1.

INTRODUCTION

The purpose of the “Distillation In A Plate Column” experiment is to analyze and apply the fundamental concepts of continuous column distillation by distilling a mixture of water and ethanol both at total reflux and finite reflux. To satisfy this purpose, the determination of the number of ideal stages and the plate efficiency for distillation of the mixture in the plate distillation column working at total reflux and finite reflux is conducted in this experiment [1]. Simply, distillation is one of the most common method for separation of the mixtures based on differences in the conditions required to change the phase of components of the mixture. In the distillation process, the liquid mixture which have different boiling point is heated to bring the components into gas phase. Then, the formed gas phase is condensed back into liquid form and accumulated to satisfy the separation process.The production of gasoline, distilled water, alcohol, xylene, kerosene, paraffin are such commercial processes which distillation process occurs [2]. Two types of distillation can be considered as important concepts of this issue. These are continuous distillation and batch distillation. If a mixture continuously fed into the process with no interruption and the separated fractions are removed continuously as output, then this type of distillation is called as continuous distillation. On the other hand, in the batch distillation, the mixture is added to the process unit at the beginning of the distillation and the separated fractions are removed sequentially in time during the distillation and also the remaining bottom fractions are taken out at the end. In this experiment continuous distillation model is handled. Moreover, the simply illustration of the process between the two trays is like in the Figure 1.1.

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While conducting the experiment total reflux and finite reflux is the main parameters. in the finite reflux ratio a higher number of theoretical stages could be obtained than total flux situation. In addition. in this situation. 2 . Moreover. Thus. so the number of theoretical stages can be obtained as minimum number [4]. All the overhead vapor is condensed and returned as reflux. total reflux condition is valid when the nearly no product removal occurs. Therefore.Figure 1. L/D ratio (reflux ratio) is infinite. it makes the operating lines the 450 line. As an information. the operating lines are as far as they can get from the equilibrium curve.1: Simple representation of distillation in a plate column [3].

EXPERIMENTAL PROCEDURES In this experiment continuous distillation column used to distillate ethyl alcohol -water binary mixture at total reflux and finite reflux.1. pump and flowmeter and there are 6 thermometers which read temperature of different parts of the system. Mixture is pumped until starts to passing to tank 3 . reboiler. Figure 2.1: Experimental setup In the first part of the experiment distillation with total reflux condition is examined. valves V1. The setup consists of a sieve tray column with seven trays. V2. V4 and V6 are closed and V3 and V5 opened in order to reboiler E1 to be filled with mixture. Sketch of the distillation unit is drawn using Edraw Max with measurements of important parts shown below Figure 2. cooling system. After the power supplied.2.

D3. E2 the cooling unit fills totally and flow rate adjust as 200 l/h.Distillation ended with switch off J1 heater. After observing the no-change of previous temperature values and initial ones it is understood that system reach steady state and samples are taken from bottom and distillate. 4 . Samples are analyzed by refractometer by using refractive index of mixtures ethyl alcohol and water. S1selonoid valve and pump G1. System reached steady state solenoid valve S1 opened on switchboard and pump flow rate settled at 50%. In the second part of the experiment the same procedure is followed until reaching the steady state. Every 5 minutes temperatures are recorded and compared previous values of each thermometer. Therefore weight fraction of bottom and distillate composition is determined by using refractive indexes. Then again samples are taken from bottom and distillate. When vapor condensed in cooling unit start refluxed into the column. then heater is switched of. Reflux ratio adjusted 5:1 on switchboard.

L/V becomes 1 and operating line of enriching and stripping section is 45 0 line [5].0709 0.1.9291 0. Table 3. Number of Ideal Stages at Total Reflux To fix the operating lines.69 Figure 3.1: Refractive indices and compositions of ethanol-water in total reflux [6].1. At total reflux. RESULTS 3.1: Number of stages at total reflux 5 .1.1.85 Mole fraction of ethanol 0.1. Number of stages is determined from McCabe-Thiele Diagram as in Figure 3.3. which means reflux ratio is infinity.3370 1. Table 3. Refractive index Mass fraction of water Bottoms Distillate 1.1. One of the limiting values of reflux ratio is that of total reflux.15 Mass fraction of ethanol 0. reflux ratio (L/D) must be set.3640 0.1 shows mole fractions of bottoms and distillate which are found from refractive indices.029 0.

3640 1. number of ideal stages is determined by using McCabe-Thiele Method and it is shown in Figure 3. q is calculated as 1.3.85 0.3370 1.14. Calculations of slopes q-line and enriching section are shown in Appendix part of the report.3.83. 6 .7734 Mole fraction of ethanol 0. distillate and feed are determined by using refractive indices as done previously.0709 0.3.15 0. operating lines of stripping and enriching section and q-line must be determined. Number of Ideal Stages at Finite Reflux At finite reflux.69 0. Also. Refractive index Mass fraction of water Bottoms Distillate Feed 1.9291 0. slope of enriching section is found as 0. Plate Efficiency at Total Reflux From Figure 3. stripping section operating line is obtained by drawing a line from mole fraction of bottoms on 450 line to cross section of q-line and enriching section line. reflux ratio is set to 5 and compositions of bottoms.2266 Mass fraction of ethanol 0. After that.14 and slope of q-line is found as 8.1. it is seen that there is 2.1: Refractive indices and compositions of ethanol-water in finite reflux [6].1.3.3630 0.57 To obtain number of ideal stages.2. Table 3.029 0. 3.2 ideal stages and 1 reboiler at total reflux and efficiency is found as. When these operating lines are drawn into equilibrium curve and 450 line.1.

1. Plate Efficiency at Finite Reflux From Figure 3.3. efficiency is.4. it is obvious that there are 2. therefore.7 ideal stages and 1 partial reboiler.3.1: Number of stages at finite reflux 3.Figure 3. 7 .

The certain amount of liquid falls to the distillate storage instead of falling into the column when the mechanism is open. condenser duty and efficiency. Although the reflux ratio is set to 5 by using a mechanism closed for 5 seconds and open for 1 seconds. The column was not isolated. sensible heat differences between the stages are also assumed negligible throughout the calculations. therefore. The heat released by one mole of vapor condensation is approximately equal to the heat required to vaporize one mole of the liquid. The heat balance for the system was not made in this report. One of the assumption is adiabatic column condition and thermal capacitance of column material is negligible. This result show that efficiency increase with increasing reflux ratio. This assumption is valid for water and ethanol mixture. neither heat given by the heater of the reboiler nor the vapor flow rate are known. Besides.422 kj/kmol. if the reflux ratio is too high then condenser duty is very large. Therefore. The heat of vaporization of water is 40. Since. there is heat loss between the column and surroundings. However.4. Proven of equal latent heat assumption also proves equimolar counter-diffusion. DISCUSSIONS The main aim of the experiment is to determine the efficiency of the plate column separating water and ethanol by using McCabe-Thiele method. the heat of vaporizations are close enough to assume that they are equal. This problem is most likely overcome by both cooling jacket and cooling coil. Some assumptions are made to use McCabe-Thiele method. There is an optimum value for each distillation column between reflux ratio. the real reflux ratio is different. The efficiency values are not reliable.626 kj/kmol while the heat of vaporization of the ethanol is 39. It is also assumed that total condensation at the top of column. One of the important assumption is that latent heats are equal. 8 . This means the number of molecules passing from the vapor phase to the liquid phase and vice versa holds. Plate efficiency at total reflux is found as 0.39 when reflux ratio is equal to 5. Constant pressure is assumed throughout the column although there is certain pressure drop throughout the column.31 whereas it is found 0.

5. real reflux ratio is different. it is supposed to falling into column when mechanism open but some amount of liquid falls distillate storage. CONCLUSIONS In this experiment main aim is to examine continuous sieve tray distillation column at total reflux condition and finite reflux condition. When results analyzed it is observed efficiency increase with increasing reflux ratio. constant pressure throughout the column. Although reflux ratio settled. Several assumptions made for using McCabeThiele method. Also it is assumed that latent heats are equal so that equimolar counter-diffusion is proved. adiabatic column. total condensation at the top column. 9 .

National Institute of Standards and Technology.J.L.Experiment 25 “Distillation In A Plate Column” laboratory manual.edu/rprice/lectures/distill4.tr/~tezsevin/ChE420/Manuals.com/cs/5/f/bldistillation. [7].Troy A.ncl.McCabe...gov/chemistry 10 . Retrieved May 4 th 2013 from http://www. 7th ed. Illinois. Smith J.about.6. Retrieved May 4 th 2013 from http://lorien.metu.nist.Distillation IV: Calculations. 4th ed..uk/ming/distil/distilint. [6]. Retrieved May 4 th 2013 from http://www. Refractive Index of Ethanol-Water Mixtures and Density and Refractive Index of Ethanol-Water-Ethyl Ether Mixtures. Retrieved May 4 th 2013 from http://facstaff.Distillation an introduction column internals.S. Harriot P.1946. W.html [5]..htm [4].ac. Unit Operations of Chemical Engineering. Massachusetts: Pearson Education Inc.C.What is distillation? Retrieved May 4th 2013 from http://chemistry. Peoria.Geankoplis C.REFERENCES [1]. New York: McGraw Hill [8]. (2005). Northern Regional Research Laboratory.htm [2]. (2003) Transport Processes and Separation Process Principles.htm [3].edu.cbu.

9 0.1 0.794 0.37 0.2 78.959 0.912 0. mole fractions are needed for diagrams.49 0.04 0.2 91.9 0.95 1 11 .942 0.377 0.1.7 0.64 0.6 0.7 83.085 0.53 0. Data is available for mass fraction of ethanol.746 0. mwA is molecular weight of ethanol.61 0. Equilibrium Data for Ethanol-Water System Equilibrium data for ethanol-water system is shown in Table A.7 0.78 0.1 78.98 1 y(mass fraction) 0 0.1 79. Table A.86 0.1 78. Therefore.8 0.3 78. T 100 98.48 0.3 84.9 0.978 1 x(mole fraction) 0 0.656 0.1 95.4 0.192 0.7.2 82 81 80.19 0.09 0. Where.43 0.96 0.008 0.86 0. however.771 0.3 0.8 87.02 0.8 0.527 0. mwB is molecular weight of water.858 0.6 0.3 0.3 x(mass fraction) 0 0. APPENDIX A.2 78. wB is weight of water for 100 kg mixture. wA is weight of ethanol for 100 kg mixture.5 0.94 0.1: Equilibrium data for Ethanol-Water Mixture [5].14 0.05 0.2 0.2 0. mass fractions are converted to mole fractions by using the following equation.822 0.57 0.95 1 y(mole fraction) 0 0.28 0.713 0.02 0.

2 0.6 0.1 0.4 0.7 0.5 0.8 0.8 0.2 0.1: Equilibrium curve for ethanol-water Boiling Point Diagram for Ethanol-Water 120 110 100 Temperature.5 0.y Figure A.mole fraction of ethanol in liquid phase Figure A.x or vapor.1 0 0 0.7 0.6 0.T(C) 90 80 70 60 50 40 30 20 10 0 0 0.2: Boiling Point diagram for ethanol-water 12 .1 0.9 1 x.5 0.3 0. mole fraction of ethanol in vapor phase 1 0.1.4 0.2.3 0. equilibrium curve for ethanol-water is drawn as shown in Figure A. Ethanol-Water Equilibrium y.2 0.3 0.4 0.7 0.8 0.6 0.1 and boiling point diagram is plotted as in Figure A.By using data in Table A.9 1 mole fraction of ethanol in liquid.9 0.

9291 0. refractive indices are used [6]. Refractive index Mass fraction of water Bottoms Distillate Feed 1.9291 0.69 0.3630 0. Table B.2: Refractive indices and compositions of ethanol-water in finite reflux [6].0709 0. 13 . distillate and feed.15 Mass fraction of ethanol 0. which is defined as [5]. Refractive index Mass fraction of water Bottoms Distillate 1.3640 1.15 0.2266 Mass fraction of ethanol 0.85 Mole fraction of ethanol 0. then they are converted to mole fraction by using Equation A.57 C.3640 0.7734 Mole fraction of ethanol 0.3370 1.B. Equation C.69 Table B.029 0. Refractive Index of Ethanol-Water Mixture To find compositions of bottom product.1 is also written in terms of enthalpies.0709 0.1. Calculation of Slope of q-line Condition of feed is represented by the quantity q. Compositions are found as mass fraction.1: Refractive indices and compositions of ethanol-water in total reflux [6].029 0.3370 1.85 0.

is heat capacity of liquid.44 2260 855 Boiling point of feed is determined from Figure A. Also. To find the value of q. feed is at room temperature which is 250C. heat capacities and heat of vaporization values of components are obtained as seen from Table C.K) Latent heat of vaporization.2 for mole fraction of 0. λ (kJ/kg) Water Ethanol 100 78. λ is heat of vaporization. Table C. feed temperature is 250C which means feed is cold liquid since water has normal boiling point of 1000C and ethanol has normal boiling point of 78. is temperature of feed. is boiling point of feed.In the experiment. Component Boiling point (°C) Heat capacity Cp (kJ/kg. q formula for cold liquid feed is [7].57 and it is obtained as 820C. Where. 14 .1.1: Properties of water and ethanol [8].187 2.3 4.30C.

D. slope of q-line is. 15 .3. During the experiment. Therefore. slope of enriching section is. Therefore. Calculation of Slope of Enriching Section Operation line of enriching section is defined as [5]. reflux is set to 5:1. q-line equation is.Substituting these values into Equation C.

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