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Supercritical CO2 for the Entheogenic Hobbyist Options
 
spaghettiman
#1 Posted : 4/16/2010 4:19:09 AM
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Is liquid CO2 a viable solvent for our favorite alkaloids?

for an initial mass extraction of something like phalaris followed by purification steps, A/Bs, distillation, column, whatever.

Any thoughts on this? Has anyone ever heard of this being done? Check this out:

http://en.wikipedia.org/...critical_carbon_dioxide

It seems to dissolve non polar things with ease, and ive heard its generally a good solvent
 

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Samadhi-Sukha-Upekkha
#2 Posted : 4/16/2010 5:01:18 AM
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Supercritical CO2 makes a great solvent, but it requires some pretty expensive equipment to use. It's likely infeasible for any single individual to find a way to do it -- but maybe I'm wrong!
 
amor_fati
#3 Posted : 4/16/2010 5:26:41 AM

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A video for extracting limonene from orange peels was posted here not too long ago, and the thought had crossed SWIM's mind. One thought that had occurred to him was to blend lime, water, orange peels and MHRB together, then to extract with SCCO2, leaving a small amount of saturated limonene to do whatever one would care to do with. One may be able to leave out the limonene altogether to achieve a product devoid of liquid solvent, but if that doesn't turn out to be a solid product or a crystallizable product of any kind, that may become mechanically difficult. Besides that, blending the basified material with orange peels may help to pretreat and prep the material to expedite the process by, as SWIM would guess, gathering the active oil droplets into a more voluminous network of limonene droplets.

SWIM would wonder whether the bit of water present in limtek procedures would lead to conversion into carbonic acid that would subsequently be neutralized by the lime, decreasing or even absorbing all of the SCCO2 before it percolates through. SWIM would guess not; however, for cactus extraction, perhaps the collection reservoir could contain water, potentially resulting in the production of mescaline carbonate.

The mechanics of such a process would also be a bit challenging, but perhaps they could be made to work the advantage of the process. SWIM wonders whether one could make a sort of solid-state aeropress? Take a vessel that can withstand a great deal of pressure, fill it partway with dry ice, fill the rest of the way with basified mixture, top it off with a cotton cloth filter, and seal it with lid (or somehow with a separate vessel) that will facilitate the collection of the solvent and precipitated freebase production when the pressure is released. Or a lid may not be necessary if orange peels are mixed in and the wet material provides a sturdy enough seal (with a screen to hold it and the filter in), then the vessel could simply be placed overtop a collection vessel.

 
amor_fati
#4 Posted : 4/16/2010 5:31:38 AM

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One way to do it may be to put a dish in the bottom of a pressure cooker, place a screen and cotton cloth overtop the dish (or bowl), pour the basified material on top of the cloth, add a layer of dry ice and seal.
 
amor_fati
#5 Posted : 4/16/2010 7:40:00 AM

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A pressure cooker isn't designed for the sort of pressure required, unfortunately, and it may be quite difficult to find a larger vessel that would.

Now SWIM's thinking something more along the lines of honeybee hash oil extraction.



SWIM's thinking small scale and a CO2 tank may be the safest route.



He's wondering at the possibility of preparing columns of dry basified plant material to prepare individual doses on the fly, possibly directly into a smoking device. He envisions great possibilities...
 
spaghettiman
#6 Posted : 4/16/2010 5:21:32 PM
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amor, hell yeah, exactly what ive been thinking.

This would be easy to do.... all you really need is a dispenser like that, some sort of modified brewing or paint ball tank. and do it like honey oil, they even say its used for that in wikipedia


for the pressure cooker, you can melt dry ice if you warm it in a container like that and let it pressurize itself to about 5atm.... sounds really damn dangerous. thats 73 psi.... If you could do it safely the dry ice melting route might be a good way.

what about butane? has anyone used butane on basified pulverized dried plant material of this sort? bad for the environment tho, CO2 is MUCH more benign, in terms of everything(planet and self).

I think this kinda thing might be a good route concerning phalaris. giant A/Bs are stupid...

either way, i think CO2 is VERY feasible, at worst your going to need to build a solid setup to do it, at least your going to need to find and/or modify a CO2 tank to give us liquid.
 
amor_fati
#7 Posted : 4/16/2010 6:59:03 PM

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spaghettiman wrote:
This would be easy to do.... all you really need is a dispenser like that, some sort of modified brewing or paint ball tank. and do it like honey oil, they even say its used for that in wikipedia


A little research into the matter has shown SWIM that this is most often a myth, but in the cases where it's not, it's not very commercially sensible.

Quote:
for the pressure cooker, you can melt dry ice if you warm it in a container like that and let it pressurize itself to about 5atm.... sounds really damn dangerous. thats 73 psi.... If you could do it safely the dry ice melting route might be a good way.


The critical pressure is 72.9 atm, though, and a pressure cooker isn't capable of this, as far as SWIM knows.


SWIM's thinking some modified paintball equipment, dry basified material packed into a tube with filters/screens on either end (acting as a syphon tube/herbal column), and the material-containing tube could be locked into a closed, pressurized system. The end opposite the tank could be outfitted with a valve and nozzle. The pressure would have to to released a couple times to get the SC-CO2 flowing into the tube. The extract could potentially be sprayed (with slow controlled pressure release) onto a dish, into a smoking device, or bubbled into an acidic solution to collect the product, which may be an oil in its freebase form though it might solidify rather quickly.
 
amor_fati
#8 Posted : 4/16/2010 9:16:46 PM

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The trick here would first be to design the experiment as feasibly as possible. No one wants to go out and buy a CO2 tank for experimental extraction process unless they may have other uses for it as well. CO2 tanks are commonly used in place of compressed air as a more efficient alternative, so SWIM wouldn't mind purchasing one for dusting, filling his bike tires, and possibly to use for power tools. As far as SWIM can tell, the siphon tube is the key to rendering SC-CO2 outside of the tank:



This wouldn't likely be something you'd want to use with your powertools, but having a larger tank on hand with a siphon tube would enable you to refill a smaller tank with an antisiphon tube or even make dry ice for whatever purpose:
http://www.practicalphysics.org...y/mov/making_dry_ice.mov

And this larger tank could also act as a SC-CO2 dispenser for extraction. One way of doing would be to take an empty CO2 tank, fill it with dry basified material, insert a siphon tube outfitted with a filter (not sure how feasible this is), fill it using another siphon tank, then expel the extract and collect. Another would be to simply stuff high pressure tubing with basified material and filters, seal it and lock it into the system, which sounds like the most realistic method to SWIM and would probably facilitate the rapid extraction of individual doses. A modified paintball tank would be cheaper route for accomplishing this, but it wouldn't be multi-purpose (unless you're into paintball).

edit:
A CO2 fire extinguisher may be another option, as they come ready equipped with a syphon tube. Here's a reference confirming the type of valve that can be outfitted to a fire extinguisher: http://www.nitrous.info/nitrous-historic/index.htm
More info here:
http://www.pyramydair.com/blog/...-bulk-fill-co2-guns.html
http://www.pyramydair.com/blog/...03/bulk-fill-part-2.html
 
amor_fati
#9 Posted : 4/19/2010 6:10:37 PM

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This thread is intended to compile and summarize the possibilities for the employment of super-critical carbon dioxide as a solvent for general extraction purposes. The potential advantage of using SC-CO2 is that it is nontoxic and evaporates cleanly and instantly under normal pressure. It was originally proposed on the forums as an eco-friendly means of extracting limonene: https://dmt-nexus.me/forum/defau...aspx?g=posts&t=10914


http://www.anoniem.org/?http://...PDF/chem122_Limonene.pdf

and was later proposed for the extraction of DMT: https://dmt-nexus.me/forum/defau...aspx?g=posts&t=11769

The difficulty presented is that SC-CO2 only exists under fairly extreme pressure that most common and household equipment simply is not capable of withstanding. While SC-CO2 is commonly used for the commercial extraction of essential oils, the equipment used to do so is well beyond the means of most hobbyists.

One way that SWIM has proposed to accomplish a fairly large scale extraction is by loading an empty CO2 tank with the material to be extracted from, inserting a filtered siphon tube of some sort, and simply performing a CO2 transfer between tanks:



The potential problems SWIM sees with this proposal is that dry ice may form if the tube is blocked or filtered in any way, thus plugging the tube and stopping the flow of SC-CO2, so this method may not be safe or viable--likely one would just end up with a broken siphon tube, though.


However, a much more safe and viable method would be to pack a tube with the material to be extracted, and lock it into a pressurized system with a CO2 tank containing a siphon tube--such as a CO2 fire extinguisher or a modified soda club (often used for paintball)--allow the tube to fill, then expel onto a dish or into a smoking device using a valve and nozzle.





With a system like this, the SC-CO2 would be forced to percolate through the material in the tube by the pressure of its release into the tube, and in theory, the pressure of being released from the tube would force out the extract.

While this may only be viable for extremely small-scale extractions (instant extraction of individual doses), it's possible that a longer tube could be packed and perhaps coiled to facilitate the extraction of larger amounts of material.

SWIM believes that the cheapest way to go about this would be to use a CO2 fire extinguisher in the manner documented here:
http://www.pyramydair.com/blog/...03/bulk-fill-part-2.html
http://www.pyramydair.com/blog/...-bulk-fill-co2-guns.html
Alternatively, practically any regular CO2 tank (with an antisiphon tube) could be turned upside down to expel liquid CO2.


The goal for DMT extraction would be to retrieved an instantly crystallized (or at least oily) freebase product, but if one were to extract from cactus, it may be possible to retrieve mescaline carbonate by bubbling through water. This may also work for other extractions, such as the extraction of harmaloids. SWIM's hope for this would be the development of a universal extraction rig using a nontoxic and efficient solvent.

While such a method may eliminate the need for limonene in extraction, most people consume oranges and have some use for limonene, so occasionally packing a tube with orange peels and extracting limonene with a CO2 tank would be a fairly practical habit to get into. Aside from that, there are plenty of other practical applications for having a larger CO2 tank, capable of filling smaller ones.
 
neuro_rocket
#10 Posted : 4/19/2010 10:03:00 PM

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Maybe the setup could be similar to a Butane Hash Oil extraction. Pack a PVC pipe with MHRB, put a screen on one end and pump CO2 through the other.
Could Butane also work to extract DMT?
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amor_fati
#11 Posted : 4/19/2010 10:53:07 PM

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SWIM was considering a very simple setup where the cone of a CO2 fire extinguisher is replaced with a setup similar to that, but wonders whether the CO2 would remain super-critical while passing through or just ice up. If the whole process were performed under pressure, rather than open, it may stand a better chance of working.
 
spaghettiman
#12 Posted : 4/20/2010 3:01:52 AM
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swim has been thinking about the viability of such extractions for bulk teks, namely phalaris

dry and powder, then maybe moisten and mix with base then dry, and do the extraction with CO2 or whatever.

then you would do an a/b and whatever work up, like a cake method.

This would surely work with butane, but it is terrible for the environment, and probably not suitable for the bulk of phalaris. It may be wise to base the material then dry it, but may not be necessary. MHRB to changa in one step....

Butane is great for this, but its sad for the environment. It is unfortunate there is no safe way to burn the butane off instead of just releasing it. This is much better for the atmosphere. hydrocarbons arn't supposed to be floating around like that.

for a single dose you may not need much butane tho. I wonder how good the yield would be. gotta do some testing...
 
amor_fati
#13 Posted : 4/20/2010 5:45:49 AM

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spaghettiman wrote:
swim has been thinking about the viability of such extractions for bulk teks, namely phalaris

dry and powder, then maybe moisten and mix with base then dry, and do the extraction with CO2 or whatever.


The problem is that the equipment necessary for bulk would be quite expensive and uncommon for home use, unless a makeshift method could be developed (like the dual tank idea mentioned in the OP). SWIM supposes that the bulk method he proposes wouldn't be too dangerous with the burst disc as a safety device; however, he can envision the possibility of a siphon tube getting clogged and costing a whole tank along with material to be extracted, as it may prove next to impossible to clear. It is hard to imagine any plant material being capable of clogging the path of that kind of pressure, though.

Small-scale extraction would be a quick and less costly way of determining the viability of such a process. At worst, one would burst a hose using the method SWIM recommends.
 
Adivino
#14 Posted : 5/4/2010 9:05:38 PM

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I'm aware of super-critical CO2 being used for the extraction of alkaloids at an industrial scale, caffeine in particular. This method is much cleaner than the previously used Dichloromethane and more environmentally friendly. However, I seriously doubt that someone will be able to perform a CO2 extraction at home. Please tell me if you succeed.

http://en.wikipedia.org/...critical_carbon_dioxide

One would have to take the CO2 to 72.9 atm and 31.1°C!
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director of sound
#15 Posted : 6/30/2010 1:39:12 PM

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you know i was looking into this too a while ago. paintball.... when its cold out you loose alot of pressure on your tank and if you invert it and fire liquid co2 comes out with your ball. why not throw a 20oz. co2 tank in the freezer for a while then attach a remote line to it and invert the tank while discharging through something like a butane honey oil extractor but larger and made of thick aluminum or stainless steel. the remote lines have a quick detach and a valve/regulator so you can slowly feed the cold liquid co2 into the extractor. maybe something like this with a screen and fritted glass disc for a filter in the discharge end.

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shoe
#16 Posted : 6/30/2010 5:10:52 PM

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SWIM Just gave away a CO2 canister unfortunately, but you can rent them for very little from BOC gasses.

If the supercritial CO2 idea comes to fruition, then all of the DMT will be extracted in a matter of moments, which would be quite impressive to say the least.
shoe

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amor_fati
#17 Posted : 11/17/2011 3:24:10 PM

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amor_fati
#18 Posted : 11/18/2011 4:18:38 PM

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from the caption:
Quote:
I built a pressure chamber from 2" pipe fittings and 1/8" brass valves to contain supercritical CO2 for drying applications. One project is to try aerogel production which generally requires that solvent be removed via supercritical drying. Normal evaporation would deform the aerogel structure as the surface tension of the solvent pulls the gel's structure tighter together and makes it dense. Since supercritical fluids have gaseous properties, they can diffuse out through the gel without affecting the structure the way that a liquid would


Also note what happens upon release: http://youtu.be/FZeaAnguXCs?t=2m51s


This could very well be a next-gen method for hobby extraction, as the fittings used are cheap enough and easy to come by and the CO2 tank and CO2 could a generally useful investment. The little porthole in this setup would also be a nice touch the purposes of extraction (I wonder what other steps could be taken to visually monitor the process). The only modification necessary for this would be a filtration device between the contents and valve--being pipe fittings, I'm sure there's plenty of options.

The only question remaining is retrieval. Judging from the portion of the video linked above, it could simply be done right into a dish, allowing the CO2 to evaporate instantly, leaving either a cold chunk or powder freebase behind, if DMT is being extracted. The other option is to connect a second chamber below so that CO2 may remain in liquid form as it enters a dish contained inside, then the pressure could be released from the top at a controlled rate, possibly forming crystal shards.

The other possibility would be to use the same process for mescaline extraction, but instead of retrieving freebase, one could bubble the CO2 through a small amount of water in a controlled pressure situation (within a second chamber), instantly producing mescaline carbonate, then retrieve in whatever way desired (I imagine a chamber like this would have plenty of options available to that end).


The followup demonstrates the intended use of producing silica aerogel, which just so happens to be a great porous insulation material withstanding heats comparable to ceramic fiber. This could mean that one could produce convection heating filter for any vaporizing apparatus.




As a sidenote, having CO2 handy would be great for flooding airtight containers for innate, long-term storage (to prevent oxidization).
 
amor_fati
#19 Posted : 11/24/2011 7:06:21 AM

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This will certainly deserve it's own thread but here's a bit more on aerogels:



note the insulative properties: http://youtu.be/kHnen2nSmDY?t=1m22s

...and what do we have here?



Some important info here, as well: http://www.aerogel.org/?p=16
 
ChickenTikka
#20 Posted : 12/27/2011 4:27:16 PM

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It was a while ago i wanted to post here but didn't have access, but if you watch that blokes videos (the one who makes silica gel) he has this chamber he made out of aluminum and acrylic that he puts dry ice into and seals with bolts, allowing the dry ice to melt will put it in a liquid state, he then heats it to make it super-critical. Much easier than messing about with fire extinguishers or co2 canisters, dry ice can be bought online and isn't too expensive. I'll have a look and see if i can find the video, the design he has would work if you add a valve or something to drain the co2, and maybe some metal screens/mesh to act as a filter. Problem with doing it this way, unless you have a cheap local source for dry ice you will be wanting to do bulk extractions to get your moneys worth.


http://www.youtube.com/w...creen&v=-gCTKteN5Y4

I suppose you'd just want to use fittings like he uses in his aerogel setup though, since this sort of thing would cost a fair bit to get made if you didn't have the equipment.
 
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