PROCESS & EQUIPMENT EXPERIMENT

DISTILLATION

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,

1.3. Raw results

Table 1
Flow rate Concentration Temperature
Locat
No ion of Distillat Distill
Reflux Distilla Feed Reflux
feed Feed (F) e (D) Feed ate (tD
(Lo) te (tF) (tLo)
(ml/ph) liquid)

1 4 30 132 5 40 88 66 54 82
2 4 30 100 10 40 88.4 67 54 81
3 4 30 74 15 40 94.75 66 54 80
4 2 30 80 10 40 76 67 54 86
5 5 30 80 10 40 74.5 69 54 83

2. EXPERIMENTAL 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:
K1
α= (1)
Kh

P1
KL= (2)
P
PH
KH = (3)
P
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.

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yL/ xL yL ( 1−xL )
α= = (4)
yH / xH xL ( 1− yL )
This can be rearranged to give
α ( xL)
yL= (5)
1+ xL(α−1)
The tradition 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 assumption 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+1yn+1=Lnxn + DxD (6)
yn+1=(Ln/ Vn+1) + (D/ Vn+1)xD (7)
where the stages are numbered consecutively, beginning with the top stage
L/V=R/(R+1) (8)
yn = (R/(R+1))xn + (1/R+1)xD (9)
Stripping section:
yn = (Ln/Vn)xn – (Bn/Vn)xB (10)
VB=V/B (11)
L/V=(V+B)/V = (VB+1)/VB (12)
yn = ((VB+1)/VB)xn – (1/VB)xB (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.

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DISTILLATION

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)

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
EM = (14)
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 retios.

3. EXPERIMENTAL RESULTS
Table 1 : Raw results

Flow rate Concentration Temperature

Locat
No ion of Distillat Distill
Reflux Distilla Feed Reflux
feed Feed (F) e (D) Feed ate (tD
(Lo) te (tF) (tLo)
(ml/ph) liquid)

1 4 30 132 5 40 88 66 54 82
2 4 30 100 10 40 88.4 67 54 81
3 4 30 74 15 40 94.75 66 54 80

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DISTILLATION

4 2 30 80 10 40 76 67 54 86
5 5 30 80 10 40 74.5 69 54 83

Table 4 : Raw results processing

Ratio mol(mol C2H5OH/total

Flow rate (ml/min)=dd*5.64
mo;l)
Location
No Distillate
of feed Reflux Bottom
Feed (F) (D)
(Lo) Feed Distillate (xW)
(ml/ph)
(xF) (xD)
1 4 169.2 132 28.2 0.0623 0.1685 0.029
2 4 169.2 100 56.4 0.0622 0.1992 0.004
3 4 169.2 74 84.6 0.0623 0.3226 0.031
4 2 169.2 80 56.4 0.0624 0.2059 0.024
5 5 169.2 80 56.4 0.0624 0.2126 0.025

Table 5 : Calculation Results

Reflux
HF(KJ/Kmol)
Location ratio HGF HLF q q/(q-1)
No of feed (R) tF (Kcal/Kmol) (Kcal/Kmol)
1 4 0.21 66 270 2983 308 1.01 72.23
2 4 0.56 67 274 2983 307 1.01 82.05
3 4 1.14 66 270 2963 287 1.01 157.20
4 2 0.71 67 274 3003 327 1.02 51.24
5 5 0.71 69 283 3005 330 1.02 57.70

Table 6 : Input line equation and Linear equation

No Input line equation Linear equation

1 y= 72.23x-6.15 y= 0.18x=0.42
2 y= 82.05x-7 y=0.36x+0.332
3 y=157.20x-13.49 y=0.53x+0.336
4 y=51.25x-4.34 y=0.41x+0.182
5 y=57.7x-4.89 y=0.41x+0.172

Table 7 : Experimental Results

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DISTILLATION

General tray
Location of Reflux ratio Theory
No xD efficiency
feed (R) plate
E0
1 4 0.21 1 0.5 0.510
2 4 0.56 2 1.1 0.520
3 4 1.14 2 1.5 0.719
4 2 0.71 2 1 0.310
5 5 0.71 3 1.7 0.293

4. GRAPH
Schematic calculation of theoretical trays
Each graph corresponds to an experiment
Graph of theoretical specimens with Lo=5

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DISTILLATION

0.9

0.8

0.7

0.6

0.5

Equilibrium curveuilib-
Đường cân bằng
0.4 rium
Đường chéo
Cross lineuilibrium
dòng nhập liệu
Cross
0.3 Inputelineuilibrium
lineuilibrium
đường cất
Stripping
đường chưng lineuilibrium
0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Input line equation Linear equation

y= 72.23x-6.15 y= 0.18x=0.42
Theory plates : nLT = 1

Graph of theoretical specimens with Lo=10

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DISTILLATION

0.8

0.6

Đường cân bằng

Đường chéo
0.4 Đường làm việc phần cất
Đường nhập liệu
Đường làm việc phần chưng

0.2

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Input line equation Linear equation

y= 82.05x-7 y=0.36x+0.332
Theory plates: nLT = 2

Graph of theoretical specimens with Lo=15

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DISTILLATION

0.9

0.8

0.7

0.6

0.5

0.4 Đường cân bằng

Đường chéo
0.3 Đường làm việc phần cất
Đường nhập liệu
0.2
Đường làm việc phần chưng
0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Input line equation Linear equation

y=157.20x-13.49 y=0.53x+0.336
Theory plates: nLT = 2

Graph of theoretical specimens number 2

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DISTILLATION

0.9

0.8

0.7

0.6

0.5

0.4 Đường cân bằng

Đường chéo
0.3 Đường làm việc phần cất
Đường làm việc phần
0.2 chưng
Đường nhập liệu
0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Input line equation Linear equation

y=51.25x-4.34 y=0.41x+0.182
Theory plates: nLT = 2

Graph of theoretical specimens with number 5

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PROCESS & EQUIPMENT EXPERIMENT
DISTILLATION

0.9

0.8

0.7

0.6

0.5
Đường cân bằng
0.4 Đường chéo
Đường làm việc phần chưng
0.3 Đường làm việc phần cất
Đường nhập liệu
0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Input line equation Linear equation

y=57.7x-4.89 y=0.41x+0.172
Theory plates: nLT = 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

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DISTILLATION

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
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 but 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 rate
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 tray is
increased then), so the achievement of purity Higher 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 of 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

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DISTILLATION

 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

6. APPENDIX
The calculation of the data for all 5 experiments was similar.
Data table:
Ethanol:
 Specific weight: r = 0.772 g/ml
 Molecular weight: Mr = 46 g/mol
 Specific heat (40 – 80 oC) : Cr = 119.6 J/mol.K
 Latent heat of vaporization at 86,5oC rr = 39741 j/mol
Water:
 Specific weight (40 – 80 oC) : n = 0.992 g/ml
 Molecular weight: Mn = 18 g/mol
 Specific heat (trong khoaûng 40 – 80 oC) : Cn = 75.24 J/mol.K
 Latent heat of vaporization at 86,5oC rn = 41200 j/mol
We need to calculate the following parameters in turn:

 It changes from the contraceptive to molar xD , xF

do ruou×ρ r
Mr
x=
do ruou×ρ r (100-do ruou )×ρ n
+
Mr Mn (12)
 Varies from flow to mol / min
Q( ml/ phut ) do ruou× ρr (100-do ruou)× ρn
Q(mol / phut )= ×( + )
100 Mr Mn (13)
 Distillate concentration.
x F . F−x D . D
xW=
F−D
 Average specific heat of the mixture C2H5OH - H2O (Chh)

C hh=x.C R +(1−x)C N
CN : specific heat of water. (Kcal/Kmol.oC)

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DISTILLATION

CR : specific heat of alcohol. (Kcal/Kmol.oC)

 Average latent heat of mixture C2H5OH - H2O (Kcal/Kmol)

r hh=x.r R +(1−x)r N
rhh, rR, rN : heat of vaporization of the mixture, pure alcohol, water at the
temperature under consideration
 Calculate CF, CLF, CGF , HF, HLF, HGF
C F =C LF =Cr ×x F +C n×(1−x F ) (14)
C GF =C r × y F + Cn ×(1− y F ) (15)
H F =C F ×t F (16)
H LF =C F ×t sF (17)
tsF : boiling point of the mixture
H GF =C F×t sF +r r × y F +r n (1−x F ) (18)
 Calculate the reflux ratio R , q
 Find out the slope = R /(R +1) , and free radical in its equation = xD / (R +1)
 Find the input slope by q/(q-1) and free radical in its equation =
xF/(q-1)
 Draw a graph to calculate the number of theoretical points, thus deducting the
overall efficiency of the distillation tower : E0 = nLT / nT
 The checklist

DISTILATE
Temperature
ρr (kg/m3) ρn (kg/m3)
100 716.20 960.60
100 716.20 960.60
100 716.20 960.60
100 716.20 960.60
100 716.20 960.60

DISTILATE
Temperature 3
ρr (kg/m ) ρn (kg/m3) ρtb (kg/m3)
44 769.23 990.06 901.73
44 769.23 990.06 890.69
42 771.01 990.76 856.71
42.5 770.57 990.59 889.38
42.5 770.57 990.59 887.18

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DISTILLATION

FEED
Temperature 3
ρr (kg/m ) ρn (kg/m3) ρtb (kg/m3)
50 763.85 987.80 947.49
51.5 762.49 987.20 946.75
50 763.85 987.80 947.49
48 765.65 988.58 948.45
48 765.65 988.58 948.45

REFLUX
Temperature 3
ρr (kg/m ) ρn (kg/m3) ρtb (kg/m3)
38 774.542 992.096 905.33
38 774.542 992.096 894.46
41 771.896 991.103 857.43
38 774.542 992.096 892.22
38 774.542 992.096 890.04

SPECIFIC HEAT
Determine the boiling point of the input stream tF sôi tb = 89 look xFtb = 0.0623

tFtb = 49.5 tF sôi tb = 89

Cetylic J/kg.K 2823.997 3333.60
CWater J/kg.K 4186 4227.86
CF 3995.320 4102.664

LATENT HEAT
retylic J/kg.K 874135.62 tF sôi tb = 89
rw J/kg.K 2390408.04 tF sôi tb = 89
rF J/kg.K 2178129.90

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DISTILLATION

KLR cuû
a Etylic theo nhieä
t ñoä
p
850
800
750
700
650
-50 0 50 100 150
y = -0.0012x2 - 0.803x + 806.51 t

KLR cuû
a nöôù
c theo nhieä
t ñoä

p
1010
1000
990
980
970
960
950
940
930
0 50 100 150
2 t
y = -0.0032x - 0.0946x + 1000.5

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DISTILLATION

Nhieä
t hoù
a hôi theo nhieä
t ñoä
cuû
a röôïu etylic kcal/kg
r
225
205
185
165
145
0 50 100 150
y = -0.000000001x 5 + 0.0000006x 4 - 0.0001x 3 + 0.0051x 2 - 0.1711x + 221.1
T

Nhieä
t hoù
a hôi cuû
a nöôù
c kcal/kg
r
600
580
560
540
520
500
0 50 100 150
t

y = -0.0012x2 - 0.4217x + 594.89

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DISTILLATION

ETYLIC
Ethylen- -Water
NÖÔÙ C

100

Temperature oC
T ÑOÄ( C)

90
NHIEÄ

80

70
0 10 20 30 40 50 60 70 80 90 100
%ETYLIC

7. REFERENCES
[1]. Voõ Vaên Bang ,Vuõ Baù Minh - Quaù trình vaø Thieát bò – Taäp 3 –
Truyeàn khoái, ÑHQG TP HCM, 2004.

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[2]. Trònh Vaên Duõng - Toùm taét baøi giaûng Caùc quaù trình vaø
thieát bò truyeàn khoái, ÑH Baùn coâng Toân Ñöùc Thaéng, 2003.
[3]. Soå tay quaù trình vaø thieát bò, ÑH QG TP HCM, 2004

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