Winterization


#102

Hey buddy so I have an in theory question on making an inline dewaxer with my CC

I’ve asked bvv they said yes should work

But I have a CC… Not cls … So if I get another open jacket column, stack under mine and put valve in middle and have guage on both columns, material top, inline dewaxer bottom…

Then since I have no nitrogen or closed loop, to move solvent from the top material column, to the bottom dewaxer column. But I’ll have gauges on each to see it move from one side to other…

And I can take my vacuum pump, pull vac through both, closing top column,then the bottom one, leaving me with negative pressure on each, and a valve in btw keeping them separate…

I’ll have to either get filter column or slide whatman slow filters in BTW viton gasket filter on each side…I know this alot info bare with me… So the negative vac will allow me to fill top and soak, then move to bottom with negative pressure left on bottom column, open valves watch it move on gauges, and if not moving good since I’m backyard, maybe take empty cans and use the gas left to move it on to the bottom if any Is left… Then I can cryo soak and evacuate.

Would this basically be a inline dewax column then? Do you think the negative pressure will move the solvent ( along with jacket column temps being colder?)
The guys at bvv told me I might be on to something… Does the idea sound feasible, does anyone know anyone that tried this


#103

Good input. Seems like something that I am going to have to play around with and see what happens :slight_smile: gotta love fresh ideas and having no clue if they will work or fail hahaha


#104

I like your idea and I think I’m following what your idea is and why you want to run it.

By pulling a vac in both chambers when introducing the solvent the vac will assist pulling solvent into the system. Similarly when you open the ball valve to dump your solvent from material column into dewaxing column the negative pressure will assist the movement. However people who use this same method in their cls sometimes have issues clearing all of the solvent from the material column to dewaxing column and this is called vapour lock. I am not exactly sure what causes it. I have seen people say that they can even start pulling vac on their recovery chamber with all valves to column open so they would stop and assume that they have recovered everything, but when they open up the system to the atmosphere they find a noticeable amount of solvent that has been trapped in their material column. This only seems to happen when running columns at cryo temps. This is why people often use nitrogen assist because it is the only reliable way as far as I’m aware to clear your loaded solvent out of your material column. In theory any gas should work to force the solvent through but use a gas WITHOUT any oxygen! Gots to keep the conditions inside the columns safe so no chances of explosions :slight_smile:

So your theory should work but I would be looking into a cheap nitrogen cylinder and regulator kit to help you out. Also because when you are filtering your solution leaving your dewaxing column you will need positive pressure to assist the movement of the solution through the filter which nitrogen is perfect for. As said elsewhere if you try and pull the solution through the filter as opposed to pushing it , you will cold boil off your solvent and damage your vac pump. Although I seem to remember you saying you used water aspiration to pull vac so I guess that isn’t really an issue for you.


#105

Hey buddy thank you so much for actually reading that! Yeah so that’s me only issue was wondering if it would have pressure to go on through the filter, it goes through it when there isn’t another columm in the middle but yeah…ok so the gas in the can contains oxygen…hmm ok that means using it dangerous huh…

Ok how much nitrogen does it take, will a quick, pop of the valve be enough? Yeah if there is another big hidden cost I’m going back wards…

I’ll finally be able to get my solvent colder -40f , this may help about grabbing plant matter, seems like if I soak it any it starts grabbing plant matter… Looks like I gotta get the cryo column back out too… Just so next easier to set it in dry ice with it piled around it… Thanks so much again…

Also I have water asiparted vacuum for my buchner funnel, I really wasn’t planning on pulling on it but before I loaded it with Tane


#106

So i guess you will have to give it a go and see if it works without adding positive pressure. You can add the pressure by adding warm solvent vapours to the top of the system but then you are using more solvent and not sure if the warm gas would counteract the cold winterising proccess.


#107

I just bought 10lb of brown alumnium oxide for use in winterization of ethanol thc extract, before evaping then into my distillation rig.

Albeit only 20.00 or so for 10lbs.

I hope I have the correct product. The celite 454 I didn’t hear about until today.


#108

I have gone through pounds and pounds of alumina. I found 220-240 grit to be about right. I have used finer grit but much finer that 400 grit and it makes more of a mud and is hella slow to vacuum through. I used to be able to get white alumina but can’t find it in abrasives anymore. No difference but the color looked cool in a column.

Alumina as a filtration agent is very hard to beat. Essentially it is very old tech and is simply a sand filter which are highly efficient irregardless of application. The alumina is often used in chromatography so there is a great body of knowledge to tap on the sites that deal with chromatography. There are TONS of peer reviewed articles and posts dealing with its use in chromatography. As you pointed out too it is dirt cheap lolz plus it is inert and can be cooked way hotter than is possible without a kiln before heat impacts it at all. You can cook it very hot. It fact one lab I did was to cover the extract in a layer of alumina in my sublimator. Then I tried to see if I could cook the gas up out of the alumina.

It was a very early stab at research and the alumina just popped dust all over inside as the extract bubbled but the point is that it is a very versatile compound.


#109

I’m a smaller scale patient, trying to make very small batches of RSO with the equipment that I have available at home (equipment: MB2E, heated magnetic stirrer, sink aspirator, Buchner filter and a counter-top domestic still). My goal is to improve the final medicine by removing the lipids, waxes and chlorophyll; but, I’m unsure about a few steps, as my starting point will be an ethanol extraction from the machine (aka nasty dark tincture). If anyone can review this and give me some feedback, that would be greatly appreciated!

UPDATE: Thank you to everyone who has responded. If you also have a MB2E, do yourself a favor and read the threads on here. The cold ethanol extraction tek is a much more streamlined process that results in a far superior end product. No comparison…

Dry Ice Assisted Cold Ethanol Extraction for RSO

  1. Drive MB2E out to the country in my trunk and give it a send off that would make Office Space proud
  2. Perform a dry ice assisted cold ethanol extraction
  3. Transfer collection flask to still (domestic counter-top still designed for water) and recover majority of ethanol (leaving enough ethanol to transfer crude from still to beaker after recovery)
  4. Transfer extraction to beaker on a heated magnetic stirrer and boil off remaining ethanol at ≈ 78.2° C until bubbles stop and temperature spikes
  5. Continue heating at ≈ 122° C for 27 minutes to fully decarboxylate extraction
  6. Transfer to syringes for dosing, plus 1 mL for testing

#110

Ditch the butter machine and use cold solvent so as not to pick up any of that stuff. See Bucket Tek (Cold Ethanol Extraction on a Budget)

You can make 70% THC with essentially the tools you have, even with only a -20 Freezer. Effective meds. Dabbable or edible


#111

@Killbill


#112

I appreciate the suggestion. I read through the tech and it looks like there is no comparison between the end product, which makes complete sense. So, thank you for pointing that out. However, that still leaves me with the issue of removing the lipids, waxes and chlorophyll. Would alumina be preferable to traditional winterization and the carbon scrub? If so, can you give me your opinion on the steps I was planning on taking to remove the lipids, wax and chlorophyll above?


#113

From what I’ve learned on here.

-40c temps, dry ice aided
Ethanol

Filter thru buchner with 220 grit aluminum oxide still as cold as -40c as possible.
May have to filter 2-3x

Bring to room temp

Put etoh in warm water bath at 145*f (I hope I have the temp corrext), add powdered activated charcoal. Stir well. Leave to warm for 30 mins. Stir occasionally.

Let cool to room temp.

New buchner funnel with celite 545 and powdered activated charcoal on top. Please follow sop.
Filter 2-3x

Ethanol should be nice and light golden.

Please correct any errors I may have made. This is going by what I’ve read on here.

I have 8lbs of trim to run.


#114

@Killbill


#115

Theres a beach in SWFL called Siesta Key… 99.9% quartz sand. Silky smooth and fine like baby powder. Never gets hot even in the blistering August sun…


#116

Thank you for the response. I’ve thoroughly reviewed the Bucket Tek (Cold Ethanol Extraction on a Budget) and plan to proceed when I have the necessary supplies and equipment. I was hoping to find a way to clean up some existing ethanol extraction. I realize that the machine I have used is not suited for making a high quality extraction.

As ethanol is polar and also forms an azeotrope with water, I thought it would be effective to boil the existing ethanol extraction, hoping that it would perform a similar function to the isopropyl method described by Beaker, as they have similar properties. This will not result in the best final product (given the route I took to make the ethanol extraction), but it would likely produce a better product without further investment.


#117

Inow we’re getting somewhere…you’ve made icky goo, and want to try and clean it up.

adding water to 30% will ppt your cannabinoids. probably not what you’re after.

see louche: https://future4200.com/search?q=louche

try following @Beaker’s boiling iso verbatim.

Edit: coffee filters will get you 25micron nominal. 20 once they’re caked


#118

Yeah but you crash out cannabinoids too. Ive tested residuals in the precipitate and about 50% is cannabinoids (this was with 20% water/80% ethanol)
At 30% water I bet it you’ll be crashing as much or more cannabinoids than the carotenes and junk.


#119

If you follow their steps, but recover your ethanol in your still, you should have your meds


#120

@cyclopath This will work great for my needs. Thank you!


#121

Also heat.