methanol winterization

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.

@tweedledew Have you had success reusing your recovered methanol?

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Yup no issues

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Awesome! Thanks, excited to try this next week… ethanol winterization always seemed so inefficient. How are you filtering? Any media used, like alumina?

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Alumina yeah

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Why would you want to use methanol?

It’s more polar than ethanol so you need less of it. You can do the winterization instantly at room temperature.

Polarity is one factor of many for a good winterization.

Waxes crash at room temp in ethanol too. I haven’t done any winterizations in meoh (room temp or cryo) but I’d bet my final dollar that waxes would crash out of a room temp winterized solution if you brought it down to cryo temps. Im not buying it.

Well yeah you can add water to ethanol and it’ll have the same effect. Just need more water and higher solvent volume.

The whole point is to not take 3-48h and however much $$ it takes you to do a cryo run.

Water is free. Methanol is cheap and readily available. Time is precious. Rent is monthly and unforgiving. Fast processes are best processes provided they’re accurate & thorough.

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https://fscimage.fishersci.com/msds/14280.htm

https://fscimage.fishersci.com/msds/89308.htm

agreed. however, there’s nothing to suggest its accurate and thorough. There’s a million reasons not to use meoh. just cause it works does not mean its the best practice. I still am not seeing an advantage to it.

unless someone can convince me meoh actually does a better job, I would stick with the process that yields best results.