Separation of Delta 8 from Delta 9

[squig]

want to be made of unobtainium if you ask me for half a million.

I could employ a team of engineers for a year and supply the materials at that price.

[squig]

A Large Spinning-Band Fractionating Column

A Large Spinning-Band Fractionating Column.pdf (456.2 KB)

[Dr_Jebril]

By the way, do you understand what is this machine ?

From here just look like 3 parallel big reactors, with pumps, stirrers, and nice pipes.
And there are two cooking pot on the rights…

And it claims “99+% removal of unwanted compounds from crude oil”.

So basically, if you personnaly aim to one specific compound inside the crude oil, let’s say a cryptic cannabinoid, or some specific fatty acid, you could get all the rest out ?
It sounds fantastic.

[Dr_Jebril]

I did not see your reply. Your are right.
I was focused on all the nice valves, and then I noticed the stirrer inside.
But where are the columns ? The columns are the fancy tubing arround ?

[Killa12345]

I thought it was interestingly vague from the description.

And just like you said. It looks like 3 reactors, with some pumps and plumbing. Some cbd guys gonna look at this and drewl

[squig]

same here not sure.

still 500k is a lot

[Dr_Jebril]

The tubing is fact manly the support for the motor transmission and the frame.
I’m not familiar with those devices. I thought there should be some sort of column.

This price you said, is it a bet or the real price ?

[Killa12345]

That’s the real price. It’s was $520k

[anon1342]

@tweedledew

Yup that’s my plan. I know some people managed to get a 90% d9 10% d8 starting up to 95% d9 fraction. They can separate via distillation better than something like CBD and d9

@spdking @squig @AlexSiegel @anon56994712 @phenethylamine1 @SoStupendous @cyclopath

Dumb idea of the moment:

Will black light help differentiate d8 d9 during distillation? Or do they come across mixed?

Anyone tried this?

Ultraviolet Fluorescence of Cannabis - Observations

I’ve made observations of UV fluorescence during cannabis processing that I’d like to share. (Fig 1) as shown from left to right is a 78% total cannabinoid distillate, 98% THCA isolate, and 99.8% CBD isolate. The distillate has a green glow and the isolates have none. [1%20first%20observation3%20annotated%20322%20by%20167] (Fig 2) is an ethanol extraction at -78C with 20 micron inline filtration approximately 190 proof. (Fig 3) is crude hydrocarbon/CO2 extract. (Fig 4) is a soxhlet extract…

[squig]

not sure you would have to see if they fluores different from pure samples I would think.

that is how they separate the different ergoloids post reaction and for separation from plant extracts
though the use a column rather than distillation.

[AlexSiegel]

Probably not. The UV-absorbance of d8 and d9 are very similar. I’m not positive about their fluorescence but I’d expect it to be similar

[nostrum]

We have one, I definitely have seen some degree of separation in cannabinoids, but indeed if I could dial in a method for this purpose, we could really make some moves until the regs officially change on D8

[nostrum]

Same here, both

[anon56994712]

I dont think they would look too different

[onemadalchemist]

Absolutely possible to separate d8 and d9 using reverse phase, prep scale HPLC.

Might be doable on flash, though loading would have to drop like 100x or so what people are generally running with their THC remediation methods.

Also relatively easy with SFC, though obviously not with reverse phase. See the following patent. It’s Waters and good old John MacKay, which usually means nearly microscale level small, ha. The same principle applies at scale, though.

US10501432B2 - Chiral separation of Δ8-THC, Δ9-THC, and related enantiomers...

Speaking of scaling, Ebbu was on that tip with SFC three years ago. Here’s the abstract for a poster of theirs from 2017.*****

"Separation of Natural Cannabinoids by SuperSep®
Martin Enmark1, Kurt Levy2, Brian Reid2 and Jin Seok Hur3,
1Horizonoid Ltd, 35715 US Highway 40, Evergreen, CO 80439 USA 2EbbuLLC, 35715 US Highway 40, Evergreen, CO 80439 USA 3Novasep, LLC, 23 Creek Circle, Boothwyn, PA 19061 USA

For the high efficiency and less organic solvent consumption, supercritical fluid chromatography (SFC) has been widely used for chiral separationsin pharmaceutical industry. Now, the SFC application is being broadened to achiral separation and purification of natural extracts, which are often very complex mixtures. This poster presents the preparative SFC purification of cannabinoids.The processwas developed using a bench-top SFC instrument and then directly scaled-up to SuperSep®1000 with a 50 mm i.d. column for manufacturing. Cannabinoid oil extracted from cannabis plants contains many different compounds such as Δ9-tetrahydro-cannabinol (Δ9-THC), which is a well-known psychoactive compound, and cannabidiol (CBD), which has been getting a lot of attention in the last few years for health benefits. For various pharmaceutical and neutraceutical manufacturing, having an access to gram to kilogram amounts of purified cannabinoids will have great value."

Plenty of references out there.

*****This is in no way, shape, or form an endorsement of Ebbu, please don’t anybody think that…

[Ennui]

I’m only just starting down the chromatography path so forgive the ignorance. Has anyone tried using the chroma methods presented in some of the isomerizations patents? In many of these academic journal entries and patents the authors claim to have good results separating unknown isomers and known ones. I’ll edit this in a minute and give an example

[tweedledew]

With a long enough column anything’s possible

[squig]

@Ennui

In many of these academic journal entries and patents the authors claim to have good results separating unknown isomers and known ones. I’ll edit this in a minute and give an example

im a looking buddy thankyou for the common sense that in this time was lacking.

[that445guy]

@Roguelab was saying he could get good separation with a longer fractioning column as long as there was no cbd.

[anon1342]

As with the initial extraction, CBD, Δ8 THC, and Δ9 THC are separated out by precipitation. The precipitation occurs from dropping the P and T in steps from high to low. CBD is precipitated at 70 bar and 50℃. Δ8 THC is precipitated at 60 bar and 30℃, and Δ9 THC is precipitated at 55 bar and 25℃.

@Roguelab @Dr_Jebril @RockSteady @bigbone @squig @JedClampet @SidViscous

https://hemphacker.com/category/cannabis-chemistry-2/

The final step described in the patent is the separation of CBD, Δ8 THC, and Δ9 THC. This is achieved by using a purification material/media commonly used in separation science – silica. As is described below in the chromatography, silica has a charge to it, that reacts with the molecules that are to be separated/purified from one another. Some molecules have a stronger interaction than others and therefore travel slower through the silica packed column. In this case, Mueller ends up with pure fractions of the three cannabinoids.

The silica used in the patent has an average size of 0.1mm, and is commonly used in separation science. Looking at figure 3, you will see that the CBD/THC mixture starts at the bottom of the column. When the supercritical CO2 is pumped into the system, the mixture travels up the column and begins to separate the mixture.

After the separation column, there are three collection vessels. As with the initial extraction, CBD, Δ8 THC, and Δ9 THC are separated out by precipitation. The precipitation occurs from dropping the P and T in steps from high to low. CBD is precipitated at 70 bar and 50℃. Δ8 THC is precipitated at 60 bar and 30℃, and Δ9 THC is precipitated at 55 bar and 25℃.