I’ve been doing T remediation with chromatography for about a year now and have very little experience with crude. A customer has about 10 liters of crude that was ethanol extracted warm in bags. The guy that extracted it has been let go. He supposedly winterized it but I have serious doubts. It smells of fumes very badly. Customer wants me to clean it up the best I can. I don’t have a loop extraction system, just some basic lab equipment a few vacuum pumps and solvents. Trying to keep costs for this project under $1200.
Scanned crc threads and such here quite a bit here lately. Found great info on clays and media to complete the task. I’m going to winterize it again with a buchner to get all the fat and waxes out for sure, I understand that process and have done it once before. After winterization, what should I try for cleanup in terms of equipment on a fairly low cost basis? Can I layer a bed in the buchner funnel with filter paper and media and vac it through or make a column that goes above the buchner flask and dry pack it with media? I know running it through a closed loop with inline crc would probably be best, but I don’t have that equipment currently. Again I’m pretty clueless on this so any keywords or links would greatly be appreciated.
Aloha! Yes-you can most certainly pack your Buchner funnel with medias and use that to clean up your crude. Will work wonders. Just be sure it’s packed really well so you won’t have any channeling and you night need to do a few separate runs.
The first run you can do with everything super cold and running over activated alumina will help hang on to fats and other crap. Then you can do some runs with celite and get some great filtering action. Carbon scrubbing works well too, if need be. And don’t forget LLE if you have a separatory funnel (or can rig one up).
Since you’re not exactly sure what you’re working with, have you thought about roto’ing it down and then adding back a known amount of fresh solvent?
Haven’t thought of rotovaping it back down. I do have a small rotovap I could run it with and access to a -40 cryo freezer. I’m going to mix it 10-1 with fresh ethanol when I winterize it again. Then rotovap it down after that. It’s got decent COA #s with 6.7%CBDV 63%cbd. Should make some quality distillate in the end. Thanks for the insight, appreciated
Oh yeah - that should come out real nice! Youre going to be amazed at how well you’ll be able to clean up your crude. You were reading the right threads and are on the right path…now you just need to get in there and play around with it a little.
Yeah, the same guy that made the crude tried to make distillate out of it like it is. Complete disaster, worst distillate I’ve ever seen. Smelled like a fish fucked a diesel fuel truck if that describes it even lol… Will do some LLE research, something I have never tried. Don’t have a sep funnel yet, but I can probably swing it for this project.
Heat to decarb temps- ensure full decarb- then as it cools hit it with 10% by weight 1:1:1 AC/T5/AA and stir for half hour or so- then dissolve 8:1 methanol to oleo and hit it with water til you see white wax crash out- filter over a bed of celite/t5/ac/and a mountain of AA that’s been wetted with distilled water- make sure your funnel is completely and totally chock full of stainless steel wool as it will keep the filter from clogging early by catching the fats and waxes that pouched out with the water addition
I use an 8x24 triclamp spool affixed to a keg for my butcher funnel, real fast
Next step is to stream a steady flow of heptane through your methanol and collect it to evap- the heptane will extract the goods from the methanol and leave a lot of crap behind-
This is version one- I added sight glasses all over- use a UV light to tell if you’re pulling methanol through your mixer settler, the heptane will be real dark at first and gradually clear up
