I’m working at a place that’s making 50kg Hemp D9 per run usi by triiso and we’re getting around 5% D8. We’ve seen non detect D8 in Hemo Derived Delta 9 THC before and are looking for a co sultans who can help us dial in our process.
Our basic protocol is to react the CBD using triiso in a reactor, transfer to a reactor and do the Liquid to Liquid extraction and then once we’re finished move onto distillation. There’s obviously a ton of nuances to it that we can discuss over the phone but looking for anyone that can offer advice or are open to doing a consult for us.
Whith triisobutylaluminium less than 2% is doable
What solvent are you using now ?
And what’s your cleanup look like ?
Are you realy attacking the aluminium out ?
You see aluminium after quench becomes aluminiumhydroxide Wich is a Lewis acid in dry conditions
And the culprit of your D8
If you can get separation on an HPLC you can get separation with chromatography on a larger scale.
I don’t know if you have the equipment for this. And I don’t think I have seen commercial scale columns, so you would need to be packing your own columns to do it. But it could be done. Then you are just evaporating again.
If you have in-house HPLC so you can constantly look for it - it will help, as you are taking aliquots, until you get to where you know how long you can run it before you start seeing D9 in there again.
Feel free to hit the DMs if you want to talk about chromatography - assuming you have equipment available as you mentioned it already as an alternative to distillation.
I’ve seen a Gilson CPC unit in action, seven foot columns you get the joy of packing yourself. It was an absolute nightmare to run, tons of solvent waste, very mediocre support from gilson and you’ll need excellent in house analytics to have any hope of dialing the process. But yeah, it can do what you’re asking.
Ive done it using large units from interchim, each column held 7kg of C18. They retailed at either 190k or 290k. Even a few years ago when prices were higher, it still didnt make sense from a financial standpoint. I was removing ~2% D9 from D8 to make compliant D8.
Ok so
At first I thought your quench to be insufficient and it might as wel be
BUT
Since you work on dcm as a solvent
I would do a test
As follows
Quench reaction as usual and recover solvent at a temperature as low as possible once the dcm doesn’t get out anymore at this low temp I would add
Some hexane or any solvent with a higher boiling point and try to evacuate all dcm from solution without raising the temp to much
Dcm gets entrained in the solution and a serious amount of heat is needed to purge it all marking the solution les viscous will help in getting it all out
Reason dcm is a very accitic solvent
And known to isomerize on it s own
Place some cbd issolate in dcm and after a few days you ll have a small % of thc
Heat is a catalyst for reactions to speed up every 10C is 4x the reaction speed
So I would not be suprised if you are able to lower the temperature to evacuate all dcm that in the end you will have a lower % of D8
Good luck
Reason I recomend hexane is that it has no azeotrope with dcm and that it s right in the upper limit to purge itself from 2stage rotary came vacuumpumps
Since solvent entrainment in the vacuum pump oil can realy screw your vacuum depth
