Methanol winterizing

Hey!

I’ve been doing primarily methanol winterization for a bit now with decent results. Ran into something odd. Usually I just do a 2 day winterize, but left some stuff for a week.

I usually run 6-8:1 for solvent to oleo.

Had some weird stuff happen, I’m guessing there might have no been enough solvent with the oil? But instead of just waxes, it seems like a ton of stuff dropped out. I was left with A beautiful red/orange methanol solution, then a slick black oil layer at the bottom.

I’m redissolving the remaining oil in methanol again and re-winterizing (there’s a bunch in there), to see how it goes. But just curious if anyone’s had this happen before?

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Get it tested

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Good call :stuck_out_tongue:

I’ll take a sample, but redissolve the remainder and winterize again. (Deadlines and rent and all that)

There’s a bit of charcoal in there so I was thinking the charcoal acted as a flocculating agent? But there definitely seems like there’s a ton of something still left in there.

Seems like theres two separate oily layers in there too. One stuck to the bottom. Then something runnier and slicker moving around on top.

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I’ve left 85gs of shatter dissolved in 350ml of methanol in the Freezer for at least a month and a week and this hasn’t happened

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Hmm, my other thoughts were there was some water in the crude when evapped. Bringing the methanol percentage down.

Some people do room temp winterizing with methanol at 80//20, so I’m guessing perhaps I got some water issues?

I dissolved ait in fresh methanol and popped it back in the freezer to test

I’m planning on using methanol + ac for winterization first time using this solvent for this purpose -adding powdered ac to the solvent, the filtering over aluminum oxide and T5 will be a problem or no?

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Seems just fine

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Have you done room temp with 80/20 yet? That’s what I’d like to do- if I was gonna freeze it I’d just use ethanol, filtering the stuff and keeping temps cold throughout filtration has been a bitch.

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@beaker always did it with great success. I do believe he’d start with 99% and then add water to watch the waxes precipitate? I haven’t tried room temp yet. Was waiting for my analytics to come in to test the efficacy of both methods

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Rip sweet prince :crown:

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I wonder if the water helps get the chlorophyll out of solution as well? I know chlorophyll has a hard time dissolving in methanol, but dramatically more so when its cold. I’ve tried 90/10 before, but I’ll try the 80/20 tomorrow at room temp after I filter what’s currently winterizing and add citric acid before tossing back in the freezer.

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I think the chlorophyll is happy to go into water? Or I think the thought around here is higher water % in your initial solvent, the higher chlorophyll pickup to expect. Though this was mostly tested with ethanol I think

I use methanol only , in my experience when it has that wierd thicker oil ifs chlorophyll

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Citric acid, what does that do?

My yields have been getting hit pretty hard freezing the 90% methanol mixture at 6:1. I’ll be distilling a room-temp only winterization at that ratio on Tuesday and see how it goes. Im wondering if the freezing is crashing cannabinoids, because it feels slick at first, then SUPER sticky.

Degumming, since I throw it into a sep funnel with water and heptane after winterization. Pulls out a TON of red.

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At that ratio you better be washing your waxes good, or just let them pile up and get the stuff extra liters later. I never noticed a huge yield difference

Not sure why it changed my name i had to log out then back in. Depending on the crude I usually do a 3:1 or so then have more in the freezer to wash the waxes. I also save rhem all unless there white as snow and then do one big pain in the ass filtering and get every last bit eventually

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Ok, so a though occurs. 80/20 methanol/water is used for room temperature winterization (or at least warmer temp winterization). Methanol is too non-polar to winterize at room temp alone, so the polarity needs to be stepped up with water. Why not do the same with ethanol/water mixtures? Since ethanol is less polar, find a workable ratio (eg. 75/25), and that way no toxicity issues or cost of chilling to -40 really cold for a long time if methanol is off the table.

I’m using non-decarbed ethanol crude so the cannabinoids are slightly more polar to retain more cannabinoids in solution.

I already found a solvent polarity chart (on a scale from 0-1). I know that’s not the most accurate way to do this, but it is better than nothing (link below).
Solvent Polarity Table - Miller’s Home (google.com)

Polarity Values:
Water: 1
Methanol: 0.762
Ethanol: 0.654

I’m not sure what kind of curve to follow, since a linear curve doesn’t really make sense, 80/20 MeOH would yield a polarity of 0.8096 (1x0.2 + 0.762x0.8), that would require 40/60 EtOH/water, which it doesn’t even dissolve at that concentration, so maybe a formula with a square curve? Not sure how to do that math at the moment.

I’m currently doing a run with 65%, 70%, 75%, 80%, and 85% EtOH by weight at 5:1 crude to solvent. I may want to bump that up in the future, but I find it’s usually best to minimize that as much as possible (depends on who ya are I guess). What are people’s thoughts on this?

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I think @Photon_noir has some insight

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