Continuous Distillation of a Binary

Mixture of Methanol-Isopropanol
By
Group 28

Arati Banu (013802) Mitchell Lim (013484) Pang Hui Ying (013387)
What is Distillation?

2
A process that separates mixtures into their constituent
components based on the differences in the components
boiling points/volatility.

Figure 1: Simple Lab Scale Distillation Schematic 3

What is Continuous Distillation?

4
An ongoing separation by which a mixture is continuously
fed (without interruption) into the process and the respective
fractions are removed continuously.

Figure 2: Simple Continuous Distillation Schematic 5

 Applications of
Continuous Distillation

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 Oil Water
Refinery Treatment

Air Separation

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Experimental Outline

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A laboratory scale continuous distillation rig
was executed to study the continuous
distillation at a constant reflux ratio.

Test mixture: Methanol-Isopropanol

Mixture phase: Liquid

9
The methanol-isopropanol flowed via the
feed stream and separated into 2 product
streams;

 Top product

 Bottom product

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Methanol (MVC)
Vaporize more & was removed in the distillate
stream.

Isopropanol (LVC)
Remained in the bottom stream.

*The bottom stream was in liquid phase,

while the distillate stream was collected by
condensing the vapour phase.
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Experimental Objectives

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• To observe and study the mechanism of a
continuous binary distillation column.

• To obtain the optimum number of stages for

continuous distillation for a given percentage of
reflux.

• To gain knowledge on the behavior of a

continuous binary distillation column at certain
conditions.

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Operating Conditions

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 Before the Experiment During the Experiment

Power Setting Power Setting

 1000W (25%)  600W (15%)
Reflux Setting Reflux Setting
 100%  68%

Throughout the Experiment

Feed Pump Capacity Cooling Water Flow Rate

 13% of 0.75 L/min  120 L/h
Evaporator Heating Capacity Volume of Feed in Feed Tank
 4.0 kW  2L
Number of Trays Volume of Mixture in Evaporator
 8 sieve plate column  5L
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Experimental Procedure

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1) Once the feed vessel and
evaporator were filled with
• the methanol-isopropanol
Once the feed vessel and
mixture, thehave
evaporator experiment
been filled
was
withstarted by turning on
the methanol-isopropanol
the rig. the experiment was
mixture,
started by turning on the rig.
2) • Initially,
Initially,the
the experiment
experiment was
was carried
carried out
out at at 100%
100% reflux; no
distillate in the top product
reflux
tank.
• Valve
Valve Setting
Setting:
- Closed
Closed
- Open
Open
- Open
Open (72%(during 68% reflux)
reflux)

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3) Once the top product was seen in the phase break vessel,
T1-T16 was recorded after 15 minutes.

4) Then the reflux ratio was changed to 72%.

5) The experiment was then carried out for 50 minutes and the
T was recorded every 10 minutes.

6) At the end of the experiment, the required refractive index

of the samples were obtained and the volume of distillate
was measured.

7) Lastly, all liquids were drained from the vessels and cooled
before being transferred back into the original storage
container.
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Results

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Temperature at different points for 100% reflux ratio

Position Temperature (⁰C)

T1 25.4
T2 22.5
T3 77.8
T4 76.3
T5 75.7
T6 75.3
T7 74.8
T8 74.5
T9 73.7
T10 73.3
T11 73.8
T12 71.2
T13 25.6
T14 24
T15 13.4
T16 16.1

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Temperature at different positions for
72% constant reflux ratio
Time(min)
10 20 30 40 50
Position
T1 25.7 25.8 25.9 25.9 25.9
T2 23 20.5 23 26.2 25
T3 78 78 78 78 78
T4 76.4 76.4 76.4 76.8 76.9
T5 75.8 75.8 75.8 76.5 76.5
T6 75.7 75.7 75.7 76.5 76.6
T7 74.9 75.2 75.2 75.2 76.6
T8 75.7 75.7 75.7 76.5 76.6
T9 75.5 75.5 75.5 76.5 73.7
T10 75 75.3 75.4 76.3 76.4
T11 73.8 74.5 74.8 75.9 75.9
T12 73.4 74 74.3 75.3 75.3
T13 25.7 25.9 26.4 26.6 26.7
T14 26.1 26.1 26.1 26.1 26.2
T15 12.4 13.5 13.7 13.9 13.8
T16 15.4 15.5 16 16.7 16.7 21
 Temperature Profile
Temperature VS Positions
90

80

70

Total reflux
60

72% Reflux Ratio @10 mins

Temperature

50

72% Reflux Ratio @20 mins

40

72% Reflux Ratio @30 mins

30
72% Reflux Ratio @40 mins
20
72% Reflux Ratio @50 mins

10

0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
Temperature at Different Point (T1~T16)

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 Composition of Sample
Position Refractive Index
Initial Mixture 1.367
Final Mixture ~Phase Break Vessel 1.362
Final Mixture ~Top Product 1.361
Final Mixture ~Evaporator 1.369

XW XF XD

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 Composition of Sample
Position % mole Volume of
Methanol fluid /ml
Initial Mixture 0.32 (XF) 7000

Final Mixture (Phase Break Vessel) 0.46 120

Final Mixture (Top Product) 0.48 (XD) 1200

Final Mixture (Evaporator) 0.28 (XW) 5130

To plot graph using McCabe-Thiele method;

𝑅 𝑥𝐷
𝑇𝑂𝐿 ∶ 𝑦𝑛+1 = 𝑥𝑛 +
𝑅+1 𝑅+1
𝑞 1
𝑞 − 𝑙𝑖𝑛𝑒 ∶ 𝑦 = 𝑥 − 𝑥𝐹
𝑞−1 𝑞−1 24
 Graph
McCabe-Thiele Method :
To determine the THEORITICAL STAGES & position of FEED PLATE

1.8 stages
(XD, XD))

(XF, XF))
(XW, Xw)) Feedenters at
the 2nd plate

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Discussion

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 For Total Reflux at 100%

1.5 stages TOL

aligned
with X=Y
(XD, XD)) line

(Xw, Xw))

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By the McCabe-Thiele method, the theoretical number of
stages was found to be 1.5 stages.

Thus, according to the formula:

𝑻𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝑵𝒖𝒎𝒃𝒆𝒓 𝒐𝒇 𝑺𝒕𝒂𝒈𝒆𝒔

𝑨𝒄𝒕𝒖𝒂𝒍 𝑵𝒖𝒎𝒃𝒆𝒓 𝒐𝒇 𝑺𝒕𝒂𝒈𝒆𝒔 =
𝑻𝒓𝒂𝒚 𝑬𝒇𝒇𝒊𝒄𝒊𝒆𝒏𝒄𝒚

Efficiency:

1.5/8 x 100% = 18.75%

∴Optimum number of stages was NOT used

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 Obtaining Rmin from methanol X-Y graph

Pinch Point

0.47 (XD, XD)

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 Determining the optimum Reflux Ratio

𝑥𝐷
𝑦 − 𝑖𝑛𝑡𝑒𝑟𝑐𝑒𝑝𝑡 =
𝑅𝑚𝑖𝑛 + 1

By substituting the Y-intercept obtained from graph and XD:

∴ 𝑅𝑚𝑖𝑛 = 0.02128

𝑅 2.5714
= = 120
𝑅𝑚𝑖𝑛 0.02128

𝑹
This value far exceeds the typical value of 𝑹 (1.05-1.3),
𝒎𝒊𝒏
thus the optimum reflux ratio was NOT used.
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Assumptions

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1) Column is perfectly insulated, thus no heat loss.

2) Vapor and liquid phases have sufficient contact time

at plates.

3) Constant molar overflow;

- Molar Hvap of the feed components are equal.
- For every mole of liquid vaporized, a mole of
vapor is condensed.
- Heat effects eg. heat of solutions are negligible.

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Provided that,
- Feed flow rate, F = 0.0975 L/min
- Distillate flow rate, D = 0.024 L/min

𝐋𝐭 = 𝑅𝐷
=0.0617 L/min

𝐕𝐭 = 𝑅 + 1 𝐷
= 0.085 L/min
𝐋𝐛 = 𝐿𝑡 + 𝑞𝐹
= 0.174 L/min

𝐕𝐛 = 𝑉𝑡 + (𝑞 − 1)𝐹
= 0.100 L/min

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Errors & Limitations

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1) Contaminated feed
- Feed was recycled for each experiment.

2) Parallax error
- Inaccuracy of readings due to the fact the eye level was
not perpendicular to the apparatus scale.

3) Improper technique of handling the instruments :

- Final volume of liquid (7.05 liter) was more than the initial
volume of liquid ( 7.00 liters).
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4) Possible defects (certain parts of the distillation column)
- Consistent fluctuations in temperature readings (T2, T10).
- T2 < T1

5) Inefficiency of the column:

- Heat loss to the atmosphere was inevitable

6) Inadequate contact time between vapor and liquid phases.

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Possible Improvements

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1) Use fresh feed for each experiment conducted.

2) Repeat measurements for the refractive index and

obtain an average value.

3) Place containers on a flat surface while measuring

volume of liquids.

4) Ensure proper and complete draining of the liquids from

the tanks.
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5) Schedule regular maintenance for the instrument.

6) Run the experiment at a lower feed rate.

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Conclusion

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 𝑅
≠ (1.05-1.30) ;
𝑅𝑚𝑖𝑛

Reflux ratio used is NOT optimum!

Theoretical number of stages is 1.8 instead of 8 stages as

present in the laboratory column.

Low efficiency of the column : 18.75%

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Appendix

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 Calculations For McCabe-Thiele Method

Given Percentage Reflux = 72%

𝑅
= 0.72
𝑅+1

0.72𝑅 + 0.72 = 𝑅

𝑹 = 𝟐. 𝟓𝟕𝟏𝟒

𝑅 𝑥𝐷
𝑇𝑂𝐿 ∶ 𝑦𝑛+1 = 𝑥 +
𝑅+1 𝑛 𝑅+1

2.5714 048
𝑦= 𝑥+
2.5714 + 1 2.5714 + 1

𝒚 = 𝟎. 𝟕𝟐𝒙 + 𝟎. 𝟏𝟑𝟒𝟒
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 𝐻𝑒𝑎𝑡 𝑡𝑜 𝑉𝑎𝑝𝑜𝑟𝑖𝑠𝑒 1 𝑚𝑜𝑙𝑒 𝑜𝑓 𝐹𝑒𝑒𝑑
q-line : 𝑀𝑜𝑙𝑎𝑟 𝐿𝑎𝑡𝑒𝑛𝑡 𝐻𝑒𝑎𝑡 𝑜𝑓 𝐹𝑒𝑒𝑑

Assumption: feed boil when enter the feed tray at T4 ,boiling point of liquid is 74.5C

0.32×32.04×2.5404+0.68×60.1×2.6342 × 74.5−26 + 0.32×35210+0.68×45340

q= 0.32×35210+0.68×45340
– q=1.154 ( indicates the feed is subcooled liquid)

𝑞 1
𝒒 − 𝒍𝒊𝒏𝒆 ∶ 𝑦 = 𝑥 − 𝑥𝐹
𝑞−1 𝑞−1
1.154 1
𝑦 = 1.154−1 𝑥 − 1.154−1 (0.32)
𝒚 = 𝟕. 𝟒𝟗𝟒𝒙 − 𝟐. 𝟎𝟕𝟖 44
Annotations

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XF : Mole fraction of methanol in feed
XD : Mole fraction of methanol in top vessel
Xw : Mole fraction of methanol in phase
vessel
Vt : Top vapor flow rate
Lt : Top liquid flow rate
Vb : Bottom vapor flow rate
Lb : Bottom liquid flow rate
TOL : Top operating line
BOL : Bottom operating line
R : Reflux ratio
Rmin : Minumum reflux ratio 46
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