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Vomaturge
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The word screen can mean many things. "a windscreen" "a computer screen" "a privacy screen of trees" Tsjerk doesn't mean fine mesh... I hope. As for
residual pressure, he has already stated his intent. He wants a pressure release valve that will let off at 6 atmospheres (or some other
pre-determined pressure lower than the vapor pressure of carbon dioxide at room temperature). As the dry ice heats up, the pressure will rapidly
build, allowing the dry ice to melt. When the pressure gets high enough to open the valve, the liquid CO2 will start evaporating and escaping. The
extract is supposed to stay in the chamber, assuming that the extraction worked to begin with. Once all the CO2 boils off, and the chamber has come up
to room temperature, the safety valve should stop venting. The chamber will still have gas under pressure. This is the "residual pressure" that has to
be vented before opening the chamber.
For some reason I to would expect extractions to be ineffective at extremely low temperatures. I know I already said that carbon dioxide may not have
to be supercritical, but I was more thinking along the lines of 0C, 30 something atmospheres or 20C, 50ish atmospheres. But again, I have no proof
that this will work better. The liquid CO2 extractions I saw on YouTube did not show the pressure or temperature.
Of course, any increased pressure will make it harder to build a pressure vessel, and will lead to a worse explosion if it fails. I am not sure
whether people should try this and be very careful, or if they should not try it at home at all. A while back, I found this story about a serious
brain injury from a bottle of ginger ale that overpressurized:
https://survivingtraumaticbraininjury.com/tag/soda-can-explo...
If it was a re-used plastic bottle, it could not have held more than a liter or two of carbon dioxide gas and water with CO2 in solution. The pressure
could not have been more than 10 or 15 atmospheres in a plastic soda bottle. But that was enough to do permanent damage. I have heard people say that
a container of liquid rupturing is less dangerous than a container of gas, because it won't expand violently once the containment is gone. But, with a
container full of liquid carbon dioxide, the EXPLOSION WILL BE MUCH WORSE THAN WITH AN EQUAL VOLUME OF GAS AT THE SAME PRESSURE.
Just for the sake of it, lets try to see how bad. Once the container breaks, liquid CO2 will spray out into the surroundings. At the triple point of
217K, 5.18 bar, the latent heat of fusion of the liquid is 197 j/gm, and the latent heat of sublimation is 571 j/gm. The density and molecular weight
are roughly 1.1kg/L, and 44 g/mol, respectively:
https://www.pacificdryice.com/physical-properties/
based on the heats of fusion and vaporization, it is clear that WITHIN MILLISECONDS, ABOUT 34.5% OF THE LIQUID WILL VAPORIZE, (around 8.6 mols of gas
from a liter of liquid) and the remainder will freeze, without the pressure or temperature changing at all. 30 liters of gas, still at around 5
atmospheres and -56C are almost instantly released from a single liter of the fluid, and this freeze-boil-expand process releases around 15 kilojoules
of mechanical energy. I would say that it takes between a gram and ten grams of chemical explosives to do the damage of a liter of CO2. The gas is
still at 5 atmospheres at this point, and will continue to expand and cool, although how much it can adiabatically expand before it just starts
condensing into dry ice is hard to estimate. Now, If the liquid CO2 were warmer than -56C, more of it would evaporate initially, and it would be at a
higher pressure, causing much more damage. That was long. Sorry. I just had to try to quantify this.
A more important calculation: (cost of apparatus blown up+cost of court fees, jail time, fines, etc for explosives and or drugs+ cost of doctor bill
because you partially blew yourself up+cost of cannabis you blew up)(shitty quality of life because you're in trouble with the law+shitty quality of
life because you blew up your stash of weed+shitty quality of life because you partially blew yourself up)(the tremendous indignity and embarassment
of this whole debacle)= how bad an exploding extractor could be.
Still a bit better than a scorching hot butane explosion-extraction:
http://registerguard.com/rg/news/local/36308727-75/feds-argu...
Edit: I didn't do all of those stupid "vaporization" calculations just to scare people out of doing this. I had done most of them for other reasons a
year or two ago (and no, I didn't blow anything up). In some ways, the results are encouraging: a small CO2 extraction chamber rupturing might be
hazardous, but not insurmountable. Trying it does not have to be an incredibly stupid or wreckless thing. If you did it in a bottle held in the hand,
and tried to control temperature and vapor pressure by tightening and loosening the cap, now That would be really stupid. But if you have a
strong chamber with a safety valve that's much better. Tsjerk, I think you are pointed in the right direction safety wise, thinking about putting the
whole setup behind a, ahem... fragmentation suppression barrier. You know that there's a good chance the thing will explode, and are finding ways to
deal with this reality. That's the way it will have to be for any amateur or "DIY professional" unit. Now, depending on what you're extracting, how
much, where you are, etc., we might have to get pretty creative with explosion fail safes. A way to recover product post-accident would be really
nice, and a way to surpress sound and pressure waves might be crucial in some installations, like in an apartment (hypothetically). I don't plan on
extracting any cannabinoids, but I am captivated by the idea of using carbon dioxide as a solvent. That's the main reason I'm part of this discussion.
Happy extractions!
[Edited on 15-3-2018 by Vomaturge]
[Edited on 15-3-2018 by Vomaturge]
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Tsjerk
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[Edited on 15-3-2018 by Tsjerk]
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happyfooddance
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Quote: Originally posted by Tsjerk  | Dude? What is your problem? I didn't read all your posts, but the once I did read are all this negative shit like you spill here.
Do you have a clue about what I mean with a screen? Apparently not as you think I'm stupid. I used to make high and low explosives, I know what an
explosion can do, I can perfectly imaging what a steal vessel at high pressure can do, I don't underestimate it. Don't worry.
Residual is relative. My over pressure valve can handle 650 liters of gas per minute. You don't have a clue about the size of
my apparatus, so you don't know how much it will have to handle. Don't make assumptions.
Semi-closed? My apparatus is completely closed with a high over pressure, which you could have known if you would have read what I said and looked at
my ugly drawing. Where is the water coming from?
Did you see the YouTube video I linked too? A brick won't extract no, the idea is to make liquid CO2. It is not going to evaporate before doing so,
and I'm not going to try doing so, thank you for suggesting though.
Do you have references saying cold CO2 doesn't extract? I can't find them, please enlighten me. I like using references when stating something not
commen knowledge, as you can see from my posts in the past.
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Research it yourself.
I don't give a fuck if you blow yourself up, willingly, or stupidly. Have fun. You can talk shit on me and my posts, but if you look carefully, I
only post to help other people, usually from hurting themselves. How many questions have I asked, how many threads have I started. I'll help you out.
0.
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Tsjerk
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I didn't think you would worry about me hurting myself.
Why do you try helping people if you don't care about them? Does it make you feel better about yourself?
I will let you know how my experiment works out.
[Edited on 15-3-2018 by Tsjerk]
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aga
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Welding is Fun ! Definitely worth learning.
In any event, testing pressure apparatus isn't too difficult. Slightly dangerous, but not difficult.
https://es.aliexpress.com/item/Hand-tool-manual-pressure-tes...
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Tsjerk
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@happyfooddance; don't like speculation while pretending you are not. I used to peer-review articles, including reviews, among others for Nature
Reviews. By my hand articles got rejected because of speculations, I just hate it. Your posts have a very strong penetrating speculation smell around
them.
[Edited on 15-3-2018 by Tsjerk]
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happyfooddance
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You both are complete rookies, which is apparent.
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happyfooddance
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| Quote: Originally posted by Tsjerk | @happyfooddance; don't like speculation while pretending you are not. I used to peer-review articles, including reviews, among others for Nature
Reviews. By my hand articles got rejected because of speculations, I just hate it. Your posts have a very strong penetrating speculation smell around
them.
[Edited on 15-3-2018 by Tsjerk] |
Tell me which of my professions are speculations. I will gladly send you pure samples of your own dumb-ass interpretations of organic chemistry.
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aga
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Chill out dudes.
No need for personal attacks etc.
All that kind of ego-crap is really boring.
Edit:
Take deep breaths, then weld some bits of scrap steel together to relax.
[Edited on 15-3-2018 by aga]
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Tsjerk
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I didn't say your posts are based on nothing, but you never give any checkable resources for any of your claims. You just say "this is true" without
explanation. Also when it is not obvious what you are claiming.
Besides that you also speculate. How do you know CO2 doesn't extract at low temperatures? Did you try it? Did you read it? Is it Common knowledge?
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S.C. Wack
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What makes you think liquid CO2 is a solvent at all? By extension this means you think industrial supercritical extractors are fools who could just be
shaking liquid CO2 in a pressure vessel.
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Tsjerk
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https://www.sciencedirect.com/science/article/pii/S026087749...
https://youtu.be/o2aIUemy9Xw
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OldNubbins
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This guy appears to know enough about what he is doing to still be alive.
Superitical CO2 - in plastic! WOOOOO! Get the pitchforks!
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S.C. Wack
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Subcritical extractions are known but the extraction power is not good. Data at higher pressure here.
Sustainable Production of Cannabinoids with Supercritical Carbon Dioxide Technologies
Hélène Perrotin-Brunel.
Attachment: H.Perrotin-Brunel-PhD_thesis-final_version.pdf (2.9MB)
This file has been downloaded 423 times
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Sidmadra
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I find this a little funny and felt that it needs to be pointed out, since nobody has done so in the last 3 pages - people are arguing about CO2
extraction, and have been posting about it since the first page, when that isn't even what OP was asking about.
It was pretty clear to that he was asking about purifying cannabinoids (separating out the low-mid BP terpenes from the high BP cannabinoids),
POST-extraction, since he was talking about short path distillation. You know, taking the sticky wax and refining it into a nice white powdered
THC/CBD/Cannabinoid mixture. His entire first post is about distillation and boiling points, which being a chemistry topic works here. There isn't
any mention or question of the extraction process, yet people are here arguing over CO2 extraction.
| Quote: Originally posted by S.C. Wack | | What makes you think liquid CO2 is a solvent at all? By extension this means you think industrial supercritical extractors are fools who could just be
shaking liquid CO2 in a pressure vessel. |
What do you mean? CO2 is a solvent in this application... Supercritical CO2 is good solvent in that it dissolves a wide range of compounds, regardless
of their solubilities. A quick google search can reveal hundreds of pages on its ability to act as a solvent, and "green replacement" for many other
solvents. If it wasn't acting as a solvent then it wouldn't do anything to extract the high BP cannabinoids.
These "industrial supercritical extractors", COULD shake liquid CO2 in a pressure vessel, but after drainage, there would still be desired compounds
left behind in the material. Shaking it makes little sense as an extraction technique, when you could use a continuous extractor and get a more
thorough extraction with FAR more ease. You can also get away with having a lower ratio of solvent:plant material.
Imagine you have 500g of plant matter, and to do a complete batch extraction, you might need 20L of solvent because of the low solubility of the
compounds. Or, you could use a loop extractor that recycles the solvent, like a Sohxlet, and get away with just using 500ml of solvent.
[Edited on 15-3-2018 by Sidmadra]
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S.C. Wack
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| Quote: Originally posted by Sidmadra | I find this a little funny and felt that it needs to be pointed out, since nobody has done so in the last 3 pages - people are arguing about CO2
extraction, and have been posting about it since the first page, when that isn't even what OP was asking about...
...What do you mean? CO2 is a solvent in this application... |
We've moved on from this limonene stupidity. I said liquid CO2. Supercritical CO2 is not liquid. When this homemade process with liquid CO2 has pumps
and/or many cycles like the 65 atm. Soxhlet of Tsjerks article it might extract something.
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Sidmadra
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| Quote: Originally posted by S.C. Wack |
We've moved on from this limonene stupidity. I said liquid CO2. Supercritical CO2 is not liquid. When this homemade process with liquid CO2 has pumps
and/or many cycles like the 65 atm. Soxhlet of Tsjerks article it might extract something. |
I feel like we're splitting hairs here... but I definitely wouldn't just outright declare it's not a liquid, as supercritical CO2 is in a fluid state
and dissolves compounds like a liquid, even though it's not technically in liquid form.
https://en.wikipedia.org/wiki/Supercritical_fluid
"A supercritical fluid (SCF[1]) is any substance at a temperature and pressure above its critical point, where distinct liquid and gas phases do not
exist. It can effuse through solids like a gas, and dissolve materials like a liquid."
https://en.wikipedia.org/wiki/Supercritical_carbon_dioxide
"Supercritical carbon dioxide (sCO2) is a fluid state of carbon dioxide where it is held at or above its critical temperature and critical pressure."
.... and I'm not sure why we moved on from the Limonene thing. Practically nobody tried to answer OP's question except for one or two people. This
thread has mostly just been an arguing place of people debating about CO2 extraction.
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happyfooddance
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I have a hard time thinking that I am "arguing" at all. I am just trying to keep someone from hurting themselves.
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S.C. Wack
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It's most very definitely not a liquid and it's not splitting hairs. There really is a huge difference between the two forms in both utility as a
solvent and physical form.
There isn't a reason to use limonene as a solvent. Because someone else has done it isn't a good reason.
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Corrosive Joeseph
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Please guys, no bitchin'........... 
Slightly off-topic, but what I have 'heard' -
All brands of lighter gas gave a similar golden oil tinged with brown and a barely discernable hint of green.
One particular brand gave a most beautiful golden oil that was far more potent than any other.
Once the oil is collected in the bottom of a glass bowl, it is placed on the (just switched on) steam bath and dissolved in about ten times it's
volume of pure EtOH.
This dissolves both oil and resudial gas (and even shitty ethyl mercaptan) and the hydrocarbons and ethanol are driven off as SLOWLY as possible.
Repeat this alcohol wash 2 or 3 times.
Now for 'winterization'. Dissolve the oil in enough EtOH to fill a glass bottle with a good seal.
Place in the freezer, packed in a crushed ice/table salt mix. This will bring temperature down to about -20c
The plant waxes will coagulate and fall out of solution.
Filter and then evaporate the alcohol (slowly again) to give a very potent oil.
This is the easiest way to produce a material of high quality and if the oil is to undergo a distillation it is the perfect starting material.
Butane that had been pre-chilled over night in the freezer and used immediately, produced a digusting oil that drew out far too many undesirable
compounds.
NO comparison to 'room tempature' cans. Just report of the effect of temperature on solubility as touched on above.
NOTE - Even 3 alcohol washes on an oil made with evil ethyl mercaptan gas left no sulpher/rotten egg smell and that stuff is detectable below 1ppm in
air. I'm not recommending anybody use this gas but only trying to showcase the efficiency of the pure EtOH washes.
I'm sure there was more but thats all I can remember for now.
[EDIT] - Nodded off on the keyboard and fired off half a post too early.
Goodnight
[Edited on 16-3-2018 by Corrosive Joeseph]
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happyfooddance
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| Quote: Originally posted by Tsjerk |
Besides that you also speculate. How do you know CO2 doesn't extract at low temperatures? Did you try it? Did you read it? Is it Common knowledge?
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Sometimes. Experience. Yes. Yes. Yes.
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Fulmen
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Can we take a step back and discuss this in a civil manner?
Happyfooddance: Do you claim that cold liquid CO2 won't extract THC specifically or that it doesn't work as a solvent at all? This video does suggest
that it could work: https://www.youtube.com/watch?v=o2aIUemy9Xw
A quick search for this method on THC did not give any results, but that really isn't conclusive evidence of anything. And while one should never
underestimate the dangers of pressurized vessels it should be possible to do this safely without too much effort.
The triple point for CO2 is 510kPa/217K, so a 6-10atm safety valve should work assuming it can handle the temperatures (-50°C).
We're not banging rocks together here. We know how to put a man back together.
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Sulaiman
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If the sale and/or trade of the product is not allowed,
what is the benefit of regular extraction/concentration ?
(once or twice as an experiment I understand)
I imagine that there is a significant risk of abuse rather than use with very concentrated extracts
and the side-effects of consuming the entire product are historically well documented,
but at high dosage, without (possibly) intrinsic 'antidotes' to some side-effects,
there will be new potential risks.
=======================
regarding butane-in-a-can as a solvent, to check for non-volatile contamination
squirt an inverted can into a clean borosilicate beaker,
(thermally isolated from external thermal conductors such as liquids and solids),
allow to evaporate, then check for residues.
(outdoors, upwind, with no ignition sources downwind)
Then do the same for any other potential solvent.
.......................
I find it difficult to believe that butane would leave more residue than limonene which has a much higher b.p.
I can imagine butane residues being more sensitive to detection than limonene,
due to the molecular similarity between limonene and THC,
and the b.p. difference between butane and the product..
......................
anecdotal: I use transparent plastic cigarette lighters, after 10's refills per lighter I have never seen any residue, liquid or solid.
CAUTION : Hobby Chemist, not Professional or even Amateur
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Tsjerk
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| Quote: | If the sale and/or trade of the product is not allowed,
what is the benefit of regular extraction/concentration ?
(once or twice as an experiment I understand) |
I'm aiming for CBD, not THC. CBD is a big hype now and as long as the concentration of THC in the end product is lower than 0.2% Dutch law has no
problems with the sell of it.
CBD is diluted to 4- 10% in for example vegetable oil.
There are breed of Cannabis sative which are very low in THC but high in CBD.
CO2 extraction is a big plus when selling the product for consumption. I don't know how contaminated butane extracts really are, but when selling CO2
extracts are way easier to get rid of.
[Edited on 16-3-2018 by Tsjerk]
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Mister E
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| Quote: Originally posted by Swinfi2 | | Quote: Originally posted by Mister E |
Furthermore there is a recrystallizing method referred to as "winterization" using ethanol. I also know this is being done to the extract after the
limonene is removed. |
Winterization is the process used to remove plant fats from the extracted material, the terpenes and canabanoid solubilities aren't too effected by
temperature but filtering while as cold as possible takes out plant fats. Then distil your ethanol back off.
I've heard this makes a product suitable for use in vape pens etc. which would be healthier than mixed combustion products. |
You're quite correct. Winterization is a recrystalization of plant fats to separate them rather than a recrystalization of the THC.
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