CH 3520 HEAT AND MASS TRANSFER LABORATORY

Title of the experiment: Plate column distillation

Date of experiment: 5/02/2013 Date of Report: 13/02//2013

For Instructors use only:

Item number 1 2 3 4 5 6 7 8 9 10 Division Experimental Diagram Experimental Procedure Precautions Experimental data Sample calculations Error analysis Results and discussion Suggestions for improvement Conclusions References Total Maximum Marks 5 5 5 20 15 10 25 5 5 5 100 Actual Marks

Batch and group number: B8 Marks:

Name
1. Gokul Krishna 2. Prabal Sabarawal 3. T G Radhakrishna

Roll Number
CH10B017 CH10B087 CH10B089

100

3.

Plate Column Distillation

Aim: To calculate the number of ideal stages required and the overall efficiency of plate distillation
column.

Apparatus: Measuring cylinders, beakers, refractometer, burette, chemicals: Toluene, CCl4, and
acetone.

Experimental Diagram:
Plate

Theory:
Any physical device that provides good contact between the vapour and liquid phases present in industrial-scale distillation columns or laboratory-scale glassware distillation columns constitutes a "plate" or "tray". Since an actual, physical plate is rarely a 100% efficient equilibrium stage, the number of actual plates is more than the required theoretical plates. We can use the following formula to calculate the efficiency of the plate column if we know both number of theoretical stages and the number of ideal stages required for a particular operation. Number of ideal stages required can be calculated from McCabe-Thiele method.

Where: Na = the number of actual, physical plates or trays, Nt = the number of theoretical plates or trays and E = the overall efficiency

For calculations we follow the McCabe-Thiele method. It is a graphical approach, considered to be the simplest and most instructive method for the analysis of binary distillation. This method uses the fact that the composition at each theoretical plate (or equilibrium stage) is completly determined by the mole fraction of one of the two components. The McCabe-Thiele method is based on the assumption of constant molar overflow which requires that: The molal heats of vaporisation of the feed components are equal. For every mole of liquid vaporized, a mole of vapour is condensed. Heat effects such as heat of solution and heat transfer to and from the distillation column are negligible.

Procedure:
Calibration: 1. Take 11 beakers with 10ml solution of CCl4 and Toluene such that volume of CCl4 varying from 0ml to 10ml. 2. Refractive index of each sample is measured using refractometer. 3. A graph between refractive index and mole fraction is plotted. Distillation column experiment: 1. Wash all the vessels and round bottle flask with acetone. 2. A 1000 ml solution of toluene and CCl4 is made with 55% (v/v) toluene and 45% (v/v) CCl4 and fed into the round bottom flask. 3. Boiler is turned on and temperature is observed at the plates and flask. 4. Vapours are condensed using cold water supply from outside. 5. After sometime the temperatures at all the levels becomes constant. This indicates that the system has reached steady state. Then Samples from the five taps are collected. 6. The samples should be cooled down to room temperature. 7. Refractive index of the samples is measured with the help of refractometer.

Precautions:
1. 2. 3. 4. 5. 6. 7. 8. 9. Clean all the vessels and round bottom flask using acetone Avoid liquid spillage over heater coils at the bottom of distillation column. Ensure proper supply of cold water in the condenser pipe and make sure there is no leakage. Shake the samples well before measuring the refractive index. Ensure that steady state is achieved before collecting samples. Wear gloves while handling hot materials. Wear safety goggles while making binary solutions. Store the collected samples in tightly closed containers. Measure the refractive index of the collected samples from plate column only after reaching room temperature.

Experimental Data:
Molecular Mass of CCl4: 153.82 g mol1 Molecular mass of Toluene: 92.14 g mol-1 Density of CCl4: 1.595 g/ml Density of Toluene: 0.866 g/ml Calibration:
Volume of CCl4 (ml) 0 1 2 3 4 5 6 7 8 9 10 Volume of Toluene (ml) 0 0.010369263 0.020738526 0.031107788 0.041477051 0.051846314 0.062215577 0.072584839 0.082954102 0.093323365 0.103692628 10 9 8 7 6 5 4 3 2 1 0 Mole fraction of CCl4 0 0.10919849 0.216187426 0.321033201 0.423799572 0.524547793 0.623336735 0.720223002 0.815261038 0.908503229 1 Refractive Index 1.49404 1.49177 1.48898 1.48654 1.48191 1.47998 1.47502 1.47141 1.47021 1.46499 1.45812

Moles of CCl4

Moles of Toluene 0.09398741 0.084588669 0.075189928 0.065791187 0.056392446 0.046993705 0.037594964 0.028196223 0.018797482 0.009398741 0

Graph of Refractive index vs. Mole fraction of CCl4

Refractive index of solution vs Mole fraction of CCl 4

1.5 1.495 1.49 Refractive Index 1.485

1.48
1.475 1.47 1.465 1.46 1.455 0 0.2 0.4 0.6 Mole Fraction of CCl4 0.8 1 1.2 y = -0.0345x + 1.4962

Linear fit for the data: y = -0.0345x+1.4962

Distillation column experiment: Tray spacing = 20 cm No. Of trays = 5 Length of column = 100 cm Total Volume of the mixture = 1000 ml Volume of Toluene = 550 ml Volume of CCl4 = 450 ml Plate number (from bottom) 1(bottom) 2 3 4 5 (top) Refractive index Temperature (oC) Mole fraction of CCl4 from : x= (y-1.4962)/(-0.0345) 0.744927536 0.777681159 0.824057971 0.882028986 0.906376812

1.4705 1.46937 1.46777 1.46577 1.46493

86 83 Not working Not working 78

Calculations:
In order to calculate the number of ideal trays required for the operations, we are going to use McCabe Thiele method. According to this method, slope of operating line of absorption or rectifying section is reflux ratio. Reflux ratio is defined as the ratio of reflux rate to distillate rate (R = L/D). In our case, distillate rate=0. So, Reflux ratio, R = operating line. Plot CCl4 and toluene vapour liquid equilibrium curve and operating line y = x on the same graph. Then drop the stages from the first point (concentration of CCl4 on the top plate) to the last point (concentration of CCl4 on the bottom plate). Then count the number of steps. This number is the required number of ideal stages to do the same separation. From the graph we can see that, the number of ideal stages required to do the same separation is around 2.5. Since, the number of stages cannot be a fraction so, the number of ideal stages required = 3. According to the formula, Efficiency of the plate column = Therefore, efficiency of the plate column = 60 % . Therefore, slope of absorption curve = = 1. Therefore, y = x is our where, R is

Vapour-Liquid Equilibrium Data for CCl4-Toluene system: Mole fraction of CCl4 in liquid phase (x) 0.025 0.05 0.075 0.1 0.125 0.15 0.175 0.2 0.225 0.25 0.275 0.3 0.325 0.35 0.375 0.4 0.425 0.45 0.475 0.5 0.525 0.55 0.575 0.6 0.625 0.65 0.675 0.7 0.725 0.75 0.775 0.8 0.825 0.85 0.875 0.9 0.925 0.95 0.975 1 Mole fraction of CCl4 in the vapour phase (y*) 0.061 0.1181 0.1715 0.2217 0.2688 0.313 0.3547 0.394 0.431 0.466 0.499 0.53 0.559 0.5879 0.614 0.639 0.6638 0.6867 0.7084 0.7292 0.748 0.767 0.7858 0.803 0.8195 0.8353 0.8504 0.8648 0.8787 0.892 0.9048 0.9171 0.9289 0.9402 0.9511 0.9616 0.9717 0.9815 0.9909 1

Graph showing number of ideal trays, VLE curve, and Operating line

*Dots are mole fraction of CCl4 on each plate (if we join these points we will get our operating line)

Errors and discussion:

Actual Efficiency of the plate column would be less than 60% because the actual number of trays required to do the separation is approximately 2.5, but we have taken the number to be 3 in our calculations. So, actual efficiency of the plate column would be around 50% which is much less than the typical efficiency of a plate column which is around 65%. The efficiency of the plate column can be improved by improving the contact between vapour and liquid by using bubble cap trays. Least count of the burette used is 0.1 ml. So, there could be a maximum error of 0.05 ml in our readings. Value of density is collected from Chemical Engineers Handbook by Robert Perry. This value need not be the same as that of the sample we used.

Suggestion:
1. The inefficiency of plates occurs mainly because of two reasons insufficient time of contact and insufficient degree of mixing. 2. Better contacting is achieved by installing bubble-caps or valve caps at each perforation to promote the formation of vapour bubbles flowing through a thin layer of liquid maintained by a weir on each tray. 3. Insulation of the round bottomed flask can be improved in order to prevent heat loss to atmosphere. 4. Few thermocouples were not working. They have to be replaced.

References:
Mass Transfer Operation by Robert Treybal, third edition Chemical Engineers Handbook by Robert Perry and Don Green Separation Process Principles by Seader and Henley