CO2 Crystallization Tech

  1. Traditional Live Resin

  2. Live THCa

  3. Live Jelly

All made with CO2.

16 Likes

Nice work dude.

That’s great, thank you so much.

Do you know the pump speed and quantity of input material used for this type of extraction? To figure out the ratio of CO2:input material to use rather than extraction time as there are so many different pumps that require different amounts of time to extract.

I was using different speeds at different times, slower to pull wax and terps, a bit faster for the THCA. Would always ramp up speed slowly.

5-10% of biomass weight in g/min of CO2 for waxes and volatiles, 10-15% for cannabinoids.

As mentioned before this can vary based on line sizes and machinery. As far as material quality, less waxy is better, so indoor material is ideal.

1 Like

very neat! you extracted fresh frozen in a neat CO2 system or you have a cosolvent?

So each subsequent pressure/temperature change requires you to pull the extract from the separation vessel prior to continuing? Also what brand of rig are you running?

1 Like

This looks absolutely fabulous. What extractor did you run with this?

2 Likes

Correct, it was a Waters. I’m not running CO2 anymore though.

2 Likes

@mtnlabs That CO2 live resin is dope. What machine are you using? Did you hook up a chiller to your extraction vessel?

I crashed out some crystals in my terpene fractions from time to time. Never got to do proper R&D so it is very cool to see you were able to make such a good looking product.

12 Likes

Hi again, getting ready to test this method of extracting THCa soon and realized I cannot operate higher than 300 bar. Do you think there would be any success in extracting at 200 bar then bumping up to 275? Or do you find you need to hit that 300-350 bar? Thanks again

2 Likes

It’s certainly possible. The Waters I was using had extremely narrow lines, so it needed a bit of muscle to move crystalline without clogging.

2 Likes

@ExTek90 :slight_smile:
can you explain the technique used in the separation and
and crystallization methods section of this paper. [(IUCr) Δ<span class="sup"><sup>9</sup></span>-Tetra­hydro­cannabinolic acid A, the precursor to Δ<span class="sup"><sup>9</sup></span>-tetra­hydro­cannabinol (THC) ]

They are subcritical CO2 using what I think is an identical
waters system to yours. There seems to be only one temp and pressure and direct release into collection vessel with all valves open? Does the collection method selectively allow only THCA
to crystallize… You seem to address this issue in some of your early posts. The method yields highest purity crystal ready for
XRD studies…but is less than 5% efficient.
Thanks in advance.

I don’t have access to it, Sci hub didn’t have it.

If they were running sub critical it definitely wasn’t the same system, I was unable to run under 150 bar and had no way to chill the columns, only heat.

1 Like

@ExTek90
using a Waters SFE Bio-Botanical Extraction
System (BBES).
system has ABPRs but all manual regulators are left open??
this is all they describe:

In the present work, liquid CO2 at 5 C rather than supercritical CO2 was used in order to avoid possible decarboxylation of THCA-A (Wang et al., 2016). The liquid CO2 flowed
at 200 g min1 through a 1.8 kg compacted marijuana sample
in a 3.3 l custom jacketed extraction chamber. All the backpressure regulators were in a fully open position. Extraction
pressures increased from 900 to 1150 psi (1 psi = 6894.76 Pa)
over the 45 min process. The collection chamber temperature
heater controls were set to 30–45 C to minimize solid CO2
formation upon expansion from the transfer lines between
chambers. Crystalline THCA-A was accumulated in the first
collection chamber in a high-purity form, not contaminated
with many of the other biomass components typically coextracted with supercritical CO2. Under these conditions, the
majority of the THCA-A remained in the extraction chamber
as part of the biomass. The quantities extracted were <5% of
the total available. No further processing of the crystalline
THCA-A was required.

4 Likes

Ohhhhhhhhhh. That’s neat, they were basically bypassing the pump and recycler and just using the system as a glorified open blast tube.

I’m sorta busy today, I’ll go over this in detail later.

5 Likes

thank you…yes…I have not been able to find anyone to discuss this with…
!!! there is so much more !!!

5 Likes

This is the most important bit, it was not a stock system. I’m totally up for helping design one, talked about it upthread I think.

1 Like

I understand…I am more interested in some of the details of that experiment:
why at 200 g/m after 40 min or 8 liters of CO2 liquid solvent over
1,8 Kg biomass…do we only get a yield of less than 5%…
but what we do get by XRD analysis is pure THCA protonated form.
This is CO2 interacting with Biomass Trichome soup at about 5C…how do you explain why CO2 is such a poor solvent.

I used to have a diagram somewhere describing the polarity of co2 at different pressures and temperatures, as well as with different co solvents. Unfortunately that’s lost.

It’s a weird solvent.

It’s generally non polar at high pressures and generally polar at lower pressures. I would imagine at 5C and ~1000 psi it’s not very effective and it’s mostly polar. This would explain why it’s not grabbing much in the way of terpenes or waxes even at that flow rate.

I have a list of solutions to these problems but need a manufacturer to work with.

2 Likes

Isn’t it the opposite? I thought polarity increased as pressure increased?

Waxes & fats are primarily non-polar, that’s why we winterize in methanol (highly polar).

1 Like