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extraction of hash using liquid CO2 at 5.2 atm

  • by Kryptos
  • Jun 11 2012 03:05 AM
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Posted 11 June 2012 - 03:05 AM

Hello, I just joined this forum with a question about hash extraction methods. So one of my friends was talking about making hash by soaking herb in everclear and letting it evaporate.
My chemist friend was wondering, would it be possible to use a liquid CO2 extraction solvent under pressure, as used to extract caffeine from coffee beans and eugenol from cloves. If possible, this method would be cheaper and a lot faster.

Intro:
-Most essential oils from plants are 100% soluble in liquid CO2
-CO2 can be made to condense to a liquid under certain conditions (-56.6 C and 5.2 atm)
-liquid CO2 can be used as a solvent to extract and filter essential oils from plants

Materials:
-15 ml Polypropylene centrifuge tube
**This one is important, make sure its polypropylene. If it's too weak you just built a hand grenade.
-Flexible wire
Paperclip should work
-Glass wool
Some cotton should work but you will likely lose product unless you run it quite a few times
-Finely ground plant material
Coffee beans for caffeine, cloves for eugenol, That sort of thing
-Dry Ice
Grab a fair amount cause it evaporates quick. 5lb=~5$
-Clean pipettes
Not necessary but make life easier
-1 liter soda bottle
Speeds reaction and blast shield
-2 liter soda bottle
Backup blast shield (Trust me, if anything goes wrong, it goes REALLY wrong)

Procedure:
Wind up the piece of wire so that it creates a coil that will fit tightly inside the centrifuge tube. This should rest in the centrifuge tube at roughly the 1.5 ml mark.make sure you leave a long tail leading to the top of the tube so that this can easily be removed. Place this into the test tube. add a tiny bit of glass wool or cotton to completely filter out particles. Keep in mind this soaks up extracts so try to use as little as possible. After you make the plug, fill the tube with finely ground plant material till around the 7-8 ml mark.

At this point you should be putting on goggles and probably a kind of thick and shitty sweater you dont care about. Think protection, leather coat is good. I've added some safety features to my original proof of concept, but that one put shrapnel through a shisha tin we used as a cover.

Cut off the neck of the 1 liter bottle and fill it with slightly warm tap water. make sure the test tube can fully submerge in the bottle. Cut neck off 2 liter bottle. Make sure that the 2 liter can be inverted onto the 1 liter without disturbing the setup.

Take test tube with wire stopper, glass wool filter, and plant material and fill with crushed dry ice. Pack it down and use gloves if possible, this stuff is REALLY cold. Pack the test tube full of dry ice and cap it. Allow the tube to float in the 1 liter soda bottle upright. PLace the 2 liter soda bottle upside down on top of the whole assembly, and make sure it is not touching anything.

At this point, if you packed it correctly the dry ice should sublimate into CO2 gas, until it reaches 5.11 atm pressure in the test tube. at that point te gas will begin to condense into CO2 liquid and will filter through the plant material, dissolving any essential oils. eventually, the test tube will begin to leak and release CO2 gas, and the liquid at the bottom will evaporate. This process will take about 15 min at least.

Once all the liquid has evaporated, you should be left with some oil at the bottom of the tube. or crystals along the sides. Carefully open the test tube, as it will release pressure. Refill with dry ice up to five more times.
Replies (10)

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Posted 11 June 2012 - 04:16 AM

The problem with your method is the last 30 seconds of this video...
[ame][/ame]

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Posted 13 June 2012 - 12:45 AM

If you leave the test tube a tiny bit open it can still build up enough pressure to liquefy, and slowly releases the pressure. It's hard to describe, but I ran this in organic lab, I was just wondering if it would work

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Posted 17 July 2012 - 01:46 AM

Bump cause the only other comment was not applicable and I would still like a chemist's (with a degree) opinion. Anyone wanna bite?
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Posted 17 July 2012 - 02:36 PM

If you want to extract the oils from your herb using an organic solvent, look into BHO (Butane Hash Oil). Its the cheapness and efficency of CO2 extraction without the nessesity to reach high atmospheric pressure or deal with the resolidification of the CO2 at STP from a liquid state. The only problem with butane is its low combustion temprature.
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Posted 30 August 2013 - 07:25 PM

Bump cause the only other comment was not applicable and I would still like a chemist's (with a degree) opinion. Anyone wanna bite?

 

well after all this time it dont look like a chemist "with a degree" is around to help....but if ya want smart help instead of having to talk all slow I,m game....

I am building my "sub-critical" extraction unit in the coming weeks, "critical" co2 extraction is NOT what ya desire for MMj essentials, the sub critical will do a far better job and wont leave the finished product bland and unfavorable.....

 

Critical co2 extracts caffine from beans, sub critical co2 exracts leonine from orange peels, lemon and lime peels and stuff of that nature....so right off the bat you should see that Critical co2 is far too agressive for soft plant tissue

and will degrade the extract by denaturing it....

 

Ctitical co2 extracts suck as far as the smoking experience goes, no worthy flavors at all.....but when ya think with a "degree" you are locked into the BS mind set of a colledge....no thanks there........why?

 

because the "degree" mindset is that if 50 sand paper cleans up my hard wood floor it will do great on my antique furniture......

 

forget the "degree" ......I make this stuff with 200 dollars in equipment and any hobby chemist can do it easily...in fact to call it what it is ....I would say....10th grade science at best....

 

think about it man...what is Critical co2 and subcritical co2....

what is all that equipment you see with the extraction units and how much of it do we need to make oils....

 

this extraction method has been used since the sixties.......Why would you think that a person with a degree in chem would know this anyway, he'll look it up as fast as anyone,...critical co2 has nothing to do with the degree.....just cuz a guy is a mechanic dont mean he knows how to work on EVERY car.....

Edited by guerilla45, 30 August 2013 - 07:28 PM.

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Posted 01 September 2013 - 09:03 PM

good info thanks. there is a super-critical unit on the market for

less than $1500. and they say their unit produces fine tasting oil.

 

But I'm interested in the sub-critical if it gets whay we are looking for.

Does not have to be super=critical for me.

 

Hope you post more on the sub-critical method.

thanksm.

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Posted 01 September 2013 - 09:58 PM

sub-critical co2 is is the same thing as critical but the pressure and temps are lowered a touch.

 

with a liquid co2 temp of 120f and pressure of about 900-1100 pounds you should float right under the critical line in most areas.

this sets up for a nice oil with a lot of essence....get into the critical and it seems to lose a lot of flavor and overall appeal.

 

mind that I am still studying the topic very hard....... 

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Posted 02 September 2013 - 04:32 PM

there are some cheap  pressure vessels on the market  & with guages

for pressure and safety relief valves. I bet a system could be made cheap for a litre size.

 

dry ice kief (trichomes) for extraction might help with volume size. the co2 penetrates the kief.

Edited by onegreenday, 02 September 2013 - 04:45 PM.


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Posted 18 January 2014 - 04:07 PM

Im about to embark on the process of extraction, and wow.. there is so much being done out there its a little mind boggeling. Im trying to get up to speed on diferent process, costs and equipment. I need to know pros and cons to types of extractions, the dangers involved. I have an abondance of material, and have the expertise to build any type of system.. Im working with a bio-chemist and we are interested in getting some expertise from the experts, so please if you have some info you would/could share, we would be most thankful...


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Posted 21 January 2014 - 12:41 AM

Ive been playing with a DIY Co2 extraction idea for awhile now, involving a high pressure vessel and dry ice. ill post somthing soon, if i can.



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