vacuum relief valve breathes in atmospheric air and protects the tank from further damage. Interlock is a device used to help prevent a machine from harming its operator or damaging itself by stopping the machine when tripped. Safety protection requirements are interlocked with the equipment operation to save the plant and person. Also called permissive. Interlock testing will be done based on the inter lock report which was already tested and certified. Interlock testing duration intervals are defined based on the criticality of the equipment. Is the condition to start or stop the equipment or valve or pump etc. 47

If the interlocks are satisfied than only you can able to operate the require operation. For example if the centrifuge lid is in open condition you can not able to start the centrifuge. Interlock check reports are available for all critical equipments and tested periodically.

48

The following controls are used in batch reactor The flow rate of steam can be controlled by the manual set point of percentage of valve opening. The flow rate of steam can be controlled by setting the requirement of steam flow rate. Based on the steam flow rate the steam control valve will be regulated automatically. Manual mode: The flow rate of cooling water to the condenser can be controlled by the manual set point of percentage of valve opening. Auto mode: The flow rate of cooling water to the condenser can be controlled by setting the requirement of cooling water flow rate based on the cooling water flow rate the control valve will be operated automatically. Cascade mode: The flow rate of cooling water to the condenser can be controlled based on the heat load of condenser. Temperature control: The flow rate of cooling water can be controlled based on the cooling water out let temperature of total condenser.

4.5 EFFLUENT TREATMENT PLANT Effluent is any water that has been adversely affected in quality by pollutants and the same drained during the process of production by production and other service department 49

4.5.1 Effluent origin: Utilities cooling waters(biocides ,heat ,slimes ,silt) Production process waste water Production process waste aqueous solution Residue from process Above Effluent Contains the Following High COD Extreme pH-from Process Traces of solvent

4.5.2 Need for Effluent Treatment: Treated effluent should comply with the local and/or national regulation regarding disposal of effluent into community treatment plants or into rivers ,lakes or ocean For the above orchid established zero discharge effluent treatment facility so that the pollutant concentrations in the effluent is treated and reused for the utilities (water make up for cooling towers, in recovery column water reflux and solvent washing ,in ETP filtration system water washing)

Effluent Treatment It is a group of unit process designed to separate ,modify remove ,and destroy undesirable substance carried by effluent sources

Effluent Quality Indicator The quality of the effluent is characterized by the following parameters pH COD (hemical oxygen demand ) BOD (Biological oxygen demand ) DO(Dissolved oxygen) TDS (Total dissolved solids) 50

 Others (silica, Iron, Fluoride)

4.5.3 Types of Effluent: Based on the incoming effluent characteristics we separated effluent into two streams for effective treatment to achieve the zero discharge The two effluent streams are 1. LPS-Low polluted stream 2. HPS-High polluted stream LPS &HPS Standard are mentioned as belove LPS 1. COD Less than 15,000ppm 2. fluoride ,iron,& traces solvent nil HPS 1. COD more than 15,000ppm 2. traces of Solvent LPS and HPS are treated as belove mentuned LPS (Low pollutant stream)is the effluent source which is treated by the bio chemical and filtration process to reuse for utilities HPS (High pollutant stream)is the effluent source which is treated by stripping evaporation and distillation processes to convert into LPS source and to reuse for cooling towers and other applicable usages

4.5.4 Effluent Treatment Processes: Treatment stages in LPS Primary treatment Secondary treatment Advanced treatment Primary treatment Primary treatment or pretreatment processes address the problem of screening ,equalization , neutralization, removal of floating scum and removal of suspended matters 51

Screening Screen grit chamber is used for screening process to separate the solid materials of more than 6mm from the LPS and to settle heavier particles at the bottom of the chamber The above said solid material from the screen and the settled particles are to be cleaned periodically By purging air at the bottom of the equalization tank for homogeneous mixing of LPS equalize the parameters (temperature, etc)and uniform feeding Any abnormal Ph is observed in the Eeropac(pH is the less than 6.5 and 8.5) neutralization to be done The total suspended solids (chemical sludge )which is collected at the center of the clarifier is taken for circulation from the neutralization tank and the settled TSS can be thickened further in centrifuge. Biological method s are cheaper ,effective and eco friendly the following biological methods are mainly used to reduce COD in the effluent by maintaining the MLSS&DO 1. Fine bubble jet aeration system 2. Coarse bubble surface aeration system By fine bubble jet aeration system we are effectively supplying the oxygen from the atmosphere air through the air blower to the bottom of the aeropac (circular tank used for fine bubble aeration)with the effluent emerging from the submersible pump connected to the FRP kit with spray nozzle .the same set up is kept in the each compartment of the aeropac. Coarse Bubble Surface Aeration System By surface aeration we are effectively supplying the oxygen from the atmosphere air through the aerator by splashing the surface of the liquid

(rectangular tank used for the surface aeration) Advance Filtration Treatment Process This process mainly used to recycle the resource (effluent) and to achieve the zero discharge. Ultra filtration system Nano filtration system Reverse osmosis system Ultra filtration system is used for following reason as mentioned below 52

 After secondary treatment we still have suspended solids in effluent. Using filtration methods we can trap all the suspended maters. If the feed water passes through the any filtration system it can be separates as two components 1. Permeate 2. Reject The permeate water from the UF is taken for NF for further treatment. The reject water from the UF is recycled in our biological system. UF filtration steps Pre filtration Cartridge filter (S.S) 250 micron pore size To avoid membrane contamination Fine porous ceramic membrane are used for filtration .

The Principle Nano filtration system is.Nano filtration working as same as the osmosis principle only filtration range is differs. When the feed water pass through the semipermiable membrane (poly amide) the movement of solvent phase (that is clear filtrate) takes place from the higher concentration to lower with continue till the applied pressure is greater than the osmotic pressure of the feed water. Dissolved macro particle shall be removed in this specific range of The permeate water from the NF is taken for RO for further treatment The reject water from the NF is send to ecology for HPS treatment NF filtration steps Pre filtration steps Cartridge filter (PP wounded) 5 micron pore size To avoid membrane contamination NF membrane filtration Membrane is made of spirally wounded fine porous poly amide 53

Reverse osmosis system Principle When the feed water (concentrated)water pass through the semipermiable membrane (poly amide) the movement of solvent phase (that is clear filtrate) takes place from the higher concentration to lower with the applied pressure the filtration will continue till applied pressure is greater than the osmotic pressure of the feed water. Dissolved micro particle shall be removed in this specific range of filtration. The permeate water from the RO is used for cooling water make up in utilities & column reflux in the recovery plants. The reject water from the RO is send to ecology for HPS treatment. RO filtration steps Pre filtration Cartridge filter (PP wounded) 5 micron pore size To avoided membrane contamination RO membrane filtration Membrane is made of spirally wounded fine porous poly amide.

Treatment process in HPS is mentioned below Stripping To remove mixed solvent in HPS Evaporation HPS is converted to LPS by evaporation (Three types of evaporator) Waste heat recovery Impure stream heat is transferred into pure stream Concentration (Concentrated as salt)

54

CHAPTER 5

CONCLUSION
A detail study of manufacture of Pentaerithritol has been completed with material and energy balance calculation for the production capacity of 600 tones per annum. Design of the reactor and vacuum tray drier involved in the process has been studied as per requirements & also plant layout, safety, with respect to environment aspects has been studied. It has been estimated that Payback period of 4.329 can be achived by suitable selection of process. The effluent treatment for this process has been studied in detail manner. Safety related to material handling, fire fighting equipments and safety features of batch reactor is studied in detail. The application of penaerithritol is studied. By product sodiumformate recovery is studied in detail with respect to material balance.in overall view it has been concluded that this method of process adopted for manufacturing of pentarerithritol and its by- product is most suitable economical process.

55

REFERENCES
1. Bhatt B.I and Vora S.M., Stiochiometry, 2nd edition, Tata McGraw-Hill publication, New Delhi, 1994, page no: 360-375. 2. Donald.Q.Kern, Process Heat Transfer, 7th edition, McGraw Hill publication, Singapore, 2000, page no: 619-635. 3. Kirk R.E and othmer D.F, Encyclopedia of Chemical Technology 4 th edition, Wiley-Interscience publication, New York, 1995 , page no: 325-340. 4. Robert E.Treybal, Mass Transfer Operations, 3rd Edition, McGraw Hill publication, Singapore, 1981, page no:665-675. 5. Robert H Perry and Don W.Green, Perrys Chemical Engineers Handbook 7 th Edition, McGraw Hill publication, New York, 1991, page no:452-459. 6. Sinnot.RK, Coulson and Richardsons Chemical Engineering, Asian Books Pvt Ltd., New Delhi, 1998, page no:456-462. 7. Sybilp Parker, Encyclopedia of Science and Technology, 7 th Edition, McGraw Hill publication, New York, 1992, page no: 391-403. 2 nd Edition,

56

57