THC isolation from crude CBD oil

Both your cbd and thc would be deprotonted under those basic conditions. This deprotonation is what aids in increased water solubility. Can you explain why you think thc will remain in the water layer and your cbd will not.

Cbd would have two free alkoxides and thc would only have one which would mean if both alcohols are deprotonated on cbd it would be more readily dissolved in water over thc.

For all, yes the pka of the phenolic proton is around 10 (the same as other phenol protons).

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So, then this could theoretically work with minor adjustments. Bring to ph of 9.5-10, do your pulls, and neutralize the solution to bring out CBD, leaving THC in your organic layer.

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I think this is a better experiment unless i am missing something. The henderssen hasselback
Equation could determine your set point of ph and adjust the experiment accordingly.

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Even deprotanated the solubility of both THC and CBD are quite low. You will lose more CBD than THC to the aqueous wash. Since the THC level in the organic phase is much lower to begin with, you will still be left with a high concentration of CBD in the organic phase, by the time that you lower the THC concentration of your crude to acceptable levels. It will take multiple washes to get the THC low enough and this method might be better done with a counter current distribution. The biggest problems you are going to run into are emulsions forming at the high pHs. Unless your crude is already impeccable clean, there are going to the compounds with similar pKas to CBD and THC that are going to act as soaps. Also be sure to have good oxygen and temperature control. If you introduce too much oxygen, you are going to be essentially running a Beem test. You’ll turn the CBD in to a deep violet quinone.

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I have a few pounds of hemp I’ll be extracting as soon as I get my ethanol. I’ll play with these methods after cleaning the crude thoroughly and report back on the results. Hoping someone beats me to it, because between waiting for my solvent and lab testing, this could take a few weeks. I’m really wishing I majored in chemistry instead of getting a useless sociology degree. :expressionless:

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I just wanted to add this educational video for those of us without a chemistry background to get a better understanding of what is being discussed using these LL extraction methods mentioned above.

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As in cbd quinone ?
Been looking for a sop dooing cbd to cbd quinone for a while
Biggest problem No testing available to do iT No one has a GC with those standerds

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So I’m starting to have some faith in what @Deleted was saying here. I tried the liquid partitioning that Future outlined with THCA in another thread on my hemp extract (which conveniently matched what Columbo outlined above in this thread) and I thought I was getting CBD in my aqueous layer. The emulsion was taking a while to clear up during the second high PH brine wash and I didn’t have any way of speeding up that process, so I called it a night and figured I’d come back to it later. What I came back to this morning was crystals forming all around the organic layer, even along the bottom. Pretty sure they’re CBD crystals. The CBD stayed in the organic layer despite the PH being well above 11. I tried to capture the crystal formations in the photo below.

Have yet to test what precipitated out of the aqueous layer of the first wash after adding some hydrochloric acid, but I think it’s pretty clear that it’s not all the cannabinoids from my extract.

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The idea is that the hemp solute has substantially more CBD than THC, and THC has more of an affinity to crash out into the aqueois layer at pH conditions above 10.6 = yes there will be SOME CBD that comes out into the water, but what remains in the organic phase will be devoid of THC. You can repeat this process several times to ensure you get a truly THC-Free result. The Cannabinoids in the water layer can be reclaimed easily afterwards for little to no “loss”. Maybe someone much smarter than me could take this concept and scale it more efficiently & effectively using more precise pH levels and more more appropriate compounds/solvents.

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I have a sample of my crude before it even touched the sep funnel out for testing now. I’ll be taking a sample of the stuff after the two washes I already did, take a sample of it after a third final wash, and post my potency results once I get them all in. Though I didn’t get super accurate PH readings, I took pretty detailed notes on volumes and weights and all that, so I’ll post those details as well so we can settle exactly how efficient this method is.

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Yeah, high pH and temperature in the presence of Oxygen will degrade your CBD into several compounds, one of them being the CBD quinone. This paper Synthesis and Antitumor Activity of Quinonoid Derivatives of Cannabinoids has a method for producing it. They bubbled O2 through an ethanolic solution of CBD and 5% KOH at 0C for 3 hours to get a 20% yeild. They then purified it with crystallization in heptane.

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Damit i have tried this on thc to get to CBN at 23 % in weeks with pure oxigen treu a nano bubble machine
And Searching like mad for cbd quinone sop. Thank You so much for the lead
Guess @cyclopath is right
I love this place

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Wondering about the result of this?

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Interested to see how this came out, any success?

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Results should be in this week!

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Ran into complications with the lab, so that’s going to delay the actual results, but long story short the way I did tried this didn’t seem to work very well. The lab tech notified me that all my samples came back hot so I have to jump through a few more hoops to get my results back.:neutral_face:

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Where are you located Coppertop?

I have an HPLC in my lab and am in Colorado. Am working on figuring this out as well and the ability to get results without weeks of delay is game changer.

Feel free to email me at allhemptrading@gmail.com to discuss some options. Anyone interested in cooperative research in this field don’t hesitate to reach out!

All the best!

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Couldnt you save the thc water layer thats left over and crystallize out any CBD if its dissolved in the water? Then wash in cold pentane to remove residual thc since it wont crystallize? Lol crazy idea but water IS a solvent.

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Agreed

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Totally down with this. I have been reading about this like crazy and very intrigued. Im going to try it with crude and multiple samples of distillate(first pass, 3rd pass, heads, tails, etc).

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