New ways to quench

It is possible to collect metallic aluminium from the rxn mixture. Apparently the aluminum hydroxide run over acidic AC will do itā€¦ pretty wild.

Also yes, @EagleChem , there are engineering solutions, but as a consultant for hire I cannot give everything away for freeā€¦ nor would I want to step on the toes of folks like yourself using trade secret methods by publishing them here, you know? On the forum, I just focus on the chemistry of the topic at hand. :wink:

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Should we understand physical ? :thinking:

Bentonites are cation exchangers. AlCl3 will not sorb on it. If you observe clogging, it means that it acts as a filter, catching large enough particles.
Anionic exchangers (e.g. LDHs) could work if you have it under an anionic form. In any case, anion exchange media can only be a solution if if AlCl3 would be used in catalytic amounts for yhe reaction. Is it the case ?

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Just some humble thoughtsā€¦

Why not turn the Aluminium chloride to Aluminium phosphate, which is insoluble in water and should precipitate in water, so by first adding a small quantity of phosphoric acid to turn the aluminum chloride to aluminum phosphateā€¦

AlCl3 + 3 H3PO4 = AlPO4 + 3 HCl

But since the phosphoric acid is not stronger than 85%, the water content will at least turn some of the AlCl3 to its hydrate form., so the reaction will beā€¦

[Al(H2O)6]Cl3 + H3PO4 = AlPO4 + 3 HCl + 6 H2O

But the phosphoric acid will also react with the DCM as followsā€¦

2 CH2Cl2 + 4 H3PO4 = 2 CH2O + 2 H2PO4- + 2 Cl- + 3 H2O

ā€¦creating formaldehyde (C2HO), which dissolves in water to formalin, and hydrogen phosphate ions (H2PO4-), chloride ions (Cl-), all soluble in water, and water (H2O).

And then adding water with excess sodium carbonate or sodium bicarbonate to neutralize the acids. to sodium phosphate and sodium chloride, which both are soluble in waterā€¦

Na2CO3 + H2O + H3PO4 & HCl =

Na2CO3 + H3PO4 = Na2H3PO4 + CO3 andā€¦
Na2CO3 + 2 HCl = 2 NaCl + H2CO3

And then finally, wash it repeatedly with water and separate the water part from the DCM.

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Yust for clearing things up

This is a short hand sop
Take solution to less than 0C AND KEEP IT THERE AT ALL TIMES
Add alcl3 to solution
Run for 2 hours and quench as cold as possible

Ok @Dr_Jebril , @Capella , @Photon_noir
The isseu is NOT alcl3 it s aluminium complexes that are formed in the process
Tetrachloroaluminate the most likely
Wich is soluble in the solvent DCM
And Wich does not wash out nor reacts with the basic salts usually used for quench and cleanup

@Capella nice write up and indeed
Using an acid in the quench helps with
Remediation of color of the solution
Sulfuric gives amber
Phosforic gives bright gold
This aluminate a solution must be found for since in europe this sop is widely used and to avoid the havoc it creates when distilling people are selling undistilled aluminate rich oils at the moment Wich is worrying

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In catalytic amounts ? Or much more ?

Would it all turning into this ? Or only a portion ?

If this is a limited quantity, then anionic exhanger may work. :thinking:

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No defenatly not all
Amounts used in general are anywhere from 40-132 gr per kg of cbd
Seems like only 8 grams is soluble in solvent at around 0C
And the reaction can be done with 0.33L of solvent per kg to 12L per kg
Exotherm is big so be aware
Anionic exchangers indeed are an option and main focus althou
some bentonites also seem to work
A solvent swap is recomended by some Wich has the benefit of making these complexes insoluble
Washing with acetone then pouching this out by water addition also has benefits
BUT the aim of the quench is waste control

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2 posts were merged into an existing topic: Spray distillate onto flower

thank you. and please I mean no disrespect. I have poured over hours of your contributions here and it is no secret even all the way in Germany that you are a chemist of chemists in the industry. If I came off prissy I do apologizeā€¦I have those. you know times of the month and dealing with a daughter and an exuberant boss who is quite frankly a bit of a butt hole. I will watch my mouth from here on.

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for smaller scale you can totally use the feizer workup and go
aluminum chloride 0c
Quench with 15% sodium hydroxide and 1:1 water:dcm under argon and vacuum simultaneously
Then you can add 1:1 alcl3:anhydrous magnesium sulfate
Warm to room temp
Filter the sludge over Celite
Dry Dcm and recover
Distill oil.
This works great at 10L BF but for some reason not the same at scale. Makes a mess. This wonā€™t help the people doing industrial work but should bless a small at home chemist with good medicine maybe.

For all others I would totally be down to tradeā€¦
I can teach 1. A filtration method 2. a 99.9% water soluble method 3. a peroxide method all with alcl3 and I can share test results if you promise not to dox me.
I would like to learn other things that a lot of you guys know and would happily collaborate on a trade for information (couple of zooms together) whatever.

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I am not on here a ton. I am only allowed two hours at work on the internet and a lot of it is taken plus I live in a small village outside of Cochem where internet is pretty much only good for an occasional text message. But I can go to the library if we have a chance! Otherwise many blessings my friends!

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Mermal? Excuse me if I came off terse or touchy! Please know that no offense or aback or insult was taken at all! I just havenā€™t conversed with you before, so I did not expect you to know my linguistic idiosyncrasies. That is, I try to set out any caveats I feel could be important to know about me for each new person I talk to. No harm, no foul, no mood, no matter! Thank you for your civility, though! It is charmingly refreshingā€¦ albeit to my chagrin.:sweat:
I must admit it feelsā€¦ pleasantishly unsettling?.. thinking about what you said of my rapport (infamy?) among other chemists in your country. Likely thatā€™s because I donā€™t get many opportunities to speak with fellow chemists at all, let alone with those in Germany! I mean, being known is cool and all, but please tell them I will gladly have conversations with whomever may want to chat! I feel I may have inadvertently driven this ā€œwedge of inapproachabilityā€ between myself and others, and I sincerely hope that is NEVER the case! I like talking with anyone about chemistry! :smiling_face:

Oh yes a couple of my colleagues followed your work all the way back to maybe 2016ā€¦ ish? about using magnetic filters to reduce iron concentrations in our vape pens. We were veryā€¦underground then but it was an amazing contribution especially given the quality of soil here leading to some heavy metal contamination.

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Iā€™m going to start by saying I have never done the reactions you are talking about but I am aware there are ways of separating aluminum via magnetism (Eddy Current Separation) it is likely not a viable solution on a small scale but on a large scale I think there is a good possibility it could work for you guys. But again like I said I have never done the reaction of which you are discussing here and so there may be pitfalls Iā€™m not thinking of at the moment that will negate the use of magnetism.

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Ok so I know quite a few people are following the ALCL3 tek so I wanted to share some interesting phenomena that I experienced over this past weekend in America.

This started out using cbda mothers milk from cbda isolate formulation. Just trying to get creative with the formulation of thca (which is apparently a big deal there) Unfortunately all of the cbda that the person had created was sold so we only had mothers milk feed stock.

Using DCM and alcl3 I went through the normal SOP/washes that we normally do.

The material was definitely much darker than I have experienced before

I thoughtā€¦well thatā€™s why you need good feedstock. Here is really the only thing that changed other than the feedstock is during the drying stage after washes I went ahead and dumped the calcium chloride into the reactor to mix for about 2 hours before discharging through a filter that honestly I just rubber band to the bottom of the discharge nozzle.

The very interesting thing is that upon my first filtration I had what appeared to precipitate. Well normally I would assume aluminum hydroxide but the way that this precipitate behaved as well as the theoretically improbable chance that (quenching the way we do) leads to aluminum hydroxide formation (gel like pain in the bottom) I was like what is going on here???! Upon secondary filtration this is what I caught in the filter reactor! THCA!! It crashed in a matter of minutes! It would seem that I donā€™t know dehydration or something with the alcl3 when exchanging with cbda (maybe under the subcritical temps?) force crashes the thca out of it.

I confirmed this with only a 1.2% yield with oil out of the rotovap when I removed DCM.

Can a more well versed chemist explain the mechanics of what is happening?

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Did you isolate the cbda first or or did you run this reaction on the mother liquor?

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You created a Medusa solution :upside_down_face:
If any amine was used in the process it s very probable
OR you are getting thc-a B. Wich is a lot less soluble

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Ok so rereading your post I am trying to understand the steps taken and I have some questions
As @oscar asked was this a crude extract winterized with some terpenes still present mother liqueur ?
Or was it a motherliquer as result of a isolation salting process ?
So after washing you dried solvent of water content by adding cacl to the solution

Please explain above quoted
There is NO alcl3 anhydrous in that solution at this time and hydrated alcl3 is very improbable

A 1.2% thc-a yield ? And what else ?
Was in that solvent free oil ? Cbd-a
Other minor cannabinoids ?
Or did it almost all disappear to unknowns ( very probable iso-thc-a)
If the temps where well below 0C and an overdose of alcl3 was used in the reaction > 80gr per kg input material

So hunch number one
Cbd-a extracted by Medusa gas (bho)
Was used as feedstock and the dea amine never gave isseus for it doesn t interact with cbd-a but it does with thc-a
And it doesn t with alcl3/alcl4
So still present and caused a Medusa crash

Hunch number 2
Cbd-a was conceived by salting and the amine used was still present in minute amounts >0.01% and created the Medusa crash

Hunch numero 3
An amine was used in the reaction as buffer to avoid decarboxilation by the aggressive nature of alcl3
Resulting in above mentioned scenario
I would then recomend
Tetra ethyleen glycol dimethyl ether

As buffer instead of an amine
In natural extracts there is always 2-5% cbd-a B present and in isomerized rxn
It became thc-a B Wich is a lot less soluble in polar solvents than the A form
@moronnabis might have an explanation about the reason the solubility of the two is difrent

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One major difference is THCA-A can make an intramolecular h-bond with the ortho hydroxyl.
THCA-B can not. this phenomenon is somewhat pH dependent.
CBDA is very different.

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@EagleChem this tread might be of interest :stuck_out_tongue_winking_eye:

WOW. Roguelab. King.

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