CO2 as a Crystallization solvent

Pretty much what Plant2pipe said. It was thick and soupy, and had been dewaxed previously. Ambient temperature was probably 8-10°C around the vacuum oven

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Did the crystals remain after returning to atmosphere? I’ve seen stuff freeze under vaccum before, just no precipitation.

Yeah, it probably never got hotter than 38°C but the seed did not go anywhere after leaving it out all day. The slab of shatter on the pyrex was warmed up and scraped (including the seed), as it still had a bit of ethanol in there. When it finished drying it was glassy and very clear

Great thread! There is a book in the data dump “Formulating Poorly Water Soluble Drugs”. Check out Chapter 12, very good info on GAS precipitation. Overall the book has a lot of interesting topics. It is in the add new info folder. Thanks for putting this project together. The openness of everyone here in the community is great!

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I might have been the one to put it there lol GAS procedures start with a pure source and are usually used to make tiny microcrystals because they great for bioavailability. Selective crystallization and growing large crystals from a complex mixture is much trickier but def possible
Partial molar volume reduction of solvent for solute crystallization using carbon dioxide as antisolvent.pdf (405.4 KB)

Any chance you could give me the ballpark ratios for doing this?
1:4 ethanol:co2 or more like 1:10 (or 1:20?) Im planning for more like 1:10 bc of what (little) i know of CXE but I’m worried thats still too much ethanol.
also temperature- with the pressure you gave I’m assuming it needs to be cold in order for it to be in the liquid region of the phase diagram…

I am assuming those two factors are the most important for getting a high yield in this step, but I guess there is also the original ratio of extract to alcohol, which I’m guessing is less important as long as your within a good range.

I am planning on reducing under low heat a winterized cryo extract, throwing it in my 20L eden extraction vessel with some dry ice… If my understanding is correct, once the dry ice liquefies, as long as my ratio of solvent:antisolvent is correct, and my temperature is not off, the THCA should CRASH out of solution very quickly, and then I can drain/push the solvent off into the separator…
I’m not going to break anything doing this am I? :grimacing:

As a side note, this should only crash out any acidic cannabinoids, and that is due to their more polar nature compared to their decarboxylated cousins, right?

Any advice before I try this would be appreciated, thank you!

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Interesting but why not just throw it in the separator and attempt to overpressure the seperator . The PRV on it shouldn’t go off if you bring it up to 1000 psi . Then attempt the rest of what he described . I am very interested in this myself . Do you pull terps on your Eden ? and how are they ?

Found the “Formulating Poorly Water-Soluble Drugs” and looks promising and possibly a good resource! It is a couple hundred bucks, can you attest to its value or do you maybe have a sample (or whole) pdf available to you?

Thanks for the help!

I sent you message with the link.

Cheers and good luck,
Strull

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Just to clarify for others following along. The book @strull is citing is in the data-dump (my reading suggests @strull dropped it there for us).

If you haven’t explored the data dump, you’re missing most of the information available here.

I’d link to the data-dump, but @EvinAtEmerald needs to go find it themselves :wink:

Heres the PDF

1-s2.0-S0928098706001151-main.pdf (772.6 KB)

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At that point why not just use etoh to make diamonds? You can dewax etoh easily, you can scale it up and you don’t need all this ridiculous co2 high psi nonsense.

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I am about to start co2 diamonds in boiling pentane and just wondered if anyone has done this. I got the soluiton in a 5:1 ratio in pentant about to bring to boiling point then I think we are gonna let it evaporate or is there a better step in the crystalization? sorry about spelling tyoing fast

That does NOT make CO2 your crystallization solvent…

So this is probably not the right thread to look for hints on using pentane.

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the extration is Co2 for the thca and can you make diamonds in the Co2 machine itself?

That was the premise. Yes.

Are there different peramaters to set Co2 machine to make them in machine itself? the way that I saw was that you get your crude extraction from Co2 then whatever solution you use to winterize it, but when you run through a rotovap you use different temps to not decarb it, then you put your finished crude in a 5:1 ratio of pentane bring it to a 36c boiling point then let it crystalize slowly after settling by putting it in colder temps over time. I just wanna know if this how we are achieving Co2 diamonds. Im thinking we have to seed it to start crystalization. just asking questions if this is wrong pls correct me!

Did you read the thread you posted in?

My take is that no, there are not.

Unless you’re using ethanol as the solvent & CO2 as the anti solvent, and that might or might not count as using CO2 as the solvent…(above my pay grade…)

Your description is not incorrect.

However, that would be growing diamonds with pentane as the crystallization solvent.

It would certainly be using the CO2 derived thca, but it would not qualify as “CO2 diamonds” (imo) and would certainly not qualify as an example of using C02 as the crystallization solvent.

Just saying that if you want to use pentane as your solvent, CO2 is a red herring…

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the way im doing it with pentane would it still work to form diamonds? Im just trying to get a basics down on making diamonds then would like to try it with Co2 machine only.

If you’ve got thc-a over 70% in your oil, you’re likely able to crystallize in pentane