Experiment 2: Distillation (Bubble Cap) : No Section

Experiment 2 : Distillation (Bubble Cap)
No Section Page
1.0
Abstract
2.0
Objective
3.0
Introduction
4.0
Literature Review/Theory
5.0
Methodology
6.0
Results
7.0
Discussion
14
8.0
Conclusion
16
9.0
References
16
10.0
Appendix
17
ABSTRACT
Separation Laboratory 1 | 3 SKB Page 1

The main objective of this experiment is to determine the effect of operation time to the composition and volume of distillate, and also wants to determine the relationship between the volumes of distillate with composition of distillate. In distillation process, the purities of distillate is dependent on some factors such as the operating time, temperature, reflux factor and chemical properties. The unit operation distillation is a method used to separate the components of a liquid solution, which depends upon the distribution of these various components between a vapor and a liquid phase. All components are present in both phases. in this experiment, distillation bubble cap has been used which is consist of several trays in the column. This device has a built-in seal which prevents liquid drainage at low gas flow rates. Gas flows through a center riser, reverses the flow under the cap, passes downward through the annulus between riser and cap and finally passes into the liquid through a series of openings or slots in the lower side of the cap. At the bottoms contain mixture of ethanol and water heated around 70oc and 90oc where is in the range of ethanol boiling point. The top product (distillate) is contains of mostly pure ethanol which is obtained from the condensation process. The purities of distillate composition is determine by reflection index measurement. This experiment is run in 1 hour, and the data taken in every 5 minutes and recorded. A table of operation data has been constructed for record all the results. The general relationship between volume of distillate and composition of distillate can be conclude as, the more volume of distillate produce, the more higher the composition of desired distillate obtained. However, the result obtained is not the exact result because there are some errors occur during the experiment. Therefore, some precautious steps have been suggested in order to improve the result.
1.0 OBJECTIVE
Separation Laboratory 1 | 3 SKB
Page 2

The main objective of this experiment is to determine the effect of operation time to the composition and volume of distillate, and also wants to determine the relationship between the volumes of distillate with composition of distillate.
20 INTRODUCTION Distillation is a separation method in which mixture components in a liquid mixture are separated based on their relative volatilities. The distillation column provides an environment where the liquid and vapour phases can approach equilibrium within a column. The existence in gas phase is due to the vaporization process at the boiling point of the component. When the mixture is heat up, the component that has higher volatility will evaporate first. Besides that, the components that want to be separated via distillation should have different composition in vapor and liquid where it is equilibrium at the boiling point of the liquid. In fact, most solutions used in distillation process are highly volatile such as ammonia-water solution and ethanol-water solution. Separations of components are easier to happen if the relative volatile mixture is high. Separation is achieved by condensed vapor flowing as a liquid down the column theoretically achieving equilibrium with the vapor flowing up the column. The distribution of components differs in each phase and results in the separation. In the case of a binary mixture in batch distillation under total reflux, the vapor condensing at the top of the distillation column will be rich in one of the components. Liquid leaving the reboiler at the base of the column rich in the other component. As the system reaches equilibrium the separation process reaches steady state for that apparatus and set of operating conditions. This experiment is designed to study the distillation of a binary mixture of Ethanol Water in a tray distillation column. As other processes, there will be a few factors that affect the system such as temperature and time that may affect the composition of the distillate. Therefore, the objective of this experiment is to determine the effects of the operation time with the composition and distillation volume beside to determine the relation between distillation volume and distillation composition. This experiment was started with the preparation of 32 liter of ethanol-water mixture solution with composition of ethanol (30%) and water (70%). The feed was allowed to be heated for a while. Ethanol which has a higher volatility or a lower boiling point compared to water will evaporate first when heated. The ethanol vapor will enter the bubble cap distillation column. Condenser will condense the ethanol vapor at the top with cooling water. The condensate will undergo a series of cooling before collected to make sure vapor is complete condense into liquid phase. After finish this experiment,

we can determined the time needed for a certain composition to distillate and indentified the relation between reflux ratios with the volume of distillate. 3.0 THEORY A group of operations for separating the components of mixtures is based on the transfer of material from one homogeneous phase to another. Unlike purely mechanical separations these methods utilize differences in vapour pressure or solubility, not density or particle size. The unit operation distillation is a method used to separate the components of a liquid solution, which depends upon the distribution of these various components in their volatilities in boiling liquid mixture. Distillation is used to purify a compound by separating it from a non-volatile or lessvolatile material. When different compounds in a mixture have different boiling points, they separate into individual components when the mixture is carefully distilled.
Figure 1 Typical Distillation
Column set up
The performance of a distillation column is dependent on many factors such as: a) Composition of feed, b) The vapor liquid equilibrium characteristics, c) Trace elements that can severely affect the Vapor liquid equilibrium of liquid mixtures

d) Internal liquid and fluid flow conditions, e) State of trays. The state of the feed mixture and feed composition affects the operating lines and hence the number of stages required for separation. It also affects the location of feed tray. Some columns are designed to have multiple feed points when the feed is expected to contain varying amounts of components. The actual number of trays required for a particular separation is dependent on the efficiency of the plates. Thus, factors that cause a decrease in tray efficiency changes the performance of the column. Trays have two main parts: a) The part where vapor (gas) and liquid are being contacted; the contacting area and b) The part where vapor and liquid are separated, after having been contacted; the down comer area. Classification of trays is based on: a) Type of plate used in the contacting area b) Type and number of down comers making up the down comer area c) Direction and path of the liquid flowing across the contacting area of the tray d) vapor (gas) flow direction through the (orifices in) the plate e) Presence of baffles, packing or other additions to the contacting area to improve the separation performance of the tray
Common plate types, for use in the contacting area: a) Bubble cap tray has riser or chimney fitted over each hole, and a cap that covers the riser. The cap is mounted so that there is a space between riser and cap to allow the passage of vapour. Vapor rises through the chimney and is directed downward by the cap, finally discharging through slots in the cap, and finally bubbling through the liquid on the tray.
Figure 2 Bubble cap tray b) Sieve trays come with different hole shapes (round, square, triangular, rectangular (slots), star), various hole sizes (from ~2 mm to ~25 mm) and several punch patterns (triangular, square, rectangular).
Figure 3 Sieve tray c) Valve tray come in a variety of valve shapes (round, square, rectangular, triangular), valve sizes, valve weights (light and heavy), orifice sizes and either as fixed or floating valves.
Figure 4 Valve tray d) Combinations of these types are applied: plates with both sieve openings and valves, as well as plates with both light and heavy valves. 4.0 METHODOLOGY 4.1Material and apparatus Bubble-cap distillation column, refractometer, syringe beaker, measuring cylinder, reagent bottle, stop watch, water and methanol. 4.2Procedures
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1. Seven set of methanol-water mixture were prepared using pipette. After that, the refractive index of the mixtures was determined using refractometer. 2. 32 liter of the feed of ethanol-water mixture of 30 % ethanol and 70 % water was prepared. 3. Every apparatus was in good condition before experiment started. 4. Then, the position of the valves were adjusted as below:
a. Opened: V2, V8, V10 b. Closed: V1, RCV1, V3, V4, V5, V6,V7, V9, FCV2
5. Electrical heater was switched on as the cooling water pump was switched on. 6. Initially power supply is the maximum, it was minimised after the feed boiled.
7. Reflux control was set at 2.0 by opening the reflux control valve (RCV 1) slowly. The distillate
was following to RI 1B and the extra distillate was following to RI 1A and return to boiler. 8. Distillate was controlled to not flow back to boiler by: a. V2 closed b. V3 opened (V3 closed if V4 opened)
c. V4 opened (to get sample) 9. The distillate collected was measured. Sample composition was analyzed using refractometer to get the refractive index. 10. Step 9 and 10 were repeated for every 5 minutes. The result was recorded as Table 4.1.
4.3 Several precautions during and after handling the experiment 1. The flow meters should be operated smoothly in order to avoid pressure surges within the equipment 2. The flow rates of liquids should not exceed the maximum rates of the flow meter 3. Safety glasses and safety helmet must be worn at all times in the laboratory and appropriate rubber gloves must be worn when organic solvents are handled 4. Check the zero errors of the manometers and adjust the reading to zero if necessary.
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5. After the process was finished, turn the reboiler power switch off and Main power control switch off. When condensate no longer collects, the cooling water to the condensers need to be shut off.
5.1
RESULT
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Volume of Ethanol (ml) Volume of

TIME 5 10 Water (ml) TI 1 79.0 2078.9 Mole ofTI 1A 78.3 79.3 Ethanol 0.000 TI 1B 76.0 76.0 15 20 25 18 79.1 78.8 15 78.7 79.0 78.9 78.8 0.034 0.086 76.0 76.0 76.0 79.4 30 35 40 10 78.9 78.8 5 78.8 79.0 78.80.257 79.4 0.171 76.0 76.0 76.0 79.4 45 50 55 2 78.7 78.7 0 78.6 78.8 78.80.343 78.7 0.308 76.0 76.0 76.0 79.2 60 78.6 78.7 76.0 79.2
10
15
18
20
(mole)
Mole ofTI 2 Water (mole) % Mole of

TI 2A Temp Refraction eratur e in Index TI 2B plate TI 2C TI 2D TI 2E TI 2F TI 3 Initial temperat u-re Tempera t-ure of cooling water Reflux TI 4 TI 5 TI 6
79.5
1.110
78.5
0.999
79.4
0.833
79.3
0.555
79.3
0.278
79.3
0.111
79.2
0.000
79.0
0.00
79.2 79.2
3.29
80.1
9.36
79.5 78.8
23.55
79.0
48.04
78.9 78.9
73.51
78.8
100.00
79.0 78.8 78.8
Ethanol (%)
1.3350
79.0 79.0
1.3370
79.0
1.3410
79.0 79.0
1.3470
79.0
1.3525
79.0 79.0
1.3530
79.0
1.3600
79.0 79.5
79.0
75.0 76.0 76.0 78.0 24.0 28.0 5.2 2.0 195 1.363 0
76.0 76.0 77.0 78.0 24.5 29.0 5.4 2.0 220 1.36 35
76.0 77.0 77.0 79.0 24.5 29.5 5.8 2.0 220 1.36 30
76.0 77.0 77.0 79.0 25.0 31.0 5.8 2.0 225 1.36 30
77.0 78.0 78.0 79.0 26.0 32.0 5.4 2.0 220 1.36 30
77.0 78.0 78.0 80.0 26.0 32.5 5.0 2.0
77.0 78.0 79.0 80.0 28.5 32.5 5.6 2.0
77.0 79.0 79.0 80.0 27.0 32.5 5.6 2.0 225 1.36 30
77.0 79.0 79.0 80.0 27.0 32.5 5.4 2.0 220 1.36 30
77.0 79.0 79.0 80.0 27.5 34.0 5.2 2.0 225 1.36 30
77.0 79.0 79.0 80.0 28.0 34.5 5.6 2.0
77.0 79.0 79.0 80.0 28.0 35.0 5.4 2.0
RI 1A RI 1B Ratio of Reflux Distillate volume Reflexion index Voltage Current
225 225 1.36 1.36 30 30 24 170
230 180 1.36 1.363 30 0
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Table 1: Table of relationship between volume of ethanol with reflexion index Data (Reference : Elementary Principles of Chemical Processes) : M.W ethanol = 46.07 M.W water = 18.016 SG ethanol = 0.789 SG water = 1.000 For 2 ml of methanol and 18 ml of water: Mole of ethanol Mole of water % mole of ethanol = = = 2 x 0.789 46.07 18 x 1.000 18.016 0.034 x 100% 0.034 + 0.999 = 3.29 % = 0.999 gmol = 0.034 gmol
Graph 1: Graph of refraction index versus %mole of ethanol Example of calculation of % ethanol from refraction index:

Refraction index = 1.3630 The equation from the graph, y = -5E-06x2 + 1.3334 1.3630 = -5 10-6x2 + 1.3334 -5 10-6x2 0.0296 =0 x = 76.94 %
Refraction Index 1.3630 1.3635 1.3630 1.3630 1.3630 1.3630 1.3630 1.3630 1.3630 1.3630 1.3630 1.3630
Percentage Mole of Ethanol
Volume of
(%) Distillate (mL) 76.94 195 77.59 220 76.94 220 76.94 225 76.94 220 76.94 225 76.94 225 76.94 225 76.94 220 76.94 225 76.94 230 76.94 180 Table 4.2.2: The % mole of ethanol at different time
Time (minutes) 5 10 15 20 25 30 35 40 45 50 55 60
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Graph 2: % mole of methanol versus time
Graph 3: Volume of distillate versus time
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6.0 DISCUSSION (A) Graph 1: Graph of refraction index versus % mole of ethanol Initially, the refraction index is directly proportional to % mole of ethanol, giving a positive value of slope. The slope is reducing as % mole of ethanol increases, and at one point, the refraction index becomes indirectly proportional to the % mole of ethanol resulting in negative value of slope. As the graph illustrates the relation between mixed refraction index and ethanol composition, it is used as a standard reference for the samples on order to determine the percentage of ethanol in the distillate. (B) Graph 2: Graph of % mole of ethanol versus time The values of % mole of ethanol are constant except for the time at 10 minutes. We can simply say that along the distillation, the percentage of ethanol in the distillate does not undergo any change. Theoretically, the composition of the ethanol will decrease as time goes on because the experiment is conducted in an enclosed system at a constant reflux ratio. The amount of ethanol left in liquid phase will decrease as most of it is distilled out via gas phase and at the same time; there is no fresh feed of ethanol to the system. The small difference of the results compared to the theory is due to the fact that the distillate is not put into the refractometer immediately. Ethanol has high value of vapor pressure and can easily vaporize. If the distillate is exposed to the surrounding for too long before being valued in the refractometer, ethanol will vaporize to the surrounding and the value read from the refractometer is not accurate. (C) Graph 3: Graph of volume of distillate versus time It can be seen that the value of volume measured are almost same. The linear equation that represents the data shows a straight line with a negative slope. Theoretically, the volume of distillate will remain constant throughout the experiment. Although the slope is negative, we can say that our results do obey the theory as the value of the slope is too small to be considered.
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Advantages of Bubble-Cap Column 1. Can overcome flood problem although the air rate used is low. 2. Range of operational temperature for Bubble-Cap Column is wider compared to the PackedDistillation Column. 3. If the flow rate of the mixture is low, the Bubble-Cap Column can provide more surface are for effective interference. 4. It is more economical compared to the Packed-Distillation Column. 5. The curly tubes acting as cooler can be arranged in a more pack arrangement in order to achieve a better result. 6. It is considered as more relevant because it is easier to be cleaned when any unwanted particle is found in the column. Errors 1. Parallax error that occurs when taking the reading of the refraction index, volume of distillate which is caused by the false position of eyes that is not parallel to the level. 2. The fluid level at RI 1B is not constant at 2.0 and always changing resulting in inconstant volume of distillate. 3. Systematical error in the usage of watch. 4. Dirty glass condition at refractometer may affect the value of refraction index.
5. There is probability that the volume of distillate may be lower than it really is as the result of
vaporization of ethanol to the surrounding. This happens when taking it out from the valve V4 i.e. the ethanol temperature is greater than the surrounding temperature. 6. Unwanted particle in the column and instrument may affect the result of the experiment. Precaution 1. The glass of refratometer must be cleaned with distilled water every time before taking the reading. 2. Eye position must be parallel with the level of distillate. 3. Reflux RI 1B must be set constant at 2.0. 4. All the instruments used must be free from any unwanted particle. 5. Operational temperature must always be under 100C to prevent the water from vaporizes. 6. All the valves must be close tightly.

7.0 CONCLUSION From the experiment, the % mole of ethanol is not changing with time along the distillation process. Mole fraction of ethanol obtained is in the range of 76.94 ~ 77.59%. The volume of distillate is also not changing with time along the distillation process. The value of the distillate volume is in the range of 180 ~ 230 mL. 8.0 REFERENCES
1. Geankoplis, Christi J., Transport Processes And Unit Operations, Third Edition, Prentice Hall
International, New Jersey, 1993.

2. McCabe, Warren L., Unit Operation Of Chemical Engineering, Fifth Edition, McGraw-Hill Inc.,
New York, 1993.

3. Perry, Robert H., Don Green, Perrys Chemical Engineering Handbook, Sixth Edition, McGraw-
Hill International Edition, New York , 1993.

4. Ronald W.Rousseau, Elementary Principles Of Chemical Processes,2nd Edition, John Wiley,
New York, 1993 .

5. Sinnott, R.K., Kejuruteraan Kimia Jilid 6, Dewan Bahasa dan Pustaka, Kuala Lumpur, 1994.
9.0 APPENDICES
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