Experiment 300: Distillation Sub-Team # 4 Team Leader: Adirene Castro Safety Officer: Annette deKloet Operator: Carlos Cardoso (Procedure) Operator: Robert St. John (Chemcad)

Objectives GC Calibration Pump Calibrations Reach Steady-State Comparison (Chemcad and McCabe Thiele)

Overview Background Safety Plan of Investigation Data and Results Discussion Recommendation Answer questions

Background Process Flow Diagram

Background (cont’d) Distillation Experiment Simple distillation. Ethanol n-Propanol Requirements 1. Second phase be formed 2. Different volatilities 3. Ability to separate phases

Background (cont’d) Material Balance at Steady-State Equilibrium Line Equation Number of Theoretical Stages

Safety Hard Hats, Gloves and eye protection Equipment valves Tank Levels Heating elements Ethanol and n-propanol

Plan of Investigation Pump Calibrations GC Calibration Achieving Steady-State

Gas Chromatograph Calibration

Pump Calibrations

Reflux Ratio

Steady-State Approach

Steady-State Approach

At Steady-State xD xB 4:37 pm Day 3 0.506 1.02 2.65 0.732 0.417 Time Reflux Flow Rate (mol/min) Distillate Flow Rate (mol/min) Bottoms Flow Rate (mol/min) xD xB 4:37 pm Day 3 0.506 1.02 2.65 0.732 0.417 Material Balance 3.5* 0.51 - 1.02 *0.7324 – 2.65*0.417 = -0.067 mol/min

Chemcad Distillate Flow Rate (mol/min) Bottom Flow Rate (mol/min) Distillate Composition (xE) Bottoms Composition (xE) 0.95 2.55 0.73 0.44

McCabe-Thiele

Discussion Nmin = 4 Nt = 3 Efficiency = 33.3 % xD,Chem= 0.73 whereas xD,Ex= 0.732 %Error = 0.27% xB,Chem= 0.44 whereas xB,Ex= 0.417 %Error = 5.2%

Conclusions Feed and Reflux Ratio Effectively Maintained Composition Fairly Constant. Did not vary more than 8% Temperature Fairly Constant Steady-State

Recommendations Do not trust rotameters Get a new air cooling heat exchanger Improve Data Collection Sheet, Procedure, Flow Diagram

References Henley, Ernest J., and J. D. Seader. Separation Process Principles. New York: John Wiley and Sons, Inc., 1998. Unit Operations Super Team, Fall 2002 Distillation Experiment. FAMU-FSU College of Engineering, 2002.

Ackowledgements Dr Loren B. Schreiber Rama Sista Mark Lescher The Audience Everyone Who Believed in Us

Questions?