Delta 9 into Delta 8

distillation

#1

Hello again everyone!

This is part 2 of my project to synthesize cannabinoids. My first one was thc acetate (link: THC-O-acetate synthesis ) For my second cannabinoid I would like to isomerize delta 9 into delta 8.

To do this I have purchased Cbleach from @ColumboLabs. Ive seen similar threads on this forum using Cbleach to remove pigments but nothing on the conversion of delta 9 into delta 8 using this product. @Future has a thread (link: CBleach Scrub) and in it states that under low temperature conditions (60C or less) delta 9 will not isomerize to delta 8. Under the Cbleach description it states, “High potential to convert Δ9 into Δ8 when used in the boiling flask with crude/distillate. Has the potential to convert other cannabinoids into Δ8 when used in the boiling flask with crude/distillate.” Does anyone have experience using cbleach in a rbf?

Let me know if anyone has any other methods of converting delta 9 into delta 8. @Photon_noir you were a big help with the last project and I would greatly appreciate it if you could help me with this one as well.

Side note: @ColumboLabs video on delta 8 is interesting and influenced this project. Thank you for the video! Check it out if you haven’t already. ( link: https://www.youtube.com/watch?v=_9Zh65FcIkg)

Thanks,
Franz


#2

Hey Franz!

Below are some helpful best practices when using CBleach as a adsorbent and co-distill-ant in @LabSociety SPD’s or @BR-Instrument “cauldron style” distillation systems.

Note:
The exact amount of isomerization varies from batch to batch and depends on multiple factors. it would be hard to achieve full conversion to THC∆8 unless starting with a highly refined compound (For example in my experience, CBD Isolate is a great pre-cursor to extremely potent THC∆8). We are currently working on a new formula called ColumboBleach-Light or CLite for short to convert 99.7 CBD Isolate into ∆8 at 97%+ Conversion. It is not a complex process but requires tight tolerances including the use of N2. For what you will most likely want to do, there is a much simpler way.

Definitely start with either highly refined crude (Water-washed, Enzymes, Winterized, Scrubbed with Carbon or Clay, and ran through MagSil) or some regular first pass distillate.
In our incubator, we usually run our Tails/Reclaim with a liberal amount of CBleach in the flask (5-10%). Our batch size would be approx 7-12L and we would wet-load some pre-dried CBleach in amounts between 500g and 1.5kg into hot material (85C or so)

If you are doing a 1000g first pass run, warm your material up to 80C and slowly add between 30g – 100g of CBleach and mix with overhead stirrer or magnetic while slowly bringing the heat up-to 140C. If the solution muffins, allow it to settle, continue to stir until there is no boil present. Pour into the Boiling flask and allow to cool to 100C while you put your system together.

The key to a successful Distillation of ∆8 using CBleach is how to spot azulene and when to swap flasks to collect main body. You need to be patient and watch the vapor temperature instruments very carefully while modulating vacuum depth and agitation rpm via stir-bar.

Make sure you are using the @LabSociety digital temperature monitors as they will provide you with the clear picture of what’s being distilled as well as integrate into the #elitelab system (Ask Mike to be part of the beta testing.) Having a few vacuum instruments wouldn’t hurt either – I usually run with one at the head for the “in-system” vac depth as well as one directly on the vacuum pump to monitor ultimate vacuum potential:

https://labsociety.com/lab-equipment/vapor-temperature-monitoring-kit/

https://labsociety.com/lab-equipment/precision-vacuum-monitor/

You can ramp up to about 140C on the mantle pretty much right away provided you degas your concoction (80C – 120C under vac depth in-system about 500 mtorr). Azulene will start to happen between 135-147C vapor temps, it will continue to turn distillate green/blue all the way 151 – 157C vapor. Its important to pull out all of the azulene prior to switching flasks otherwise you will have blue or green disty that smells like boof.
Recently in collaboration with other friends in the industry, we started to rep the recent @labsociety full-bore kits. The vacuum depth and speed of degas which you can achieve with a full-bore system will outmatch any GL fitted system with comparable vac pump. Conversion kits can be found here:

https://labsociety.com/lab-equipment/full-bore/

https://labsociety.com/lab-equipment/condenser-kit/

Its also helpful to Burp your azulene fraction. What this means:

Once your no longer see any blue in your condenser and vapor temps are steadily dropping from approx. 149C - increase your stir bar rpm by 5-10% RPM until at maximum. Give each change in parameters 5-10 minutes to produce an effect in the system before ramping up temps or RPM’s. You will at some point “Pop” your THC fraction (Usually at 155-158C vapor at approx 150 mtorr in-system.) Once you feel comfortable that all the blue has stopped, shut off RPMs + Heat and proceed to drop Vapor temps 40% before re-engaging the stir-bar to MAX.) If you no longer see blue once the vapor temps climb once again past the 147C point, you are in the clear (literally).

I usually like to stay under 175C vapor while collecting my main body which allows me a 500ml/hour flow-rate on a 12L Mantle set to 185C with a top jacket;

https://labsociety.com/lab-equipment/heating-mantle-system/
https://labsociety.com/lab-equipment/heating-mantle-system-top/

The best I’ve ever made was about a year ago – we started with some really nice BHO material which was extracted properly with fresh trim. We took our time degumming and winterizing. The second pass had 10% cBleach in the flask and we produced this:

Sadly, we never got batch results back for this run, but it didn’t oxidize even after 3 months of storage!


Delta8 vs. Delta9
CBleach Scrub
CBD Isolate crystallization questions
#3

Great stuff!!!


#4

Why would we spend the money on the short path to perform this experiment? What is the short path doing other than providing heat?

Also what is the clay doing in the flask?


#5

You don’t absolutely have to have a SPD, it’s just the simplest method.

You could reflux with the clay, carbon, or an acid, then attempt to filter out/neutralize that activating ingredient, then distill the mix again in a wiper if you want.


#6

What is the clay doing?


#7

Zeolites are often catalysts. Really big in the petroleum industry to crack selectively. They have active sites and can hold ions


#8

So you think the clay is acting catalytically? Then are you using a molar equivalent or is it a catalytic amount? How much clay per gram distillate?


#9

That’s literally just the first link, but they zeolites can have bronsted and lewis acid sites. Went to a lecture by one of the head WR Grace chemists who designs and qualifies new catalysts (he has a ton of patents and even more trade secrets). Not only can the activation energy be lowered by the catalyst, but the catalysts can crack very specifically like I said before.


#10

I have no idea about the amounts. I think people use around 3-10% by weight. Catalysts don’t appear in a rate law because they also assist the reverse reaction so adding a ton wouldn’t really do that much for you if it is purely a catalyst and not a reactant at all.


#11

Our acidic clay has lewis acid sites due to activation with sulphuric acid prior to water leaching. What some people in this industry have acted on is the fact that acidic zeolite is easy to use and remove, without having to handle high purity sulphuric.


#12

I’m sure you could decipher a specific load rate.

For right now we operate on a heat/load or load/heat function. So higher heat uses less zeolite, more zeolite(20%+) requires less extra heat energy.


#13

So why would i use your clay rather than a catalytic amount of a lewis acid if you are claiming this process is catalytic?


#14

I would say because the clay is useful for other things as well, and you can use the clay in bulk amounts without running into serious occupational safety concerns. If you don’t mind using high purity lewis acid and turning small batches then do that instead.


#15

TBH initially we were using the adsorbents in the flask for color improvement, the isomerization was a side effect.


#16

And I was bringing T41 online for pesticide remediation before we found out what it was doing for color…the clay world has been like a Russian nesting doll.


#17

How would you compare T-5 to T-41 for color removal vs. other uses? I’ve only experimented with T-5 so far and not really sure it did much using it in a dry or wet bleach protocol similar to C-bleach.


#18

I encourage you to seek out information of chemical catalysis. It is a process by which you have a basic understand but your knowledge seems unfortunately riddled with misconceptions.

Two massive misconceptions.

  1. Catalysts are used in catalytic amounts and never calculated by weight. They are generally 0.1-0.5 molar equivalents to whatever the limiting reagent is in a reaction.

  2. They are also not lowering any activation energy for the reaction. They affect the reaction in a few ways, sometimes by raising the energy of the reactants or very commonly stabilizing the transition state among others but these are the most common two I believe.

  3. lastly but generally egregiously offended is the fact that for a catalyst to be considered a catalyst it must be regenerated at the end of the reaction being formed. Without the reformation of the catalyst it is simply a reagent. This is why only small (catalytic) amounts of these chemicals are necessary for the reaction.

The paper you posted seems somewhat applicable but no where in the paper is there any generalizations stated that the zeolites used are the same zeolites in our favorite over-marketed attapulgite, bentonite, clay mixed with activated carbon.

My purpose is not to troll, my purpose is provide free information that is the closest to the truth as possible, I encourage you to challenge my statements to reveal more truth to the community.


#19

My point is that this overpriced clay should be marketed to do what it has been shown to do and explained in such a way that is not misinformation. To use the buzzword of catalysis when selling this clay is wrong and it is misinformation. I am not saying it wont help you make delta 8 but it is not catalytic.

If the sellers do not understand the chemistry they should not be saying it has catalytic activity as a selling point. By saying this the sellers are taking advantage of those who do not have a chemical background and do not fully understand what catalysis is. The sellers may not be doing this on purpose but rather due to their own ignorance. I hope my explanation of catalysis in this thread gives people the free information to make an educated purchase.


#20

I have no evidence but What we “know”:

-acidic conditions favor conversion
-zeolites have active sites

That article wasn’t supposed to be conclusive it was just the first one I found describing them as catalysts when I googled zeolites as catalysts. That’s all I was trying to say there.

The activation energy can be lowered by catalysts, that’s definitely true. Most catalysts provide an entirely different mechanistic pathway. Haber-bosch is a great example.

Yeah catalysts -should- be regenerated but they can be poisoned. And if the zeolite is functioning as an adsorbent holding a non-cannabinoid molecule, the cannabinoid cant be in the active site. Unlikey to occur so quickly after one batch so I dunno just a counter point.

You are also right that you only need “catalytic” amounts. I think for most peope its easier to throw enough in there to say “that’ll do”. And like I said if water, hydrocarbons, pesticides, etc get adsorbed then you would probably lose catalytic activity too.

Final disclaimer im talking out of my ass and stoned off my ass​:call_me_hand::v: