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supercritical c02 extraction

smurfin'herb

Registered Cannabis User
Veteran


OK, So how much are we talkin to build this? Where can one get the parts and are they obtainable to the public?
 

boroboro

Member
I'm a fan of extractions, and would certainly like to see this happen. Where did you get this diagram? I think I've seen (legal) herbal supplements made using this process.

The thing that jumps out at me is the pressure indicated: 300 bars for about half of the system, including the chamber the weed is in. That's about a metric buttload of pressure. Natural gas powered cars I used to work on had about 200-250 bars of pressure. Steel lines, valves, and fittings were readily available through suppliers like Mcmaster-Carr. Tanks and big chambers exist, but not inexpensively at those pressures.

I wouldn't build it myself, though, because of the pressures involved. Don't want to make a mistake with 4500 psi. Ouch.

I don't know these companies, but it looks like plenty of people would sell you a complete functional unit:
http://www.accudyne.com/b12_supercritical.html
http://www.supercriticalfluids.com/sft100xw.htm
http://www.edenlabs.org/supercritical_extraction.html
 

3dDream

Matter that Appreciates Matter
Veteran
bump...

I am curious if people have looked into this. I have found entry level models like SFT-100, but can't find pricing. Is there anybody out there that can help put together a DIY SFE?
 

3dDream

Matter that Appreciates Matter
Veteran
as a rule of thumb the extraction of marihuana with carbon dioxide of density 0.9 g/ml at 40 degrees C for 34 min and of hashish for 18 min can be suggested. The application of the proposed extraction times ensured at least a 95% recovery for the main neutral cannabinoids.

Walter White - I would like to explore this a bit more for sure.

Here's a patent...

http://www.patentstorm.us/patents/7344736/description.html

In PCT/GB02/00620 the applicant discloses a method of preparing a herbal drug extract (botanical drug substance) from medicinal cannabis. The process comprises: 1. a heating step to decarboxylate the acid form of the cannabinoids to theirneutral form; 2. a first extraction with a specified volume of liquid carbon dioxide for 6 8 hours; and 3. a step to reduce the proportion of non-target materials, referred to as winterisation, which step precipitates out waxes.

More specifically, PCT/GB02/00620 describes a process wherein: step 1 comprises heating chopped cannabis (2 3 mm) at 100 150° C. for sufficient time to allow decarboxylation; step 2 comprises CO2 extraction using: a) a coarse powder(the particles are passed through a 3 mm mesh); b) a packing density of 0.3; and c) supercritical conditions of 600 bar at 35° C. for 4 hours, although other combinations of temp and pressure ranging from 10 35° C. and 60 600 bar (bothsuper critical and sub critical conditions) could, it is acknowledged, be used; and step 3 comprises conducting an ethanolic precipitation at -20° C. for 24 hours and removing the waxy material by filtration.

The supercritical method disclosed in PCT/GB02/00620 produced: a) a high THC extract containing: 60% THC (Δ9-tetrahydrocannabinol) 1 2% CBD (cannabidiol) 4 5% other minor cannabinoids including CBN (cannabinol) (Quantative yields were9% wt/wt based on dry weight of medicinal cannabis); and b) a high CBD extract containing: 60% CBD 4% THC 2% other cannabinoids (Quantative yields were 9% wt/wt based on dry weight of medicinal cannabis).

Clearly as the resulting BDS is to be used in a pharmaceutical product it is essential that the process is safe, scalable to GMP and gives high degrees of product consistency and, preferably also good yields.

The principles of supercritical fluid extraction (SFE) have been known since the work of Baron Cagniard de le Tour in 1822 when it was noted that the gas-liquid boundary disappeared when the temperature of certain materials was increased byheating them in a closed glass container. From this early work the critical point of a substance was first discovered. The critical point is the temperature above which a substance can co-exist in gas, liquid and solid phases. It was later found thatby taking substances to or above their critical temperature and pressure they could be used as sophisticated solvents for extraction and fractionation of complex mixtures.
 

clide

Member
People have been talking about supercritical fluid extraction of essential oils of cannabis online since OG's dawn and before I imagine. I can only personally attest to the talk at OG but perhaps others remember when butane extraction was referred to as supercritical fluid extraction. The Lycaeum and its ilk may have been responsible; I believe supercritical fluid extraction was the name given to the first successful butane extraction of DMT performed at the DMT Vaults in the fall of 1998.

What I have yet to see is anyone posting the results of a true supercritical extraction. To claim that there's no reason to pursue this as the above poster does is willful ignorance. There's no point in informing someone as to why CO2 and organic solvents might be slightly different to inhale at high temperatures should complete evaporation of solvent prove impractical if the person clearly thinks that CO2 and all organic solvents on that list are equally kosher to put in your resin.

Alright look at the last section of the last link posted at the top here. Because it is extremely awesome and will blow everyone's mind I will post a portion here below.



Looks like Eden Labs is violating INDRA's patent huh.

i can attest to this! the flame wars were massive, if we dont respect this they would have been flamed for nothing!

but seriously, there are people still looking into this, im sure foaf will be the first one to figure out how to do it on your own if it ever becomes possible. to be honest it would be thousands of dollars for each unit regardless of where you get it, is anyone wiling to invest 10K+? doubt it. if you are, buy a commercial unit! jeez, sometimes it dangerous as fuck to do somethings and sometimes regular laypeople shouldnt have access to dangerous as fuck things. im not talking like chainsaw or table saw or like hunting rifle. i mean more like a grenade which you cant find the pin to, and when you do, you find that it wont fit, so you have custom mill a new one, also the grenade is balancing on a pin in a vacuum sealed dome surrounded by landmines.

sooooo......be grateful your mind/body can grasp the butane process and complete that without(hopefully) blowing yourself up, some of you have stories im sure, i know i do. why cant people just be happy with what they have?
 

3dDream

Matter that Appreciates Matter
Veteran
Sundance - my understanding is that distillation is not the right thing for weed. The steam is too hot and will ruin the product.
 

clide

Member
More than that, I'm grateful you've taken the time to inform me of the error of my ways and to remind me to be grateful that my feeble mind can understand current methods. Now I can stop trying to improve my product and can rest assured that things are as good as they're going to get.

your very very welcome, someone has to inform you of your limits!

listen to HMK, he knows what hes talking about.

if youd spend thousands on a home extractor try one of these extractors,
http://tamisiumextractors.com/

they wont kill you as easily.

if you just want to be the first kid on the block to have co2 extraction, you should squash that.

if you havent witnessed a flame war over something as silly as super critical extraction then your lucky. there is already consensus on this topic, there has been for years, even bubbleman was in on some of those threads back in the OG days.
 

3dDream

Matter that Appreciates Matter
Veteran
clide - it's been a few years has it not? Maybe we can re-evaluate SFE. I wasn't around for the board that no longer exists.
 

Shcrews

DO WHO YOU BE
Veteran
It's a good thing you don't want to start a flame war over anything silly. You're a fucking bitch, I bet your oil gets about as hard as your dick.

i tink he's right, your wasting your time....

BHO has tested at 98-99% THC according to Cannabis Culture and PAul Hornby, so why not just fucx with that and leave the co2 for the plants to breathe
 

flubnutz

stoned agin ...
Veteran
4500 psi man thats like workin with a bomb. just the safety shielding and locks and stuff would cost a mint.
 

3dDream

Matter that Appreciates Matter
Veteran
Found this. Even though it is for catnip, I think it is interesting to hear what the steps are w/ a commercial device.

Oil of catnip was extracted via the supercritical fluid carbon dioxide in an
SFT1000 Supercritical Fluid Processing Unit (SFPU). The dried catnip (consisting of
Page 4 leaves, stems, and buds) was crushed and 17.533g were packed into a 50mL stainless steel vessel. After securing the vessel into place, the SFPU was set to the appropriate conditions. The conditions were checked using the “system status” function, and conditions were altered using the “rest parameter editor” function. The initial
temperature for the SFE/SFR was set to 40°C while the initial pressure setpoint was
2000 psi. During this time, the vessel filled with liquid carbon dioxide. The pressure was
raised in increments of 2000 psi by use of a pneumatic pump until the desired pressure
of 6000 psi was obtained. The SFPU operated in the static mode for 30 minutes
allowing the carbon dioxide time to soak through the catnip. After this time, the unit was
set to dynamic mode for 7 minutes, and the restrictor valve was opened manually 13 full
turns (completely opened is 17 turns) in the counter clockwise direction. It was
important to monitor the restrictor valve temperature at this time using the “system
status” function. If the temperature, set to approximately 60°C, fell below 5°C, the
restrictor valve had to be turned in the clockwise direction to maintain the temperature
above the freezing point. During this time, supercritical carbon dioxide extracted the oil
from the sample and carried it to the collection jar. After the completion of the 7
minutes, the pressure setpoint was reset to zero using the “rest parameter editor.” (The
mode was still dynamic). The restrictor valve was turned in the counter clockwise
direction allowing a rapid fall in pressure. When the pressure fell below 1200 psi, the
“open depressurization valve” function was selected to provide the final rapid
depressurization.
 

SuperConductor

Active member
Veteran
You can also check out the patent for Sativex http://www.patentstorm.us/patents/7344736/fulltext.html which is a sophisticated professinal supercritical co2 cannabis extraction for the pharmaceutical industry, it also describes a decarboxylation process but don't think it says what temp or how long for, it's pretty vague to my eyes actually but it's there. Bet they're equipment is home made.
 

clide

Member
there is a difference between muddling your way through something and knowing what your doing, its having a degree to prove it that keeps your digits and appendages attached.
 

SuperConductor

Active member
Veteran
Where's your sense of humour clide? Would they be able to sell these machines to the general public if they were as dangerous as you say? Why should a man who smokes as much bho as I presume Mr White does not be able to explore better and possibly cheaper in the long run alternatives. In fact why is he not even allowed to talk about it?
 

foaf

Well-known member
Veteran
Its all fun stoner McGuiver type talk, but without some clear benefit you arent gonna get someone like me, who has the money and the skills (chemistry degree, welding equipment, and balls to do it) , to do it.

So what's the potential benefit? It is obviously more dangerous by virtue of the pressure, more expensive, and technically more demanding. If it provided some benefit, then Im all for it, but I havent heard of one valid known benefit. I'm not afraid of complicated, expensive, or dangerous. Look at the complicated goofy ass contraptions I've built to improve my hash/pot smoking life so far.

98%, not likely in most cases and even if it was, I dont know that that is "good", shit, the dark "weak" oil I sometimes make from a longer steep or second run is still too strong for me to smoke much of. and you can change the characteristics by using other solvents and varying steep times. cheaper? no way. easier, no way. larger amounts, not likely, pressure vessels get much more expensive as they get larger.

Low pressure room temperature solvent extractions are generally safe, inexpensive, quick, and make a product that I can't imagine improving on much, at least not taste wise or potency wise.

Its an interesting discussion, but from a reality standpoint, it aint happenin round here any time soon, and with good reason.
 
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