Sustainable Production of Cannabinoids with Supercritical Carbon Dioxide Technologies

12-7-17

Check out the 212 page study done in the Netherlands on the study done on Sustainable Production of Cannabinoids with Supercritical Carbon Dioxide TechnologiesISBN 978-90-8570-730-1
https://thealchemistresource.thealchemistresource.com/p/normal-0-false-false-false_7.html

The following are some notes from the 212 page report by Hélène Perrotin-Brunel in the Netherlands, ISBN 978-90-8570-730-1, Copyright © 2011,

Their copyright forbids copying, but I can share some of their critical results and suggest that you read the whole thing at:

https://repository.tudelft.nl/islandora/object/uuid:c1b4471f-ea42-47cb-a230-5555d268fb4c

According to the report, between 315-345 K and pressures up to 26 MPa, the solubility of 9-THC increases as the CO2 pressure rises. Solubility decreases with decreases in temperature up to about 15MPa.

Feasible extraction conditions, with solubility above 1x10-4, requires pressures above about 20 MPa and temperatures above 325 K.

9-THC decomposes into Cannabinol (CBN) and between 314 and 334K, and pressures from 13.0 to 20.2 MPa, showed a molar solubility ranging from 1.26 x 10-4 to 4.16 x 10-4
and demonstrated different behavior as compared to 9-THC, with regard to molar solubility.

The Peng-Robinson equation of state in combination with quadratic mixing rules were used to correlate the data. Deviations between calculated results and the experimental data ranged from 4.14 to 4.46 % AARD (Absolute Average Relative Deviation).

9-tetrahydrocannabinol (9-THC) is recognized for medical application as an neuroprotective and an analgesic, showing about an equal affinity for the
CB1 and CB2 receptors.

It isn’t the only biologically active compound present in cannabis however, as there are more than 400 volatile compounds, including 66 cannabinoids all producing biological activity.

Cannabinol (CBN) is one of these cannabinoids and is mildly psychoactive, with sedative or stupefying properties. It’s the primary degradation product of 9-THC , with low presence in fresh plants, but after harvest increases as 9-THC degrades through exposure to light and oxygen in the air.

This dehydrogenation chemical reaction changes the 9-THC cyclohexene ring to an aromatic benzoic ring.

In the Sustainable Production of Cannabinoids with Supercritical Carbon Dioxide Technologies (SPOCWSCDT) study, the solubility of the cannabinoid CBN in supercritical CO2 was measured between 314 and 334 K, at pressures between 13.0 to 20.2 MPa.

The highest solubility was achieved using highest pressures and an intermediate temperature of 326 K.

CBD’s solubility behavior differs that of 9-THC, in CO2, which demonstrates greater higher solubility at higher temperature.

Due to those differences, the SPOCWSCDT study concluded that supercritical CO2
could be a good solvent for isolating CBN and 9-THC by extraction.

The solubility of cannabigerol (CBG) and cannabidiol (CBD) in SCFE CO2, were established at 315, 326 and 334 K, between 11.3 to 20.6 MPa pressure.

Within those parameters, the molar solubility of CBG ranged from 1.17 to 1.91 x 10-4 and the molar solubility of CBD ranged from 0.88 to 2.69 x 10-4.

Arranging the different cannabinoids by solubility in supercritical CO2, at 326 K, they fall in the order 9-THC < CBG < CBD <CBN.

Actual results deviated from calculated results and the experimental data from 0.81 to 6.35% AARD, with the exception of CBD at 334 K, with an AARD of 18.4%.

I was wondering when you'd get around to reading that ^_^

Pretty cool. She's a little redundant on her disapproval of current methods using organic solvents but her presentation is pretty amazing. Sure would be cool to have a girlfriend that smart. Be nice to have someone to talk to. LOL

Chemistry was not my major but I think I understood most of it.

One thing I found odd was the time and temp they used to decarb cannabis flower.... 240F for temp was about what I have always known to be accepted but they said they decarb'd for 100+ minutes. I don't recall the exact number but it was close to 3 times the normal accepted.

Another thing I didn't totally understand was the study by Chuchev and Sulu (or whoever that was) on decarboxylation. Am I to understand that they used formic acid to decarb? I recently read something about citric acid decarb'ing and just wondered if there was some correlation.

I would love to see that CPC in action. There are certain things in this study that could never be done (cost effectively) for personal use (like the CPC) but I wonder just how difficult it would be to make a DIY CO2 extractor. Maybe a pressure cooker. Tap a few holes for input and output. Hmmmm?

Thanks for the info Gray Wolf. I have found this is one of the few canna sites where this type of info is pretty prevalent. Thanks for being a contributor.

EDIT: pp 7.2.1 decarb 110 min at 110C.

Ringodoggie said:

Pretty cool. She's a little redundant on her disapproval of current methods using organic solvents but her presentation is pretty amazing. Sure would be cool to have a girlfriend that smart. Be nice to have someone to talk to. LOL

Chemistry was not my major but I think I understood most of it.

One thing I found odd was the time and temp they used to decarb cannabis flower.... 240F for temp was about what I have always known to be accepted but they said they decarb'd for 100+ minutes. I don't recall the exact number but it was close to 3 times the normal accepted.

Another thing I didn't totally understand was the study by Chuchev and Sulu (or whoever that was) on decarboxylation. Am I to understand that they used formic acid to decarb? I recently read something about citric acid decarb'ing and just wondered if there was some correlation.

I would love to see that CPC in action. There are certain things in this study that could never be done (cost effectively) for personal use (like the CPC) but I wonder just how difficult it would be to make a DIY CO2 extractor. Maybe a pressure cooker. Tap a few holes for input and output. Hmmmm?

Thanks for the info Gray Wolf. I have found this is one of the few canna sites where this type of info is pretty prevalent. Thanks for being a contributor.

EDIT: pp 7.2.1 decarb 110 min at 110C.

Click to expand...

Currently working on differences in decarb results between the different studies, and note one difference is how they tests were conducted. On bare glass in an open container, versus in a solution in a closed container for instance.

I sent a collection of charts, including a couple I drew, to Dr Fischedick and asked his take. More when I hear back.

The formic acid decarbing caught my attention as well, so I passed the study on to Pharmer Joe for his take. More when I hear back.

I agree ICM is a premier site for actual details vis a vis hubris. That brought me here almost a decade ago and has kept my attention every since.

DIY SCFE CO2 is more convoluted than it might appear on the surface. Check out: http://thealchemistresource.thealchemistresource.com/p/blog-page_13.html

Gray Wolf said:

Currently working on differences in decarb results between the different studies, and note one difference is how they tests were conducted. On bare glass in an open container, versus in a solution in a closed container for instance.

I sent a collection of charts, including a couple I drew, to Dr Fischedick and asked his take. More when I hear back.

The formic acid decarbing caught my attention as well, so I passed the study on to Pharmer Joe for his take. More when I hear back.

I agree ICM is a premier site for actual details vis a vis hubris. That brought me here almost a decade ago and has kept my attention every since.

DIY SCFE CO2 is more convoluted than it might appear on the surface. Check out: https://thealchemistresource.thealchemistresource.com/p/blog-page_13.html

Click to expand...

I noticed another difference in the studies on decarb'ing is that some are using flowers (as in this study by Dr. [FONT=Arial, Helvetica, sans-serif]Perrotin-Brunel[/FONT]and), while others (like the study on SkunkPharm) are using extract like rosin or BHO. I use almost exclusively rosin for edibles so I am definitely more interested in that data vs data on flowers.

I'm also looking for a final purification step other that Winterizing with ethanol. I use rosin and I like to be 100% solvent free so I don't Winterize and my rosin is always a little dirty.

As for building a DIY CO2 extractor, I have been a reverse engineer since 1963 when I took my families brand new Magnavox Color TV apart with my Handy Andy Tool Kit. I was 10 years old at the time. I managed to remove the back panel, removed every vacuum tube and was working on removing the last speaker when Mom finally caught me. She tried to get it back together before Dad came home but she couldn't get it working. The TV probably wasn't a week old when I did that. Boy, did I get a beating. I remember watching Johnny Quest IN LIVING COLOR. LMAO

Point being, in the last 54 years since I got that Handy Andy Tool Kit (which I still have, by the way) I have accumulated a pretty sweet stash of equipment. LOL What I can't afford to buy, I usually manage to Rube Goldberg a substitute. So, you can bet that I'll be accepting this CO2 challenge with glee. LOL

The part that will be tough to Rube is the CPC. I have a pretty nice centrifuge but nothing like that thing in the study. Wow!

Albeit, my interest in separating the cannabanoids is only for potency testing so TLC is going to have to work for me. I don't need to isolate and collect any specific canabanoid for medicine or anything. Really just want to know exactly what it is that I have. Curiousity is more my motivation. I am shooting for CBD (aren't we all LOL). I just planted a few MedTree high CBD seeds and I am curious to see if I respond to CBD in the same manner as is working in most others. I doubt it. LOL I suffer from pain, anxiety, and dozens of other issues that cannabis is supposed to help and after consuming a couple ounces a week I get zero relief from any of them. LOL Just wondering if CBD will be any different.

Once again, thanks so much to you and your associates for sharing all this information. It puts the rest of us on the path.

Peace

Gray Wolf said:

Currently working on differences in decarb results between the different studies, and note one difference is how they tests were conducted. On bare glass in an open container, versus in a solution in a closed container for instance.

I sent a collection of charts, including a couple I drew, to Dr Fischedick and asked his take. More when I hear back.

The formic acid decarbing caught my attention as well, so I passed the study on to Pharmer Joe for his take. More when I hear back.

I agree ICM is a premier site for actual details vis a vis hubris. That brought me here almost a decade ago and has kept my attention every since.

DIY SCFE CO2 is more convoluted than it might appear on the surface. Check out: https://thealchemistresource.thealchemistresource.com/p/blog-page_13.html

Click to expand...

https://jyndustriez.blogspot.com

Here's a thread I started about this with GW's input,

"Cheap, easy, and pretty CO2 extracts..."

https://www.tokecity.com/forums/showthread.php?51120-Cheap-easy-and-pretty-CO2-extracts

Ringodoggie said:

Albeit, my interest in separating the cannabanoids is only for potency testing so TLC is going to have to work for me. I don't need to isolate and collect any specific canabanoid for medicine or anything. Really just want to know exactly what it is that I have. Curiousity is more my motivation. I am shooting for CBD (aren't we all LOL). I just planted a few MedTree high CBD seeds and I am curious to see if I respond to CBD in the same manner as is working in most others. I doubt it. LOL I suffer from pain, anxiety, and dozens of other issues that cannabis is supposed to help and after consuming a couple ounces a week I get zero relief from any of them. LOL Just wondering if CBD will be any different.

Click to expand...

Which MedTree strain did you get? I finished some Richness a few months ago. They were weak stemmed that needed support but ended up bulking up quite nice. I am planning to make to make my first round of shatter with it this weekend. I am a bit mixed on the flowers so far, as if you are used to consuming large quantities of THC, the CBD has almost the opposite effect. I have smoked it before bed a few times, and gotten absolutely amazing sleep for the first 3-4 hours, and then the CBD wears off and you are high, which for me creates absolutely terrible dreams and very bad sleep after. I am going to experiment with nothing but cbd dabs and edibles for a few days, and really see how it effects my anxiety and general mood.

Gray Wolf said:

DIY SCFE CO2 is more convoluted than it might appear on the surface. Check out: https://thealchemistresource.thealchemistresource.com/p/blog-page_13.html

Click to expand...

Damn dude... that's not putting me on the path, that's a paved highway. You did everything for me. You're too easy. LOL

Very nicely done. I like your work.

WaterFarmFan said:

Which MedTree strain did you get? I finished some Richness a few months ago. They were weak stemmed that needed support but ended up bulking up quite nice. I am planning to make to make my first round of shatter with it this weekend. I am a bit mixed on the flowers so far, as if you are used to consuming large quantities of THC, the CBD has almost the opposite effect. I have smoked it before bed a few times, and gotten absolutely amazing sleep for the first 3-4 hours, and then the CBD wears off and you are high, which for me creates absolutely terrible dreams and very bad sleep after. I am going to experiment with nothing but cbd dabs and edibles for a few days, and really see how it effects my anxiety and general mood.

Click to expand...

I grabbed something called Continuum. It's Suzy Q (50:1) x Tocitonic (20:1). I have heard of Suzy but never Tocitonic (no doubt a Cannatonic run).

I picked this one because it was the only fem seeds they had and I just don't have the space or time for males right now.

You did say something that really grabbed me. I have been into lucid dreaming for decades and it's hard when you smoke pot because pot inhibits the dream cycle. However, for the first time, you have made me wonder if it's THC or CBD that is affecting the dream state. Another research project in the making. Inquiring minds want to know. LOL

Here's a couple shots of mine. The big one is about 5 to 6 weeks from seed and the other 2 are a couple weeks behind. The cups are Lemon OG clones that are on about week 3 or 4.

Nice. The smaller 2 pots look similar to mine, which were very branchy. I topped a bunch (12+) and they stayed short but were huge yielders for the space they took up. They are not the frostiest, but easily in the 20%-22% cannabinoid range, and Richness (Valentine-X x Rainmaker) being a 20:1 variety, the math is pretty simple with around 20% CBD and 1% THC. You did great with Continuum, as I have a pack of that in vault as well. It should be even better than Richness, with higher CBD and lower THC.

As to dreams, it is a most interesting topic. I find it hard to sleep unless both physically and mentally tired, and have used THC in some form to help. At various times for work, I have gone months with zero canna, and while the transition period is rough for 7-10 days, I will say definitively that my sleep was not better or more restful in the absence. If anything I would wake more often at night. As to my few sleep experiences with CBD, I think what is really jarring is that it is the equivalent of smoking a joint while in a dream state, because if you have enough thc in your system, especially if consuming edibles, your default state is being "high" from thc, and the cbd effect is the temporary one that wears off suddenly (to me). Our brains are one of the most biologically advanced organs on the planet, and as such, everyone's reacts differently to different stimuli. Hope that makes sense.