Post-Ethanol Extracted Crude to Crystallization - Crystals Without Distillation?

If you do a good job of controlling your extraction variables such as solvent temp and soak times, you can easily acheive a high enough purity to be able to crystallize straight out of the crude. Ethanol -46°C usually is the magic number for lipid-free extract. You will however still pull terps, gums, and other chlora. Also, if working with room-temp solvent - remember to roto down your tincture to 15:1 or 10:1 before attempting winterization otherwise nothing will coagulate out.
Cheers!

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My question is mainly about your actual step of isolating the crystal. I am assuming you are just going to dilute and freeze which seems like what the patent suggests and that is the same free tek found on here. You may be able to get some cbd to crash out doing that it may just take quite some time. I think that SOP has about a week wait in the freezer before you see crystal.

Good luck and let us know how it goes.

With disty, warm dissolution + supersaturation with rapid cooling afterward (colder the better, -86°C is best) - we usually see significant crystallization after only a few hours.

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what is the time of maximum crystal growth or rather when do you pull the jars out of the freezer?

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The patent suggests that crystallization can be completed in 24-48 hours with the distillate under ideal conditions, or as little as 12 hours. I haven’t tested it though so who knows if it works as well as the patent suggests or with a lower purity starting material :man_shrugging:

“The exact period of time required for complete crystallization of the CBD will depend on the exact conditions. Typically, in accordance with the invention, the CBD solution is kept under the temperatures recited above for a period of at least 12 hours, preferably for a period of 12-60 hours, more preferably for a period of 24-48 hours.”

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@Deleted how are you cooling to -86?

Cryo-freezer

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Nice, the reason i like to take crude to dist before i induce crystallization for isolation is because i can crash in about 15-20 minutes, also it is useful to sell the intermediate processed distillate

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Interesting, from distillate to crystallized product approximately how much do you yield?

60-75% yields

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what is the time of maximum crystal growth or rather when do you pull the jars out of the freezer?

Few hours - usually overnight.

So you’ve confused me on this one… I assumed winterizing meant filtering frozen. The reason I ask is because I winterized with dry ice before and filtered nothing after having done the original wash at around -15°C. You make me wonder if there was too much solvent for the waxes to precipitate out. This makes much more sense I think… Awaiting for backup before I dwell on it for too long, hard to get the wrong thoughts unstuck.

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That’s exactly what he meant. If the fats aren’t supersaturated in the ethanol solution, they won’t crash out when chilled

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So if you are using generous amounts of solvent then you should vaporize/catch some solvent off to increase the saturation of the ethanol solution and THEN freeze and filter. This is a game changer for me, thanks for all of the help.

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Correct. Although it’s typically cheaper to extract colder and skip winterization entirely

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You have just stumbled into the #1 mistake we all made lol… (By “we all” I mean etoh extractors).

I find also a good SOP to force lipids to materialize is to recover ALL the etoh, then reintroduce etoh to make 1:1 dilution. Bring this 1:1 suspension to just below the Etoh boiling point, then slowly add super-chilled Etoh until you are at -20°C or colder for the whole mixture or you’ve acheived 10:1 dilution whatever happens first. If the color and texture doesn’t seem to change or there’s a few small lillypads floating around (kind of like fish-flakes), put the container in the freezer and continue to chill past -40°C. If the whole solution turns kind of a murky miso-soup-like texture, let it sit out for 30 mins, then filter through 25 micron - then back into the freezer overnight.

Staging filtration this way will make your life alot easier if you have exceptionally fatty material. :sunglasses:

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Can I see the patent please?

the link IS posted up thread…

You can find it by scrolling, or practicing your use of the search bar

http://future4200.com/search?q=@munkdooligan+patent

you might want to check out some of the other advanced search features as well

Last day vote @Beaker award

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