New ways to quench

Layer of carbon on top and t5 on bottom mixture of silica, alumina and bentonite in the middle

Something about that crc mix loves heavy metals and high proofing solutions

Salt out quench and then filter

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You might try Chitosan. For a solid R-NH2 or R-NH3+
Compatible with dcm. Just do quick batch pour over…in a beaker…stir…see if it works…

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or better yet, in a glass column with a filter with a round bottom collection flask. choose what you put in the round bottom, if anything, for secondary safety, and a gas trap with a vac adapter if using a 3 neck round bottom for even more safekeeping of your actives.

beyonce had one of the best videos of all time, but if cotton balls and pressure equilizing funnels ever did a collab they’d give her a run for her money.

@Roguelab I can provide lotsa info relative to experience with pTSA, AlCl3, and ZnCl2 (or Zn itself and the utility of such relative to your questions) in DM if you wish!

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Liquid liquid extractions can be done inline aswell, use float valves with different densities to create a fixed bed height and use counter current flows. Take pipes protruding thru the bottom and make them different heights so they pull different substances based on which layer it ends up in.

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Still liquid
I am well aware of technical improvements that can be implemented
But a singel pass treu a crc should be able to cut it
It s 10 grams per kg of cbd that needs to be remediated of a highly reactive substance

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True, i was more so thinking another solvent that doesnt mix with dcm but still dissolves some basic stuff to neutralize. Im also trying to minimize water liquid as much as possible. But loading powders gets annoying

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Well depends
If only 10 grams of a kg needs to be neutralized a 6” stack with grain /powders can hold enough for 170kg neutralizing so if your rolling once a day :stuck_out_tongue_winking_eye:

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Well if ur getting that kind of efficiency then hell yeah

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First test off bicarbonate oven dried is good so pretty convinced this is gona be a viable route
2” x36” triclamp spool filled with bicarbonate and pass over it
First thing I noticed is your solids have to be dry or else nothing happens
There is probably a film of water Wich rejects the dcm but attracts the alcl3
Ph of dry powder flushed is 4.2
Ph of plain bicarb is flushed is 2.2 this is yust dcm alcl3 passed over the bicarbonate then ph is taken on the first
LLE of the water Wich was mixed with the dcm

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Back at the drawing board finnaly reagents are in first liquid quenches
All at 4 C
Heavy mix
Basic water solutions
Basic alcohol solutions
Alcohol amine solutions
Straight amine solutions
Keep you posted
Solids are next

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Ok so some good news the quench in general does not affect yield of your thc s when done with high mixing speed and at cool temps
Some quenches make emulsions some don t
Some affect color positively some don t
The examples shown are on dcm at -20 with an additional reagent in the flask to slow down reaction speed with alcl3
60 min start of taking samples 80 min last sample was pulled 8 different quenches tried
First quench bicarbonate soda
1:1 with water

All samples have had the same workup and are now placed under heat to check for isomerizations when heated from residual reagents

This is meoh+Potasiumsulfate +h2so4.

This is meoh with amine

Based on the isomerization results from heating i ll plan the length of crc stack with solid support reagents and filtration
For rxn residents times

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Arggg worked all this time to fuck it up
Pfffff darn members with their good idea s :stuck_out_tongue_winking_eye:

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Is that your disty?

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Yep fucked up big time
Used a amine that’s barely water soluble as quench and not in stociometric amounts thought I had it all figured out out WRONG by the time I realized damage was done
O well shit happens

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could always do a biphasic acid wash to remove trace amines but that may defeat the purpose of your ‘new way to quench’ venture!

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Well still in the wet amine versions and washing them out with water the regeneration of the sieves they can not be dryied as usual for you’ll destroy the amine it s loaded with so
And some amine i ll need to load on silica so checking now Wich makes most sense for that function
Salts formed must be preferably insoluble in solvent as to catch them with the 02m filter at the end
It s an interesting journey

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Arrggg so next mistake on the list hope some off you can learn
So for the tests I need to make isomerization product to pass treu the solid supports then distill them to see if at least my color stays good and if so to the hplc a before and after result

Now I dry solvent with mgso4 since it s quick and had a slip of hand when pouring in the reactor
Mgso 4 is fairly interactive with Lewis acids so decided to proceed
BUT when turning on the mixer on the reactor these mgso4 specks started nucleiation sites and within 5 min it was all crystelized
So evaporate solvent off
Melt cbd
Drain cbd
Add back solvent
Dry the goo
Back into reactor
And you are back where you wished to be 6 hours earlier :tired_face:

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Who doesnt love this? I am locked in on this one.
Thank you @Roguelab for always sharing such great research and tek.

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So why did my cbd crash to wet
BUT once dried and starting over it crashed again and yet again
Not even at a cold temp 14C
So WTF after carefull inspection of the reactor I noted this thin line
Wich turns out to be crystelized alcl3/cbd from the previous run and
Did not go away with the concentrated iso/hcl I use to clean the reactor after a run and at a glance hardly visible
Only now with a better background it is
So another lesson learned
Reactor has to be clean with no nucleation points on the glass

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Same line since I proceeded no really shows the havoc it can create
Not interested in numbers yust the quench so I proceeded but if numbers are the aim think we’ll before you proceed

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