How could one test that there is still catalyst remaining without distillation? Having to work up the mixture all the way thru distillation is gonna eat the lab hours alive. Being able to rapidly test whether there is still catalyst in there would be imperative to rapid quench prototyping. I understand it would probably take mass spec as GC-FID wouldn’t cut it.
Yes. There are often wet-bench chemical verification tests for presence of a species… usually colorimetric or otherwise visible, at least down to low percentages or sometimes trace levels, just because our eyes have maximum resolutions for degrees of difference (i.e. a smallest detectable change or separation, based on the properties of structures in the eyes & visual system) for things like hue, opacity, particle size, etc.
@Roguelab 300g AC per kg precursor might as well be a metric fuckton, no? Yikes! It really depends on the target species and solvent system, so I hope you are referencing some detailed parameters he provided that I must have missed… I don’t know what catalyst, solvent, or even what rxn @MedicineManHempCo is performing! Too many different things going on at once!
Yes, ion exchange media is often used for this type of thing, but they are usually resins, aka the solid supports for which rogue was talking about DCM being too aggressive.
Ultimately, we need to find a replacement solvent for DCM. It is a nasty one for health, anyway, and its proper disposal is costly, in part due to it being largely phased out of commercial use.
I propose 2-methyl tetrahydrofuran or a similar, greener solvent. This particular solvent has enough similarities to DCM that I think it could work well. Like DCM, it has some Lewis Base potential to destabilize the would-be 9C for the Δ9-THC; a similar polarity index (I believe) to DCM, yet low solubility (also inverse with temperature, in fact) with water for better separations; and not so high a boiling point that recovery distillation is hindered.
So what you are saying is that anion exchange resins could break the complex formed between the AlCl3 and 2MeTHF? If that is the case, I wonder if the 2MeTHF would dissolve polystyrene? I have some anion exchange resin lying around that would be cool to play with but have no THF. I just wish there was a way to functionally immobilize the AlCl3 similarly to how sulfonic acids are crosslinked into the polystyrene beads. I have heard of AlCl3 being functionalized on silica gel, but so far it has been wildly expensive to think about buying, and “making” my own proved difficult and still didn’t work.
I wouldn’t expect a complex to form, but anyway I thought the issue was upon quenching the aluminum chloride…? You see? Too many different topics for me to follow. My point was just that DCM needs to be replaced by something safer for the workers and the environment… although I guess that’s yet another topic in the froth!
I just did some preliminary searching when you mentioned the solvent, and found this. I assumed it did.
https://www.sigmaaldrich.com/US/en/product/aldrich/553417
The problem is that no matter the number of washes or various different adsorbents in a cake, completely ridding the mixture of all trace catalyst in whatever form it may be in proves very difficult. I understand that DCM is a hazard, and I appreciate you for suggesting a potential alternative.
If you use ion exchange resins the right way, you get the job done without a single drop of water. You can completely skip LLE and can avoid any kind of further isomerization at the distillation process.
You can even add specific types of resins to
your setup to remove heavy metal contamination that comes along with the AlCl3 (e.g.: Al, Fe, Cu, Cr, Ni, Pb, Zn)
Curious what solvent you would suggest. Been tricky to find one that is compatible with both AlCl3 and polystyrene.
I think the ideas being discussed here are way super incredible and might even lead to further discovery so I’m not going to dampen that BUT I will drop another small crumb…
Instead of focusing so much on the chemistry aspect focus your efforts instead to the engineering aspect and the answer is right in front of your face. Probably quite literally.
Crumbs are fun… not the first time you piped up about something with no direction/proof of the statement…
Go back to falsely accusing people, suits you better opposed claming it’s an engineering problem that only you understand and everyone else has clearly overlooked…
please go away…at least until you realize the SOP that everyone is trying to figure out…is my SOP and we do it all the time. go envy someone else bye
I tried this with mixed results a while ago. I wish I had more time to study it.
I don’t care if it, or isnt, i have no interest in it as…
If it didn’t occur naturally in the plant, made by the plant/extracted solely from the plant in it’s natural state, it’s garbage!
What you’ve done (or claimed to have done) is significantly laughable.
I figured it was JUSTIFIED to make sure people know the “input” and “engineering observations” coming from you are coming from a mind feeble enough to falsely accuse people of actions related to rape.
Were you using that for reaction or workup? I believe that particular product would produce d8 and am unsure of its utility in catalyst removal.
Could you just shut the fuck up and let the adults talk? I couldn’t care less of your biases and am interested in sharing ideas with other chemists involved in the art.
Oh we’re swearing at people now? Your feelings must be hurt…
The only ideas I’ve ever seen you share are that of a garbage brain’s ramblings. You really should get the whole meth lab poop soup imagery out of your head because there are some talented folks out there making truly good product. A concept I’m sure that you are completely unfamiliar with.
Now that’s an insult! (I fixed it for you).
Bit of a reach, once i realized a thing or two about things and twos… i stopped publicly sharing and making threads.
“Meth lab poop soup” isn’t the image i have in my mind… but keep reaching…
Artificial/Synthetic/Converted = “Truly Good Product”
Noted.
Meh, you can think what you want because I wouldn’t wipe my ass with your opinion. How much analytical chemistry experience do you have? How many tests have you personally run?? What does your testing equipment consist of? Is gakass fishhash all you got brother? Do you have anything other than mindless ramblings and baseless opinions to share with the class? Kindly, sit the fuck down unless you have anything meaningful in your noggin worth anyone’s time.
I’ve got multiple cancer patients that rely on my products to get them relief while my state legislators drag their feet. I listen to the people that actually use and rely on my products because the rest is just noise…
MeTHF as solvent is basic in it s own and will probably not work
Somewhere between Mtbe and thf
It’s polarity is also on the high side
It’s water misibility sounds daunting to dry out prior to distillation
So not very hopeful it will work
Tolueen works and so do the other chlorinated solvents
Chloroform, dicloroethane, And 1.1.1 trichloroethane (works best)
Lewis acidity/basis properly of the solvent matter
There are some solvents that react with alcl3 and taking solution to the low (-20c) prior to adding the alcl3 avoids unwanted rxn with alkanes it s actually interesting to note that the addition of very minimal amounts of dcm will avoid the crashing of the cbd at low temps (<0) all in all quiet a rabbit labyrinth
As for the use of dcm with loaded beads
After contact with producers and reading some patents several can be used and althou some swelling might occure leaching should not
As for the alcl4 @EagleChem has the solution so probably available for the right price saving you a shit load of r and d
And honestly setting up a pressure filtration skid for the AC is fairly easy and takes little effort yust some additional equipment still need to do some r and d but seems that B80 (oildry)
Also snags it out
Since @eagelchem mentioned an engenering approach also works
I wonder if the 0.2um filtration is doing
Something as well since I am catching something in the filter and bentonites
Clog in time so maybe it s that easy