BUTANE EXTRACTION AND RECOVERY SYSTEM

Gray Wolf · May 6, 2011

jump117 said:
for the laugh! Let me ask a few questions.

Lengthening the duration of extraction at atmospheric pressure does not damage the quality and increases the amount of good extract.
Have you experimented with the duration?

Solvent should wash material. In still solvent effect of saturation of the contact layer slows down the extraction.
Certainly need to stir. How do you solve this problem?

Sorry I haven't much yet bro! I am still trying to speed it up and get it reliable running fan leaves. I will most definitely be experimenting with duration if the new pump works out.

We have discussed this issue, and considered multiple columns mounted in an array on a vibrating frame, connected by PTFE hoses instead of stainless tubing.

A vibrator could be mounted to our existing assembly, but would most likely loosten fittings and create leaks without a dampening hose or mechanisim between them.

We built a couple of simple closed system prototypes, incorporating vibrators which worked well at ambient, but did not reclaim the butane.

They also rose to about 25 psi at ambient, during a 10 to 20 minute vibratory soak. It improved the yield but actually required more butane, due to the increased volume of the non packed portions of the systems.

The material also exhibited more of a green hue than our flow through extraction of the same material and required more subsequent polishing.

foaf · May 6, 2011

Lengthening the duration of extraction at atmospheric pressure does not damage the quality and increases the amount of good extract.
Have you experimented with the duration?

That isn't true in my experience. Longer "steep" times make my oil darker for sure. I run two quick steeps, the first run is lighter and tastes better to me. The second run give about 1/2 again the yield of the first, it is darker, and while still great oil, it isn't as "clean" tasting as first run. I do approximately a 1 minute steep on the first run and maybe a couple of minutes on the second. When I initially did this, I did about a 10 minute "steep" and the oil was darker than what I wanted, which led me to the slightly cumbersome double runs I do now.

Gray Wolf · May 6, 2011

foaf said:
That isn't true in my experience. Longer "steep" times make my oil darker for sure. I run two quick steeps, the first run is lighter and tastes better to me. The second run give about 1/2 again the yield of the first, it is darker, and while still great oil, it isn't as "clean" tasting as first run. I do approximately a 1 minute steep on the first run and maybe a couple of minutes on the second. When I initially did this, I did about a 10 minute "steep" and the oil was darker than what I wanted, which led me to the slightly cumbersome double runs I do now.

Have you tried any method of agitation during soak?

foaf · May 6, 2011

Yes. The way I do it now is a bit different than the diagrams in my thread. I "push pull" the butane from the storage tank into the "steep" vessel, keeping the "evaporation" vessel between the pump and the steep vessel. Once the steep vessel fills up, based on my sight tube, I turn the liquid spigot off, wait part of a minute, then just turn it upside down, leaving the pump running all the while. The top port in the steep vessel becomes the bottom, so the liquid butane and oil mix moves into the evap vessel. While this is happening, I manually swirl/shake the upside down "steep" vessel. It takes about 20 seconds for it to empty, so it gets swirrled/shaken for this amount of time. I do this on both runs. I don't know if it helps any.

jump117 · May 6, 2011

Hence, by your description at room temperature, butane is behaving the same way as ethanol or isopropyl,
the extraction time is somewhere between them.

During the extraction in an open thermos, butane with its own temperature below -0,5°C (31°F) does not dissolve lipophilic mud for two hours.
I have repeatedly applied the scheme of 1 hour + 1 hour in an open thermos,
and always extract the second hour is almost no different in quality from the extract of the first hour.

I always suspected that the high selectivity of butane is due to its low temperature during extraction.

Gray Wolf · May 6, 2011

jump117 said:
Hence, by your description at room temperature, butane is behaving the same way as ethanol or isopropyl,
the extraction time is somewhere between them.

During the extraction in an open thermos, butane with its own temperature below -0,5°C (33°F) does not dissolve lipophilic mud for two hours.
I have repeatedly applied the scheme of 1 hour + 1 hour in an open thermos,
and always extract the second hour is almost no different in quality from the extract of the first hour.

I always suspected that the high selectivity of butane is due to its low temperature during extraction.

Good insight! Thanks bro!

foaf · May 6, 2011

Temperature is part of it, I'm sure, but I do think butane is still more selective. Has anyone done QWISO with super cold alcohol?

I have chilled the butane before the extraction on several occasions, and it makes a small difference in how clear the oil is. You do it by cycling the butane through the pump in a closed loop, and it gets cold pretty quick. My first post on my honey pot thing.

.... mostly my oil is now clearer than the early pics (shorter steep time and maybe even precool the butane using the recovery pump)

Before I built my rig, I tried using butane chilled with dry ice. It allowed me to just pour it, I poured it over pot in a collander and let it steep for a while, everyting chilled down, and I tried to make a recovery vessel from a pressure cooker. It worked, I recovered by chilling the storage vessel, like the satsuma thing. This is the only picture of that 2003 experiment that I can find. The oil I got from the butane chilled by dry ice was almost clear and there was very low yeild. It was like the vodka of hash oil, it really was the clearest stuff, I wish I had photographed the oil. It tasted very "pure".

This picture could be the first closed system ever, I dunno. Late 2003.

Rednick · May 7, 2011

jump117 said:
The effectiveness of the solvent depends on temperature. Dissolution goes faster with higher temperature of the solvent.

Liquid butane can be heated only to boiling point, which increases with increasing pressure.
At atmospheric pressure the boiling point of butane -0,5 ° C.
Under pressure in the can butane remains liquid at room temperature.

The higher the pressure in the extractor, the higher the temperature at which butane is a liquid solvent,
the better the efficiency of dissolution.

When using a simple tubular extractor, dense packing not only increases the pressure, but also lengthens the duration of extraction.

And it seems that the colder the extraction (within reason), per Dope Roors pics, preserves the other more volatile components than the cannabinoids that give good smoke that familiar flavor.
Following SCF theory, it is a combination of temp and pressure to achieve the supercritical state.
Which, from others obersvations when smoking the expensive co2 hash, doesn't preserve the compounds that appeal to the hashaseur...However, I am sure they yield the most product in the end.
So what we a really looking at is sub-critical extractions, or wash (liquid) extractions to more thoroughly preserve the compounds that are of interest to us?
Without some good spectro equip I cannot see a good way to define what compounds we are trying to isolate, thus enabling use to determine at what max pressure degredation of the compound would occur.
FSL sure as hell doesn't do that testing, or if they do (which they may), they don't commercialize it.
Not sure where I was going with this, except to say, this is what I see as the impetus going forward and fuck all the peeps (disp douches) that drove me to look at CO2 b/c it was 'healthier' than butane.
I'll use SCF CO2 when I get Superfund funding for cleaning up a site. (much literature from the gov on that, btw)
:blowbubbles:

Gray Wolf · May 7, 2011

Rednick said:
And it seems that the colder the extraction (within reason), per Dope Roors pics, preserves the other more volatile components than the cannabinoids that give good smoke that familiar flavor.
Following SCF theory, it is a combination of temp and pressure to achieve the supercritical state.
Which, from others obersvations when smoking the expensive co2 hash, doesn't preserve the compounds that appeal to the hashaseur...However, I am sure they yield the most product in the end.
So what we a really looking at is sub-critical extractions, or wash (liquid) extractions to more thoroughly preserve the compounds that are of interest to us?
Without some good spectro equip I cannot see a good way to define what compounds we are trying to isolate, thus enabling use to determine at what max pressure degredation of the compound would occur.
FSL sure as hell doesn't do that testing, or if they do (which they may), they don't commercialize it.
Not sure where I was going with this, except to say, this is what I see as the impetus going forward and fuck all the peeps (disp douches) that drove me to look at CO2 b/c it was 'healthier' than butane.
I'll use SCF CO2 when I get Superfund funding for cleaning up a site. (much literature from the gov on that, btw)

The outstanding news is that Oregon Green Lab has agreed to GC test our panoply of different extractions as shared research, so soon skunk pharm will be sharing empirical numbers, vis a vis subjective patient panel subjective and anecdotal results with ya'll!

Ya'll Oregonians might also check OGL out for your own research needs, as most certainly the principal's head appear to be on straight and they will soon be privy to more selective process data than ostensibly any of the national (International?) alternatives that I have found available to us simple minded patients to date and thus far.

The same results, from the same batch of material, extracted and treated in a variety of different ways.

I suspect that this data is already readily available amongst circumscribed medical research and other brothers and sisters that are not sharing, for any number of reasons outside the scope of this thread.

Anything this simple to extract and formulate a bunch of different ways, can't be a deep, dark secret, or privy only to this oooold retired manufacturing engineer generalists, whom last attended a chemistry class in the early 60's.

I also recognize that OGL services are not available beyond Oregon borders, in recognition of federal interstate jurisdiction, but these lab folks kiss and hug, shake hands, and share resources, so it may soon be coming to your state soon!

Check with your favorite local lab and encourage them to contact and stay in touch with OGL's principal Richard, for what we come up with, that may interest ya'll.

Hee, hee, hee, snicker, snark, snort, ahwoooooooooooooooo!!!!!!1

Ohmmmmmmmmmmmmmmmmmmmmmmmmmmmm!!!!!!!!!!!1

Rednick · May 7, 2011

Gray Wolf said:
Anything this simple to extract and formulate a bunch of different ways, can't be a deep, dark secret, or privy only to this oooold retired manufacturing engineer generalists, whom last attended a chemistry class in the early 60's.

We've got a witch! We've found a witch, can we burn her?
http://www.youtube.com/watch?v=yp_l5ntikaU
:blowbubbles:

Gray Wolf · May 13, 2011

Bingo! Hee, hee, hee, snicker, snark, snort...........

Got my total cycle time down to 49 minutes, with 41 of those being the vacuum purge to full recovery. Under my hour target.

Thanks to Ricky's Bong for the heads up on the Appion G5 Pump, it works slick.

I also upsized the line from the pump to the collection vessel to 3/8" and sat the recovery tank in an ice bath. I had already added collection vessel heat, in previous trials.

I replaced the electronic vacuum gauge with an analog one, after it died of infant mortality.

The way my cycle works, is I first pull a vacuum on the entire system using the CPS 6.2 cfm AC vacuum pump, to -28.5Hg.

I then close the lower valve that isolates the column to the collection vessel, but leave the top vent valve open.

I turn off the AC vacuum pump, and close the ball valve to isolate it.

I turn on the Appion G5 refrigerant pump connected to the collection vessel and open the valve that feeds liquid butane to the bottom of the column. The Appion pulls the butane up through the column and out the top vent valve.

As soon as the chill of liquid butane is felt flowing through the stainless line that runs from the top vent valve to the lower collection tank, the butane flood valve is closed, as is the vent valve.

I allowed the column to soak for 3 minutes, and then opened the lower valve between the column and the collection tank underneath, and allowed the butane to drain down into the tank.

I pumped for 41 minutes until I reached -25"Hg

Here are some pictures of the final configuration:

iSMOKE.KUSH · May 13, 2011

Gray Wolf said:
Bingo! Hee, hee, hee, snicker, snark, snort...........

Got my total cycle time down to 49 minutes, with 41 of those being the vacuum purge to full recovery. Under my hour target.

Thanks to Ricky's Bong for the heads up on the Appion G5 Pump, it works slick.

I also upsized the line from the pump to the collection vessel to 3/8" and sat the recovery tank in an ice bath. I had already added collection vessel heat, in previous trials.

I replaced the electronic vacuum gauge with an analog one, after it died of infant mortality.

The way my cycle works, is I first pull a vacuum on the entire system using the CPS 6.2 cfm AC vacuum pump, to -28.5Hg.

I then close the lower valve that isolates the column to the collection vessel, but leave the top vent valve open.

I turn off the AC vacuum pump, and close the ball valve to isolate it.

I turn on the Appion G5 refrigerant pump connected to the collection vessel and open the valve that feeds liquid butane to the bottom of the column. The Appion pulls the butane up through the column and out the top vent valve.

As soon as the chill of liquid butane is felt flowing through the stainless line that runs from the top vent valve to the lower collection tank, the butane flood valve is closed, as is the vent valve.

I allowed the column to soak for 3 minutes, and then opened the lower valve between the column and the collection tank underneath, and allowed the butane to drain down into the tank.

I pumped for 41 minutes until I reached -25"Hg

Here are some pictures of the final configuration:

wow. love this. i want one....

Gray Wolf · May 30, 2011

Hee, hee, hee, progress is being made!

After shaking the system out with fan leaves, we switched to prime U of Dub bud and ran successive 3 minute cycles to determine at what point we reached the point of diminishing returns.

After four three minute cycles at about 60F ambient temperatures, we ran the last cycle for five minutes, which appears close to utility at the margin (break even bang for the buck) for oil extraction from this strain.

Oil yield was low with this strain at approximately 10%, but that is not an unreasonable return on a number of strains. I have never gotten more than 21.6% using a simple column and the strain makes a big difference. More research required here.

We removed the oil at the end of each cycle by washing it out with hot ethanol, and the first two produced an amber oil. The last three cycles produced an oil with more green pigment, but which when vaporized, still produced a floral flavor that was still extremely smooth.

Now that we see where the break is, we will try running the first two flood and soak cycles back to back, without fully vacuuming off the butane soaked into the plant material in between, as the system reaches vacuum state relatively fast, but takes along time to scavenge every last bit of butane under vacuum. Limiting the cycle to only one hard vacuum evacuation, will shorten it by about 30%.

300 grams is a good size for fan leaves, but most of our extractions for specific patients require less capacity, so we made two more columns, to supplement the existing 1 1/2" X 48" column. We made a 12" and a 24" column.

The 12" column is on my stove in a pot of hot soapy water being boiled out for test later yet today, and should also be a perfect size for running samples.

Ahwoooooooooooo!!!!!!!!

Rickys bong · May 31, 2011

GW, I'd recommend putting a filter/dryer on the pump inlet. I had to rebuild one of mine due to sweet sticky oil accumulating in the piston ring groove and causing them to leak.

It only takes a minute amount of hash oil in the butane stream yer pumping to accumulate and cause the rings to stick and stop sealing properly. A filter won't restrict the flow enough to be a problem.

RB

Gray Wolf · May 31, 2011

Rickys bong said:
GW, I'd recommend putting a filter/dryer on the pump inlet. I had to rebuild one of mine due to sweet sticky oil accumulating in the piston ring groove and causing them to leak.

It only takes a minute amount of hash oil in the butane stream yer pumping to accumulate and cause the rings to stick and stop sealing properly. A filter won't restrict the flow enough to be a problem.

RB

Good input! Thanks!

BudGood · May 31, 2011

Just finished reading, great thread! :lurk:

Bobo Bolinsky · Jun 2, 2011

Howdy Do Gray Wolf :tiphat:

I was fortunate to get thru HS Science. Your take it another level innovations make we wish I'd have spent more time in the lab. Excellent work

Gray Wolf · Jun 2, 2011

Bobo Bolinsky said:
Howdy Do Gray Wolf I was fortunate to get thru HS Science. Your take it another level innovations make we wish I'd have spent more time in the lab. Excellent work
<aka Jolly Roger in other locales >

Thanks bro! Wish I had too!

Gray Wolf · Jun 2, 2011

Well the 12" column works slick and I have been playing with it, doing thing film vacuum purging of BHO.

I have been using the vacuum gauge to monitor progress and have noted that the recovery system will only pull to around 19" while butane is still evaporating from the column and the column is frosted.

By the time it is able to pull to 21", the frost is gone, indicating boiling has ceased.

At that point, I tried something new. I switched over to the hard ((100 micron) AC vacuum pump and pulled it down to under 29 in/hg and checked leak up rate to determine if some out gassing was still occurring.

None was detectable after 30 minutes wait and the extract was bubble free when the pot was opened.

Last night I left a thin film of oil in the warm collection pot under 29 in/hg vacuum over night with no discernable loss of vacuum. Pictures attached.

foaf · Jun 4, 2011

Have you considered fitting some "extension" tube at the bottom of the column so that the butane oil mixture can flow into the bottom of a teflon bag for evaporation? It's mighty nice not having to deal with the extra step of scraping or rinsing with alcohol.

BUTANE EXTRACTION AND RECOVERY SYSTEM

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