1.

ABSTRACT
1.1. Experimental purpose
The objective of the experiment is to understand and apply basic concepts in distillation of
binary mixtures. Continuous distillation of ethanol water mixture will be investigated:
- Determine the overall efficiency of the column
- Investigate effect of reflux ratio on the product composition
- Investigate effect of location of feed flow on the product composition
1.2. Experimental methods
This lab is mainly designed to separate binary components including ethanol and water using
distillation with 5 stages batch column
2. EXPERIMENT THEORY
The separation dynamics are most heavily dependent on the vapor pressure of the
species in the column. The more volatile component is also known as the light key, the less
volatile component is also known as the heavy key. For a two-component separation:

All symbols are defined in the nomenclature section at the end of the text. By Raoult’s
law, this means that relative volatility can be described in terms of mole fractions in the liquid
and vapor phases.

This can be rearranged to give:

The traditional approach to modeling distillation processes is known as the

McCabe-Thiele approach. This model requires making the following assumptions:
- That the relative volatility is constant over the temperature range in the column
- That the components have equal and constant molar enthalpy
- That enthalpy changes and heat of mixing are negligible
- That the pressure is uniform within the column
 These assumptions allow equations to be derived relating flow rates to molar
compositions in each stage of the column. The column is divided into the vapor phase, and
the rectification section, in which the less volatile component is selectively condensed. In
each section, the liquid and vapor compositions can be related to flow rates.
Rectification section:
𝑉𝑛+1. 𝑦𝑛+1 = 𝐿𝑛𝑥𝑛 + 𝐷𝑥𝑝 (6)
𝐿 𝐷
𝑦𝑛+1 = ( 𝑉 𝑛 ) + ( 𝑉 ). 𝑥𝐷 (7)
𝑛+1 𝑛+1

where the stages are numbered consecutively, beginning with the top stage
𝐿 𝑅
𝑉
= (𝑅+1)
(8)
𝑅 1
𝑦𝑛 = (𝑅+1)
. 𝑥𝑛 + (𝑅+1)
. 𝑥𝐷(9)

Stripping section:
𝐿𝑛 𝐵𝑛
𝑦𝑛 = 𝑉𝑛
. 𝑥𝑛 + 𝑉𝑛
. 𝑥𝐵(10)

𝑉
𝑉𝐵 = 𝐵
(11)

𝐿 𝑉+𝐵 𝑉𝐵+1
𝑉
= 𝑉
= 𝑉𝐵
(12)

𝑉𝐵+1 1
𝑦𝑛 = 𝑉𝐵
. 𝑥𝑛 − 𝑉𝐵
. 𝑥𝑛(13)

Given equilibrium data for the components of the distillation, these equations can be
used to model the stages graphically, as shown in Figure 1.

Figure 1 : Sample McCabe-Thiele diagram. Each step indicates a theoretical stage

going to complete equilibrium. The calculations are shown for the rectification section only.
Reprinted from Seader (1998)

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 Because true vapor-liquid equilibrium is unlikely to be achieved on each stage, this
method must be adapted in order to properly model the distillation system. A widely used
method for this is known as Murphree Efficiency

Where y* used in this equation is derived from experimentally measured liquid-phase

composition values. The Murphree Efficiency can be used to alter the equilibrium line in the
McCabe – Thiele graph. This adapted graph can be used to more accurately predict the
separation under different conditions of feed composition and reflux ratios.
3. EXPERIMENTAL REPORT
Table 1: Raw results
Concentration of
Flow rate (reading level) Temperature (oC)
EtOH
Reflux
No. Tray position Overhead
Feed (F) (Lo) Feed Distillation Feed Distillation Reflux Bottom
(D)
(ml/min) (ml/mi (xF) (xD) (tF) (tD liquid) (tLo) (tw)
(ml/min)
n)
1 4 150 60 76 20 60 56 32 233 93
2 4 150 36 64 20 65 57 19 75 93
3 4 150 28 44 20 77 61 17 73 93
4 2 150 50 40 20 73 55 15 74 92
5 5 150 60 56 20 80 56 16 73 92

Table 2: Raw results processing

Flow rate (Reading level) Concentration of EtOH

Experiment Tray position
Feed (F) Overhead Reflux (Lo) Distillation
Feed (xF) Bottom (W)
(ml/min) (D) (ml/min) (ml/min) (xD)
1 4 846 60 428,64 0,07002 0,31530 0,05130
2 4 846 36 360,96 0,06997 0,36564 0,04537
3 4 846 28 248,16 0,06977 0,51000 0,02569
4 2 846 50 225,6 0,07007 0,45712 0,03352
5 5 846 60 315,84 0,07002 0,55450 0,01943

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 Table 3: Calculation results

Experiment Feed tray position tF HF(kJ/kg) HV,F HL,F q q/q-1

1 4 56,00 219,69 2521,24 383,28 1,08 14,0689

2 4 57,00 223,76 2528,22 323,99 1,05 22,9913
3 4 61,00 240,07 2527,73 383,28 1,07 15,9738
4 2 55,00 215,63 2527,77 383,28 1,08 13,7914
5 5 56,00 219,69 2527,77 383,28 1,08 14,1088

Table 4: Input line equation and linear equation

No. Input line equation Linear Equation

1 y = 14,0689 x - 0,92 y = 1+ 0,07x

2 y = 22,9913 x - 1,54 y = 1+ 0,05x

3 y = 15,9738x - 1,04 y = 1+ 0,07x

4 y = 13,7914x - 0,9 y = 1+ 0,12x

5 y= 14,1088x - 0,92 y = 1+ 0,12x

Table 5: Experimental results

No. Location of feed Reflux ratio (R) Theory plate 𝑥𝐷 General tray efficiency 𝐸0

1 4 0.06 1 0.315 0%

2 4 0.1 1 0.365 0%

3 4 0.09 2 0.510 50%

4 2 0.05 2 0.457 50%

5 5 0.05 3 0.554 66.67%

Where 𝑛𝑟 = 5 (real experiment number of stages)

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 4. GRAPH
Schematic calculation of theoretical trays
Each graph corresponds to an experiment

Graph 1: Graph of theoretical specimens with 𝐿0 = 5

Input line equation Linear Equation

y = 14,0689 x - 0,92 y = 1+ 0,07x

Theory plate: 𝑛𝑡ℎ𝑒𝑜𝑟𝑦 = 1

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 Graph 2: Graph of theoretical specimens with 𝐿0 = 10

Input line equation Linear Equation

y = 22,9913x - 1,54 y = 1+ 0,05x

Theory plate: 𝑛𝑡ℎ𝑒𝑜𝑟𝑦 = 2

Graph 3: Graph of theoretical specimens with 𝐿0 = 15

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 Input line equation Linear Equation

y = 15,9738x - 1,04 y = 1+ 0,07x

Theory plate: 𝑛𝑡ℎ𝑒𝑜𝑟𝑦 = 2

Graph 4: Graph of theoretical specimens number 2

Input line equation Linear Equation

y = 13,7914x - 0,9 y = 1+ 0,12x

Theory plate: 𝑛𝑡ℎ𝑒𝑜𝑟𝑦 = 2

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 Graph 5: Graph of theoretical specimens number 5

Input line equation Linear Equation

y= 14,1088x - 0,92 y = 1+ 0,12x

Theory plate: 𝑛𝑡ℎ𝑒𝑜𝑟𝑦 = 3

5. EXPERIMENTAL THEORY
5.1. The effect of the flow on the product's purity, on the performance of the wheel and
the overall performance of the column
5.1.1. The effect of the flow on the product's purity
It is clear from the experiments 1,2,3 that as the flow of circulation increases, the
purity of the product increases.
This can be explained on the basis of heat. With a constant supply of heat, the molar
mass of the Go is constant.
We have Go = Lo + D. As the flow of circulation increases, this also means
decreasing the flow of product. For the whole tower powder, the amount of heat entering the
boiler has the function of separating the mixed phase. Individual dosing rates will be
calculated according to the amount of heat supplied separately - calculated on 1 molar peak.
Thus, when D decreases, ie the heat supplied separately increases the separation, ie increasing
the purity of the product (including top and bottom products).
5.1.2 The effect of the flow on the performance of the wheel
By experiment, it is clear that as the flow increases, the process efficiency increases.
Increased productivity means that the system works as close to the theory

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 However, it must be noted that general performance does not allow for an assessment
of the economic viability of the equipment. Our goal is to produce the desired purity product.
As the flow increases, the efficiency of the tray increases, which means that the number of
trays needed will be reduced, thus reducing the initial cost of manufacturing the device.
However, as the flow increases, as noted above, the individual supply will increase. Want to
get the desired amount of product to spend more heat. This cost sometimes accounts for a
huge percentage of the total cost of the
5.1.3 The effect of the flow on the product's purity, and the overall
performance of the column
During the distillation, the liquid stream as well as the vapor stream will change the
concentration as it passes through each tray (change in concentration). However, the change
of concentration when passing through each tray also depends on the ability to exchange in
the tray. It is clear that when inputting the trays near the bottom, the number of exchange
rates increases, resulting in peak product purity increase; when the input tray near the top, the
result will be the opposite. However, when the input position is not the same as the
theoretical position, the exchange capacity of the trays will decrease (although the number of
theoretical trays is increased then), so the achievement of purity is not sure.
Through experiment, we find that the input tray does not affect the efficiency of the
tray. The effect of the input trays on the performance of the trays cannot be concluded based
on its high or low position, but based on its deviation from the theoretical position as close to
this position as the efficiency the higher the tray.
5.2. The phenomena and processes taking place in the tower when operating stable
- On each tray there is the boiling of the mixture. The boiling temperature of the
mixture in each tray is different and gradually reduced to the final tray.
- Stable operating system is proper operation of the heat exchanger in order to ensure
the heat supply to the currents
- The flow meters should be stable
- Thermometer on the trays of different values, the higher the temperature the lower the
temperature
5.3. The causes of the error and how to overcome
- During the experiment
+ The valves are not fully opened so the flow is unstable
+ Marbles are always drop so always monitor the flow
+ Measurement of alcohol by incorrect design by the reader error due to flow
measurement (press incorrect clock, unstable flow)
+ Do not read the measured values at the same time
- In the calculation process: data rounding, table lookup, unit conversion, plotting
inaccurate
+ Restricted and corrected
+ Experiment must be careful, the operation of the members must coordinate rhythm
+ Always adjust the flow of input and flow at the correct value measure the values at the
same time

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 6. APPENDIX
The calculation of the data for all 5 experiments was similar.

Table 6: Data table for ethanol

Specific weight ρ𝑟 = 0. 772 𝑔/𝑚𝑙

Molecular weight 𝑀𝑟 = 46 𝑔/𝑚𝑜𝑙

𝑜 𝐶𝑟 = 119. 6 𝐽/𝑚𝑜𝑙. 𝐾
Specific heat (40 –80 C)
𝑜 𝑟𝑟 = 39741 𝐽/𝑚𝑜𝑙
Latent heat of vaporization at 86.5 C

Table 7: Data table for water

Specific weight ρ𝑟 = 0. 992 𝑔/𝑚𝑙

Molecular weight 𝑀𝑟 = 18 𝑔/𝑚𝑜𝑙

𝑜 𝐶𝑟 = 75. 24 𝐽/𝑚𝑜𝑙. 𝐾
Specific heat (40 –80 C)
𝑜 𝑟𝑟 = 41200 𝐽/𝑚𝑜𝑙
Latent heat of vaporization at 86.5 C

We need to calculate the following parameters in turn:

𝑑𝑜 𝑟𝑢𝑜𝑢 × ρ𝑟
𝑀𝑟
It changes from the contraceptive to molar: 𝑥 = 𝑑𝑜 𝑟𝑢𝑜𝑢 × ρ𝑟 (100 − 𝑑𝑜 𝑟𝑢𝑜𝑢) × ρ𝑛 (12)
𝑀𝑟
+ 𝑀𝑛

Varies from flow to mol/min:

𝑄 (𝑚𝑜𝑙/𝑚𝑖𝑛) =
𝑄 (𝑚𝑙/𝑚𝑖𝑛)
100
× ( 𝑑𝑜 𝑟𝑢𝑜𝑢 × ρ𝑟
𝑀𝑟
+
(100 − 𝑑𝑜 𝑟𝑢𝑜𝑢) × ρ𝑛
𝑀𝑛 ) (13)

𝑥𝐹×𝐹 − 𝑥𝐷×𝐷
Distillation concentration: 𝑥𝑤 = 𝐹−𝐷

Average specific heat of the mixture: 𝐶ℎℎ = 𝐶𝑅 × 𝑥 − 𝐶𝑁 × (1 − 𝑥)

Where:
𝑜
𝐶𝑁 – specific heat of water (Kcal/Kmo𝑙 C)
𝑜
𝐶𝑅 – specific heat of alcohol (Kcal/Kmo𝑙 C)

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 Average latent heat of mixture: 𝑟ℎℎ = 𝑟𝑅 × 𝑥 − 𝑟𝑁 × (1 − 𝑥)
Where: 𝑟ℎℎ, 𝑟𝑅, 𝑟𝑁 – heat of vapourization of the mixture, pure alcohol, water at the
temperature under consideration.
Calculate 𝐶𝐹, 𝐶𝐹𝐿, 𝐶𝐺𝐹, 𝐻𝐹, 𝐻𝐿𝐹, 𝐻𝐺𝐹
𝐶𝐹 = 𝐶𝐿𝐹 = 𝐶𝑅 × 𝑥 − 𝐶𝑁 × (1 − 𝑥) (14)
𝐶𝐺𝐹 = 𝐶𝑟 × 𝑦𝐹 − 𝐶𝑛 × (1 − 𝑦𝐹) (15)
𝐻𝐹 = 𝐶𝐹 × 𝑡𝐹 (16)
𝐻𝐿𝐹 = 𝐶𝐹 × 𝑡𝑠𝐹 (17)
𝐻𝐺𝐹 = 𝐶𝐹 × 𝑡𝑠𝐹 + 𝑟ℎℎ (18)
Where: 𝑡𝑠𝐹 – the boiling point of the mixture

- Calculate the reflux ratio R, q

𝑅 𝑥𝐷
- Find out the slope = 𝑅+1
, and free radical in its equation = 𝑅+1
𝑞 𝑥𝐹
- Find the input slope by 𝑞+1
, and free radical in its equation = 𝑞−1
- Draw a graph to calculate the number of theoretical points, thus deducting the overall
𝑛𝑙𝑡
efficiency of the distillation tower: 𝐸0 = 𝑛𝑇

Table 8: Density of ethyl alcohol and water based on Fahrenheit temperature

Feed
Temperature
ρethanol (kg/m3) ρwater (kg/m3) ρave (kg/m3)
56,00 752,00 998,57 499,29
57,00 751,00 984,71 492,36
61,00 747,00 982,67 491,34
55,00 753,00 985,70 492,85
56,00 752,00 985,21 492,61

Reflux
Temp
ρethanol (kg/m3) ρwater (kg/m3) ρave (kg/m3)
233,00 565,11 823,10 694,11
75,00 735,00 974,81 854,91
73,00 737,00 976,00 856,50
74,00 736,00 975,41 855,71
73,00 737,00 976,00 856,50

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 Distillation
Temperature
ρethanol (kg/m3) ρwater (kg/m3) ρave (kg/m3)
32,00 776,00 995,05 497,53
19,00 788,00 998,38 499,19
17,00 789,00 998,74 499,37
15,00 791,00 999,06 499,53
16,00 790,00 998,91 499,46

Bottom
Temperature
ρethanol (kg/m3) ρwater (kg/m3)
93,00 718,00 963.27
93,00 718,00 963.27
93,00 718,00 963.27
92,00 719,00 963.95
92,00 719,00 963.95

Table 9: Specific heat of ethyl alcohol, water and feed based on the temperature at boiling
point
tF sôi tb
T 56,00 57,00 61,00 55,00 56,00
= 87.75
Cp (etylic)
2902,15 2914,37 2963,74 3316,15 2889,99 2902,15
J/[Link]
Cp water J/[Link] 4183,00 4183,00 4183,00 4216,00 4183,00 4183,00
Cp of Feed 3923,05 3925,53 3935,55 4033,37 3920,58 3923,05

Table 10: Latent heat of ethyl alcohol, feed and bottom product
Latent heat

r ethanol J/kg.K 871524,46 TF sôi tb = 87.75

r nước J/kg.K 2297070,03 TF sôi tb =87.75

2197248,75 56,00
2204233,56 57,00
r F J/kg.K 2203746,20 61,00
2203780,35 55,00
2203777,96 56,00

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Figure 2. Density of alcohol ethylic according to temperature.

Figure 3. Density of water according to temperature.

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Figure 4. Heat of vaporization of ethyl alcohol (kcal/kg) according to the temperature

Figure 5. Heat of vaporization of water (kcal/kg) according to the temperature

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 Figure 6. Ethyl alcohol - water graph based on temperature

7. REFERENCE
[1] Võ Văn Bang, Vũ Bá Minh - Quá trình và Thiết bị - Tập 3 - Truyền khối, ĐHQG TP.
HCM, 2004
[2] Trịnh Văn Dũng - Tóm tắt bài giảng Các quá trình và thiết bị truyền khối, ĐH Bán công
Tôn Đức Thắng, 2003
[3] Sổ tay quá trình và thiết bị, ĐH QG TP. HCM, 2004

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