THC isolation from crude CBD oil


#21

:+1:

Just wanted to be sure we were attacking the right problem.

Crystallizing the CBDA, or chromatography (over C18? @Shadownaught)


#22

I know it isn’t the only method. I have a trusted source that has told me they don’t do it by chromatography at their facility. They are barred by contract from explaining anything more than that.


#23

Thats not how i do it. But also this technology other than chromotography is worth alot of money so doubt youd be able to obtain it for free


#24

neglect tek!


#25

I wouldn’t expect so!


#26

https://watermark.silverchair.com/42-3-130.pdf?token=AQECAHi208BE49Ooan9kkhW_Ercy7Dm3ZL_9Cf3qfKAc485ysgAAAjkwggI1BgkqhkiG9w0BBwagggImMIICIgIBADCCAhsGCSqGSIb3DQEHATAeBglghkgBZQMEAS4wEQQML2SKSBCRVWG0tDohAgEQgIIB7EagpmVTWbmY5Y5auEb1P-dDBoQaNMq_vgRCKsaCaVSAy-cRe4g_Ah-pFehGzkLbzBLOz-tEEQLNC90Iup3acKKeSLgojlOQCJSEgL5x57MeuVFtQjzIz76U1V_HAEkKzTQ4vN8WWRruwgNpcKoAuONw5-PxeTnZSGfHZgNOPiRliE-3a-bCIpyvXcjCWBmJEtaZy_KIkUDWSf506HVEaXCJ7lkfvB_FQMGutZmiYsIr8m_8AphOBUh_8DIzJ-HHwHyOmSOmodQmNSwa3z9ENYIVNBlV3w3o4Lq_9ahgzTO1vEFsqciXACfa5_CWW7lI-62Ztw_A8dIrSnjAhvB0LhEJWCjxDzdC-xt56m2ubJShBJZE9eFKvVBKmqJn8ZuQdAUI9ihJlSrgdfkEqaAj6_58pcoe9zsaUDZOVUDsEfNhN8_quqTowsyXSosHQRXBb7GwbR-blkKSijljyAsJFCCmqCHoRxjlBVc-870XV56hulBER3cMlyFsQ_sVStPI57kiGWFW4D4aao1xUj-OXts1o-sGxDrwhkJSJ2nxPUCNhXccRrG-yTuwFDpAC2btKzO5Wb8EEnmCTeThFn9bpZiBFu6fYMqJWItttjgyMBppYgabTYkFEX-6ipXRpxtnFEY94lnoxrc-hzhQ

Can be done with normal phase. It’s probably probabilitive to buy your own unit that can do kg scale. One of these systems can do both normal and reverse phase. Inline solvent recycling systems exist.

Has anyone tried the separation on kilo scale to see if the proper loading? I haven’t had time to read every post.


#27

The link is too long, can you provide a tiny URL?


#28

Better?


#29

Yep that works, thx!


#30

Good paper but with regards to full scale production of THC-free CBD distillate there isn’t anything there that would appear to be any more scalable than any other method of chromatography. Unless I’m missing something.


#31

I have been told there is a method much better than chromatography by a company making it. They paid for the proprietary SOP’s though


#32

Decarb the crude fully, then dissolve in your favorite alkane solvent (pentane, Hexane, Heptane). Do several flushes with a highly caustic brine (spike your salt water with sodium hydroxide to acheive a pH of 12+). Bring the solution back to neutral by flushing with distilled water and verify that neutralization has taken place or you will have isomerization issues later. Also make sure you dry out your suspension with a dessicant (mol sieve like Cbeads) prior to recovering your solvent.
The reason this works is the kpa of THC is 10.6 - we are essentially making it water soluble by exposing it to a pH of >10.6 - THC levels are very low in your Hemp-Based extract and after a few rinses we should have a remainder of mostly CBD + other minor cannabinoids.
Save all your water if you care to neutralize and extract the THC from the byproduct :sunglasses:

Cheers.


Looking to buy IP/SOP for stripping THC
#33

I think we have a winner! thank you @ColumboLabs

while not technically “crude”, the above product is neither an “isolate” nor a “distillate”, and although it’s going to be missing a few components other than just the THC, it is certainly going to have the general spectrum one would expect from “THC free crude”.

As a bonus, I’m wrong again, which should mean I’ve learned something.

Which would be way more satisfying if it was the first time I’d heard that trick…

Doh!


#34

:raised_hands:


#35

Looks like I need a bigger sep funnel. Is there an ideal solvent to crude ratio? Or will just enough solvent to dissolve the extract do?


#36

I can’t find any real data with a quick search. Does anyone have a good source for the pKa’s of the neutral cannabinoid phenols? I would have guessed that CBD has pKa’s similar to resorcinol, 9.32 and 9.81.

I literally cannot find where my glassware has been moved


Chromatography Units for CBD Isolation
#37

Pubchem?


#38

Why doesn’t the CBD become water soluble as well?


#39

What is the pKa of CBD?


#40

@scoteburk Looks like 9.13?

https://www.drugbank.ca/drugs/DB09061