Sunday, May 31, 2020

Distillation of Methanol from Water







Simple and Fractional Distillation

Institution Affiliation

Date



Table of Contents



PURPOSE

The objective is to help understand the concept of distillation by separating a mixture of methanol and water using fractional and simple distillation methods. Water and Methanol are miscible. Simple and fractional distillation methods will be used to demonstrate how to separate miscible substances. Although the distillate that is collected from this experiment is not expected to be 100% pure, the effectiveness and efficiency of the process will be discussed with respect to each distillation process to help compare and determine between the two which one is more effective and why. These experiments will help learners understand the complex industrial distillation process done on a large scale.

 INTRODUCTION

Miscible liquids are separated through the process of distillation. A solution is heated until it starts to vaporize, then cooled down to back to liquid. Liquids which have different boiling point evaporates at different stages (Nicholas 2017).  Simple distillation is used to separate liquids which has a wide gap in boiling point, while fractional distillation is suitable for separating substances which has a closer gap in boiling point. The liquid with a lower boiling point will change to vapor first, passed through the condenser where it turns back to liquid and is collected container as distillate (Nicholas 2017).

EXPERIMENT PROCEDURE

Simple distillation

Apparatus required

Round bottom flask, Vacuum Adapter, Water condenser, Thermometer adapter, Thermometer, ‘Y’Shaped multipurpose adapter, Jack, Woodblock, Clamps, Graduated cylinder, Boiling chip, Water tube and Heating mantle.

Preparation for Simple distillation

I.            Set up the apparatus above as shown in fig 1.1
Figure 1.1 a complete set-up of apparatus for simple distillation
II.            put 20ml methanol and 20ml water in round bottom flask
III.            Add a boiling chip to the mixture
IV.            When the set up is complete turn on the water and the heat source.

Observations from simple distillation experiment

        I.            The table below contains the reading of the Volume of distillate after every 2ml against their respective temperature.
Vol ml
0
2
4
6
8
10
12
14
16
18
20
22
24
25
Temp C)
63.4
63.7
65
66.3
67.8
68
70
70.8
72.8
75.5
78.2
83.3
87.8
88.6

Fractional distillation

Apparatus required

Round bottom flask, Vacuum Adapter, Water condenser, Thermometer adapter, Thermometer, ‘Y’ Shaped multipurpose adapter, Clamps, Graduated cylinder, Boiling chip, Water tube, Heating mantle, Fractional column.

Preparation of Fractional distillation

        I.            Gather all the apparatus required and set-up a fractional distillation as shown in fig 1.2 below.
Figure 2.1 complete set up of apparatus for fractional distillation.
     II.            Mix water 20ml and Methanol 20ml into a round bottom flask.
  III.            Add a boiling chip into the mixture.
  IV.            Switch on the heating mantle to Start heating the mixture.
    V.            Connect the water source and ensure that cold water is continuously running through the condenser.
  VI.            Continue heating the solution even after it start boiling.
VII.            Once the first drop is collected in the graduated cylinder, read the temperature on the thermometer.
VIII.            Take the reading of the thermometer after every increment of the distillate in 2ml.
  IX.            After all the readings are taken, disassemble the apparatus once they cool down.

Observations from fractional distillation experiment

a)      The table below contains the reading of the Volume of distillate after every 2ml against their respective temperature.
Vol ml
0
2
4
6
8
10
12
14
16
18
20
22
24
25
Temp (°C)
58
60
60.7
61.5
62.3
63.1
63.9
65.0
66.7
68.0
73.8
86.2
90.8
91.3

DISCUSSION

Graphical illustrations



Distillation Process

Add 20ml water and 20ml methanol into a round bottom flask, then set-up the apparatus as shown in fig 1.1. Start heating the mixture by adjusting the power knob that supplies power to the heating mantle. Continue heating the mixture until it boils. Ensure a continuous flow of cold water through the condenser. Take note of the temperature when the first drop falls to the graduated cylider. Continue recording the temperature after the distillate increases at an interval of 2ml in the graduated cylinder.

Differences between simple distillation and fractional distillation

Fractional distillation is a more complex process that uses fractional column while simple distillation is a simpler process and the fractional column is not used. The reason why the fractional column is used in distillation is to separate a mixture of fluids which has a relatively closer boiling point (Mia et al. 2017).

Explanation of Observations from the Graphs

The first drop in the fractional distillation came out at 580C while that of simple distillation came out at 63.40C. Also, both lines increase at almost the same gradient up to at around 20ml after which the gradient for fractional distillation becomes steeper as compared to that of simple distillation. This implies that most of the all methanol had vaporized and the remaining solution has to be heated harder for it to vaporize.

Boiling point of methanol

From the graphical illustrations, both graphs have two different boiling points. The boiling point of methanol is 63.4 0C in simple distillation and 580C in fractional distillation. 64.70C is the accepted boiling point for methanol (Jerry et al. 2014).
Contrary to my expectation, the accepted boiling point at 64.70C is closer to the boiling point of methanol at simple distillation. This should not have been the case if the error discussed hereunder wasn’t there. The boiling point of fractional distillation should have been closer to the accepted boiling point because it does not have the fractional column which contains steel wool or glass beads meant to increase the surface area. This makes the vapor to condense and return back to the boiling mixture many times before vaporizing and reaching the topmost of the column, due to the aspect of condensing and re-vaporizing the boiling point reading becomes more accurate than that of simple distillation method.

Waste Disposal

At the end of our distillate, we need to dispose of the distillate into the non-halogen organic solvent bin. After disposing we should ensure that the bottle where we put the waste is closed always.

Safety Protection and Precaution

Methanol is poisonous and therefore, after the experiment one should always wear lab coats, Protective eyewear, gloves, and closed-toe shoes at all times when experimenting. It is also highly flammable and therefore one should take caution not to sprinkle it so as not to cause fire. We should not eat anything in the laboratory as it might be contaminated and dispose properly laboratory waste (Peter 2016).
1n 1926, the federal government intentionally increased the amount of methanol used in industrial alcohol to poison alcohol in an attempt to curb alcohol consumption.

Distillation of Ethanal

Ethanal can be distilled from a mixture of water using both methods because they have different boiling points (Jerry et al. 2014).

Distillation Real-world applications

a)      Separation of oil products
Crude oil comprises different petroleum products, these petroleum products in crude oil have different boiling points and therefore they are separated using fractional distillation (Sukasem, Hareemao, & Sudawong. 2017).
b)      Distillation of salty water
A large distillation plant can be used to purify salty water and supply many people with clean drinking water and also be used to cook.

The precision of the Thermometer

The precision of the thermometer is the fraction to which a thermometer can be read, it can also be defined as the nearest whole number or decimal to which a thermometer can be read.  In our experiment the precision of the thermometer is 0.10C.

Errors and Omissions in the experiment

There was a critical error made during the transition from simple distillation to fractional distillation. The instructor did not completely change the entire set of apparatus he used for simple distillation. Instead, he only added a fractional column and proceed with the experiment on fractional distillation.

CONCLUSION

Distillation is the most commonly used method of separating a mixture of two or more liquids. The process applies a simple rule of separating mixtures based on their boiling points. It has traditionally been used to perform complex industrial separation of substances in the food industry, chemical, and petroleum industry. It should be understood that distillation is an irreversible process, and is commonly used alongside other procedures to ensure that the distillate is 100% pure.


REFERENCES

Pater, L. (2016). The mimic of fractional distillation technology distillation process          modeling. arXiv preprint arXiv:1605.00097. Jerry . M., David G. A., Gretchen E.
Mia, M., Islam, A., Rubel, R. I., & Islam, M. R. (2017). Fractional distillation &    of tire-            derived pyrolysis oil.
Sukasem, N., Hareemao, T., & Sudawong, C. (2017). The mimic of fractional distillation technology      for the development of homegrown pot distillery for ethanol     distillation. Energy Procedia138,     985-990.
Jerry R., Paul F. S., & Christina N. H. (2014) Laboratory Techniques in Organic Chemistry.         Library of             Congress Control Number: 2013955847
Dr. Nicholas L., (2017). Fractional Distillation. URL: https://www.jove.com/science-        education/5700

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