Ethanol Crude Winterization

Hi Guys! So real quick, I’ve been working with BHO crude for the past 6 months without fail from winterization to distillation. My current process for BHO is melting the crude with a hotplate (never measured the temperature of the hot plate - just melted it down) using a 9:1 ratio (99% room temp isopropyl to crude) placing about 1000grams in a 5 gallon bucket. I’d place the bucket with the warm mixture in a -20c freezer for 12 hours. After the 12 hours, i filter the winterized crude using a pump filter funnel system to remove the fats and then scrub using carbon and bleach. The tincture is then roto’d to remove the excess alcohol then placed in a short path mantle for distillation. The mantle terms from 160f to 195f, then starts pumping clear from ~199f to 220f. This is the process I’ve had success with BHO crude.

I tired following the same recipe for Ethanol Crude, but failed in my first attempt. The end result was very dark clear.

My last attempt was doing a 10:1 ratio of 99% isopropyl to ethanol crude, warming both of them before mixing (Temps were not recorded of either, just warm them enough to get them warm:|) via a hotplate. I put the warm mixture into a 5 gallon bucket and put in a -20c freezer for 24 hours.

This batch was then filtered, scrubbed, put in a roto and finally into a short path for distillation with temps of 230f to 310f to yield clear( we were told that we should turn up the heat and blow through sp1 *whqt temp should this be??) from there it was ran again for a second time via a short path. the amount we yield was very little and still had good amounts of fat in the clear. and Very very dark.

After some research on this forum and online, it sounds like my winterization process isn’t correct.

Any insights or tips would be greatly appreciated!

Why are you using ISO? Use ethanol. Look into the quality of your trim, grind size, extraction temps, and then try multiple winterization.

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^ I second what he said. Or better yet, use methanol if you’re planning on throwing it in a still. :sunglasses:

That being said, I would reduce your solvent to extract ratio as well. I noticed 6:1 ethanol to crude ratio was much more effective than the 10:1 everyone says to use. Some folks around here are using a 4:1 or 5:1 ratio.

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@Jay-TL thanks for the insight! i used ISO for BHO so thought it would work with the ethanol crude. Unfortunately i can’t look at the trim since i’m buying the crude already made. do you have any tips for winterization?

@coppertop i’ll definitely try reducing the solvent to extract ratio, esp the 6:1 ;). any tips for how you winterize your ethanol crude? thanks in advance!

read Iso vs ethonal to understand why ethanol.

what temp did you extract with ethanol?
or are using purchased crude?

“clear”?!? call it distillate. please.
because as you’ve noted, it is anything but clear!
calling it “clear” suggests you’ve got a fair amount of reading to do.

why would you expect the distillation temp be sooo much different? you’re trying to boil the same molecule, from a similar matrix.

how much reading have you done on winterization?
https://future4200.com/search?q=winterization I’d start with the top hit, and then work your way through the next 1/2 dozen or so.

Same goes for your scrub. https://future4200.com/search?q=ethanol+color+remediation

then dig into distillation. I’d suggest I make terrible distillate....why? as a start.

You’ll also notice that relevant (posted) crosslinks are provided right below the first post in a thread. So you can explore topics in more depth.

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How do you like the methanol? Doing the room temp winterizing tech with methanol? Or same SOP as ethanol winterization? I agree with the lower solvent ratio I’m experimenting similarly, only problem with that is slower filter speeds with thicker solution

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@Siosis I am loving methanol winterization. Afa SOP, it depends on the crude I’m using. I only add 10% water to the methanol as 20% was giving me slightly sticky wax which I assume means that cannabinoids are starting to crash along with the wax (can’t wait to get in house testing to confirm that suspicion). If I immediately see waxes precipitating after dissolving the crude I will filter over alumina before throwing into the freezer at -26c to make the cold filtration easier. If I don’t see anything precipitating I’ll add about a tablespoon of B80 or T5 clay before throwing into the freezer to help flocculate the waxes to the bottom and make filtration much easier.

Lately I’ve been adding citric acid to the whole lot before throwing into the freezer to simultaneously degum as I’m dewaxing. I’ll filter everything over 240 grit alumina, then throw into the sep funnel with heptane to neutralize the acid and do some LLE before filtering through a CRC column, reclaiming the heptane, then decarbing/devolitalizing under vacuum in preparation for distillation. I’m able to hit 88% CBD with a single pass and a very light color with zero red.

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Thanks for the feedback! I really appreciate it.

So far I’ve been using ISO with BHO crude and it worked like a charm! From winterization to distillate .

For the Ethanol crude, I didn’t extract it, I purchased it from a vendor. I tried using the same steps that I used for BHO crude, but failed terribly. Again, my experience is comes from working with BHO. I thought the same steps would yield the same results from the Ethanol purchased crude, but I haven’t had success. :sob: I’m learning that Ethanol Crude is very different from BHO crude and requires its own process… I’ll report with more once I get more insight…:slight_smile:

you shouldnt use methanol unless you want to go blind. save it for the fellas doing basement extractions

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Is this scalable tho? Say for 1000 pounds a day?

Cough cough
We just had this debate in a thread the other day.

@Kingofthekush420

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not looking for a debate - just someone with a chemistry degree who has been banging his head against a wall reading all of this. anytime i see someone recommend something i know is wrong/not safe I feel obligated to speak up. you can listen to an expert(s) or your buddy - only one actually knows what theyre talking about.

*trying to avoid an argument from authority, but at some point, it needs to be said. stop “consulting” chemical processes if you are not a chemist.

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I’ll tag you in another thread there derailing with this

Ppl over here acting like we drink methanol (which we actually do when we consume alcohol)

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RIP beaker

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Exactly
The master used it and with excellent results.

I guess this guy thinks he’s the only person with a chemistry degree who has an opinion on this? There are plenty of folks here on the forum who are also formally trained chemists who have no problem using methanol or instructing others to use it as long as proper PPE is worn and safety procedures are followed. As I said on the other thread, if you can’t handle methanol without accidentally poisoning yourself, you have no business around any other flammable chemical we often use or heavy machinery for that matter and should probably get a desk job where your only occupational hazard is a paper cut.

Anyway, @Siosis it’s definitely scaleable with the right equipment. LLE is done at scale in plenty of other industries. As far as doing it safely with methanol, it just comes down to preventing skin contact and inhalation of vapor. Which doesn’t require any kind of new, innovative technology. Just common sense measures used in plenty of other industries.

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They make a system for continuous LLE.

It’s a pump that pumps 2 solvents opposite directions

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75 ton reactors baby :sunglasses:

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I’m gonna look into this. So tired of freezer tech and filter trolleys

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