Custom supercritical CO2 chamber with easy-to-use lid clamp
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- เผยแพร่เมื่อ 29 ก.ย. 2013
- I built another supercritical CO2 chamber for extraction and drying. This time, I wanted a chamber that was easier to open and close, and could be expanded to larger volumes with the same closure system. The chamber is built from 2" OD .25" wall stainless steel, and I welded a plug into one end and a ring with O-ring gland onto the other.
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I think the technique is called "stitch welding." I made 6 tack welds, then welded between two of the tacks. Then I rotated the piece 180* and welded between those two tacks, then rotated the piece again, etc. This spreads the heat out in a way similar to tightening engine head bolts in a pattern. This was a pretty beefy weld that required a lot of filler metal (three passes), which probably caused the cupping.
Impressive and beautiful work as always. Nicely explained with that. Each of your video is a pleasure to watch. Thanks for sharing Ben !
That steel Split clamp is amaz balls. your a class A machinist for sure
Pure unadulturated genius!!!!
I would love to see you make an industrial size cylinder, about 3 in wide and 3 ft long, with gauge and input output ports.
the extraction would yeield more if the liquid phase is allowed to dwell near the extraction port, at the lowest portion of the vessel .. also: making the vessel work by gravity and super cooling your extraction vessel will trap more of your VOC's .
the super critical reaction only needs to happen for as long as it takes to strip the oils from the material . it would also help to have a strainer screen made to the standard of 70 micron filtration to hold your raw product near the filling port at the top of the tank . filtration in the process and longer offgassing times for the finished oils or caffeine can drastically reduce the moisture of the CO2 extraction process , and eliminate many of the compound destroying acids that can form with liquid CO2 exposure .
you sound like you know what you are talking about
Great job. I loved the video! I do similar things for a living but not at your level. You're very talented.
You never cease to amaze. In the next video, could you explain the flow-paths in the device, so we can better understand how the product actually makes it to the collection tube?
Your vids are always a hit with me and my friends.
Hi Ben,
You might want to try some difficult cleaning experiments. We did some development with supercritcal CO2 for cleaning stains out of cloth and clothing. If you search google patents for Liquid/supercritical carbon dioxide dry cleaning system it shows the schematic of our setup. Great video.
On your welding if you project the tube through your flange and do the weld on the ID you will get much less distortion on the flange.
Kind regards,
Tom Lipton
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What you've built resembles a Grayloc hub assembly which I've seen used in my line of work for flanges (Oilfield, 3,000 PSI+ working pressure service). You might look into them in the future, you can find flanges and clamps on ebay.
It's always the highlight of my day when he uploads a new video.
the clamp is indeed very neat!
great job on that clamp
I might be able to look up the ASTM or ASME codes on the pressure vessel you built. I am taking Mateials Engineering Technology in school and as I am learning more and more about metallurgy and NDT, the more and more I am interested in your videos and can understand what you are explaining. Thanks for the videos!
7 years ago, I watch your vid and I thought that might be handy one day, since that day 7 years later I need this DIY supercritical CO2 method for CBD extraction from Hemp/Cannabis$$$.
Just had an idea for a larger
Critical Chamber. Using a two small CO2 bottles cut the top off just after the curve (leave a small piece of the curve to catch the cover). Cut the top of the second bottle at the begining of the curve. The opening has to be slightly oval for the lid to fit inside the critical chamber, like some of the European pressure cookers, also many large vessel's use the for maintenance access covers.
It's easy to make a critical co2 extractor with out a pump, you just add the co2 to your vessel with your weed, then warm that chamber with a simple heating pad for your back until it becomes liquid at that super critical stage, then open the release valve and collect your extraction, and recapture and recompress the co2 if you set it up. No o rings, all metal check valves etc. That way you can use a scuba tank and collect much more per run.
Yes, stitch welding - the term eluded me - just like my welding skills - elusive!
The welds on my vacuum chamber are all internal, inert gas purged on 5mm thick pipe. The KF/NW flanges held up fairly well, with minimal/acceptable distortion on the mating face. I used the thicker pipe instead of thin walled tube to help absorb the heat from the welds, otherwise the mating flanges would have looked like bananas after welding! I agree with you - weld first & machine later (where possible)...
I absolutely love your videos. You have been pressure testing remotely up to your working pressures. I am curious why you don't hydrostatically bench test your rigs?
Thank you. Greetings from France !
If you make the main pipe longer, you will need to add belt bands to support the pipe and keep it from rupturing.
You have shown that the existing length will hold 4000 psi, so place the band spacing at the same length.
Walter White wouldn't had so many problems if a guy like you had shown up.
For the stresses in the pipe next to the weld, you could probably anneal it the whole thing, or use a band heater just to heat the pipe if you don't want to treat the seal.
Extract the gingerol compounds from ginger. I saw a GC/MS report of 1-1.5% by mass of the gingerols via CO2. I'm also curious what an ethanol co-solvent will do.
Wow...you are awesome. Bravo!
if you have an input for high pressure co2 then you should be able to implement recirculatation of that dry ice co2. Just realized its 8 years old but still lovely work
I hate when explosive decompression destroys my o-rings, but taco night is so worth it.
It's interesting hearing you talking about pressure testing. I was wondering how I could do this safely if I ever did anything like this. My idea was to fill the whole thing with brake fluid and connect to a brake master cylinder, then put the pressure vessel in a dustbin full of water. It's easy to get 1000s of psi with automotive hydraulic brakes and because everything is filled with relatively incompressible liquid, if it does fail then there's not that much energy stored in it.
really cool dude!
I have MS and use CO2 extracted cannabis for spasms. Would be interesting to see how it is done. Not sure if you are in a state where you can do that though.
Very innovative, DYI is a special talent now days, may i ask would you be able to use this for MEDICAL cannabis extraction at home?
Bro it needs a ball valve on the bottom with a high pressure pump on the inlet and a vac chamber to pull into on the outlet side... 2 pumps and you got it
In all of the very low pressure CVD and MBE chambers at my lab (some of which are cylindrical and some of which are spherical and operate on the order of 10^-9 torr), we use copper gaskets to seal the vessels. Have you thought about using copper gaskets to seal the high pressure chamber instead of silicone?
I want to see what you wrote on your blogs... Im thinking about making hops oil extracts.... did you try it?
So, if you place the dry ice with the coffee grinds in the vessel and close it, the pressure inside it exceeds 2kpsi as the dry ice goes from solid-liquid-gas & as it's doing so, it extracts the soul n all the glory out of the grinds... How do you get it out w/o it soaking back into the grinds (being that the pressure is so high in the chamber)? Man your skills are rather impressive. Thank 4 the videos!
Hi, by any chance, do you have instructions or the specification on how to build del Supercritical extraction chamber?
This chamber is much larger than 50mL, and the size is required to get a usable amount of product. Do you have a source of 50mL tubes (or any tubes) that can actually hold 200 atm?
Why not put the bevels on the lid and chamber instead of the clamp?
Easy to do on a lathe.
The work is awesome, but, would not have been easier to machine the clamp´s internal groove in the late?
When you need to fill the critical chamber, place the critical chamber in a deep vacuums, invert the CO2 canister so liquid only comes out. Open the schrader valve to the critical chamber and weigh out the CO2 from the CO2 canister.
I believe you could do it with a quartz window as typically done with high pressure reaction vessels when you need to see inside.
Surplus oxygen and scuba tanks and fittings are rated for 3000 psi, CO2 reaches supercritical liquid state around 110 degrees F at 1,600 psi or so one could make many methods using cheap surplus materials.
Hi I was wondering if perhaps I can run a few things by you pertaining a SCCO2 machine I designed. I am having a few technical issues, and wanted to know if you had any information on condensing and recirculating the exhausted gas.
Home made Tri-Clover clamp nice!
You can use water and a grease fitting. Fill the chamber with water and put a lid on it with a standard grease zerk. A typical grease gun can produce 10kpsi.
Have you considered making a clamping style flange end to connect to a pre-manufactured steel pipe vessel as you've used in the past? It seems like that would allow you to change the size of your vessel easily while maintaining the easy opening/closing of the clamping end.
Hi, I was wondering if this would be something I could DIY? And how would a DIY(done properly) compare to an expensive one, like for example eden labs?
have you considered compressing the dry ice into slugs? or what if you put 2 valves on the chamber, one on top one on bottom then you fill the chamber full of"extraction medium" and simpley inject liquid co2 using a SIPHON CO2 tank used for arrow soft guns
Extract Angelica archangelica (Umbelliferae) it contains a perfume and some medical compounds. As always very interesting video.
Would your acrylic design work with glass lining the inside to avoid the CO2 penetrating the acrylic? It was cool to see what was going on...
I know this video is really old but, for future viewers, the other thing you could have done regarding the weld, is assemble the cap/clamp and weld with that all on
Or just make the cap/clamp with pipe thread. It would attach just like his original threaded cap via teflon tape and a pipe wrench, but the clamp would be available for everyday use. The threads would only be used at initial setup, or if you wanted to upgrade to a larger or smaller extraction chamber like he seemed to immediately want to do.
Zoinks, what a conversation starter. The Holy Grail of medicinal whole plant extraction. Personally having spent the time, money, and bulk vegetable matter needed to explore most "medicinal herb" extraction methods I have come to realize that simple, clean kif is hard to beat in todays world of 'Dabs" of unknown origin. I know mine(dabbage) is free of mercaptan,"upper cylinder lube", residual solvents, spider mite gut juice, sweat, hand oils, etc. I can't really tell other than taste and a 10 power loupe, what, if any crap is in the concentrates available in California pot co-op's today. I'm glad to see a trend among like minded people toward superfluid extractions using co2. Yield with traditional solvent methods ranges from shitty to barely tolerable. I was shocked the first time I used dry ice in my 80 micron shaker rig instead of dry shaking. The dry shake yielded about 8-10% by wt. vs. 21% with dry ice crushed in the plant material (which tested at 22% at my local testing lab). Naturally I'm dying to build an extraction vessel for CO2 now. The vid helps a lot but I'm blown away with the helpful, intelligent comments on this post. I subscribed yesterday, thanks.
I assume you tig welded it? Stainless is difficult when it comes to heat but there are some tricks that work. When you put a tack down, give it about 5 seconds of argon afterwards, then give it a 5 to 10 second blast with compressed air, the change in temperature should be enough to flex it back in to place, a second man comes in handy here. A colleague of mine who does alot of flanges puts ice cubes on flange when welding, didn't try this myself be he says it works great? Good video!
extract the soul of a ginger
Blood from a turnip
maybe you should do a project on hydrotesting, since it looks like you would be testing many more DIY high pressure chambers in the future. it's definitely safer than putting a heater to CO2 filled steel pipe!
When Ben was talking about the difficulties machining the inside surfaces of the clamp, was I the only one involuntarily yelling "lathe!" At the screen?
Rob Mckennie I did too. Machine ur grooves before splitting it.
what about foam made with sCO2 and recycled PET?, I want to make a small sheet foam extruder with this system
how does this device extract without a siphon ? or does it have one and im not seeing it
slop == margin ;)
Would a small high pressure gas bottle work as the pressure vessel?
use a cooper gasket to deal a flat surface, cooper will cold flow slightly to seal the end
yay new vid from ben
your the man
The length of the chamber if you choose to make a longer one, will be a weakness, I don't remember about how much of a weakness though so test it thoroughly, also if it should fail at longer lengths, you could probably cure that by using some kind of clamps at the distance of the current chamber or using extra material welded on at that distance and maybe something welded through the chamber, keeping it from expanding on the inside.
Thank you for the real science .How did you calculate the the pressure rating for the cylinder
bgianzin10 My blog shows the calculations for a smaller, but still cylindrical chamber. The biggest unknown are the welds. The metal itself will be weaker in the heat affected zone of the weld, but the weld bead should be larger in cross section to compensate.
Tank you very much again.You sum up very much knowledge in a few minutes of video that is awesome.
+Applied Science Industry rule of thumb is ~50% reduction in the heat affected zone with no additional heat treatment for a weld. Thank you for these videos, always enjoyable to watch.
Hi! Defining weldings is not an easy task in the proffesional field anyway. I'd reccommend you to weld a couple of collars on the tube if you make it longer and to mind the fatigue of the material if neccesary. Hope the typos are not so many :P
The brass fittings become grenades at these pressures and temperatures.. Be safe sir.
the little fleck of debris on the interface next to the O-ring gland made me OCD for a bit there.
He used a very thick acrylic window, did not seem to flex. The only problem was the CO2 seeping into it to cloud it. But a bit of flex would break the glass.
Is it possible to so the extraction in a single chamber rather than adjusting co2 than running it into a second chamber?
any chance i could hire you to build one for me? i have a few changes i could suggest as well
Why not machine your coupling flange with the inside tapped and then thread the tube and screw it on instead of welding?
That way you could experiment with different flange designs or switch to a longer tube if desired and you wouldn't have to worry about heat damage to the flange and tube.
And no loss of strength or warping from the heat of welding.
I had exactly the same problem when welding stainless steel KF/NW fittings to stainless steel pipe - the mating flange warps due to the heat from the weld. Did you weld it quickly, or did you do small passes and allow it to cool between passes?
This seems ideal for some culinary applications I've been wanting to play around with. Does anyone know of a commercial option that doesn't involve the machining?
This is basically a High pressure reaction vessel.they are expensive
Sooo rad, that CNC porn got me going. Subbed!
Id like to see ( be educated about) the mechanical interface that actually picks up the oils as the CO2 extracts them. I see a tube closed at one end with a fitting on the other but no dip tube no way to gather up the extracted material. How does it make to from the CO2 as it reverts to a gas into that little poly tube?
once the co2 has evaporated, it leaves the material at the bottom of the chamber. then you just tilt it upside down to empty out the spent trimmings and scrape the thc gunk off the bottom.
Can't stainless steel be welded under water? I think I saw something about stainless steel dishwasher tubs being welded that way to reduce warpage.
Hi,
I admire your manufacturing capabilities. The vacuum pump fittings you referred to are called "Sanitary Tri-Clamp" and they are widely used in food, drug and brewing environments in sizes up to 6" in diameter. I found a nice reference guide to the types & sizes of clamps & gaskets available on gvc.net. I have a Flash Chromatography system that uses billet aluminum tubes and stainless tri-clamp ends that it useful for ethanol & butane solvent extractions, but would prefer using CO2; do you think a 1/4" thick x 4.5" ID billet aluminum tube would stand up to 3,000 PSI?
I look forward to watching your subsequent videos.
Some nice eucalyptus extract could be nice
Aren't copper gaskets sometimes used instead of soft O-rings in high pressure seals?
On a different subject: there are plenty of videos where people use a Soxhlet extractor to get a slurry of oils and capsaicin from chili peppers. But there's one method I've never seen: Ultrasound augmented supercritical CO2 extraction. One author claims that using ultrasound in combination with supercritical CO2 increased yield by 77% when extracting capsaicin from chili peppers compared to supercritical CO2 alone.
Hi there, fascinating experiment! Have you further explored this since the video posting years ago? Am very interested in hiring you to custom build a unit for me. Please let me know.if this is a possibility. Thanks - Mick
can you show us co2 stain removing?
I bet you could have made that angular face really easily on a lathe.
You clamp it in the "closed" position, and use a boring bar and the compound slide.
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"This can happen".
This being your head if you open the visor in your space suit in space.
I have often wondered about pressure tests like the one you did. You ran it to 4000PSI once. But is that a "semi destructive" test? Do such tests weaken the container? Or does your test mean that you can run the pressure up to 4000PSI as often as you want and for as long as you want?
Perfect materials can be stressed within their elastic limit an infinite number of times and show no damage. In the real world, many materials will degrade a small amount with each loading/unloading cycle -- this is known as fatigue. The material's properties, shape, and loading severity will determine how much the material degrades, and failure due to fatigue can be estimated via statistical methods. Airplane fuselages have a rated number of flight cycles after which the aluminum body is in danger of failing due to fatigue (many 10's of thousands). This is partially why old planes are decommissioned even though they are still functional. In the case of the pressure vessel, one rather high loading cycle will not reduce the fatigue life by any noticeable amount. High pressure cylinders for welding gas are tested at over their rated pressure every few years, and this is not considered damaging to the cylinders at all.
you can put some pressure ring around the pipe. isn't it?
OOOPS I was thinking of high pressure instead of low pressure, this makes it easier the lid does not have to be oval, And can be held down with a "Y" yoke.
I read somewhere that you can extract oil from honey. It would be cool to see you attempt that.
Nevermind. Honey oil is apparently a quality of cannabis oil and not oil extracted from honey.
The obvious choice for many of us with this kind of solvent would be to try it with some marijuana buds, depending on your state laws of course. Usually we use something like regular butane in the freezer, so it would be really interesting to see what kind of product this way of doing it produces. Another extract I personally would like to see is that of szechuan pepper. Lastly of course, goes without saying, the Internet favorites Bhut Jolokia or Moruga Scorpion. All fat soluble substances.
I think you should make some CO2 hash oil, Ben!
Organic rose pedal extract to use in Mediterranean cooking, cognac or tea.
What does theese extracts taste like?
Re-preform the cinnamon, coffee and vanilla extractions to determine how much of an efficiency increase this setup delivers.
Lycopene from tomato waste please it is my final. Yr project please help me out
not really a stress guy but you'd derate to the annealed state in the heat affected zone and add in another 30-50% or so for thermals and porosity...ish...
Nutmeg extraction
Testing pressure containers is ALWAYS best done in "hydraulic mode" - fill it up with incompressible liquid (water, hydraulic oil), and then exert the pressure. Even if the whole thing craks there'll be just a small splash, and that's it.
About the welds: I'd be concerned not only whether they can withstand the testing pressure, I'd be also concerned with how they are going to stand up to repeated stress (from repeated extraction cycles) - weld and base metal are tad dissimilar, and have different properties. Repeated stress can lead to developing cracks - keep that in mind.
Also, there might be some stress introduced into the material by welding iitself, although in the case of TIG welding this probably won't be a real concern (from what I can see the apparatus was TIG welded).
Anyway, once you get the whole rig filled completelly by liquid, you can use some hydraulic pump (like modified hydraulic jack) to rise the pressure inside - or you could easily to make own "pump" from a section of a thick-walled steel pipe, custom made piston and some ACME threaded bolt. Plain, easy and safe.
Cheers.
I have a question for you MrKotBonifacy,
The video said that more ports may be added for injecting liquid co2.
What suggestions would you have concerning threads for gauges,
adding thermocouple wells into the cylinder for regulation.
thanks.
@@jackgreen7273 , I'm not sure I understand that question... The technical side of "gauge threads issue" is pretty simple and obvious - if a gauge has a measuring range of 4000 PSI then it's thread must withstand that force - as simple as that. You get a certain gauge, with a given thread, and you have to make corresponding female thread in the lid of the extractor. Gauges come in different sizes, so you have to match the size of the gauge to the size of your apparatus, and that's it.
As far as mounting thermocouples or cartridge heaters, taking the size of the apparatus AND safety concerns into consideration, the best way IMO would be machining a matching aluminium block, or thick split sleeve, or collar, mounted tightly around the main pipe (something like that: cdn.mscdirect.com/global/images/ProductImages/7309036-11.jpg), with "parallel" holes for abovementioned parts drilled into that block/ sleeve/ collar (paralel to the walls of the vessel, that is).
It could be round, or it could be a square block with a hole bored into it and then split, it doesn't really matter - the only thing here to keep in mind is the bigger that collar is, the bigger it's thermal inertia will be. (For machining hints take a peek here: th-cam.com/video/3cOoJ-en_M8/w-d-xo.html)
Preferably I'd make TWO of these collars, one (bigger) for cartridge heater(s), the other one (much smaller) for the thermocouple, in order to separate them somewhat thermally, so the temperature readings would be more accurate. (When you put both of these elements into one block, the thermocouple would heat much faster thn the content of the vessel). Or, you can just make a block only for heaters, and place the thermocouple somewhere else directly onto the vessel, and wrap some insulation around it.
Then I'd wrap a thin layer of slightly crumpled aluminium foil onto that pipe, in a section where I'd want to fit that sleeve/ block, and then I'd put that collar around it and tighten it well (the purpose of aluminium foil is to fill up any gaps that might be there, as stock pipes typically are not perfectly round, and thus improve thermal conductivity between the vessel and the collar). Of course, thermal conducting paste (industrial grade, like this one, euro-industry.com/main.php?index=details&cat=1267&prod=23204452) would be a better solution - but it will add to the cost, and might be tad messy, even for that "non-flowing" types - but condictivity wise, with good vessel - collar fit, it will be better option.
Then I'd place thermocouple(s) and/ or heater(s) into proper holes, filling the gap wit thermal paste, and that's it.
Having said that...
As they say, there's more than one way to skin a cat, it all depends on your experience, equipment, budget, and willingness to do your homework.
And, obviously, the best option "measurement accuracy wise" and "quick heating wise" would be to place all those elements INDIRECTLY inside of the vessel - but this will interfere with filling up and emptying it , and - last but not least - it will introduce the issue of safety and hermeticity of that rig (remember, this is a small diameter pipe, and you'd need to make and weld some housings for them).
It all depends on what is your main goal and what would be reasonably feasible in your case.
Hope it helps : )
@@MrKotBonifacy,
thanks a whole lot. I wish you would build your version of a CO2 extractor cylinder and put it on youtube.
Do you have a web site?
thanks
@@jackgreen7273 Be my guest. : )
But don't expect anything from me on TH-cam ever, period. No CO2 extractor, no atomic-powered lawn mower, not even "learn how to use a hammer in 26 easy steps" ;-)
I'm just not this kind of guy - I have my knowledge, I have my experience and expertise, I have no problem with sharing it - but making, editing, or (God forbid!) posting any video? No no no no.... That would be a transgression, or maybe even worse.
(Besides, I dont have any equipment for that, I'm I just too lazy ;-)
tea tree oil?
I can't see that working because the acrylic would have some elastic "give" to it and that flexing would make the glass break.
Would please send to me the cost of such extractor
Why didn’t you bucket test it with a hydraulic bucket pump, much safer?