Experimental Strategy and Learning Objectives Distillation

Group:
Demonstrator:
Names:

Stream:

Supervisor:
Arjun Ahluwalia, Glen Davies, Natalie Jones, Mark Thomas

Learning Objectives
To revise and gain understanding of the distillation process.

To take into account the economics and costs of a process.

To understand the environmental and safety issues of a distillation process.

Experimental Objectives
To recover 85% of the initial methanol as a distillate of composition 97
mol% methanol.
Experimental Method
Firstly a calibration curve needs to be created for the refractive indices in order
to see what compositions are achieved from the distillation at the various stages.
This will be done by making up different concentrations of methanol to deionised
water at 10% intervals. After mixing, a refractive index is taken, ensuring a
constant temperature is maintained with each sample.
Make up a solution of 10%v/v methanol and 90%v/v deionised water.
The distillation column will be set up according to the operating manual.
First run the distillation column at each reflux ratio for a set time to be
determined. After each run, the composition and volume of the distillate is
measured. From the results, the optimum reflux ratio can be found.
The column will then be run at the optimum reflux ratio to see how the
composition varies with time.
The column needs to be heated to 64C which is the boiling point of methanol.
This temperature needs to be maintained to ensure the temperature doesnt
reach the boiling point of water.
After each run, a sample is taken of the distillate and then the remaining
distillate is put back into the still with the remaining solution. Taking a sample
will affect the concentration of methanol in the still and this will need to be
considered along with the results.
For consistency, the same team member will be assigned to the following roles:
Monitoring temperature of distillation column.
Timing of the experiment.
Taking samples of distillate at the end of each run.
Analysing the samples using the refractometer and/or gas liquid
chromatographer.

Experimental Variables

Theory
Initially the process is run at varying reflux ratios in order to find which is the
optimum reflux ratio. For the second part of the experiment, the reflux ratio is
kept constant, but at a constant reflux the composition of the distillate will
decrease with time.
Analysis of Data
A calibration curve will be plotted as detailed above.
Talk about density and calcs.
Suitability
Health and Safety
Refer to the appropriate Risk Assessment and COSHH form for this experiment.
References
I. M. Smallwood. Handbook of Organic Solvent Properties. Elsevier, 1996, Section
2. Alcohols.