Unit operation lab

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Faculty of Chemical & Natural Resources Engineering

BKF3731 Unit operation lab

Name Matric No. Group Program Section Date

Sem. II - Session 2011/2012

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CONTENTS

Exp 1: Gas Absorption Adsorption Unit Exp 2: Sieve Shaker Exp 3: Thin Film Exp 4: Rotary Evaporator Unit Exp 5: Solid Liquid Extractor Unit Exp 6: Absorption Column Unit Exp 7: Short Path Distillation Exp 8: Sieve Tray Distillation Exp 9: Plate & Frame Filter Press Exp 10: Pressure Swing Adsorption

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EXPERIMENT 1: GAS ABSORPTION ADSORPTION UNIT

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OBJECTIVE 1. To absorp and adsorp gas through a packed column in a batch process, eg. the absorption of CO2 into water and adsorption of CO2 into activated carbon. 2. To observ the effect of liquid flow rate on the absorption-adsorption process.

INTRODUCTION The gas absorption-adsorption unit is design to demonstrate the basic principles of absorption (gas-liquid) and adsorption (gas/liquid-solid) processes. Gas absorption is a process in which soluble components of gas mixture are dissolved in a liquid phase. The gas and liquid normally flow counter currently among some packing which serve to provide the contacting of interfacial surface through which mass transfer take place. Meanwhile, adsorptions involve the binding of molecules from their liquid or gaseous environment onto the surface of solids. It is a separation process for the selective removal small quantities of components from a fluid mixture or solution. Two packed columns filled with ceramic berl saddles mixed with activated carbon granules are provided for absorption-adsorption experiments. Each column are to be run individually. Air and carbon dioxide (CO2) are fed into the bottom of a packed column. Water is transferred to the top of the column either from feed vessel B1 using a centrifugal pump P1, or entered directly from the laboratory supply. Counter current flow among the carbon bed will cause the transfer of CO 2 from the air mixture into the water and subsequently onto the activated carbon. The lean air mixture will exit at the top whereas the spent water will accumulate at the bottom of the column and overflow out into either the feed vessel B1 or receiving vessel B2. Some CO2 will present in the water can be stripped or desorbed in the feed vessel B1. The spent water is heated in feed vessel B1 to decrease the solubility of CO2 in water. Circulation of the hot liquid around the feed vessel through pump P1 will release the dissolved CO2 into vent. To remove adsorbed CO2 from the activated carbon, hot air can be passed through the column while the vacuum pump is in switched on. EQUIPMENT/APPARATUS/MATERIAL 1. Gas absorption-adsorption unit 2. Beakers 3. Digital balance 4. Stop watch 5. Deionized and co2 free water

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EXPERIMENTAL PROCEDURE

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1. Perform the general start up procedures (Refer Procedure to Work Instruction). Fill feed vessel B1 with water (3/4 from maximum level of B1) and start with packed column K1. 2. Switch on circulation pump P1, then open and adjust valve V12 & V11 to give a water flow rate 50 L/hr. Allow the water to enter the top of column K1, flow down the column and accumulate at the bottom until it overflows back into feed vessel B1. 3. Open and adjust valve V2 to give a flow rate of 50 LPM air into column K1. 4. Open and adjust valve V1 to give a flow rate of 10 LPM CO2 into column K1. 5. Allow the air mixture to flow through the packed column for 5 minutes. 6. Start the timer and record the concentration of CO2 Inlet and Outlet for every minutes until no further changes. 7. Throughout the experiment, monitor and maintain the air, CO2 and water flow rates by adjusting the appropriate valves. 8. Drain all liquid from the feed vessel B1, K1 or K2 by opening valve V10, V6 / V7. 9. Repeat step 1-8 for next 2 different water flowrate (Water Flowrate Range: 25 L/Hr 200 L/Hr). 10. At the end of the experiment, close valve V1 & V2 and switch off circulation pump P1. Drain the liquid from the bottom of column K1 / K2 by operating valve V6 / V7. 11. Shut down the system.

RESULTS
Setting I Water Flowrate: Time Inlet CO2 Vol % Outlet CO2 Vol % Setting II Water Flowrate: Inlet CO2 Vol % Outlet CO2 Vol % Setting III Water Flowrate: Inlet CO2 Vol % Outlet CO2 Vol %

Concentration, Concentration, Concentration, Concentration, Concentration, Concentration,

0 1 2 3

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DISCUSSION

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1. Review about each operating condition of the CO2 composition in the outlet water flow as a function of time. 2 . Give two examples the application of this concept in the chemical/petrochemical industries. Briefly discussion about the process. 3. State the different between absorption and stripping. 4. Summarise the calculation principal of absorption/desorption.

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EXPERIMENT 2: SIEVE SHAKER OBJECTIVE 1. To introduce the basic principles of Sieve-Shaker.

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2. To obtain the particle size distribution and grading characteristics of the soil particles in a given soil sample.

EQUIPMENT/APPARATUS/MATERIAL

1. Vibratory Sieve-shaker 2. Balance sensitive to 0.1g. 3. Containers. 4. Sieving Tray 1mm, 800 um, 630 um, 315 um and collecting pan. EXPERIMENTAL PROCEDURES

1. Collect a representative dry sample of approximately 500g. 2. Determine the mass of your sample accurately to 0.1g. Record as W. 3. Prepare a stack of sieves. A sieve with a larger opening is placed above a sieve with smaller openings. 4. Pour the soil prepared in step 2 into the stack of sieves from the top 5. Place the cover on the top of the sieves. 6. Run the stack of sieves through the sieve shaker for about 5 minutes and set it amplitude to 0.5 1.0. 7. Stop the sieve shaker and remove the stack of sieves. 8. Weigh the amount of soil retained on each sieve and the bottom pan. Record as W1. 9. Calculate the total weight of soil retained on all sieves. The percentage loss during sieve analysis=(W-W1)/W*100

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EXPERIMENT 3: THIN FILM OBJECTIVE

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1. To demonstrate the separation of ethanol - propanol mixture using the thin film evaporative process 2. To determine effect of heating temperature and vacuum pressure on the separation efficiency.

INTRODUCTION The thin film evaporation unit is a complete evaporation system including feed input, heating and vacuum generation for continuous plant operation. The unit is designed to evaporate materials in the pressure range of atmospheric down to 8 mbar. The lower the pressure, the lower the temperature required to effect evaporation, thus lowering the chances of damaging the product. The thin film evaporator adopts a rotating film system, where molecules are continuously evaporating from a film which is spread by a rotating wiper.

EQUIPMENT/APPARATUS/MATERIAL 1. BP215 Thin Film Evaporator 2. Stop watch 3. Beakers 4. Refractometer 5. Cooling Water Supply 6. Ethanol 7. Measuring Cylinder 8. Propanol

EXPERIMENTAL PROCEDURES 1. Prepare a set of mixtures containing ethanol and propanol within a specified range of composition between pure ethanol and pure propanol. Determine refractive index (RI) for each mixture using a refractometer. 2. Prepare 15L of ethanol-propanol mixture at a composition at composition 60:40 v/v. Obtain a sample from the feed liquid at valve V2 and analyze the sample to determine its actual initial composition. 3. Perform the general start-up procedures with the following default settings: metering pump P1 : 60% stroke, 60 stroke/min heating thermostat T1: 60C vacuum controller PIC-1 : 400 mbar

4. Allow the unit to run for about 5-10 minutes to achieve steady state. Steady state is reached when the distillate temperature doesnt change significantly over time. 5. Record the distillate temperature.

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6. Measure the distillate and bottom product flow rates.

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7. Collect the product from both distillate and bottom product vessels B2 and B3. Analyze the collected liquid to determine its compositions 8. Repeat the experiment by reducing the vacuum pressure down (Range 750 350 mbar). 9. Return the vacuum pressure to default. Repeat the experiment by increasing the heating thermostat up (Maximum 90 oC).

RESULT Initial Feed Composition :

P1 : 60% stroke, 60 stroke/min N o. Heating Temp.

o

Vacuum Pressure mbar Temp

o

Distillate Flowrate mL/min RI Composit ion

Bottom Product Flowrate mL/min RI Composi tion

Constant Temperature at 600C (Setting at T1 = 750C) 1 2 3 60 60 60

Constant Pressure at 500mbar 4 5 6 500 500 500

*Use Antoine Equation to determine the right temperature/pressure setting Log10P = A- B/(C+T) Antoine Constant [Temperature in oC and Pressure in mmHg)
Component Ethanol Propanol Propanol A 8.1122 7.74416 8.37895 B 1592.864 1437.686 1788.02 C 226.184 198.463 227.438 TMin[ C] 20 60 -15
o o sat

TMax[ C] 93 106 98

P [mmHg] 1693.832048 845.657321 828.5394222

**Temperature setting at T1 should be 15oC higher than calculated temperature due to heat loss.

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GUIDES FOR DISCUSSION
1. Plot the calibration curve of RI versus ethanol-propanol composition.

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2. Plot a graph of distillate temperature, bottom and top composition and percentage feed vaporized versus feed flow rate and vacuum pressure. 3. Compare between the distillate temperature, bottom and top composition and percentage feed vaporized at different heating thermostat temperature. 4. Calculate the separation efficiency at different operating conditions.

Efficiency

distillate flow rate x distillate composition x100 % feed flow rate x feedcomposition

5. Compare the separation efficiencies between different operating conditions to determine the effect of feed flow rate, composition, temperature and pressure.

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FEED RATE SETTING DIAGRAM FOR FEED PUMP

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EXPERIMENT 4: ROTARY EVAPORATOR UNIT OBJECTIVE

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1. To introduce about the principles of the binary mixture separation process using rotary evaporator. 2. To separate the binary mixture, eg. ethanol-propanol using rotary evaporator unit in the vacuum condition

INTRODUCTION A rotary evaporator or rotavap, is a device used in chemical and biochemical laboratories for the efficient and gentle evaporation of solvents. The main components of a rotary evaporator are a vacuum system, consisting of a vacuum pump and a controller, a rotating evaporation flask which can be heated in a heated fluid bath, and a condenser with a condensate collecting flask. The system works because lowering the pressure lowers the boiling point of liquids, including that of the solvent. This allows the solvent to be removed without excessive heating. Evaporation under vacuum can be performed in a standard distillation rig. However, the rotary evaporator has a key advantage. As the evaporating flask rotates, the liquids are forced to the outside of the flask with the centrifugal motion. This creates a larger surface area of the liquids and hence allows for quick, gentle evaporation. Rotary evaporators are highly effective at removing the majority of organic solvents during the extraction process. The remainders of the solvents are usually removed using a high-vacuum line. EQUIPMENT/APPARATUS/MATERIAL 1. Rotadest R50 Rotary Evaporator 2. Stop watch 3. Beakers 4. Refractometer 5. Cooling Water Supply 6. Ethanol 7. Measuring Cylinder 8. Propanol

EXPERIMENTAL PROCEDURES 1. Prepare a set of mixtures containing ethanol and propanol within a specified range of composition between pure propanol and pure ethanol. Determine refractive index (RI) for each mixture using a refractometer. 2. Prepare 4L of ethanol-propanol mixture at a composition 50:50 v/v.

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3. Perform the general start-up procedures with the following default settings: a. b. c. Bath temperature T1C-1 : 65C Rotation speed SI-1 : 25 rpm Vacuum controller PIC-1 : 400 mbar

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4. Open valve V5 to collect the distillate in receiving vessel B2 5. Once all temperature readings are constant, close valve V3 and open valve V4. Observe the flow of distillate from condenser W2 through liquid cooler W3 into receiving vessel B2 6. Start the timer once liquid starts to enter vessel B2. 7. Record the distillate temperature every 5 minutes. 8. After 5 minutes, collect the product from receiving vessel B2 and measure its volume. Analyses the collected liquid to determine its composition using refractometer. 9. Combined all the collected distillate in a container and at the end of the experiment, measure its overall volume and composition. 10. Repeat the previous step by switching back and forth between both receiving vessels B2 and B3 every 5 minutes until they are no more flow of distillate observed in the unit. 11. Stop the experiment and switch off vacuum pump P1, heating bath W1 and rotary sphere drive M1. Lower the heating bath by opening the pressure release valve below the hydraulic jack. 12. Wait for the concentrate in rotary sphere B1 to cool down before collection. Determine the volume and composition of the concentrate.

RESULT Initial Feed Composition Time Minute Distillate Temperature o C : Distillate Volume mL RI Distillate Composition Vol % Distillate Flow Rate mL/min Volume of Ethanol in Distillate mL

5 10

Volume and Composition of Concentrate:

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DISCUSSION 1. State the difference between evaporation and distillation. 2. Briefly explaination about the used evaporator in the industrial world. 3. Review the main component of modern rotary evaporator. 4. Draw and shortly describe about the equilibria curve of ethanol-propanol.

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EXPERIMENT 5: SOLID LIQUID EXTRACTOR UNIT OBJECTIVE 1. To recognize the solid/liquid separation using extractor unit.

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2. To determine the extractable component using solvent, eg. salt extraction from sea-shore sand.

INTRODUCTION Separation processes are a fundamental part of almost every chemical process. Indeed, there are usually far more separation stages in the overall process than there are chemical reactions. Separations start with the extraction. Solid-liquid extraction can be defined as the removal of one or more components from a solid phase (or mixture of phases) by using a liquid to selectively dissolve the required fraction. Generally, the process can be considered in two steps: Contact of solid with liquid and selective dissolution of one or more components of the solid phases. Separation of the resulting solution from the residual solid.

EQUIPMENT/APPARATUS/MATERIAL 1. CTS6 Solid Liquid Extraction Unit 2. Steam supply 3. Portable Conductivity Meter 4. Stop watch 5. Digital balance 6. Tap water as solvent 7. Sand (from sea-shore) as the solid 8. Table salt (50g) 9. Six 250mL beakers 10. 100mL graduated cylinder 11. 2L measuring jug

EXPERIMENTAL PROCEDURES 1. 2. Prepare standard salt solution and get its conductivity by using conductivity meter. Solid charging Weigh out the appropriate quantity of solids into the fibre bag (typically 2 kg). Carefully remove the solvent food line and vent line fitted to extraction vessel cover. Open extraction vessel cover and place the fibre bag containing the solids into the extraction vessel, ensuring that the top of the bag is open for downward solvent flow. Replace the vessel cover and hand tighten the securing clips. Replace the vent and solvent food lines. 3. Solvent charging

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Open charge valve V4. Fill the water carefully until its reach the level of the vessel equator. 4. Extraction by continuous downward displacement.

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Ensure that the solvent feed line from below the distillate cooler is firmly attached to the top of the extraction vessel. Close V5. 5. Start up this equipment by follow General Start Up Procedures - Pre Start Up Checks; Start-up Circuit 1 Cooling Water; and Start-up Circuit 3 Heating in Work Instruction (attached on equipment). 6. 15 minutes after solvent has begun to pass through the product cooler, measure the flowrate FI 1 and adjust the heat input to give a flowrate of approximately 500ml/min. To measure the solvent flowrate, follow this step: Set the equipment for return of solvent to reboiler section by close valve V5. When the solvent reaches the bottom mark on FI 1 begin timing and stop the timing when the solvent reaches the top mark of FI 1. Open valve V5. 7. When a steady value for FI 1 has been determined, records its value its value and the values indicated by TI 1 and PI 4. 8. Carefully take a sample from the reboiler by open sampling valve V2 and remove sample. Close V2 when sample is removed. 9. Close valve V5 and begin solvent transfer to the extraction vessel. Close stop valve V8. Carefully open sampling valve V3 and remove sample. Close sampling valve V3. Open stop valve V8. 11. Record the collection of this sample as T=0. 12. Sample reboiler contents and effluent every 2 minutes for the first 10 minutes, then every 5 minutes until 30 minutes then at T=45. 13. Record the final temperature indicated by TI 1. 14. Determine the conductivity for each sample taken. 15. Shutdown the equipment by following the instruction in part of General Shut Off Procedures in Work Instruction.

10. Take a sample of the first effluent:

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RESULT Experimental Data Weight of solid charge FI 1 TI 1 (Initial) : : : TI 1 (Final) PI. 4 : :

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Time (min) 0 2 4 6 8 10 15 20 25 30 45 Conductivity

Reboiler Salt Conc. g/L Conductivity

Effluent Salt Conc. g/L

DISCUSSION 1. Review about the correlation between concentration and time for reboiler and effluent. 2. Briefly explaination about the used solid liquid extraction in the industry. 3. Discuss about mass transfer in the solid liquid extraction. 4. Summarise the principal of solid liquid and liquid liquid extraction.

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EXPERIMENT 6: ABSORPTION COLUMN UNIT

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OBJECTIVE 1. To determine the effect of air flow rate and water flow rate on flooding point in an absorption column. 2. To explain the relationship between water and air flow rate changes and their effect on pressure drop, P of an absorption column.

INTRODUCTION Absorption column is one of the separation techniques that involve liquid and vapor. One or more component of a gas mixture can be separated when a certain liquid flow through it countercurrently. The liquid absorbs the component(s) and mass transfer process which separates the component(s) from gas mixture occurs. Packed material is used to increase the contact surface area in absorption process which enhances the efficiency and shortens the duration of the process.

EQUIPMENT/APPARATUS/MATERIAL 1. Packed Absorption Column 2. Air Compressor 3. Water and Air 4. Stop watch

EXPERIMENTAL PROCEDURES 1. Check and make sure the valves for right column for sadle pack are opened. 2. Set the water flow rate at 2.5 L/min. 3. Set the air flow rate at 100 L/min. Start the stop watch and leave it for 5 minutes. Make sure the water and air flow rate are always constant. 4. After 5 minutes, take the data for pressure drop, P from Digital P Meter. 5. Repeat Steps 3 and 4 by increasing air flow rate by 10 L/min until the flooding point is observed. 6. When the flooding point is achieve, read the P from Digital P Meter and reduce the air flow rate back at 100 L/min 7. Repeat Step(s) 3 to 7 for water flow rate at 3.0 L/min respectively. 8. Then, maintain the air flow rate at 50 L/min and, read the pressure drop every 2 minutes at different water flow rates range from 2.0 to 3.5 L/min with an increment by 0.5 L/min

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RESULT Table 1 Water flow rate, W (L/min) Air flow rate, G (L/min) Pressure Drop, P (cm H2O) Time (every 5 minutes)

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2.5

3.0

Table 2 Air flow rate, G (L/min) Water flow rate, W (L/min) 2.0 50 2.5 3.0 3.5 Pressure Drop , P (cm H2O) Time (every 2 minutes)

GUIDES FOR DISCUSSION 1. Plot a graph log P versus log air flow rate for each water flow rate (refer table 1). Find the relationship between P and air flow rate. 2. Plot graph log P versus log water flow rate for fixed air flow rate (refer table 2). Find the relationship between P and water flow rate. 3. Describe the following terms: a) Flooding point b) Flooding velocity c) Loading point

4. List down 5 applications of this process that is used in petrochemical industries. 5. Explain roughly one of the applications that are listed above.

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EXPERIMENT 7: STUDY ON THE EFFECTS OF THE PARAMETERS ON THE THERMAL SEPARATION EFFICIENCY USING SHORT PATH DISTILLATION OBJECTIVE 1. To introduce the short path distillation principles using continuous system. 2. To observe the effects of stirrer speed and temperature on the efficiency of separation, e.g ethylene glycol-water.

INTRODUCTION This Short Path Distillation is a thermal separation process for thermal sensitive products. Short residence time and low evaporation temperature will cause a minimum thermal stress to the distilled product. Typical applications are high molecular organic compounds particularly from the field of chemistry, pharmaceutical and food industry. Distillation is one of the most important thermal separation methods. Short path distillation is a continuous separation process working under vacuum conditions. Evaporation takes place from a heated wiped film. Caused by the pressure drop between the place of evaporation and the vacuum system the operating pressure in typical wiped film evaporators with external condenser is limited to some millibars. The considerably lower pressure in the short path evaporator is obtained by the short distance for the vapours on their way from the evaporator surface to the condenser. In addition, the cross section area of flow is equal to the evaporator surface, so that there is only a minor pressure drop between evaporator and condenser

EQUIPMENT/APPARATUS/MATERIAL 1. Short Path Distillation Unit 2. Ethylene glycol water mixture

EXPERIMENTAL PROCEDURES 1. Mix the ethylene glycol and water with a ratio of 7:3 at total of 1 litre in a beaker. Then stir the mixture homogeneously. 2. Check that all valves are initially closed except the valves HV04, HV05, HV11 and HV12. Ensure that the cold trap is filled with dry ice. 3. Switch ON the main power supply at the control panel.

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4.

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Set the thermostat at 70C, Chiller at 12C and vacuum pump pressure at 250 mbar. Manually maintain the pressure throughout the experiment. [To adjust vacuum pump pressure, manually adjust valve, V14. To adjust the desired flow rate, adjust the opening valve HV03. To adjust the desired stirrer speed, adjust knob button at stirrer].

5.

Once the chiller temperature and thermostat temperature have reach the set points, the equipment is ready for experiment.

6. 7.

ON feed pump and set it to 10 rpm and then ON stirrer (set to desired speed). For every set of experiment, run for 5 minutes. After 5 minutes, records down the volume of distillate from V-104 and volume of concentrate from V-105-107.

8.

Repeat the experiment with different operating parameters as shown in the table in result and discussion.

9.

Follow the operating procedure to shut down the equipment. DO NOT let the wiper roller to run without the flow of feed.

GENERAL SHUT-DOWN PROCEDURES 1. 2. 3. 4. 5. Switch off vacuum pump. Switch off feed pump and stirrer motor. Turn off thermostat. Open valve HV 06 and HV 07. After 15 minutes, switch off chiller and turn off the main power. NOTE: DO NOT attempt to remove any vessel while the vacuum pump is running.

RESULT 1. Effect of stirrer speed Vacuum pressure, PT-200 Evaporator Temperature, TT-100 Feed Flow rate Contact time EG-water ratio 100mbar 70C ml/min 5 min 7:3

Time Start

Stirrer Speed(rpm) 50 100 200

Distillate Volume (ml)

Concentrate Volume (ml)

Separation Efficiency (%)

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220

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2. Effect of evaporator temperature Feed flow rate Stirrer speed, M-500 Vacuum pressure Contact time EG-water ratio ml/min 220rpm 100mbar 5min 7:3

Time Start

Temp (C) 70 72 74 76 80

Distillate Volume (ml)

Concentrate Volume (ml)

Separation Efficiency (%)

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V-100
Feeding Funnel
Material: Boro. glass Capacity: approx. 2000 ml c/w tempering jacket; pressure equalizing tube, needle valve Inlet: GL45; Outlet: NS29/32

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V-101
Cold Trap
Material: Boro. glass For dry ice usage c/w drain valve DN6 Vacuum: 2x KF15/3 Outlet: NS29/32

V-102, V-103
Graduated Cylinders
Material: Boro. glass Capacity: 250 ml c/w/ DN3 valves for inlet outlet & venting Inlet: NS29/32; Outlet: NS29/32

V-104 to V-107
Product Vessels
Material: Boro. glass Capacity: 250 ml Round bottom

V-108
Vessels
Material: Boro. glass Capacity: 20 ml Round Bottom

T-200
Short Path Evaporator
Material: Boro. glass c/w roller wiper cage (Rulon rolls); magnetic stirrer sealing, heating jacket (0.03 m2); cooling coil (0.05 m2); Feed: NS29/32; Outlet: NS29/32; Vacuum: NS29/32

E-300
Heating Jacket
Material: Boro. glass Surface: 0.03 m2

E-301
Cooling Coil
Material: Boro. glass Surface: 0.05 m2

B-400
Thermal Oil Bath
Range: 28 to 280 C (0.01 K) Heater: 3000 watt Bath capacity: approx. 12-L Pump: max. 24 LPM

B-401
Chiller
Range: 5 to 25 C (2 C) Cooling capacity: 18,000 BTU/hr Bath capacity: 50-L Pump: 50 LPM

M-500
Stirrer Drive
Power: 100 W Torque: 250 Ncm Speed: 8 to 2000 rpm Output: 0 10V

P-100
Vacuum Pump
2-stage Rotary Vane Type Ultimate Vacuum: 6 x 10-3 mbar Pumping Speed: 2.9 m3/hr

HV 01

V-100
HV 13

HV 02

TIC TT 100 100

SIC 500 ST 500

M-500
El.

M
HV 03

B-400

TT 102

T-200
PT 200

(E-300, E-301)
V 14

Vent

P-100

V-101

HV 04

TT 103

HV 05

HV 06 HV 10

HV 07

V-102 V-108

V-103

HV 12

TIC TT 101 101

HV 11 HV 08 HV 09

El.

B-401 V-104 V-105 V-106 V-107

Short Path Distillation Unit

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DISCUSSIONS:

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1. Plot a graph of stirrer speed vs. separation efficiency and evaporator temperature vs. separation efficiency. 2. Discuss the effects of the parameters on the thermal separation efficiency. 3. Briefly explain the importance and application of short path distillation system in industry.

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EXPERIMENT 8: BATCH DISTILLATION AT TOTAL REFLUX USING SIEVE TRAY DISTILLATION

OBJECTIVE 1. To determine the height equivalent theoretical plates (HETP) at total reflux.
2.

To determine the effect of liquid and vapor loading on the HETP at total reflux.

INTRODUCTION The principle for sieve tray distillation is the same as for normal distillation: when a liquid mixture is heat so that it boils, the composition of the vapor above the liquid differs from the liquid composition. If this vapor is then separated and condensed into a liquid, it becomes richer in the lower boiling component(s) of the original mixture. This is what happens in a sieve tray distillation column. A mixture is heated up, and routed into the distillation column. On entering the column, the feed starts flowing down but part of it, richer in lower boiling component(s), vaporizes and rises. However, as it rises, it cools and while part of it continues up as vapor, some of it (enriched in the less volatile component) begins to descend again. Figure 1: shows a simple continous fractional distillation tower for separating a feed stream into two fractions, an overhead distillate product and a bottoms product. The lightest products (those with the lowest boiling point or highest volatility) exit from the top of the columns and the heaviest products (the bottoms, those with the highest boiling point) exit from the bottom of the column. The overhead stream may be cooled and condensed using a water-cooled or air-cooled condenser. The bottoms reboiler may be a stream-heated or hot oil-heated heat exchanger, or even a gas or oil-fired furnace. In a continous distillation, the system is kept in a steady state or approximate steady state. Steady state means that quantities related to the process do not change as time passes during operation. Such constant quantities include feed input rate, output stream rates, heat and cooling rates, reflux ratio, and temperatures, pressures, and compositions at every point (location). Unless the process is disturbed due to changes in feed, heating, ambient temperature, or condensing, steady state is normally maintained. This is also the main attraction of sieve tray distillation, apart from the minimum amount of (easily instrumentable) surveillance; if the feed rate and feed composition are kept constant, product rate and quality are also constant. Even when a variation in conditions occurs, modern process control methods are commonly able to gradually return the sieve tray process to another steady state again.

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EQUIPMENT/APPARATUS/MATERIAL 1. Sieve Tray Distillation Unit 2. Refractometer

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3. 7L of binary mixture (ethanolpropanol). 4. Beakers.

EXPERIMENTAL PROCEDURES 1. Prepare a set of mixtures containing ethanol and propanol within a specified range of composition between pure propanol and pure ethanol. Determine refractive index (RI) for each mixture using a refractometer. 2. Ensure all valves are closed. 3. Prepare a mixture of ethanol and propanol at desired composition (for instance 5 L mixture containing 3 L of ethanol and 2L of propanol). 4. Record initial volume and refractive index of the liquid mixture. 5. Open the charge port cap and charge the reboiler B1 with the ethanol-propanol mixture. Close the charge port cap. 6. Make sure all the valve are properly close except V15 and V14 for cooling purposes. 7. Turn on the main power on the control panel. 8. Ensure the reflux control is 0 position(total reflux) 9. Switch on the cartridge heaters W1 and set the heater power regulator to 1.0 kW and allow the reboiler temperature reach approximate 85oC. 10. As the top column temperature sensor TT 112, reach steady state, record the temperature. 11. Set the reflux control to position 1(Total distillate offtake). When the level in phase separator reaches 100mL, start the timer. As distillate reach 200mL, stop the timer and determine the flowrate of the distillate. 12. Open valve V9 and collect 10 ml sample distillate using conical flask. Close valve V9 and set the reflux control to position 0(Total reflux). 13. To collect bottom product sample, adjust the level adjuster to a suitable level to let the product overflow into the product tank, B5 after passing through the product cooler, W3. Open valve V2 and V3 to collect 10 ml of sample bottom product using conical flask. Close valve V2 & V3. 14. Measure the refractive index of the samples and record the value into data table. 15. For different liquid and vapor loading, adjust the heater power settings in W1 according table below: Heater Power (kW) 1.00 1.50

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2.00

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17. Wait for approximately 5 minutes and allow the distillation unit to achieve new steady state. Repeat steps 9 to 13. 18. Switch off heater power and allow the system to cool down to ambient temperature.

RESULT Table 1: Data Collection for Distillate and Bottom Product Heater W1, W2 Power (kW) 1.00 1.50 2.00 Temp (oC) Distillation Refractive Index Mole Fraction Bottom Product Temp (oC) Refractive Mole Index Fraction HETP (mm)

GUIDES FOR DISCUSSION 1. Fill up Table 1 for data collection 2. By using ethanol-propanol equilibrium diagram, mark the top and bottom compositions on the diagram and determine the theoretical number of plates in the distillation unit using the McCabe-Thile Method. 3. Calculate the height equivalent theoretical plates (HETP) by dividing the effective column height with the number of theoretical plates. 4. Plot a graph of HETP versus heating power. 5. Discuss the relationship between HETP and heating power.

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Figure 1: Chemical engineering schematic of Sieve tray Binary Fractional Distillation tower. A binary distillation separates a feed mixture stream into two fractions: one distillate and one bottom fractions.

Figure 2: Process Flow Diagram for sieve tray unit

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EXPERIMENT 9: PLATE & FRAME FILTER PRESS

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(Filtration of solid particles suspended in a liquid)

OBJECTIVE 1. To introduce the operation of plate & frame filter press process. 2. To observe the influence of an increasing filtration time on the volume of filtrate. INTRODUCTION The task of filtration is to separate solid particles suspended in a liquid or in a gas. There are deep bed, surface and cake filtration. A familiar example is the separation of solid and liquid on a filter. Here, the filter is impinged with a suspension of solid particles and liquid. Filtration separates suspensions into a solid (residue) and liquid (filtrate). This is achieved by a pressure change using a porous material, the filter material. The liquid passes through the pores or openings in the filter material, while the solids are retained by the filter material. The driving force is a pressure difference between the suspension on one side of the filter material and the filtrate on the other. The difference is created by a vacuum on the filtrate side or excess pressure on the suspension side (hydrostatic or pressure generated using pumps). In cake filtration, the solid particles are deposited on a filter material. The filter cake is the total of the separated solid particles on the filter material. Ideally, a fully solid-free liquid is obtained after the filter, which is known as the filtrate.

Figure 1 Principle of filtration process. In this experiment, the suspension is conveyed through the cleaned plate and frame filter press. The filter inlet pressure and the volumetric flow of the filtrate are measured.

EQUIPMENT/ APPARATUS / MATERIAL 1. Plate and frame filter press

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2. Stop watch 3. 4. Diatomite 150 L water

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EXPERIMENTAL PROCEDURES Inserting the filter layers and filter plates 1. Measure the weight of filter layers and filter plates. 2. The first filter layer should be placed with the inlet side against the black inlet plate. 3. The other filter layers are then placed alternately outlet side to outlet side and inlet side to inlet side between the filter plates that are still to be inserted in the plate and frame filter press. 4. After the black inlet plate with filter layer inserted (2), a white, hollow filter plate (type a) is placed on the guide bar and a filter layer is inserted with the outlet side against it. 5. A filter plate with finned surface (type b) is then inserted and a filter layer is inserted with the inlet side against it. The remaining filter plates are inserted alternately in the same way. 6. Finally, the black outlet plate is inserted. NOTE The filter layers should be aligned by hand in such a way that they are gripped on all sides by the pressing edge of the filter plates and protrude evenly by around 2mm beyond the sides of the filter plates (5). Start-up 7. Place the experimentation stand on a flat surface and secure against rolling. 8. Set the master switch(1) to the 0/Off position. 9. Connect the experimentation stand to the mains electricity supply. 10. Fill the suspension tank with approximately 15 L of water, i.e. the liquid level should be around 20 mm above the immersion pump. 11. Fully open the stop valve on the bypass (3). 12. Close the diaphragm valve at the filter in feed pipe (2). 13. Switch on the unit at the master switch (1). 14. Switch on the pump. 15. Scoop out about 1 jug of diatomite (using 1000mL jug) and add to the suspension tank. NOTE During all experiments, always continue agitating the suspension in the suspension tank until it has been used up. 16. Connect a hose to the drain fittings on the collecting tray below the filter plates and attach it in such a way that any leaked suspension is fed back in to the suspension tank. Open the stop valve (4).

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17. Close the stop valve at the measuring tank outlet (5). 18. Create the suspension.

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NOTE While preparing the plate and frame filter press to perform the experiment, the suspension can be conveyed in a circuit to keep the solid particles in a state of suspension in the liquid. Before inserting, check filter layers for damage, then place the filter layers and plates onto the guide bars in turn. Make sure that the filter layers and plates are inserted in the correct order. The suspension flow can be varied by changing the setting of the stop valve on the bypass and using the diaphragm valve. Performing the experiment. 19. Slightly open the stop valve on the bypass. 20. Fully open the diaphragm valve at the filter in feed pipe. 21. Measure the filter inlet pressure. Read the filter inlet pressure on the pressure gauge immediately after starting the pump and note it. 22. Measure the time required by using stopwatch for the volume of water in the measuring cylinder to rise from 0 to 20 L. Note the elapsed time, for example at 5 L intervals, V = V/t. 23. At the end of experiment, measure the weight of the filter cartridge loaded with solid particles and liquid. RESULT Volumetric flow (L) 2 4 6 8 10 12 14 16 18 20 Inlet pressure (bar) Time (s)

Filter weights taken without solid particles = Filter weights taken with solid particles =

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Discussion

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1. Plot the graph of filtrate volume versus filtration time and filtrate inlet pressure versus filtration time. 2. Discuss the correlation of filtrate volume and filtrate inlet pressure with time. 3. Shortly describe the application of plate and filter press in industry.

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EXPERIMENT 10: PRESSURE SWING ADSORPTION (Adsorption of O2 from gas stream for single column) OBJECTIVE

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1. To adsorp O2 from a gas stream using an adsorber filled with sample carbon molecular sieve. 2. To plot the breakthrough curves using adsorption data.

INTRODUCTION Gas adsorption is a process in which one or more components from a gas stream are adsorbed on the surface of a solid. Separation is accomplished because differences in molecular weight, shape, or polarity give rise to some molecules being held more strongly on the surface than others or because the pores are too small to admit the larger molecules.

The solid that take up the gas is called the adsorbent, and the gas taken up on the surface is called the adsorbate. Many adsorbents are highly porous materials, and adsorption takes place mainly on the walls of the pores or at specific sites inside the particle. In most applications, the adsorbing component (or adsorbate) is held strongly enough to permit complete removal of that component from the fluid with very little adsorption of other components. Regeneration of the adsorbent can then be carried out to obtain the adsorbate in nearly pure form.

In this experiment, the Pressure Swing Adsorption (PSA) technology is used to separate some gas species from a mixture of gases under pressure according to the species' molecular characteristics and affinity for an adsorbent material. It operates at near-ambient temperatures and so differs from cryogenic distillation techniques of gas separation. Special adsorptive materials (e.g.carbon molecular sieve) are used as asborbent, preferentially adsorbing the target gas species at high pressure. The process then swings to low pressure to desorb the adsorbent material.

Breakthrough Curve

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A plot of the outlet concentration with respect to time is called the breakthrough curve as shown in Figure 1.

Figure 1: Breakthrough curve

The S-shaped mass transfer region moves along the bed with time as the fluid continues to flow. At times t1, t2 and t3, the exit concentration is practically zero. It remains zero until the mass transfer zone starts to reach the end of the bed at a time before t4. Then, the outlet concentration starts to rise until it reaches some limiting permissible value, or break point. The break point concentration, cb, represents the maximum allowable concentration of the outlet fluid, and is often taken as a relative concentration, c/c0of between 0.01 to 0.05. After the break point is reached, the relative concentration rises very rapidly until time t*, then more slowly approaching cd, which is the end of the breakthrough curve where the adsorption bed is considered ineffective. The value for cd is usually equal to the feed concentration, c0. It can be shown that the area between the curve and the c/c0 line at 1.0 is proportional to the total solute adsorbed if the entire bed reaches equilibrium with the feed. The ideal adsorption time for a vertical breakthrough curve is taken at time t*, in which the rectangular area to the left of t* is proportional to the amount adsorbed. For a symmetrical curve, t* is the time when c/c0 reaches 0.5.

EQUIPMENT/APPARATUS/MATERIAL 1. SOLTEQ Pressure Swing Adsorption Unit (Model: BP202A)

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2. Carbon Molecular Sieve 3. Nitrogen Gas 4. Air

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EXPERIMENTAL PROCEDURES 1. Check that all tubings are properly connected. 2. Ensure that V1 and V2 are closed. 3. Fill the column with the required adsorbent. 4. Turn on the power. 5. Ensure that the columns are regenerated prior to running any experiment by following all the steps below: a) Depending on which column to use, set valves to the following positions: Valve V1 V2 SV1 SV2 SV3 SV4 K1 desorption Closed Opened OFF OFF ON OFF K2 desorption Closed Opened ON ON ON ON

b) Supply N2 gas to the pipeline c) Open and adjust pressure regulator to 2.0 bar. d) Open valve V2 and adjust flowmeter for OT2 at 0.5LPM. e) Turn off the N2 supply when OT2 analyser shown 0%. 6. Now, the unit is ready for experiment. 7. Unplug N2 gas supply and plug in compress air where adjust the pressure regulator to 0 bar (anticlockwise). 8. Record the result by using DAS (Data Acquisition Software) and turn on the pressure regulator (clockwise) until 2 bars to start the experiment. 9. Continue collecting samples until the oxygen sensor reading are constant. 10. Repeat step 1 to 13 by using different flowrate and pressure. NOTE: Make sure that the column has been regenerated before use. GENERAL SHUT-DOWN PROCEDURES 1. Switch off the vacuum pump or compressor. 2. Turn off the power for the control panel.

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3. Close all valves for the gas supply lines.

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RESULT Pressure (bars) Flowarate (L/min) Time (s) Inlet concentration of Oxygen, c 2 30 5 10 15 Outlet concentration of Oxygen, c

40

5 10 15

30

5 10 15

40

5 10 15

DISCUSSION: 1. Determine the adsorption efficiency of oxygen. 2. Discuss the effect of pressure and flow rate on the adsorption efficiency of oxygen. 3. Plot and discuss the breakthrough curves using adsorption data.

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4. Shortly describe about the adsorption time. SOLTEQPRESSURE SWING ADSORPTION (Model: BP 202A)

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Figure 4: Process flow diagram for the pressure swing adsorption BP202A unit

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FORMULAS 1. Molarity = Mole / Liter = (Specific Gravity x Purity x 1000mg/L) / Molecular Weight 2. Mole = Mass / Molecular Weight 3. M1V1 = M2V2 M1,M2 = Molarity; V1,V2 = Volume

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