Experiment on Distillation Principles

Abstract

The general objective of this experiment is to investigate and understand distillation principles, the parameters affecting the operation of distillation columns and how to determine optimal operating conditions. To achieve this, two experiments were carried out. Experiment one was carried out to investigate the relationship between the column pressure drop and the boil-up rate, the second experiment was performed to determine the composition of the mixture of dichloromethane-trichloroethylene. The data obtained in experiment one and two were used to determine the overall column efficiency.

In order to investigate the pressure drop of the column, the power was set to 0.65 kW, 0.75 kW, 0.85, and lastly 0.95 kW. For each power input, the sample was collected for 10 seconds and then the procedures were repeated for each increment. Afterward, a graph of pressure drops against the boil-up rate (log/log) to determine the relationship between the two parameters. It was observed that the pressure drop and the boil- up rate increased as the power input increased and also that the degree of foaming increases as the power was increased from gentle at 0.65 kW to violent over the whole tray at 0.95 kW. The samples collected were tested for its Refractive Index. It was observed that the degree of foaming increases as the power was increased from gentle at 0.65 kW to violent over the whole tray at 0.95 kW.

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The overall efficiency of the column for a power of 0.65 kW is 42.5%. However, that may not be the most optimal condition since it was not possible to test for other three power input due to some systematic and technical errors.

Table of Contents

Nomenclature…………………………………………………………………………..

Introduction…………………………………………………………………………….

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Objectives………………………………………………………………………………

Methodology………………………………………………………………………………..

Results…………………………………………………….………………………………..

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Discussion of Results…………..………………………………..………………………..

Conclusions ………………………………………………………………………………..

References ………………………………………………………………………………..

Nomenclature

n = number of theoretical plates

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X_A = mole fraction of the more volatile component

X_B = mole fraction of the least volatile component

α_av = average relative volatility

Subscripts D, B or d, b indicates distillate and bottoms respectively

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∆H̅_vap = average latent heat of vaporisation of DCM-TCE mixture (J/mol)

R = 8.314 J/mol*K

T_b(TCE) = boiling point of trichloroethylene (K)  

T_b(DCM) = boiling point of dichloromethane (K)

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Introduction

Distillation is defined as a process in which a liquid or vapour mixture being made of two or more components is separated into its component fractions with the desired purity, by the input and removal of heat.

Distillation is one of the most common liquid-liquid separation processes and can be carried out in a continuous or batch system. The basic theory behind them is very simple and relies on separating a mixture being made of two or more components of different boiling points, though partial vaporisation of a liquid mixture or by partial condensation of the gas mixture. As the mixture is fed to the column, some fractions may vaporise and move up the column. The vapour components will condense and leave the column at different levels as the temperature is lower at the top of the tower. Based on a binary mixture, the more volatile component will leave at the top of the tower, and the less volatile component will leave at the bottom as a liquid.

Objectives

The objectives of this experiment are:

1. To investigate the pressure drop of the distillation column for four boil-up rates, and observe the degree of forming for each power supply
2. Use of refractometer to determine the overhead and bottom mixture composition
3. To determine the overall column efficiency

Literature Review

Distillation columns are usually made up of a vertical tower containing a series of plates. As liquid runs down the tower vapour goes towards the top. In order to understand its working principle, consider what happens when heating a liquid. At its boiling point, the molecules of the liquid possess enough kinetic energy to escape into the vapour phase (evaporation) and if the temperature decreases some molecule in the vapour phase return to the liquid phase (condensation). The same with the mixture of dichloromethane and trichloroethylene for this experiment. As heat is applied to the column, the eventually the most volatile component (in this case trichloroethylene) begins to vaporize. As the trichloroethylene vaporizes it takes with it some part of dichloromethane. The vapour mixture is then condensed and evaporated again, giving a higher mole fraction of the least volatile component in the liquid phase and a higher mole fraction of the most volatile in the vapour phase.

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For this experiment, the column was be set to operate at total reflux. Which means that all the overhead products are be condensed and fed back into the top of the tower and allowed to flow to the bottom of the column, i.e. overall no top product is taken out of the system while the column is operational.

The total pressure drop across each tray is the sum of that caused by the restriction of the holes in the sieve tray, and that caused by passing through the liquid (foam) on top of the tray.

As the velocity of the vapours passing up the column increases then so does the overall pressure drop. The velocity can be monitored by varying the boil-up rate which is done by changing the power input to the reboiler. Under certain conditions where only the vapour phase is present, the trays will act as an orifice and in that, the velocity will be directly proportional to the square root of pressure drop. However; this relationship does not become visible until the head of liquid has been overcome and foaming is taking place. In a graph of log pressure drop vs. log boil-up rate, at low boil-up rates, the pressure drop will remain almost constant until foaming occurs when the pressure drop would be expected to rise sharply for unit increases in boil-up rate.

Key Definitions

Column efficiency:  The overall efficiency is defined as the ratio of the number of theoretical trays to the actual number of trays required for an entire column.

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Foaming: Foaming regarding distillation column is defined as the expansion of liquid due to the passage of vapour, or gas. Although it provides good liquid-vapour contact interfacial, however, excessive foaming may lead to liquid build-up on column trays.

Boil- up Rate: Also called the distillation load. It is the rate at which the mixture is being distilled in the column.

McCabe Thiele Diagram. It is a diagram where y is plotted as a function x along the column provides an insightful graphical solution to the combined components. It is mainly used to determine the minimum theoretical plates required in a distillation column for separation of binary mixtures.

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The Fenske Method: similar to McCabe Thiele Diagram, it is a method used to determine the minimum number of theoretical plates required in a distillation column for separation of binary mixtures. It uses equation (4).

Methodology

APPARATUS