LLE room temp maybe… Idk.
I love methanol winterization, I’ll never go back to EtOH. I am curious, have you tested any of you filtrate at 2:1 MeOH to oil? That’s a lot less solvent than we usually use and I’ve been concerned about dropping THC at tighter ratios but I’d love to use less solvent
Beakers methanol method was add water to the methanol so it’ll precipitate all the fats at room temp
It is harder to filter like see this
What method do you use ?
I find anything south of -5c precipitates the fats out quite well which leave me with no water in the filtration
I throw mine in a 27 cubic foot regular freezer for a few hours, once it hits -20 filter and youre good to go
I agree you dont need to go super cold
I got 5 on it lets start a crowdfunding page
Me over here looking at my chiller budget like…
Okay so it’s for the loop only!
Methanol:oleo 8:1louche, chill in freezer, filter, roto down to approx 2:1 meoh/oleo, LLE to heptane using an excess of brine, wash a few times with bribe for good measure and then run through a silica plug and elute with Ethyl Acetate
I can guarantee I have a unique method that will answer the op’s questions about
And I have to add 10K for THAT!
What kind of yield are you seeing with that method? Very similar to a process we are piloting minus the chromatography for us
Use it to chill the retentate (the part you circulate in the membrane system)
These high pressure systems create some heat, and heat changes the pore size of the membrane significantly
https://www.instagram.com/p/CGGMM-2Bfew/?igshid=ht18m2uu8ahl
These 2 were the same material and membrane only difference is the right one had the chiller running 5 degrees colder
Close to my LLE sop
6:1 in methanol, winterize, wash 1:1 with heptane till the heptane comes out clear (at 1:1 itll take 13 washes), then wash the heptane 1:1 with water once to remove any polars that jumped to the heptane.
You dont need brine when you LLE heptane and methanol, they seperate quickly you’ll just be ruining your methanol by using water and brine IMO
Dewaxing column (open ended to fill with salt water and ice), hemispherical heads on top with sight glass (sight glass optional), shower head (once again, optional), and bottom with 1/2 inch injection ports on top and bottom with sintered disc before bottom hemi. Add a gauge as well (be safe and monitor pressures).
Mix product to be winterized 3:1 with methanol and heat to 30c to achieve full saturation.
Put into solvent tank (install pressure gauge) and pressurize with argon to 30psi with braided line to top of hemi head (recommend valves on both tank and column to throttle flow).
Make a slurry of Activated Alumina (220-240 mesh). Drop a medium filter paper onto sintered disk, attach to column and pour slurry in. Depending on amount filtering will dictate amount of AA.
Let gravity do it’s thing to let the bed settle (also make sure column is level). Once down to about 3 inches of slurry, add another paper (so not to disturb the bed when injecting solution) then hand fill the dewaxing column with pre made methanol/extract solution.
Pack dewaxing columns jacket with water, salt, and ice.
Slowly open solvent tank valve (forgot to mention be sure to have dip tubes in the solvent tank heads and a relief valve for bleeding pressure), then slowly open the hemi head to the column.
Use whatever method to catch dewaxed solution into whatever catch basin you choose (I normally use another tank that leads into my rotovap and use the vac to pull material/solvent into ball).
You can add other filter media’s into another column and cycle from one into the other making for a continuous flow of filtration or add spacers with media of choice UNDER the AA.
Yeah skids and membranes have me completely lost. Definitely am due some reading on them in comparison to reactor / centrifuge setups.
The membranes are more for solvent recovery, and hopefully winterization directly… So in lieu of a FFE, RFE (That’s my limited understanding)
Methanol is cheap
It will always be cheaper to save solvent then to re buy it
The only reason you need salt is for faster seperation which IMO you dont really need with methanol / heptane
Only time I ever use salt is for high PH washes since they like to make emulsions, salt helps prevent this
The winterization membrane also seperates out, sugars, chlorophyll and other colored pigments.
They can also be used for terpene seperation (and solvent seperation)
Membanes allow for the use of screw presses which allow for a truly continuous extraction with no down time
Centrifuges suck IMO, the only reason we haven’t been using screw presses on a large scale is they mangle the outer cell wall and release alot of chlorophyll, membranes can remove this
The processing plant im designing will extract wet biomass using a serious of screw presses, and use membranes to clean it up and seperate out the fats and lipids, cannabinoids, terpenes and solvent
Think of membranes as filtration on a molecular level, youre literally filtering based on molecular weights
If I had a membrane thats 500 dalton, only things smaller then that will make it through. Fats, lipids and sugars are all over 600 daltons so they wouldn’t permeate through the membrane
Cannabinoids, terpenes, and solvent are all under 500 so they’d pass through, then youd use another membrane to seperate out the cannabinoids, another for the terpenes, then a final membrane for the solvent
Its all based on molecular weights