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Fractional Distillation Questions

Hey all,

I'm interested in learning about fractional distillation of concentrates. I'm sure this has been answered before, so please excuse me, I am trying to get a more clear idea and could use your input.

What vacuum pump would be good for a small scale setup? I'm not going to be running it daily. I understand a low micron pump is needed, but is it necessary to buy one of the 2-3k$ ones?

Is it possible to process small amounts in a larger boiling flask, or does the flask size need to be adjusted depending on how much crude extract your starting with? For example, can I run 100 grams in a 3000ml boiling flask?

For starting material, I was hoping to use cold 99% ISO to make the crude concentrate and use winterization/filtration to clean it up. I was hoping to avoid using a closed loop system if possible, is anyone using this type of method?

Thanks, any input is much appreciated!
 

troutman

Seed Whore
They sell vaccum pumps on EBAY or Amazon for a few hundred $$$ that are good enough to get you started.

I don't think there's a problem running 100 grams in a 3000 mL flask.

Running small amounts in a small flask make it easier to clean and process that's all.

Why heat up or dirty a large flask if you don't need to?
 
Thanks for the reply. I am starting to get a better idea of what I will need to get. I have a 3000ml heating mantle with distillation glassware and was thinking of using that to start out, but I don't plan on processing large amounts and the glassware is only setup for simple distillation.

I am thinking I should get a smaller, 1-2L setup designed for fractional distillation with the rotating flasks and cold trap. Then If I want to use a larger sized boiling flask I can use the 3000ml with the new short path glassware, seeing how the ground joints are the same size.

Another question is, how important is the chiller? Will a ice water bath or hydroponic chiller be enough or does it have to get a lot colder?
 

troutman

Seed Whore
If you have ice left in your ice water bath it's cold enough.

Try to get as big of a cooler or container as possible for your chilling setup.

I chill my condenser with a 500 GPH aquarium pump and the glass gets very cold.
 
Brickweeder, I saw a soxhlet apparatus in one of the videos, but no distillation. Was this what you were referring to? I might have missed the one you were thinking of. There are a few videos on short path distillation on youtube but not as many as I hoped for. It seems people are fairly tight lipped about there processes.

I am planning on trying a cold ethanol extraction to use as the starting material. Luckily I have a dry ice supplier nearby, so I should be able to keep nice and cold. I'll try to post some pics of the process.
 

brickweeder

Well-known member
Its been a while since I watched them, but I seem to recall a vid where he showed an after extraction process where he had a setup to distill off the solvent, and condensed it to a separate container for later reuse, leaving behind the oil extract. I think his setup was akin to a makeshift pot still rather than a fractional still. I hope I am not confusing someone else's vids with the MG vids.
 
After reading quite a bit on the subject, I'm steering more towards cold ethanol extraction than ISO. I like the idea of using super chilled ethanol with dry ice and hopefully bypass the winterization step. I'm still trying to decide if it would be better to do a room temp or warm extraction to try and get all of the thc and then try to dewax/degum with filtration methods. Something tells me it is better to just extract cold, because there would be quite a bit of loss in product with all the filtration steps used with really crude oil.

I have a simple distillation apparatus that works well for recovering smaller amounts of solvent. Also, I was thinking a regular moonshine still would be good for larger amounts and then finish it off in the simple distillation setup.

Most of the product will be going into vape cartridges so I am not to worried about it getting decarbed in the recovery process. The recovery setup does have a vacuum adapter so I could distill at a lower temp if necessary. I tried running it with a vacuum, but the heat mantle doesn't have a stirbar so I was getting serious bumping in the boiling flask. I still have a lot to learn about running a still under vacuum. The solvent boils way faster and is way more sensitive to temp changes compared to a open air system
 
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