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Distillation Distillation Pre-Lab Plan Unit Operations Lab # 5 Date 10/31/2023 Group 1, Tuesday, 1PM section Angelo Giles Emmanuel Risasi Kevin Malec Zuhai Wang Unit Operations ChE-381 Group No. 1 p. 1 Fall 2023 10/31/2023

Distillation 1. Experimental Objective (5 pts) In this experiment, a 10 wt% ethanol-water solution is separated through binary distillation to observe how the reflux ratio and reboiler temperature influences the quality of both the bottom and distillate streams. This quality is determined by the compositions of each stream. Experiment A will vary the reboiler temperatures while keeping the reflux ratio constant to determine how each boil-up rate influences the column efficiency. For Experiment B, the reboiler temperature will be kept constant while varying the reflux ratio of the column to a constant value to change the distillate and bottom stream compositions. Additionally, the McCabe-Thiele method will be used to determine the equilibrium at each stage of the column. 2. Experimental 2.1 Apparatus (5 pts) The Armfield Distillation Unit consists of a distillation column, a reboiler, condenser, top and bottom collection tanks, a vacuum pump, and associated valves, piping, and thermocouples (figures 1 and 2). The column has nine stages, each with their own thermocouple. The material to be distilled can be placed in the feed tanks and then pumped to the column with a vacuum pump. There are valves to get samples of the top and bottom products as well as a manometer to measure differential pressure between the top and bottom of the column. The pump and heater are controlled by the circuit control unit (figure 3). The control unit supplies power and also displays temperatures sensed by the thermocouples. There is a computer with software used to log data (figure 4). Unit Operations ChE-381 Group No. 1 p. 2 Fall 2023 10/31/2023

Distillation Figure 1. Front view of Armfield Distillation Column Unit Operations ChE-381 Group No. 1 p. 3 Fall 2023 10/31/2023

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Distillation Figure 2. Side view of Armfield Distillation Column Unit Operations ChE-381 Group No. 1 p. 4 Fall 2023 10/31/2023

Distillation Figure 3. Armfield Circuit Interface Figure 4. Computer Table 1. Armfield Distillation Apparatus Components Unit Operations ChE-381 Group No. 1 p. 5 Fall 2023 10/31/2023

Distillation Number Component Description Unit Operations ChE-381 Group No. 1 p. 6 Fall 2023 10/31/2023

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Distillation 1 Distillation Column An eight stage distillation column connected to feed piping, a recoiler, and a condenser. 2 Temperature sensors T1 - T8 Thermocouples that sense temperature for each stage. 3 Reboiler A tank with an attached heater to reheat the bottoms to cause more product to evaporate. 4 Reboiler level sensor Senses the level in the reboiler 5 Bottom product receiver Holds the bottom product that comes from the reboiler 6 Heat exchanger Cools the bottom product before entering the bottom product receiver 7 V-11 Drain valve that drains the bottom product receiver 8 Vacuum pump Pumps liquid from the feed tanks to the distillation column 9 V-1 Valve that controls flow from reboiler to heat exchanger 10 Feed tanks Hold the liquid to be distilled 11 V-12 Valve that drains top product receiver to the reboiler 12 V-4 Top product sample valve 13 Top product receiver Holds the top product that comes from the decanter 14 Decanter Collects top product from the condenser. Sends top product to the top product receiver and reflux valve 15 V-10 Valve that controls flow going from decanter to reflux valve 16 Condenser Cools the top product with water so that it condenses into a liquid 17 T-12 Thermocouple that senses temperature of cooling water leaving the condenser Unit Operations ChE-381 Group No. 1 p. 7 Fall 2023 10/31/2023

Distillation 18 T-11 Thermocouple that senses temperature of cooling water going to the condenser 19 V-15 Valve that controls flow from the vacuum pump. 20 Cooling water flow meter Shows the flow rate of cooling water going to the condenser 21 V-5 Valve that controls flow rate of cooling water 22 V-14 Valve that controls flow of cooling water leaving the system 23 V-7 Valve that controls flow from the top of column to the manometer 24 Manometer Measures differential pressure between the top and bottom of the column 25 V-8 Valve that controls flow from the bottom of column to the manometer 26 T-13 Thermocouple that senses temperature of the reflux 27 Reflux valve controls how much top product is returned to the column 28 T-10 Thermocouple that show temperature of top product leaving the column 29 Electric heater Heats the contents of the reboiler. Power is controlled by the circuit interface unit. 30 V-2 Reboiler sample valve 31 Armfield circuit interface Supplies power to the apparatus. Has controls for pump speed and heater power. Displays temperature data from the thermocouples 32 Computer Computer that has software for logging systems parameters and time. 2.2 Materials and Supplies (5 pts) Unit Operations ChE-381 Group No. 1 p. 8 Fall 2023 10/31/2023

Distillation Table 2. List of Materials Item Description Water Main component for the lab. It is distilled first in a binary mixture Stopwatch Used to record/measure the times required to collect a certain amount of condensate Graduated Cylinder Used to collect the condensate Heat resistant gloves Protect hands from the extremely hot apparatus or from any heat while collecting samples Monitor Displays all the necessary graphs to be analyzed, specifically, utilizing softwares to output a McCabe-Thiele graph Tape/Marker Used to label different test tubes/beakers/samples to make it easy to differentiate them apart Wattmeter Used to measure the power (electricity in kW) Armfield Console & Process Unit Provide experiment with power (electric) and they control the variables Test Tubes Used to collect the desired samples for whom we measure the densities once cooled down 200-Proof Ethanol It is in a binary mixture 2.3 Experimental Plan (10 pts) Pre-Procedure: 1. Ethanol will be found in a fume hood. Do not remove the ethanol from the fume hood. All solutions will be made there. 2. Make a 10 L, 10 wt% ethanol solution by diluting 1.27 L EtOH with DI water. 3. Fill the reboiler tank with the ethanol solution. 4. Completely open valve 10 for reflux. 5. Power up the control panel 6. Open valve 5 and set the cooling water flow rate to 3 Experiment A: 1. Set the reboiler power to 1.5 kW (the heating element light should be on). Unit Operations ChE-381 Group No. 1 p. 9 Fall 2023 10/31/2023

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Distillation 2. Open valve 6 and 7 to ensure the manometer reading is 0. Close both valves if this reading is 0. Request assistance from a TA/Instructor, otherwise. 3. As the reboiler heats up, vapor will begin to flow throughout the column, condense and reflux back into the column. Turn the reboiler power down to 0.75 kW once total reflux has been achieved in the column (bubbling has occurred on every stage of the column). 4. Wait until the column temperature has reached equilibrium (T1-T8 has stabilized). 5. To measure the boil-up rate, time the collection of condensate in the top section by partially opening valve 3. When the valve is open, the flow rate will be unsteady and is not the start of sample collection. Discard this initial condensate volume and start timing the sample once flow out of valve 3 has stabilized. 6. Using the installed manometer, record the pressure drop over the top and bottom section of the column by opening valve 6 then valve 7. Close both valves in the order they were opened. This is to prevent vapor from entering the manometer. 7. When collecting samples from the bottom section, use a heat resistant glove. Partially open valve 2 and collect 10mL of sample from the bottom section. When the valve is open, the flow rate will be unsteady and is not the start of sample collection. Discard this initial condensate volume and start timing the sample once flow out of valve 2 has stabilized. 8. Take 3 samples from both the top and bottom section of the column. Keep all samples upright. 9. Repeat steps 4-8 at reboiler powers of 1.00 kW, 1.25kW, and 1.5kW. 10. Measure the composition of each sample using the Snap 41 Densitometer (%v/v). Independent variables: Reboiler power. Dependent variables: Boil-up rate, composition of top and bottom products, pressure drop throughout the column, column efficiency, the temperature profile throughout the column, and foaming in each tray. Experiment B: 1. Use the remaining solution in the column from Experiment A. 2. Set the reboiler temperature to 0.75kW with total reflux. 3. Wait 15 minutes for the column to reach equilibrium and its tray temperatures to stabilize. Record T1-T8. 4. Vary the reflux ratio to 5:1 by setting 20 seconds back to the column and 4 seconds for distillate recovery. 5. To measure the boil-up rate, time the collection of condensate in the top section by partially opening valve 3. When the valve is open, the flow rate will be unsteady and is not the start of sample collection. Discard this initial condensate volume and start timing the sample once flow out of valve 3 has stabilized. 6. When collecting samples from the bottom section, use a heat resistant glove. Partially open valve 2 and to collect 10mL of sample from the bottom section. When the valve is open, the flow rate will be unsteady and is not the start of Unit Operations ChE-381 Group No. 1 p. 10 Fall 2023 10/31/2023

Distillation sample collection. Discard this initial condensate volume and start timing the sample once flow out of valve 2 has stabilized. 7. Take 5 more samples from both the top and bottom section of the column by repeating steps 1-6 every 10-15 minutes. Keep all samples upright and sealed. 8. Repeat steps 1-7 but varying the reflux ratio to 2:1 and 3:1. 9. Measure the composition of each sample using the Snap 41 Densitometer (%v/v). Independent Variables: Reflux ratio and reboiler power. Dependent Variables: sample composition and temperature profile throughout the column. Project Safety Evaluation (10 pts) Project Title: Distillation Date: __________________ 10/31/2023 ________________________________________________ Yes/No Potential electrical hazards? Yes If yes, identify conditions: Stay water away from the computer and wires. Potential mechanical hazards? Yes If yes, identify conditions: The computer program and the UOP3CC distillation column might stop running. Potential pressure hazards? Yes If yes, identify conditions: The pump is running dry. Potential temperature hazards? Yes If yes, identify conditions: The heater, reboiler, and heat exchanger might get hot. Hazardous/toxic chemicals involved? Yes If yes, hazards involved: Ethanol. Causes severe eye irritation. Flammable liquid and vapor. Causes respiratory tract irritation. May cause central nervous system depression. Gloves required? Yes If yes, specify type: Heat resisting gloves. MSDS reviewed by all team members? Yes List MSDS sheets reviewed: DI Water [CAS# 7732-18-5] Ethanol [CAS# 64-17-5] Process Parameters Max Expecte d List location and possible hazards and precautions Temperature (ºC) 100 Minimize contact with heat, use heat resistant gloves and stop using it for a while. Pressure (psia) 14.7 Turn off the pump to lower the pressure. Unit Operations ChE-381 Group No. 1 p. 11 Fall 2023 10/31/2023

Distillation Safety Controls yes/no If yes, Provide description Yes Turn off all power for the main circuits. I have read relevant background material for the Unit Operations Laboratory entitled: “___________Fluid flow in pipes______________________________________________” and understand the hazards associated with conducting this experiment. I have planned out my experimental work in accordance to standards and acceptable safety practices and will conduct all of my experimental work in a careful and safe manner. I will also be aware of my surroundings, my group members, and other lab students, and will look out for their safety as well. Angelo Giles 10/31/2023 signature of team member date Emmanuel Risasi 10/31/2023 signature of team member date Kevin Malec 10/31/2023 signature of team member date Zuhai Wang 10/31/2023 signature of team member date Unit Operations ChE-381 Group No. 1 p. 12 Fall 2023 10/31/2023

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