Removal of MCT Oil from hash oil

Hash and Stuff Pre/Post-Processing
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Perhaps this will be useful to someone out there.

Recently came into a decent amount of hash oil that was mixed with MCT ~1:1 ratio that I’ve been asked to purify. They want it for edible formulation, not for a vapable product. Apparently it was too fluid for the specific edible formulation at that ratio. Distillation appears not to work.

I think I’ve been successful in removing the bulk of the MCT oil. Took the MCT/hash oil mixture and diluted with ethanol (10:1 ethanol:oil mixture) and put it in -80C freezer over night. Came back to find this:

IMG_20200223_170740
IMG_20200223_1707403456×4608 2.4 MB

At this point I diluted it with more ethanol, about 2x as much as I had originally (20:1) and froze again for 24hr and while it was still “gelled up” it became pourable with a little ambient warming. Filtered on a buchner and then back into freezer. Repeated this a couple times until no more MCT oil was visible.
Here’s some of the MCT that was filtered off. Saving this to rerun.

IMG_20200223_192447
IMG_20200223_1924473456×4608 2.57 MB

Then concentrated the solution on rotovap and back in freezer. After 24 hours still visible precipitate:

IMG_20200223_170749
IMG_20200223_1707493456×4608 3.07 MB

Eventually got to a point where there was no visible precipitate - where I am at now. Currently rotovaping off ethanol. Doubt one can remove all components of the MCT oil this way. But I’ve definitely removed a lot.

Also, acetone may be a better solvent to do this. I did some tests with MCT oil + acetone and MCT + ethanol, and when using acetone there appears to be less “gelling”. Not sure how to describe it other than the solution turns into a single solid blob. With acetone the solution is much more fluid and easier to filter cold. Maybe due to ethanol being a hydrogen bond donor to the carboxyl group of the triglyceride? Or maybe the -CH2CH3 interacting with nonpolar tail of triglycerides? Dunno.

Also, save the MCT oil that gets filtered out as it clearly still has some hash oil in it. I’ve collected this and will be repeating the process with more solvent to recover as much as possible.

Kind of a pain in the ass. Everything is slick with MCT oil now, fucking hate it. Don’t recommend, but if you have to, freeze precipitation works.

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I would think saponification might do a better job

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Probably your best bet is exactly what you’re doing. Be sure to do a few washed in your mct fraction to ensure you get all your goods

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Smart. I still have a lot of this mixture to process. Will give that a shot.

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Throw it into some heptane or something and get some pH12 water into the mix. Let me know how it goes. I think you could avoid the contamination issues that way.

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neat! here’s a thought… if you could keep the solution stirring/agitated while chilling, then maybe you could decrease the amount of hash oil and solvent that gets ‘trapped’ inside frozen MCT.

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Yeah good idea. Cooling in a dry ice bath on a stirrer or something like that should be easy.