Is it possible to load an ethanol/crude mix into a jacketed column then chill it and use N2 to pass it through a series of filters or crc with celite in it? Instead of using a normal buchner style setup for winterization
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Do you plan of freezing it to -45 to -65c for up to 18+ hours? Then pushing the coagulated mixture through after somehow homogenizing it back together first?
I would either do an acetone dry ice slurry in the open jacket and let it sit then filter it or pre chill the solution then load it and push it through real quick followed by clean but chilled solvent
Grab a jacketed feed vessel with over head stirrer, can even use a reactor if you plum it properly from the stopcock on the bottom. But the idea would be to freeze prior to filter, but you’ll have to mix the solution back together after it coagulates for a efficient seperation, the more surface area you have for the fats n lipids to be ran through the better. But a long column for winterization with media is un necessary as it’ll trap the fats n lipids waxes on top & once you push more through those will melt & run through with & or you’d have tons of clogging & slow efficiency, you’d have to reset the column a few times to fully pull all unwanteds. With a @SamboCreeck.com trolley, I can do one pass with a 4-5” plug on the 400mm & pull all I need in one pass, I do two passes for qc.
But ideally will have to let ethanol sit longer than you would methanol which would be a more viable option in your process for this
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then I’d just chill the tincture and mix it then load it in the column. wouldn’t the nitro push it through the waxes better? it’ll definitely take longer to clean waxes out in a stainless column but what I’m wondering if it would still save time. those trolleys are badass the wide surface area is definitely better for vac filtration
More than one way to skin this cat.
Settling and decanting, then just filtering the sludge is a perfectly valid response!! (Yeah you should filter the supe too, but that’s trivial)
@TheFire210 of course you can push through the filter rather than pull. You can push harder than you can pull too. Sucking only gets you 15psi across your filter and at that point you’re cold boiling your solvent.
The only caveat is how long you need to stall in this situation. 24+ hrs is ideal.
The trick to filtration is surface area, so a 24” buchner will work a lot faster than a 6” column.
Bag filters have more surface area, and a centrifuge is fastest/most efficient method imo
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I’ve used the positive air side of my diaphragm vac pump at 30 psi in my cls to do what you want to do. I say do it up, it’s safer than what I did too cause it’s an inert gas. Here’s a pass thru a. c. And d. e. The Pepsi challenge/etho color remediation thread - #56 by GroovyOctopusLabs that’s the result
I used these 1.5Ă—2 inch triclamp thingies I got from glacier tanks as carts for the powders
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Pushing an ethanol tincture with air is plenty safe at -20C (and lower), and shouldn’t be a problem for most PE to sign off on.
Using the outlet side of a diaphragm vacuum pump is well tested option
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Yes, but do it in stages. Room temp, slightly chilled, colder, then sub -60c. Or you’ll likely clog straight away
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Or you can stage the filtration, i do 25 micron > 15 micron > 10 micron > 5 micron > 1 micron.
If you can filter through a a series of cartridge or bag filters, you will go fast
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Staging the filtration would be recommended, for sure. But if he went straight to -60 or so. He’d clog
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That’s with one 5 micron filter.
exactly, you won’t have a need for a cold trap for solvent boiling off and a crc could be filled with celite that you just scrape the top layer off of every so often depending on how much waxes you’re trying to filter out.
And can use the bag filters for dewaxing really cold?? i use them at room temp but never thought to winterize in them, can you just pour the tincture in and dump dry ice in the bag as it’s filtering?
wish i had the $$ for a centrifuge
good idea, have you tried that for chromotography? the inert gas would be cleaner for sure but your idea is a lot easier
hell yea. you got a link for the cartridge filters?
Is that a diaphragm pump?
This is what I use. I also rigged up a small piece of hosing to one of these little 50 micron particle filters that I put on the vacuum side in hopes of picking up less crap from the atmosphere.
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yea that’s how i usually do it, room temp, freezer, chilled with dry ice for 24 hours
nah it was actually a vac pump, didn’t see he said diaphram
hell yea! that’s badass