US20170008870 Thca Crystallization Patent

I read through this Thca Crystallization Patent and it helped just solidify some understanding for me. It made me understand the necessity to remove any possible solids (Lipids and Fats or Otherwise) that would hinder the crystallization of Thca or cause the purity of your crystals to diminish.This step usually referred to as the dewax that many do inline, I believe needs to be done again cryo post extraction also. Even if your running your Closed Loop under cold conditions an extensive post dewax for maximum extract purity is essential. Once you have your Extract Filtrate as the Patent talks about you can try and Cryo Cold crash out your Thca crsystals or try some of the other methods that Unspokenpeace’s video talks about such as seeding, diffusion, or slow evaporation. Getting your Solution as pure as possible Pre-crystallization is best way to ensure crystallization success. Ill be posting some results soon with data for the new Forum.

Thca Crystalization Patent.pdf (118.1 KB)

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Interesting. Definitely a useful primer.

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take 100 grams and add to approx 500ml hexane isomers, direct from any extraction. non decarbed and non winterized, however winterized can be used. but virgin extract is preferred.

take 500ml distilled water and add sodium hydroxide until ph of solution rises to 13.

now take the dissolved hexane and extract solution and place in sep funnel. add slowly the ph 13 water.

allow to separate until emulsion layer breaks.

separate water out. at this point the water at ph13 will also have the thca, as well as some other compounds have now converted to thca as well. some. the water itself is what you keep, and a second wash may be done on the hexane wash with water, but the yield is very small, and not worth the time.

take the ph13 thca water and now add hcl to bring ph to 4-7. around 4-5 is best from what we have heard. the thca will precipitate out and cloud everything up. this may also cause a small foaming to occur so mix slowly and be careful. this is a chemical reaction from two components that do not solute together and begin to separate naturally.

once that water thca solution is back to neutral add back to sep funnel. then add new clean hexane isomers in the same ratio into the sep funnel with the thca water.

allow separation and emulsion layer to break. the hexane isomers with absorb the thca and it will separate from the water. remove the water and just flush a tad bit of hexane solution as well. remove contents of sep funnel inot rotovap and evaporate hexane, then place slightly liquid thca/hexane wash in vacuum oven.

turn oven up to 160-180f and vac off for abut 30 minutes and thc crystals will form.

**** replace hexanes with DCM, we are currently using dcm with great results.

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This A-B reaction works better with dicyclohexylamine, or better yet, choline chloride!

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Where do I get hexane that considered ok for me to use without having to distille or anything first

Any idea? I’m washing crystals and having the hardest time finding hexane that’s ok for me to use, I’m not exactly sure what grade to use or where to get

I would recommend against using hexane as it is believed to accumulate overtime in your system and is a nerotoxin. That’s why people started switching to pentane and heptane.

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Yeah I’m not, I can’t find either of those, restrictions against just anybody buying, I have 200 proof organic grain alcohol made for extraction to use, food grade,. I’m just trying to do quick wash,I have crystals already dried up, dry ice everything then buchner funnel it, with vac

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Or try pyridine instead of dicyclohexylamine, as it is soluble in non-polar solvents, though it doesn’t smell much better.

So they won’t return the hexane, if I distille it would it be ok then?

Will this work without distaliting

https://m.ebay.com/itm/n-Pentane-99-HPLC-Grade-125ml/273160486029?hash=item3f99a23c8d:g:IfAAAOSwfHBa0zyy

Man that’s pricy, yes it will work. For that price I would try to use it as many times as possible.

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DCM would allow for successive brine washes with very effective results. However how are you removing your DCM via simple distillation, then thin film?

I wouldn’t trust it with out and solvent CoA, even then I would be hesitant.Check this out for more info. https://www.epa.gov/sites/production/files/2016-09/documents/hexane.pdf

I believe it’s pentane hplc grade now not hexane, I took it off the list while back when I got that same reasons. Definitely not for me thanks bro

Hey Future ! Could you please elaborate on Choline Chloride in A and B reaction?
I was under impression it’s not soluble in hydrocarbons and barely soluble in alcohols.

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can citric acid be used instead of HCL or will the reaction not take place?

No cold crash, no dewax, no cryo.

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Ok so now that you have explained what you did not do, let’s talk about what you did

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Are you able to expand on the choline chloride? Isn’t it a solid?

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