THC Remediation By Degradation (a quick/affordable how to)

Hash and Stuff Pre/Post-Processing
, ,
1

I figured this post needed its own thread, This is the bare bones most basic run down on how i did some r&d for thc remediation by degradation in something everyone has, a short path and or a reactor. I will say this isnt the solve all answer for thc remediation and it should still be cleaned up with post processing and a distillation. I personally never put this into production myself as I was more focused on THC free acidics so doing this wasnt an option. but it will get your thc to compliant levels very affordably when compared to chromatography.

I wouldnt suggest doing this without in house analytics.

Wanna convert your thc to cbn and get to compliant levels???

Take a boiling flask with a stir bar or a reactor, load your oil and set temps to 130-140c and stir max speed, make a gas trap on the outlet to trap the gases escaping or pull a sight vacuum and have a proper cold trap set up and let your reaction run while testing every hour or couple of hours.

Heres some data… this was samples taken ever hour for 8 hours. I believe this was done on 100g of some thc fractions from chromatography.

CBNconversion11.25-no.1.pdf (17.0 KB) CBNconversion11.25-no.2.pdf (16.9 KB) CBNconversion11.25-no.3.pdf (17.1 KB) CBNconversion11.25-no.4.pdf (17.2 KB) CBNconversion11.25-no.5.pdf (17.3 KB) CBNconversion11.25-no.6.pdf (17.0 KB) CBNconversion11.25-no.7.pdf (17.1 KB) CBNconversion11.25-no.8.pdf (17.2 KB)

I did not provide potency results for all these tests as I think reading through these results and understanding them is part of learning this process better. I also dont wanna spoon feed the Chads

The starting material was mother liquor from making cbd isolate.
65.5% cbd
1.3% cbg
1.4% cbn
4.5% cbc
7.9% thcd9

Retention times are as follows
CBD 5.3
CBG 5.0
CBN 8.3
THC D9 10.9
CBC 14.25

Watch the cbn go up and the thc go down.

Did i say you shouldn’t do this without in house analytics and a plan to post process and clean up further??

23 Likes
2

Good man! A crystal spoon for the masses!
This post could save someone $400K who boss is considering the purchase of that “harmonic-crystal-magic distillation” scam of a “system” thats (still?) being sold.

cant imagine how much dough that company made off folks. Ive seen facilities with 2 running and considering buying more! (Ive tried since day 1 to stop folks from buying that BS kit)

8 Likes
3

You should make up an entire system that sells for 100k less with the same results and more profit!

3 Likes
4

I think thats exactly what Sub Zero Sci did. I wanna say they offer a 20-30k stainless vessel that does 10kgs at a time. it would be pretty easy to scale this as large as you want though.

3 Likes
5

They do, but the sop is the key.

6

A de carb vessel would work for this as well, correct?

2 Likes
7

yessir

3 Likes
8

Edit:

Forget it… Well played sir!

9

Wow, that’s really a game changer for someone like me, small scale, late to the game without a lot of money in a tax inefficient state.
I do have a handful of questions, a few clarifying and some open ended ones that could push this foreword. (I will try to give my best guesses in a preceding post)

Clarifying
What do you mean by slight? A run of the mill pump for rotovaping gets to 0.1 ATM (76 torr) Is too much?

I have a regular shortpath (not a wfe) so I distill at around 200C, is there a thermal degradation pathway from CBD to THC at that heat that would undo all the work I just did.

Probing Questions
Would using an inert carrier gas prevent unwanted degradation of CBD and compliant minors, or would it slow down the reaction because oxygen helps initiate or catalyze the reaction?

What is the ΔG of this reaction and are there any negative consequences of running at 150 instead of 130-140 for time sake?

10

Possible answers to my own questions:

Inert Carrier Gas
Upon first look I’m unsure if oxygen would help or hurt. I did some r&d with a friend a while ago doing something similar using a range of oxidants and addly enough, we found that oxygen actually selectively degraded CBD (to a point) more than THC. We noticed CBD was degraded to a by-product that didn’t have a peak on an HPLC. Since there was no peak and the degradation tapered (sharp drop in the first two hours ~10-15%) , it was likely a CBD quinone species that formed and acted as an antioxidant. Once enough had formed, it protected the rest of the CBD.

I see in your chromatographs, you have a drop in CBD potency between hour 2 and 3 of 15%, but it stops after that. Then from hour 3-8, minimal degradation of CBD (within standard error of machine) and THC starts to convert.

Now the part where I’m torn: what causes the THC to convert? There needs to be something that facilitates a redox reaction on the THC since it will need to oxidize, losing four hydrogen atoms whether it be to hydrogen gas or water/hydroxide species. Regardless, I don’t think it can work in inert conditions. I’ve had enough organic chemistry to know that reaction doesn’t happen at 130-140 on its own (that’s what my gut tells me). It’s likely a quinoid species being formed and acting as a redox catalyst Considering. The first pair of redox reactions going from a tetra-hydro species to a di-hydro species is the slow step, but then the di-hydro to cannabinol is fast because gaining aromaticity is energetically favorable.

However, if you graph the THC peak, THC drops in relative abundance even faster than CBD (60% in the first two hours), which is profound since it is much less concentrated.

So my best guess would likely be that there is both a thermal and oxidative reaction at play in the experiment @thesk8nmidget posted. I’m planning on trying this (against advisement) under a deep vacuum (the only inert atmosphere I can afford) and oxygen-present conditions. Hopefully we can figure something out!

2 Likes
11

Possible answers to my own questions:
Can you run hotter at 150C to speed up the reaction? And the converse: can I run at 120C and have less degradation.

Lets start with degradation; the best thing to start by looking at relative chemical equilibria. For the THC to CBN reaction, heating this will likely make it go faster since there is no real reason it wouldn’t, so it would likely go faster. However, we are also affecting the CBD degradation as well and increasing the temperature would likely push the equilibrium of CBD:CBD quinone up, making the losses much more drastic. So likely a bust on 150 unless oxygen is not required to make this run (ideally CBD thermally stable, THC thermally degradable).

What about running at 120C? In countless organic systems, a strategy to eliminate close diastereomers and enantiomers from a synthesis is to lower the temperature of a reaction lower than expected to leverage either an unwanted side product reacting faster, or your product reacting faster for easy separation. This may actually be something we can do, but it will depend on the results of the oxidation study. If the solution is the ideal one (CBD thermally stable while THC degrades) and we need just an inert atmosphere, then this is pointless since we have an easy answer. Pull vacuum and cook her hard! If oxidation is required to make this work, then this would be an interesting experiment to decrease losses. Running at a lower temperature would make this run a lot longer so block off your schedule but lower by 10C would likely halve your loss (long boring thermodymic calculations, but 6-10C about a doubling speed for a reaction is a good rule of thumb).

Updates
So I ran a test of this experiment using a heating mantle, covered in tin foil, a vacuum pump and cold trap. I heated the CBD to 140 for 8 hrs under a strong vacuum (0.05torr). The starting and ending material tests are as follows. (Cannabinoid/starting potency/end potency)

CBD: 82.21% / 61.15%
THC: 4.74% / 4.77%
CBN: 0.38% / 0.57%
CBG: 1.08% / 1.26%

So looking at this, it looks like the CBD degraded and the THC did not at all, which was surprising to me. It looks like there is a thermal degradation occurring with the CBD, even under vacuum, but the rest stayed more or less the same.

This is also very interesting because it seems like the CBD is degrading into some other product, and not a quinone (oil was not dark, which is interesting, quinoidal bands are known for their strong colors). This may mean that the CBD was degrading into something like CBE, but wasn’t able to act as a redox catalyst since there wasn’t any oxygen to form the quinone. Regardless, I really don’t recommend you do this under vacuum because the results speak for themselves!

3 Likes
12

Let’s sell this to some linkedin Chads

3 Likes
13

Does anyone know of a lab that is competent at measuring minor cannabinoids? The ones I know do the big 10, but not one that I trust to test minors. This would be to confirm or disprove my hypothesis and results above.

1 Like
14

@kcalabs does a great job for minors.

6 Likes
15

@Neutral we’d be happy to test for minors. A significant portion of our clients are remediators and are looking for the same thing. Message me if you need help.

3 Likes
16

I have found out about “degradation-while-decarboxylating” a few weeks after purchasing a Gilson CPC in 2019 :grimacing:. I still have the baby…nice for visiting customers ! Impressing looking machine. I don’t post that much on the forum, but I have learnt a lot thanks to all…so, my time to contribute by giving my humble experience : I gradually/slowly heat 2L of purified extract (63% to 66% CBDa, 3% to 6% THCa, and other "a"s) in a 5L reactor to 130°C while rapidly agitating (180-200 RPM). To reach 130°C, it takes me 4-5 hours but no rest regarding agitation. I raise temp according to amount of decarb bubbles to avoid spilling (although I often stir manually to lower bubbles level). Once I have reach 130°C, I leave it for 30 minutes and then stop my heater. I leave it for 24 hours as it is. Next day, I re-heat to 70°C to empty the reactor. Results are : CBD has increased (+2%/4%), THC is below 1% and CBC has exploded to 3%-6%. No other cannabinoids had a different behavior than expected. Don’t ask me why…this is the way I cook scramble eggs. T

5 Likes
17

Where can I get the SOP?

18

CBC or d10?