Large amount of solvent getting stuck in my closed loop system.

Fadedawg

Well-Known Member
So I received my filter in the mail today and I'm a little bit skeptical about this plastic ring on the top??? Do you cut that off? Also how do you wash it? Thanks for all your advice! I really appreciate your time.
I leave the plastic ring. The bottom vee shape sits on top of a raised ring, and is sealed against it by pressing down on the top of the plastic ring.

By hand in hot soap and water, but it could probably be run in the washing machine.
 

cannabineer

Ursus marijanus
For starters, may I note that other than proving the process and Lil Terp equipment, the balance of my R&D has been with active systems using a pump?

I've also never inline de-waxed with a passive system, but let's first talk about how they work and how to figure out pressures, so as to keep things in perspective.

Passive systems move the butane around using differential pressure created by differences in temperature. The Gay/Lussac law says that the pressure of a given amount of gas, held at constant volume, is directly proportional to it temperature Kelvin. P is a constant function of T, so P/T=C, and P1/T1 = P2/T2 = P3/T3........

That makes equipment sizing critical, and too many brothers try to run columns too large for the base. With a 10" X 12" collection pot and 3 X 18 column, you have about a 7.4:1 ration and should be more than adequate.

Kelvin is Celcius minus -273.15 degrees, so at 21C/70F ambient, we are at 294.15K, and the volume of your 10" X 12" pot is 942.5 in/3 at 29.92" Hg, and your columns 127 in/3 each.

29.92:294.15::1:X=19.5K or C /35F temperature differential in temperature needed per inch Hg of vacuum. As you can see, passive systems operate with relatively low pressure differentials, so they don't gracefully tolerate much resistance to flow.

You can also see why water ice and brine give little vacuum for inline filtration, so suggest using dry ice and alcohol.

Predistill your butane and have everything in the system connected and vacuumed to as close to -29.92" Hg as possible to remove all the atmospheric oxygen, and to eliminate any non-condensable gases in the system. After vacuuming, close the valve between the collection and recovery tank and open the recovery tank valve.

Note, if your injection and recovery tank are the same and you can't plumb it to do both without disconnecting it in the process, install a tee fitting in the line between the recovery port and the tank, that allows you to vacuum out the line again after re-connection.

I suggest packing and freezing the material column to ~-18C/0F, and wrapping insulation around it, but installing swiftly and not putting coolant and ice in the jacket.

If it is warmer than -.5C/31F, when the butane hits it, it will vaporize and impede further butane flooding the column, without a vapor vent.

Chill the pre-distilled n-butane to -30C and use an auxiliary hot vapor tank to provide tank head space pressure. You can also use N2 for this, but I prefer hot vapor, so as to not require subsequent burping.

I would put alcohol and dry ice in the de-wax column jacket, and set the collection tank in an alcohol dry ice bath, as well as the storage tank connected to the collection tank by hose.

I would use a screened gasket and a couple wadded up commercial sized coffee filters between the extraction column. You just have to keep the chunks out, as you will be filtering again. I would use a 1 micron 4" X 8" polyester felt sock filter between the dewaxing column and the collection tank. Face filters blind rapidly when filtering wax.

An alternative is a roughing filter, followed by finer face filters, but you need to get down to around 25 microns or below.

I would inject through the material column, into the de-wax column, and let it sit for 30 minutes to an hour, before opening the valve under the de-wax column, and pulling the butane through a 1 micron sock filter.

I would remove the insulation from the material column after injection and when I got ready to filter, I would add warm water into the material column to warm it up and drive off butane.

Open the dump valve and allow the 29.92" vacuum in the collection pot provide the initial boost for vacuum filtration.

Once that vacuum is lost, open valve to recovery tank.

Once the column is drained, I would set the collection pot in ~100/110F warm water, leaving the recovery tank in dry ice and alcohol for final recovery.
It is nice to see a scientifically literate writeup like this.

I have two questions.
1) What do you mean by passive v. active system?

2) How does the dewaxing column work? With what is it packed?
 

cookie master

Well-Known Member
Passive uses temperature differential to move the fluid/gasses from the storage tank, through the material, to the base tank, and then back to the storage/recovery tank. Active uses a pump to move the fluid/gasses.
A dewaxing column has a jacket around it to either put dry ice or supercooled fluid. The column is empty and you put the oil in it while its still full of butane. Then you leave the oil in the dewaxing column for an hour or 2 while the oil gets so cold that the waxes congeal. then you run it through a filter to catch the congealed waxes.
 

Fadedawg

Well-Known Member
It is nice to see a scientifically literate writeup like this.

I have two questions.
1) What do you mean by passive v. active system?

2) How does the dewaxing column work? With what is it packed?
A passive system uses heat and cold to recover the LPG, while an active system uses a refrigerant recovery pump.

A dewaxing column is typically jacketed, in which a solvent and dry ice mixture can be used to drop the temperature of the solution inside the column to subzero temperatures.

As the temperature falls, the solvent loses ability to hold the marginally dissolved plant waxes in solution, and they precipitate out, so that they can be removed by the filter at the bottom of the column when the dump valve is opened.
 

cannabineer

Ursus marijanus
A passive system uses heat and cold to recover the LPG, while an active system uses a refrigerant recovery pump.

A dewaxing column is typically jacketed, in which a solvent and dry ice mixture can be used to drop the temperature of the solution inside the column to subzero temperatures.

As the temperature falls, the solvent loses ability to hold the marginally dissolved plant waxes in solution, and they precipitate out, so that they can be removed by the filter at the bottom of the column when the dump valve is opened.
Thank you for the explanations!

Is Soxhlet-style system in these categories, or different?
 

Fadedawg

Well-Known Member
Why did you not select that process? Is there an advantage that offsets the hassle of working under pressure?
With a polar extraction, soxhleting extracts copious chlorophyll and anthocyanins. With a non polar, plant waxes, beta carotene, and pheophytin.
 

cannabineer

Ursus marijanus
With a polar extraction, soxhleting extracts copious chlorophyll and anthocyanins. With a non polar, plant waxes, beta carotene, and pheophytin.
I am aware of polarity effects on solvent selectivity and power. My question is, what about the pressurized process confers sufficient advantage to offset the increased labor and risk that are part of that process?
 

Fadedawg

Well-Known Member
I am aware of polarity effects on solvent selectivity and power. My question is, what about the pressurized process confers sufficient advantage to offset the increased labor and risk that are part of that process?
LPG's low boiling point makes it easier to remove while not removing or effecting the monoterpenes.
 

cannabineer

Ursus marijanus
LPG's low boiling point makes it easier to remove while not removing or effecting the monoterpenes.
I achieve that result when recovering my extraction solvent by distillation through a column. At this time I see more trouble than benefit in running a pressurized, non-recirculating system.

I am not interested in the monoterpenes. They confer aroma but pharmacologically I think of them as dead weight. My process is tuned to go for max potency, so I remove them.
 

Fadedawg

Well-Known Member
I achieve that result when recovering my extraction solvent by distillation through a column. At this time I see more trouble than benefit in running a pressurized, non-recirculating system.

I am not interested in the monoterpenes. They confer aroma but pharmacologically I think of them as dead weight. My process is tuned to go for max potency, so I remove them.
If all tastes were the same, us'n man childs would have killed each off over the same woman long ago. If you don't care about the monoterpenes, I suggest subzero ethanol or QWET.
 

cannabineer

Ursus marijanus
If all tastes were the same, us'n man childs would have killed each off over the same woman long ago. If you don't care about the monoterpenes, I suggest subzero ethanol or QWET.
I dewax using methanol; it's super convenient and it has good extraction values in hydrocarbon/water.

I am something of a yield freak, so I'll be sticking with Soxhlet as the first step.

Ethanol would be more viable if I had a working Rotavap, sigh ... recovering EtOH by distillation is a misery.

Btw I am one of T&T's two admitted homosexuals, so while you were scoring with the woman I'd be raiding your larder :joint::bigjoint:
 

Fadedawg

Well-Known Member
I dewax using methanol; it's super convenient and it has good extraction values in hydrocarbon/water.

I am something of a yield freak, so I'll be sticking with Soxhlet as the first step.

Ethanol would be more viable if I had a working Rotavap, sigh ... recovering EtOH by distillation is a misery.

Btw I am one of T&T's two admitted homosexuals, so while you were scoring with the woman I'd be raiding your larder :joint::bigjoint:
Yield of what? http://thealchemistresource.thealchemistresource.com/p/normal-0-false-false-false_20.html

Check out: http://thealchemistresource.thealchemistresource.com/p/normal-0-false-false-false-en-us-x-none.html

http://thealchemistresource.thealchemistresource.com/p/normal-0-false-false-false-en-us-x-none.html

Something for everyone at T&T!
 

cannabineer

Ursus marijanus
I estimate my product to be about 90% delta-nine-tetrahydrocannabinol.

When I had access to column chromatography, I was able to get the yield figures by direct gravimetric analysis of the fully purified (vide infra) cannabinoid. A sample of Indica in 2001 titrated 11.3 per cent, and the primary pentane extract was 89% THC after decarboxylation (argon, thermostated silicone bath, 120 degrees for 10 min)

A chromatography and molecular distillation yielded water-white THC that was one spot by TLC (thin-layer chromatography, ceric sulfate visualization) and no evident impurities by 300 MHz NMR spectroscopy.

My best yield of high concentrate has come from a GG#4 extraction. Bioassay showed high potency, and the yield of finished 3-stage concentrate (extract, dewax in alcohol, 2-stage molecular distillation) was just over 20% of initial flower weight.

I have not yet been able to separate CBD from a THC-rich isolate using hobbyist chemistry. I've seen crystalline CBD isolates and would like to be able to make such myself. It's an irritant to an experienced organicker to have not yet succeeded at that. I haven't had a confirmed CBD-rich isolate to work with, so that might be a factor.
 
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