Hey Everyone
I have learn a lot from this lovely site, and here is something I write up that I believe will be useful for people who is looking for Crystallization SOP. SOP for 100L Glass Filter Reactor by Jimmytian8 at Future4200.pdf (355.6 KB)
I have write it up based on my personally usage, and it can be improve as well.
And here is a photo of CBD isolate I got based on this SOP:
Any commend or suggestion is welcome.
Thank you for this write up. Informative and good for visualising the process, i dont know much about the subject but its much clearer now.
Definetly deserves more replys and thank yous from the comunitys side.
So a 100 thx from me!
Hey man thanks for the post 
keep up the good work
have you attempted to dry CBD isolate in the filter reactor? My thought would be to heat the jacket to 30C (to evaporate pentane), pull a good vacuum, and agitate slowly. Maybe even sparge a little nitrogen through the bottom. This way no vacuum oven is needed to dry your isolate, and thus less vessel changes.
After drain all pentane from reactor, I found it is hard to agitate the crystal. If you got a bigger motor and have a VFD that can control motor spin in both clock and counter clockwise, then your drying method may work.
In factory, my client prefer loading this crystal into professional powder dryer machine for 2 hr to make sure there is no solvent left.
Thank you for sharing this SOP! I especially appreciate the note on chilling capacity for the run size!
One Question:
Do you continue stirring/mixing the vessel during the temperature plunge? This was a little unclear from the SOP. I was under the assumption that mixing during the cooling process would prevent / slow down the nucleation / recrystallization, so I was wondering if you wait to resume mixing until the harvesting of the “supersaturated slurry”.
Unfortunately, my reactor does not have a filter bottom, so I believe I will have to drain the slurry and perform vacuum filtration with a buchner funnel.
Thanks,
AG
You have it backwards my friend, agitating while dropping temps will cause a lot of nucleation points and will cause the solution to remain as a slurry vs a large hard chunk of cbd that you have to then have to pulverize.
thesk8nmidget is right.
If you dont turn on mixing when dropping temperature, you will end up with a big crystal.
And it take a much longer time to make same amount cbd isolate by weight as well.
Those big CBD crystal are good for Instagram photo or trade show display, but not so good for making into product. They melt down slowly.
Ahhh ok, that does make sense. thank you so much for the quick response! I appreciate the help!
Does it matter if the agitator/paddle is submerged in the cake after the final rinse or should it be raised to maintain the structure of the cake prior to removing from the vessel? How important is it that the agitator be raised and lowered in/out of slurry/cake? I understand the importance of agitation during crystallization process but unclear during/after washing cycles.
@LydiaDeetz during my homegenization phase i have it hot at 37c and i stirr at 500rpm… once its all uniform * roughly 10 min or so* i start my ramp program and turn agitation down to 350… once nucleation begins or if i have to seed the solution i ramp it back up fast to 500 to increase nucleation points. i keep agitation going throughout the entire program. once i need to decant my ML thats when i stop my paddle. and i keep it where it is throughtout the washing phase and when i drop the isolate.
You will find your agitator stuck in the cake when you drain your liquid phase out of the tank.
You can either stop the agitation before drainage (to prevent your motor from burning) or raise the agitator.
