1.

0: OBJECTIVES
Experiment 9: Batch distillation (structure packing) at total reflux To study the effect of liquid and vapor loading on the height equivalent theoretical plates (HETP). To determine HETP at total reflux in batch distillation column.

Experiment 10: Batch distillation (structure packing) at constant reflux Students are required to study the change of top and bottom composition sample over time in batch distillation at constant reflux. To determine height equivalent theoretical plates (HETP) in constant reflux batch distillation column.

2.0: INTRODUCTION
Batch distillation is one of distillation process types. In batch distillation a fixed amount of charge is added to the still to separate into its component and then repeated. This is in contrast with continuous distillation; the other type of distillation where it is an ongoing separation in which a mixture is continuously fed into the process and separated fractions are removed without interruption as output streams. Top product composition varies with time. It depends on bottom product composition, number of trays and reflux ratio. There is no steady state as long as compositions are changing with time. At start, top product; distillate (D) is rich in more volatile component since it is easier to vaporize and going up the column. After a few time, more volatile component become lesser at distillate (D). A batch column is like the top half of a continuous column where it has a rectifying section only. Batch distillation is preferred method for separation when feed quantities are small and composition varies widely with time. It is hard to observe when the process is handling through continuous distillation since its product withdrawn continuously as the feedstock. Others, batch distillation is used while high purity streams are required for curtain product such in the pharmaceutical industry and in wastewater treatment units, and when the process requires frequent cleaning which would interrupt continuous processing.

The simplest and most frequently used batch distillation configuration is the batch rectifier, including the alembic and pot still. The batch rectifier consists of reboiler, rectifying column, a condenser, some means of splitting off a portion of the condensed vapor (distillate product); reflux drum, and receivers. The reboiler is filled initially with liquid mixture and heated to vaporize the solution. The fast-moving atom will escape as vapour and flows upwards in the rectifying column and condenses at the condenser. After passing through the condenser, some of the condensate either is forcing back to the column as reflux or flows down as top product (distillate) and collected at its receivers. Returning back the portion of condensate will provide intimate contact between vapour and liquid to improve the separation process. As the supply of the material is limited and lighter components are removed, the relative fraction of heavier components will increase and the refractive index will decrease as the distillation progresses.

Figure 2.1: Diagram of Batch Rectifier

The other simple batch distillation configuration is the batch stripper. The batch stripper has same parts as the batch rectifier but only the charge pot is located above the column. During operation (after charging the pot and starting up the system) the high boiling constituents are primarily separated from the charge mixture. The liquid in the pot is depleted in the high boiling constituents, and enriched in low boiling ones. The high boiling product is drawn into the bottom product receivers. The residual low boiling product is withdrawn from the charge pot. However, batch stripping process seldom practiced in industry.

Figure 2.2: Diagram of Batch stripper Reflux is the liquid condensed from the rising vapor which returns to the pot flask. The Reflux ratio is the ratio between the boil up rate and the take-off rate. Or in other words, it is the ratio between the amount of reflux that goes back down the distillation column and the amount of reflux that is collected in the receiver (distillate). If 5 parts of the reflux go back down the distillation column and 1 part is collected as distillate then the reflux ratio is 5:1. In the case where all the reflux is collected as distillate the reflux ratio would be 0:1. If no distillate is collected then a reflux ratio is not assigned. Instead we call this "total reflux" or equilibration.
3

The higher the reflux ratio, the more vapor and liquid contact can occur in the distillation column. So higher reflux ratios usually mean higher purity of the distillate. It also means that the collection rate for the distillate will be slower. Reflux ratio is dependent for the overall efficiency of batch distillation column. An increase in the reflux ratio will cause the overall efficiency to drop. A better overall efficiency is obtained thus the number of stages will increase if reflux ratio is smaller. Furthermore, different reflux ratio will give a different operating line in graphical method.

The remainder of the report provides detailed analysis of the Theory and Working Equations for the experiment. The experimental procedure is outlined in Material and Methods section. Presentation of the findings and detailed discussion of the results can be found in Results and Discussion section. Finally, summary of the report and recommendations are included in Conclusion and Recommendation section.

3.0: THEORY AND WORKING EQUATIONS Distillation is a common process in engineering, basically used to separate various components of a liquid solution which depends upon the distribution of these components between a vapour phase and a liquid phase, as stated by Christie John Geankoplis, in his book, Transport Process and Separation Process Principles. He also stated that, all

components must be present in both phases, and the vapour phase is created from the liquid phase by vaporization at the boiling point. Taking the principles from the stated book, the author also stated that, the basic requirements for the separation of components by distillation is that the composition of the vapour be different from the composition of the liquid with which it is in equilibrium at the boiling point of the liquid. It is concerned with solutions where all components are appreciably volatile- such as ethanol-water solutions. Advancement in technology has created many types of distillation process, but in this experiment, the method used is batch distillation. Two types of batch distillation tested are batch distillation with total reflux, and batch distillation with constant reflux. First of all, in batch distillation, solutions are heated in the fractionating tower until the boiling point is reached, then the evaporating vapour will be condensed and the product is collected as the distillate. So, theoretically the distillate should contain more of the more volatile component, which is Ethanol, where the bottom product will contain more of the less volatile component, which is water. In the book, Geankoplis wrote that in actual practice, total reflux can be defined or realized by returning all the overhead condensed vapour from the top of the tower back to the tower as reflux. Also, the liquid in the bottom is reboiled. This means, all the products distillate and bottoms are reduced to zero flows, as is the fresh feed to the tower. In the constant reflux case, a reflux ratio of the distillation process is chosen, which actually mirrors the ratio of which the vaporised liquid is recycled back into the tower and flows into the distillate. Technically, reflux ratio of 3 means that for 30 seconds of vaporised liquid flows back into the tower, 10 seconds of it goes into the distillate. Stage distillation with reflux is also known as rectification. In tray towers, a theoretical tray is defined as tray in which equilibrium is attained between the gas or vapour leaving and the liquid leaving the tray. HETP in m (ft) is defined as the height of the packed column necessary to a give a separation equal to one theoretical plate. The design of mass transfer towers requires evaluation of the number of theoretical

stages or transfer units. Hence, the height of packing H in m (ft) required to perform a given separation is; Height of packing, H = 1m

The equation of the operating line for enriching section: Reflux ratio = 3 At t=0,

The Rayleigh Equation is useful in the analysis of simple distillation, as it shows how the concentration and quantity are related. As the process is unsteady state in nature, the derivation is based on a differential approach to changes in concentration with time. The equation to be derived (known as the Rayleigh Equation) shows the relationship between total moles remaining in the still and the mole fraction of the more volatile component in the still. (Source: http://www.separationprocesses.com/Distillation/DT_Chp02a.htm) Rayleigh equation: In L1-In L2 = L1 = initial moles of liquid originally in still L2 = final moles of liquid remained in still x1 = initial liquid composition in still (mole fraction of ethanol) x2 = final liquid composition in still (mole fraction of ethanol) y= initial composition of ethanol in the vapour

4.0: MATERIALS & METHODS Experiment 9: 1. A set of water-ethanol mixture within a specific range (0% to 100%) is prepared. 6 readings of refractive index (RI) were obtained from 6 different concentration of water-ethanol mixture. A graph is generated based on the data. 2. The initial volume and refractive index of the liquid mixture in the reboiler is recorded and heater power is set to 1.5kW. 3. The temperature of reboiler is set at 85oC. The reflux control is ensured at total reflux positioned. 4. When the readings reached were stable, the top column temperature is recorded. The sample distillate and bottom product is collected. 5. The refractive index is measured and the value is recorded into table. (Note : the sample should not be discarded as it is used to perform material balance at the end of the experiment). Step 4 and 5 is repeated to different heating power such as 2.0, 2.5, 3.0 and 3.5 KW. 6. The theoretical number of plates for each sampling time is determined by using McCabe-Thiele method and HETP is calculated. The graph of HETP versus heating power and distillate flow rate versus heating power is plotted and the relationship is observed.

Experiment 10: 1. A set of water-ethanol mixture within a specific range (0% to 100%) is prepared. 6 readings of refractive index (RI) were obtained from 6 different concentrations of water-ethanol mixture. A graph is generated based on the data. 2. The initial volume and refractive index of the liquid mixture in the reboiler is recorded and heater power is set to 3.5kW. 3. The reflux ratio is 3 ( reflux timer is set to 30 second for set 1 and 10 second for set 2) and the reflux control is set to timer controller reflux. 4. When steady state is reached, the top column temperature is recorded. The sample distillate and bottom product is collected. 5. The refractive index is measured and the value is recorded into table. (Note : the sample should not be discarded as it is used to perform material balance at the end of the experiment). Step 4 and 5 is repeated for 60 minutes.

6. The theoretical number of plates for each sampling time is determined using McCabe-Thiele method and HETP is calculated. The amount of ethanol left in the evaporator is calculated and plotted against time using the Rayleigh equation.

5.0: RESULT AND DISCUSSION Experiment 9: Batch Distillation (Structure Packing) At Total Reflux Volume of ethanol Volume of water ethanol mol refractive index, (ml) (ml) fraction RI 0 10 0.0000 1.34418 2 8 0.0717 1.35237 4 6 0.1709 1.36317 6 4 0.3168 1.36818 8 2 0.5528 1.36989 10 0 1.0000 1.36718 Table 5.1: Data for refractive index and ethanol mol fraction for a set of mixtures containing ethanol and water In experiment 9, we are required to study the effect of liquid and vapor loading on the height equivalent theoretical plates (HETP) and to determine HETP at total reflux in batch distillation column. Total reflux is a condition which exists when the reflux valve is totally closed and all the condensed liquid is being returned down the column. First of all, the refractive index of 6 samples with different volume of ethanol and water is taken to determine the compositions of distillate product, XD and bottom product, Xw.

Graph Of Refractive Index (RI) Vs Ethanol Mol Fraction

1.375 1.37 refractive index (RI) 1.365 1.36 1.355 1.35 1.345 1.34 0.0000

0.1000

0.2000

0.3000

0.4000

0.5000

0.6000

0.7000

0.8000

0.9000

1.0000

Ethanol mol fraction

Figure 5.1: Graph of refractive index (RI) verses ethanol mol fraction for a set of mixtures containing ethanol and water

Distillate product Bottom product Mole Mole Heating fraction fraction Power HETP Refractive of Flow Refractive of (kW) Temperature Index ethanol Rate Temperature Index ethanol o o ( C) (RI) (xD) (ml/min) ( C) (RI) (xW) 1.5 75.3 1.36498 0.200 17.43 90.1 1.35453 0.088 1.518 1.36679 2.0 87.3 0.206 53.17 90.5 1.35324 0.076 1.392 1.36788 2.5 87.6 0.248 75.00 91.3 1.35213 0.065 1.137 1.36818 3.0 87.7 0.303 85.71 91.7 1.35220 0.063 1.075 1.36934 3.5 93.5 0.381 101.41 91.9 1.34910 0.040 0.767 Table 5.2: Data for distillate and bottom product for the selection of different set of heater power

5 sets of heating power (1.5kW, 2.0kW, 2.5kW, 3.0kW, and 3.5kw) are used in this experiment and data obtained is tabulated in Table 5.2. Graph of refractive index (RI) versus ethanol mole fraction is plotted as above as Figure 5.1. The compositions of distillate product, XD and bottom product, XW can be calculated from this graph by using molecular weight and density. Figure 5.1 shows that when the composition of ethanol in the mixture increases, the refractive index increases. This is caused by the density of the mixture. Since the refractive index is inversely proportional to the overall density of the mixture, when the composition of ethanol increases, the overall density of the ethanol decreases and thus the refractive index increases. From Table 5.2, it is shown that when the heating power increases, the distillate product, XD increases while the bottom product, XW decreases. Besides, the value of distillate product is always greater than the bottom product disregard of the heating power. Since ethanol is a volatile component, the concentration of ethanol is increased in the vapor from each stage going upward but increased in the liquid from each stage going downward. HETP is defined as the height of the packed column necessary to give a separation equal to one theoretical plate. The ethanol equilibrium data is plotted as in Figure B-1, B-2, B-3, B-4 and B-5 in appendix A. Then, the theoretical plates can be determined from the graph by using the Mc-Cabe Thiele method. From the graph, the number of theoretical plates for different heating power is 0.6588 (at 1.5kW), 0.7182 (at 2.0kW), 0.8798 (at 2.5kW), 0.9302 (at 3.0kW), and 1.303 (at 3.5kW). Thus it can be said that the number of theoretical plates

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increases with greater value of heating power. Finally, the value of HETP can be calculated from the number of theoretical plates as in appendix A.

Graph Of HETP Vs Heating Power

1.6 1.4 1.2 1 0.8 0.6 0.4 0.2 0 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 heating power(kW)

HETP(m)

Figure 5.2: Graph of HETP vs heating power

Graph Of Distillate Flow Rate Vs Heating Power

Distillate flow rate(ml/min) 120.00 100.00 80.00 60.00 40.00 20.00 0.00 1.5 1.7 1.9 2.1 2.3 2.5 2.7 2.9 3.1 3.3 3.5 Heating power (kW)

Figure 5.3: Graph of distillate flow rate vs heating power From the graph of HETP versus heating power, it is shown that the value of HETP is decreases when the heating power increases. The value of HETP at heating power of 1.5kW, 2.0kW, 2.5kW, 3.0kW and 3.5 kW is found as 1.518, 1.392, 1.137, 1.075 and 0.767 respectively. While for the graph of Distillate Flow rate (mL/min) versus Heating power (kW), the distillate flow rate is directly proportional to the heating power. When the heating power increases, the distillate flow rate also increases.

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Experiment 10: Batch Distillation (Structure Packing) At Constant Reflux The second experiment that we have conducted is experiment 10. In this experiment, we are required to study the change of top and bottom composition sample over time in batch distillation at constant reflux (reflux ratio = 3) and to determine the height equivalent theoretical plates (HETP). Before conducting the batch distillation process, the refractive indices of a series ethanol-water mixture of different composition were measured by refractometer. Bottom product Mole Mole Time(min) Refractive fraction Refractive fraction Temperature Index of Temperature Index of o o ( C) (RI) ethanol ( C) (RI) ethanol 5.0 97.6 1.36263 0.159 92.1 1.35226 0.0658 10.0 97.7 1.36317 0.165 92.2 1.35214 0.0647 20.0 98 1.36527 0.224 92.2 1.35213 0.0646 30.0 98.1 1.36657 0.248 92.2 1.35209 0.0640 40.0 98.1 1.36731 0.256 92.2 1.35208 0.0639 50.0 98.1 1.36825 0.303 92.2 1.35206 0.0638 60.0 98.1 1.36827 0.305 92.2 1.35199 0.0629 Table 5.3: Data for distillate and bottom product for each sampling time The refractive index of distillate product and the bottom product can be read from Table 5.3. The sample is collected at every 10 minutes of a 60 minute operation process. For each mixture, their respective compositions of distillate and bottom product are calculated by using their molecular weight and density. All the details are listed in Table5.3 as time passed by, it can be seen that the top product become richer in ethanol while the bottom product has leaner ethanol. This is due to the lower boiling point of ethanol (78.3 C) than water (100C). Therefore, at each time interval, the mole fraction of ethanol is higher in the distillate product rather than in the bottom product. For example at time= 10min, the mole fraction of ethanol in the distillate product is 0.165 but only 0.0647 mole fraction of ethanol found in the bottom product. In appendix B, Figure B-6 to Figure B-12 shows the equilibrium diagram for system ethanol-water at different time interval for a 60 minute operating system. The number of theoretical plates is calculated by using McCabe-Thiele method. In order to use this method, one assumption is made which is there must be equimolar overflow through the tower between the feed inlet and the top tray and the feed inlet and the bottom tray. From the Distillate product

HETP

1.481 1.446 1.274 1.185 1.124 1.099 1.053

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experiment result, it is shown that the number of theoretical plates increases with time. For t=5 minutes to 60 minutes, the number of theoretical plates obtained is as following: 0.6754, 0.6917, 0.7852, 0.8440, 0.8893, 0.9095, and 0.9495 respectively.

Graph Of HETP Against Time

1.6 1.4 1.2 HETP(m) 1 0.8 0.6 0.4 0.2 0 0.0 10.0 20.0 30.0 40.0 50.0 60.0 70.0 Time(min)

Figure 5.4: Graph of HETP against time Figure 5.4 shows the HETP against time. The calculation of the value of HETP can be found in appendix B. Theoretically, the HETP is inversely proportional to the number of theoretical plates. The higher the number of theoretical plates results in lower value of HETP. From the graph, the HETP decreases when time passed by. This obeys the theory which mentions that when the total bed height considered constant, the higher the number of theoretical plates, the lower the value of HETP in order to fulfill the high number of theoretical plates needed. From this experiment, the highest value of HETP is 1.484m, which is at t= 5 min. Time(min) 5.0 10.0 20.0 30.0 40.0 50.0 60.0 Amount of ethanol left(litre) 3.6972 3.6861 3.6851 3.6791 3.6781 3.6771 3.6680

Table 5.4: Data for amount of ethanol left for each sampling time

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Graph Of Amount Of Ethanol Left In The Evaporator Against Time

Amount of ethanol left (litre) 3.7000 3.6950 3.6900 3.6850 3.6800 3.6750 3.6700 3.6650 0.0 10.0 20.0 30.0 40.0 50.0 60.0 70.0 Time(min)

Figure 5.5: Graph of amount of ethanol left in the evaporator against time

Figure 5.5 shows the amount of ethanol left in the evaporator against time. It can be seen that when time passed by, the amount of ethanol left in the evaporator decreases. The final volume of the ethanol is less than the initial volume of ethanol left in the evaporator. This is true since more ethanol is used as time goes by. In both experiment, the liquid-vapor is assumed to be in equilibrium state when leaving tray in ideal conditions. However, there is always insufficient time for the liquid and vapor to contact and mix. Therefore in actual condition, the equilibrium state for liquid-vapor always cannot be achieved. This results in reducing of actual mass transfer.

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6.0 : CONCLUSION AND RECOMMENDATION For experiment 9, the number of theoretical plates obtained for different heating power is 0.6588 (at 1.5kW), 0.7182 (at 2.0kW), 0.8798 (at 2.5kW), 0.9302 (at 3.0kW), and 1.303 (at 3.5kW). The higher the heating power, the higher the number of theoretical plates is needed to distil off ethanol. Besides, the value of HETP for heating power of 1.5kW, 2.0kW, 2.5kW, 3.0kW and 3.5 kW is found as 1.518, 1.392, 1.137, 1.075 and 0.767 respectively. This shows that when the heating power increases, the number of theoretical stages increases but the value of HETP will decrease. The distillate flow rate is directly proportional to heating power, which means that as heating power increases the distillate flow rate also increases. For experiment 10, the number of theoretical plates obtained for different time interval (each 10 minutes for a 60 minutes operating process) is 0.6754, 0.6917, 0.7852, 0.8440, 0.8893, 0.9095 and 0.9495 respectively. The number of theoretical plates obtained is very small, which is not more than 1 stage. Since the actual number of stages must be greater than 1 stage, this result deviates from the actual result. As time goes by, the value of HETP obtained is decreasing from 1.481m to 1.053m. There is some precaution steps are recommended for result improvement of the experiment. First of all, the start-up operation should be taken with care before the experiment begins. The drain valve and the sample taking valves should be closed before the stable condition of the operating condition is achieved. Besides, we should only start the experiment when the operating condition has reached 85C to ensure the ethanol boils and the mixture is at equilibrium condition. We should also be extra careful when the sample of bottom product is taken since the liquid is hot. Apart from that, human errors should also be avoided when the sample reading is taken. For example, the reading of the refractive index should be repeated at least three times to get the average reading in order to get a more accurate result.

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7.0: REFERENCES 1. Perry, R. H., and D. Green, Perrys Chemical Engineers Handbook, 6th edition, McGraw-Hill, 1988. 2. Christie John Geankoplis. Unit Operations: Transport Processes and Separation Process Principles, Fourth Edition, Pearson Education International, 2003. 3. Jaime Benitez. Principles and Modern Applications of Mass Transfer Operations, Second Edition, John Wiley & Sons Inc. 4. Sharma. Principles of Mass Transfer, PHI Learning Pvt. Ltd., 2007. 5. http://lorien.ncl.ac.uk/ming/distil/distil0.htm 6. http://academic.evergreen.edu/curricular/whatscookin 7. http://www.fpharm.uniba.sk/fileadmin/user_upload/english/Fyzika/Refractive_index. pdf 8. http://www.solvent--recycling.com/reflux.html 9. http://www.separationprocesses.com/Distillation/DT_Chp02a.htm

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Appendix A Experiment 9: Batch distillation (structure packing) at total reflux Volume of Volume of Mole of Mole of Ethanol mol ethanol (ml) water (ml) ethanol, ne water, nw fraction 0 10 0.0000 0.5541 0.0000 2 8 0.0343 0.4433 0.0717 4 6 0.0685 0.3324 0.1709 6 4 0.1028 0.2216 0.3168 8 2 0.1370 0.1108 0.5528 10 0 0.1713 0.0000 1.0000

Refractive index, RI 1.34418 1.35237 1.36317 1.36818 1.36989 1.36718

Table A-1: Data for refractive index and ethanol mol fraction for a set of mixtures containing ethanol and water

Mol fraction of ethanol in liquid, x Mol fraction of ethanol in vapor, y 0.0000 0.0000 0.0190 0.1700 0.0721 0.3891 0.0966 0.4375 0.1238 0.4704 0.1661 0.5089 0.2337 0.5445 0.2608 0.5580 0.3273 0.5826 0.3965 0.6122 0.5079 0.6564 0.5198 0.6599 0.5732 0.6841 0.6763 0.7385 0.7472 0.7815 0.8943 0.8943 1.0000 1.0000 Table A-2: Ethanol- water equilibrium data (Perry, R H.)

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Distillate product Mole Heating fraction Power Refractive of (kW) Temperature Index ethanol (oC) (RI) (xD) 1.5 75.3 1.36498 0.200 1.36679 2.0 87.3 0.206 1.36788 2.5 87.6 0.248 1.36818 3.0 87.7 0.303 1.36934 3.5 93.5 0.381

Bottom product Mole fraction HETP Flow Refractive of Rate Temperature Index ethanol (ml/min) (oC) (RI) (xW) 17.43 90.1 1.35453 0.088 1.518 53.17 90.5 1.35324 0.076 1.392 75.00 91.3 1.35213 0.065 1.137 85.71 91.7 1.35220 0.063 1.075 101.41 91.9 1.34910 0.040 0.767

Table A-3: Data for distillate and bottom product for the selection of different set of heater power Experiment 10: Batch Distillation (Structure Packing) At Constant Reflux Distillate product Bottom product Mole Mole Time(min) Refractive fraction Refractive fraction Temperature Index of Temperature Index of (oC) (RI) ethanol (oC) (RI) ethanol 5.0 97.6 1.36263 0.159 92.1 1.35226 0.0658 10.0 97.7 1.36317 0.165 92.2 1.35214 0.0647 20.0 98 1.36527 0.224 92.2 1.35213 0.0646 30.0 98.1 1.36657 0.248 92.2 1.35209 0.0640 40.0 98.1 1.36731 0.256 92.2 1.35208 0.0639 50.0 98.1 1.36825 0.303 92.2 1.35206 0.0638 60.0 98.1 1.36827 0.305 92.2 1.35199 0.0629 Table A-4: Data for distillate and bottom product for each sampling time Time(min) 5.0 10.0 20.0 30.0 40.0 50.0 60.0

HETP

1.481 1.446 1.274 1.185 1.124 1.099 1.053

Mole fraction of ethanol,x2 0.0658 0.0647 0.0646 0.0640 0.0639 0.0638 0.0629

In L2 4.14819 4.14518 4.1449 4.14326 4.14299 4.14272 4.14026

L2 63.3194 63.1288 63.1115 63.008 62.9908 62.9736 62.8192

Amount of ethanol left(litre) 3.6972 3.6861 3.6851 3.6791 3.6781 3.6771 3.6680

Table A-5: Data for amount of ethanol left in the evaporator for each sampling time

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Appendix B Experiment 9: Batch Distillation (Structure Packing) At Total Reflux Sample Calculation At 20oC, Density of water, Density of ethanol, =0.99823 g/cm3 =0.789 g/cm3

Relative molecular mass of water = 18.016 g/mol Relative molecular mass of ethanol = 46.07 g/mol

To find the mol fraction of ethanol:

n = no. of mol of ethanol = density of ethanol = volume of ethanol used = relative molecular mass of ethanol

n = no. of mol of water = density of water = volume of water used = relative molecular mass of water mol fraction of ethanol = For example, volume of ethanol used = 2 ml and volume of water used is 8 ml

Mol fraction of ethanol =

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To find the HETP, 1. Find the theoretical number of plates in the distillation unit using McCabe-Thiele method. 2. Calculate the HETP.

Height of packing, H = 1m

When heating power is 1.5kW,

Figure B-1: Equilibrium diagram for system ethanol-water when heating power is 1.5kW Number of theoretical plates = 0.6588 HETP = HETP= 1.518

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When heating power is 2.0kW,

Figure B-2: Equilibrium diagram for system ethanol-water when heating power is 2.0kW Number of theoretical plates = 0.7182 HETP = =1.392

When heating power is 2.5kW,

Figure B-3: Equilibrium diagram for system ethanol-water when heating power is 2.5kW Number of theoretical plates = 0.8798 HETP = HETP= 1.137

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When heating power is 3.0kW,

Figure B-4: Equilibrium diagram for system ethanol-water when heating power is 3.0kW Number of theoretical plates = 0.9302 HETP = HETP= 1.075 When heating power is 3.5kW,

Figure B-5: Equilibrium diagram for system ethanol-water when heating power is 3.5kW Number of theoretical plates = 1.303 HETP = HETP= 0.767

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Experiment 10: Batch Distillation (Structure Packing) At Constant Reflux The equation of the operating line for enriching section: Reflux ratio = 3 At t=0,

When time is 5 min,

Figure B-6: Equilibrium diagram for system ethanol-water when time = 5 min Number of theoretical plates = 0.6754 HETP = HETP= 1.481

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When time is 10 min,

Figure B-7: Equilibrium diagram for system ethanol-water when time = 10 min Number of theoretical plates = 0.6917 HETP = =1.446

When time is 20 min,

Figure B-8: Equilibrium diagram for system ethanol-water when time = 20 min Number of theoretical plates = 0.7852 HETP = HETP=1.2735

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When time is 30 min,

Figure B-9: Equilibrium diagram for system ethanol-water when time = 30 min Number of theoretical plates = 0.8440 HETP = HETP=1.185 When time is 40 min,

Figure B-10: Equilibrium diagram for system ethanol-water when time = 40 min Number of theoretical plates = 0.8893 HETP = = 1.124

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When time= 50min,

Figure B-11: Equilibrium diagram for system ethanol-water when time = 50 min Number of theoretical plates = 0.9095 HETP = HETP= 1.099 When time= 60min,

Figure B-12: Equilibrium diagram for system ethanol-water when time = 60 min Number of theoretical plates = 0. 9494 HETP = HETP= 1.053
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The amount of the ethanol left: The initial volume of ethanol in still, Vethanol = 4 Litres The initial volume of water in still, Vwater = 12 Litres The original number of moles of ethanol:

The original number of moles of water:

Mol fraction of ethanol = Rayleigh equation: In L1-In L2 =

L1 = initial moles of liquid originally in still L2 = final moles of liquid remained in still x1 = initial liquid composition in still (mole fraction of ethanol) x2 = final liquid composition in still (mole fraction of ethanol) y= initial composition of ethanol in the vapour The feed composition of ethanol, x1 = 0.0934 The final composition of ethanol, x2 = 0.0629 From the equilibrium diagram of ethanol water mixture, the initial mole fraction of ethanol in vapor, y = 0.43

( (

) )

( (

) )

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The amount of the ethanol left in the evaporator = = 3.668 litres The same method of calculation is repeated to calculate the amount of ethanol left in the still for different interval of time.

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Appendix C

Figure C-1: The flow diagram of batch distillation unit (structured packing)

Figure C-2: Batch Packed Distillation Column (Model: BP81-SP)

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