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Affordable DIY CO2 Extraction???

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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I don't know about ya'll, but I have been watching CO2 Super Critical Fluid (SFE) with interest and have wanted to sample some cannabis essential oils extracted by that method, but the cost of conventional SFE equipment, is outside the range of most of our finances.

For the rest of ya'll just learning of the process, let's quickly examine what SFE is, by looking at what Wikipedia has to say about it, followed by us'n kicking off a project to develop a small affordable DIY CO2 extractor, that more of us can afford and build:

Supercritical carbon dioxide


From Wikipedia, the free encyclopedia



Carbon dioxide pressure-temperature phase diagram
Supercritical carbon dioxideis a fluid state of carbon dioxide where it is held at or above its critical temperature and critical pressure.
Carbon dioxide usually behaves as a gas in air at standard temperature and pressure (STP), or as a solid called dry ice when frozen. If the temperature and pressure are both increased from STP to be at or above the critical point for carbon dioxide, it can adopt properties midway between a gas and a liquid. More specifically, it behaves as a supercritical fluid above its critical temperature (31.1 °C) and critical pressure (72.9 atm/7.39 MPa), expanding to fill its container like a gas but with a density like that of a liquid.
Supercritical CO2 is becoming an important commercial and industrial solvent due to its role in chemical extraction in addition to its low toxicity and environmental impact. The relatively low temperature of the process and the stability of CO2 also allows most compounds to be extracted with little damage or denaturing. In addition, the solubility of many extracted compounds in CO2 vary with pressure,[1]permitting selective extractions.
Soooo, in us'n layman's terms, we use plain old CO2, that we have gotten hotter than 31.1C/87.98F, while under at least 1086 pounds per square inch pressure.

In that state, the CO2 becomes a super solvent, which has higher penetration power, and can be fine tuned to focus in on specific constitutes, by varying the pressure, temperature, and by the use of co-solvents like ethanol or hexane.

Fair enough, and easy enough to accomplish several ways that immediately come to mind and ah'm hoping some of ya'll experienced SFE brothers and sisters will jump in as this project progresses, and add your two cents!

Traditionally a high pressure intensifier pump is used to achieve the required pressures. They use two different sized pistons on opposite ends of the same shaft. If they put hydraulic pressure on the larger piston, the force it generates is applied against a much smaller piston area on the other end. The difference in surface area's of the two pistons is how much more pressure the smaller piston will generate. It there is 60 times less area, it will produce 60 times more pressure.

Cryo-pumping also works. You start with liquid CO2 or dry ice and heat it in an enclosed space. Gas expansion takes care of all the rest!

My first conceptual of a system that was semi affordable, was a simple minded system using liquid CO2 and heat to run it at about 1500 PSI. That eliminated the pumps normally used and by using a liquid Dewar with a dip tube, with both a gas head and a liquid tap, the need for any liquid pumps is eliminated as well.

It is designed to use readily available Schedule 160 austenitic stainless pipe and its largest component is small enough to fit in my 7" X 36" lathe. My original plan was to use an existing hydraulic cylinder for my vessel, but alas, carbon steel embrittles excessively at cryogenic temperatures.

My design calls for achieving pressure by simply heating the pipe with available pipe band heaters.

Pressure was controlled using a conventional, though expensive back pressure regulator. Please note the attached conceptual, which reflects my thinking four to five years ago:

I put the project on the back burner after reading the SFE CO2 patents for extracting cannabis, and noting that CO2 isn't a very aggressive solvent and the patented processes used significant fluid exchange rates, as well as relatively long spans of time.

To compound that, reports from those testing SFE CO2 extractions reported poor taste and effects, so I put CO2 extraction on the back burner to just watch for awhile.

Within the last couple of years several folks have done some interesting work starting with dry ice. The first that I noted was able to maintain high enough pressure in a test tube to keep dry ice from sublimating as it warmed, so as to extract some Limonene from an orange peel.

That led me to question whether super critical pressures were required to extract the essential oils from cannabis that we typically extract with other solvents, and further experiments by others on this forum and others, suggests that it is not. Some even report better results at subcritical pressures, especially with the use of co-solvents.

Sub critical extraction presents an interesting twist from a simplicity standpoint, so of course my simple mind immediately envisioned replacing the test tube with a pressure vessel containing dry ice in the bottom, and a basket of material suspended above it. Screw down lid and bring it up to temperature with a pipe clamp heater for pressure.

Flooding is achieved by simply turning it upside down to soak the material and right side up to drain. That step could be repeated back and forth, to soak the material and keep the boundary layers diminished. On setting it upright the final time, we could bleed off the liquid into an expansion chamber and then to atmosphere, leaving behind the oil.

I have decided to build a 2″ X 24″ prototype, and have acquired two resources on this project that emboldens me. One is the offer from a dear old friend, to allow me the use of his pressure and vacuum equipment manufacturing facilities for giggles and old times sake.
The other is an serendipitous agreement with another old friend, who owns a cryogenic equipment manufacturing plant back east and is familiar with SFE.

We have a mutual engineering support agreement in effect, in exchange for my support on one of their projects with a former aerospace customer of mine, who is now their customer as well.
For my support interfacing their equipment with my customer's equipment of my own design and manufacture before retirement, they will support me in developing a simple minded DIY SFE system, that hopefully more of us’ns can afford to build, or have built.
So here is my first simple minded conceptual using liquid and my latest starting with dry ice, but you will have to watch this space for the latest using dry ice.

After promising someone that I would publish yesterday, and after working all day on the drawing, my 2002 32 bit Auto Cad program in XP Pro virtual mode, is not able to access my printer on my 64 bit processor, and I’m not smart enough to figure it out.

I will add that drawing after I find a computer hero or heroine, but the way my conceptual works, is the bottom of the Schedule 160 316L pipe cylinder is filled with dry ice , on top of which sits a wire basket of plant material. Clamp on band heaters turn the dry ice to liquid, which is circulated and soaked through the material by simply turning the cylinder upside down.

After flipping it about a few times, over an extended soak, the vessel is set upright and attached to the lower expansion chamber via a hydraulic quick disconnect. The liquid is bled off, decompressed, and the oil collected from the decompression vessel via the bottom drain valve, as well as via the detachable bottom.

This was written especially for ICMag from data taken from:
http://skunkpharmresearch.com/affordable-diy-co2-extraction/
 

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prune

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I have no doubts on your ability to design and build either of these devices, my only question is how you will define affordable! lol
 

hammalamma

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You must spread rep before giving to gray wolf again....
Sick! Finally some real talk about c02 extraction, not just "somebody gave me this c02 wax" or "he took my trim and came back with c02 hash". Can't wait to see what you can do GW!
 

knowhere

Member
From what I was reading on edenlabs and several other websiites related to co2 extraction subscritcal co2 might be far better suited for our purposes, I would think using schedule 180 SS 304 NPT pipe fittings to make a simple blow through unit would be the best place to start with this? 2x 1500wp valves maybe a heater cable with temperature controller,

just make sure not to use high carbon steel as it becomes brittle at low temps generated by the liquid co2 and tends to explode with deadly splinters at cryogenic temps under lower pressure then the pipe / vessel is rated for. Heaters, valves and compressors to recirculate the co2 and recover it is where the system would start to cost much much more. a simple blow through system should only cost a few hundred at most to get up and testing with?

I think I saw some of the same videos and read peoples blogs on the subject as you, I saw another where a guy was extracting caffeine from coffie beans, the extract was black, the coffee beans looked bleached, I would think we would pick up allot of stuff we don't want using super critical co2 and possibly even sub-critical co2. he had to soak the coffee beans in water first for it to work I recall..

he basically had a 8 inch long 2" ID pipe nipple and two end caps with teflon tape, one of the end caps had a T on it with a pressure gauge and a 1500 psi valve, he would put the coffie beens down onto a screen that was set in place at one end of the pipe nipple before the screw on cap, on top of the beans he put in some chunks of dry ice, and screwed the other cap with the pressure gauge and valve ( in open position) onto the top, wrapped some heat cable around it, closed the valve and heated it up while watching the pressure gauge, I believe he let temps / pressure drop some before he slowly opened the valve releasing pressure, After he unloaded the unit under the screen in the bottom end cap there was black sludge, this he had to purify with other methods to get powdered caffeine. I believe he used a vice and large pipe wrench for each loading / unloading.

either way, I eagerly look forward to watching you bring forth this new system and wish you the best of luck with your en-devours :)
 
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paladin420

FACILITATOR
Veteran
I have had no need to 'watch' CO2 SFE. I just watch out for gray wolf.

sir on another note? I spotted an electric pressure cooker in walmart,and it looked very adaptable to your work reclaiming solvents..picture is on cell and am too much of a dork to upload it
 

foaf

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I've never tasted any. Good luck on building a prototype.


pressure cookers generally have silicone gaskets, and they deform with butane. and they are designed to work at pretty low pressures, like 1.5 atmospheres. I used a pressure cooker in my first designs and it was a fail because of the gasket material, and it wouldn't have been safe.
 

Rickys bong

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After re-reading one of GW pharma's patents they state a clear improvement with using sub-critical CO2 over supercritical.

Which makes me wonder if the reason why the few examples we've seen of supercritical extracts come out so reddish and have had such poor reviews.
It would seem Supercritical extraction pulls EVERYTHING out of the plant, and many of these compounds are undesirable. Innnnteresting.

They also state using 2% ethanol in a supercitical extraction improves yield but I didn't see anything about using co-solvents in liquid CO2 extractions. (this is from US7344736) Patents are frequently written to confuse competitors so who knows.

Back to liquid CO2 however, the mass flow they used was huge. 1250kg/hr for 60kg of plant material, over 10 hours. eek!

The pressure required for subcritical extraction is still way up there though, and to get a decent safety factor you'll still need to design for way over 1500psi.

I can't see liquid CO2 as being practical but I'm very interested to see some un-biased results as to whether it will work with a flow through system and if co-solvent will help. I wouldn't rule out using alloy steel since you presumably won't be using cryogenic temperatures and a chunk of seamless tube is going to be a lot cheaper in steel. Obviously ss is preferred but I wouldn't rule it out for experimental use...
What about a simpler test setup. Make a column with a valve at both ends and fill it with plant material. Get a small 2.5lb or 5lb. bottle of CO2 and connect it to one end of the column. The heater really isn't needed for sub-critical use.
If you kept the bottle valve and connecting column valve open you could flip it back and forth for soaking. Obviously liquid expansion needs to be considered but if the column is not closed off the bottle headspace takes care of that. I suppose you could dump the liquid co2 into another tank or just vent it onto a plate and see what comes out...

Awesome project dude, look forward to seeing results. A really awesome thing would be if you could do a hplc comparison test of say... ISO vs Butane vs liquid CO2 for the same plant material.

Peace RB
 

Gray Wolf

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Back to liquid CO2 however, the mass flow they used was huge. 1250kg/hr for 60kg of plant material, over 10 hours. eek!

Yeah, that!!!

The pressure required for subcritical extraction is still way up there though, and to get a decent safety factor you'll still need to design for way over 1500psi.

Good point for trying it at home! The maximum recommended operating pressure of 2" Schedule 160 is 1840 psi, and its rated burst is 14,681 psi. Since CO2 becomes super critical at around 1086 psi, there is clearly not much room to operate at super critical pressures, without using the safety factor.

If we wanted higher SFE pressures, we could just gun drill large diameter round stock, and be capable of what ever pressure we wanted.

A really awesome thing would be if you could do a hplc comparison test of say... ISO vs Butane vs liquid CO2 for the same plant material.

Peace RB

My thoughts too! Closing in on finishing the new lab and will hopefully soon at least be able to do GC.

Mostly I'm hoping to find a safe cheap simple low volume home process for maw and pa. Right now it is a spendy way to extract, even if it was ambrosia from the Gods.

Maw and pa usually have more time than money, so extended soaks are less of an issue, making cost, yield and quality the tipping points.

I am confident I can get what ever temperature and pressures I need, but am not willing to bet the farm until I see some results justifying the expense and effort.
 

mendo420

Active member
Veteran
I bought some Blue Dream Full Melt. They said it was CO2 extracted. 50 a gram.
It was light yellow with a honey comb structure.
I think it was vac purged BHO.
It was tasty, smooth and liquified instantly with flame.
Wish I had a pic

Grey You F'n Rock!!
 

Gray Wolf

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I have no doubts on your ability to design and build either of these devices, my only question is how you will define affordable! lol

Good point, a relative term! My goal is under $500, so Ma and pa may have to share it with a circle of friends.

We'll see, because I certainly under estimated what machine shops are charging these days when I designed the different butane recovery systems, but this is even simpler.

My prototype may be more spendy even with me building it, because I have to buy, borrow, or build a back pressure regulator for R&D purposes.
 

Gray Wolf

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Well thank the Great Spirit for ex-brother in laws, who can sort out computer problems, so that I can print from virtual mode. Hee, hee, hee, kept him at tossed the sister..........

Here is my simple minded conceptual of how such a dry ice system might work. More detail prints once I have exercised some resources.

After further discussion with another experimenter, I have decided to build the system to operate at 5000 psi and below. Instead of using schedule 160 stainless pipe, I will gun grill a billet of stainless, but will keep the bore at one inch.
 

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Gray Wolf

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How did the turn out, GW?

It hasn't yet, because of the flood of information that came in once I announced my intention, and it has caused me to rethink my design.

My goal is not to just do a SCFE CO2 extraction, but to have the control to produce a product that is competitive with BHO, QWET, or QWISO in flavor and effect, and preferably better, so as to justify the added trouble and expense.

I am now considering two pressure vessels, one smaller one with the material in it, and a larger one to build up the pressure in.

Building up the pressure in the same vessel that the material is in, will ostensibly start extraction in the subcritical stage and extract throughout the pressure/temperature curve, until it reaches the ultimate high set points. That seemingly negates the principle advantage of SCFE, which is highly selective extraction, by close control of the parameters.

I am also getting some good feedback on the use of co-solvents, which help in that selectivity.

I'm headed back to the drawing board and will then present my conceptual to a peer in the cryogenic equipment industry for review and comment. More after that:

Here are some pictures shared with me, of CO2 SCFE extraction using commercial equipment, where they were able to control the parameters. No credits, as they are anonomous:
 

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vertigo0007

Member
Well what do you know? I had a guy show me a quick video of a unit he is involved with using. It was a video of that first picture spewinf the extract out the tube into a jar. Its being made on a machine that supposedly is in a state inspected lab. Any idea what type of lab would have this machine amd allow its use for cannabis? I was thinking a struggling 'micro-brew' coffee company, or maybe a flavor extract company. Its a yellow goo that seperates an orange red oil as it sits. It smells and tastes like raisins and tests at 50%ish. It smells like ethanol extract i tried once, but looks completely different. Oh and it sparks and pops like hell when you put a flame to it. Is that the carrier solvent they claim they dont use and the local lab claims its certified free of? Give the some truth Lord Wolf
 
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