methanol winterization

Looking to use methanol for winterization. I run warm etoh ~23c. Quick carbon scrub and comes out looking great. I’m limited on freezer temps and dry ice consumption. Current freezer gets to -26c. 2 days and quick pass through celite. I repeat this 2-3x and its eating up way too much time. Curious if methanol would be a good fit for winterization. And info/pointers would be appreciated.

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There’s a search bar it has a little magnifying glass logo you can find things with it

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No need to be a dick, as I’m well aware of its function :grin:. All those posts got derailed. Looking for feedback mainly. Sorry I didnt specify. Is it working of others with similar limitations? Is it cost effective? Better end result?

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But that’s my nature friend LOL I’ve messed around with it some but I haven’t done a controlled test all I know is when I get this s**t on my skin I start feeling really good and go take a nap LOL

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Fair enough, I shall bathe in it…

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Great way to wind down after a long day of work

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As long as you are entering the ICH tables Class 2 solvents, you could try DCM. Dichloromethane has no flash point and a lower boiling point so it would go through your solvent recovery process quicker.

We were planning on doing some testing with it down the road but lol money.

Methanol is a good solvent for winterizing with advantages in it nature
It does not like waxes
And does not form an azeotrope with water

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8:1 seems to be the winning ratio. Dilute, filter at room temp, throw a teaspoon of T5 in it and freeze overnight in that -26c freezer, then refilter. I like to filter at room temp first just to make it easier on my filter when I do the cold filtration. RT pulls half the fats, cold pills the other half.

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DCM has so so so many more drawbacks though.

It eats plastics like crazy, smells foul, is way more toxic via inhalation than methanol on an order of a magnitude, and will make your balls shrivel up into raisins. its also incredibly difficult to dispose of properly because of how powerful of a solvent it is.

Storing the stuff is a nightmare, it loves to escape its bottle and needs to be stored super cold.

I can go on and on.

Suuuper useful for some things, but very specific things that are not like trying to winterize at any sort of scale

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dilute with what>?

Ah, should have specified. Methanol.

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So since methanol doesn’t form an azeotrope with water, does that mean solvwnt recovered via simple distillation (I.e. rotovap) can just be used again as is without reproofing like ethanol?

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@Rowan I used to work with DCM a lot in my polymer work. I avoid that stuff like the plague - inhalation hazard was always what freaked me out!

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ok cause I tried doing the louche method where yuo add water to crash out the fats n waxes and it turned into a living breathing nightmare of a day.

a top layer of activated alumina that is spritzed with a little water stops waxes like a brick wall but lets the rest of the good stuff through and is essentially the same principal

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That makes WAY more sense. How much water did you add to the methanol that made the mess?

When I distilled some water laden methanol the water seemed to stay behind pretty easily. But that was only at 20% water. With a more diluted mixture you might have to distill twice since it’s still pretty hydrophilic.

well theres the thing… I added enough to get it to 20% H2O but I realize now that it must have evapped quite a bit - the original volume of methanol had dropped substantially after sitting in a fume hood without a lid for a few hrs. I had to warm the crude and methanol to get it to come together cause it was v saturated, so as it cooled under the fans it just left the lab and I made no account for this.

learning things all the time.

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yes only watch for acidity of methanol along the way it might become accitic

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I usually run 5-7:1 solvent to resin, freeze overnight.