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Fractional Distillation Newbie - Couple Questions

Fractional Distillation Newbie - Couple Questions

Fractional Distillation Newbie - Couple Questions

(OP)
Hi All,

New to the forum, electrical by schooling but tasked with dialing in a process for a spinning band fractional distillation system. I searched and read through all pages here on the subject but was hoping a nice person could answer a few things...

Details:

- Can pull vacuum down to 1 torr as needed
- Looking to distill high purity in single run of one compound while allowing all others around it (boiling point) to mix in a different collector
- This is a lab setup but has full computerized control of heating rate, reflux ratio, open/close cut temps, equilibration time
- The substance has fairly unknown properties (we can't test every lot every time) but we know the ratio of the substance we want is about 2:1 to all other substances combined when filled into our flask
- The compound we wish to capture in high purity begins degradation near its standard atmosphere boiling point

My main questions are:

- How do we provide enough heat rate without causing the material to degrade? It seems that in the process of collecting the lower boiling point materials, our flask temp reaches too hot of temp
- The column is already insulated. Would heating the outside be helpful?
- We never seem able to lock in on our vapor boiling point for long. The temp will either start to fall drastically at which point we increase the heat rate which seems to disturb the fractioning, or the temp will simply fluctuate wildly. Some root causes to check for and/or possible solutions?
- We see a lot of refluxing down the column back into the flask, my understanding is that we're flooding the column. Is that correct and why is it occurring? Too aggressive heat rate?

Any help at all would be greatly appreciated!

Look forward to contributing on the electrical side where I can.

Thanks

- Mike

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