Degumming (Citric Acid + Enzymatic), Winterization, Saline Scrub Critique

Hash and Stuff Extraction
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Update: If you use pentane to partition your cannabinoids to a non polar layer, you’re gonna have a BAD TIME

Update 2: Considering that EtOH has been acidified and enzymatically treated, it makes sense to neutralize the solution AFTER winterization, THEN recover the ethanol and THEN introduce hydrocarbon (heptane is the only hydrocarbon I will be using for LLE anymore).

If you do not do this, you’ll be fighting pH the whole time, because “pH change” of the hydrocarbon layer is going to be majorly reliant on agitation and will not be as completely neutralized as it would have been had pH steps been carried out in EtOH/water.

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Update 2: Decided to skip degum, because this was a clean first pass 93% TAC.

Acid wash @ pH = 3 in Brine (Citric Acid)
Base wash @ pH = 8 in Brine (Sodium Bicarbonate)
Neutral Wash @ pH = 7 in Brine

T41 scrub @ 60C for 10 minutes, passed through a wetloaded column of MagSil and Silica.

I jumped from there to the roto without a neutralization wash and BAM purple…

I think I know why @Photon_noir suggests AGAINST pH washes unless absolutely necessary.

Anyways, reintroduce heptane, purple disappears completely, neutral wash with only distilled water and I lose 50% of initial yield to emulsions.

Recover heptane again, toss into a short path. Reflexed up to 205C at 250micron and it wouldn’t pull over—but in the BF it looked CLEAR—as soon as I reintroduced atmosphere, the walls of the flask turned purple again and streaks fell into the clear disty which looked red when poured into a jar.

Suggestions, pats on the backs and/or absolutely unfair ridicule accepted and appreciated.

I want to reiterate something I’ve said several times—a good chemical engineer does not a good chemist make. Know the difference and don’t assume you’re the best at both because you’re good at one of them.

Love,
Phil

P.S. Shoutout to all the homie that have been helping me out with this, I am absolutely relentless when it comes to reaching out to people and everyone in the community has responded graciously and with kindness.

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Just curious, do you think a centrifuge might help boost yield losses to emulsions or speed up your LLEs?

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Yes, they actually even sell centrifuges specifically for lle.

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Can you post a link? Or point me in the right direction?

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I would be interested in what kind of product you want to make. A process that complicated for what?

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Try this:

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Safety, Quality, Purity, Potency.

You remove impurities so you can R&D what it might look like to create high quality end-product at scale.

If you’re processing thousands of lbs of biomass weekly, phospholipids, carbohydrates, etc can and will hinder the quality of output.

If you’re not trying to make the best end product, you’re gonna get left behind.

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A research paper demonstrating the use of Citric Acid to remove Mycotoxins from rice

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Honestly, a cold ethanol extraction hardly pulls any gums…

Have you checked potency with and without degumming? Or have you noticed some gum-like compounds actually falling out?

I’ve only ever seen a need for degumming with a non-polar initial solvent.

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Definitely noticed precipitated gums after an enzymatic degum. They’re in the crude regardless of cold extract, but they won’t destroy product quality in smaller quantities

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Just following a KISS principal, your enzymatic pull might be enough to get the job done.

But I mean, if the end goal is 99% thc distillate. Then there’s no such thing as too many steps I guess.

But very few people appreciate my 99% over 95% or at least their wallets don’t care

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I agree, but I’m finding that Citrix Acid has more use than as a simple degumming agent—check the article I linked above.

Considering that it is often difficult to detect mycotoxins in bulk plant material, it might be beneficial to just use a citric brine wash anyways

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hello could be more specific about using Yang et al from 2018,can’t find it its about citric acid and enzymatic degumming,

many thanks

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Will saponification in water wash prevent need
For winterization?