New patent for In-Line Winterization / Real-Time Winterization

[GreenSolvent]

I think many people don’t know you can use liquid CO2 at negative temperatures and make winterized oil straight out of the extractor. If you didn’t have a high pressure system, then this was the way you would go after decarb. However, if you don’t want to spent all of the time decarbing all of that biomass in advance and you still want a 2-hour run with 90% + efficiency, then you can use supercritical pressures and temps (like 275 bar and 35C) but then you pull more waxes…unless you winterize in-line.

It seems that Thar Process patented it : US20210079315A1 - Process for producing refined oils from botantical plant matter using a supercritical fluid - Google Patents

It also appears that Green Mill is doing something like this on a smaller scale.

[Jdilley]

Why is no one walking about this?

[AdamExtracts]

Do you have more info on the CO2 winterization that Green Mill is doing? Is it an add on to the machine or just different parameters?

[GreenSolvent]

I don’t know. It seems like Thar changed focus back to hops and agricultural applications.

[GreenSolvent]

I heard that both companies are offering add-ons. I heard that both are 30-60% add-ons to the normal price. So that’s $200k + maybe $120,000 for a 500 g/min flow rate Greenmill. I don’t know how much savings you get there. Its a bit better if you are scaling up to a larger system like a 2x25 from Thar that generates about 1kg of extract every hour (decarbed) or 90 minutes (non-decarbed) because the flow rates on that system = 2.5kg/min. Then, do the math and that’s a lot of winterization. On LinkedIn, it seems that Thar runs a CO2 re-extraction winterization. They put the oil back in after a campaign and run it on their big boy machines.

[SoStupendous]

The dollar cost of CO2 extraction for hemp or cannabis is too high for the throughput. If on the other hand CO2 crude itself were in high demand it might be useful, but CO2 cannabis crude is too much of a pain in the butt to refine further compared to alkane or alcohol extracts.

[GreenMill]

The Green Mill Real-Time Winterization module is about the same cost as an ethanol winterization workflow, which you no longer need. The winterization happens in-process (hence “real-time”) and the product that comes out of the extractor is wax-free with high potency. It is shipping now, unlike competing offerings which are still in R&D.

Here is data to back up the claims made about RTW.

[BrotanicalMatt]

Growers hemp has had this tech for a long time.

I use to take their crude and throw it into a SPD right from extractor.

[GreenMill]

Do you have a link to their product page? I would be interested in knowing how long it took to extract and how much cannabinoid loss there was. RTW adds nothing to run times and involves near-zero loss of targeted compounds.

[BrotanicalMatt]

They don’t sell it. They bought old Russian subs and built this things from scratch. Wicked smart dudes. I have pictures of it on my old phone.

[TharProcess]

We did the R&D in 2019 and patented it. Looks like good news for CO2 extraction if multiple vendors are doing this. Seems like CO2 has lost out quite a bit lately to hydrocarbons in the MJ market. The opposite is true in hops and other products. However, there is definitely only one patented process for CO2 winterization so far to our knowledge. Plus, Thar is likely the only one doing it on an industrial scale. We have run over one ton of product. We showed the data at MJ Biz but can upload here.

[GreenMill]

The Green Mill RTW equipment and methods are novel, and the only ones that have succeeded in winterizing with CO2 to de-wax inline without extended extraction times or huge loss of cannabinoids. Almost all of our new extraction system sales are to smart operators who are also ordering RTW modules because the business case is rock solid.

Below is oil from the extractor (left) and a cannabinoid-free wax fraction (right) after a single, standard-length CO2 extraction:

[GreenMill]

Flow rate is very important. However, faster is not always better. Our philosophy is that the most crucial aspect of solvent flow is that you have a smooth flow profile, which will prevent channeling and give you a more efficient extraction. Furthermore, at a certain point, simply increasing flow rate will alter solubility and start to negatively affect your Extraction Kinetic Curve.

[TharProcess]

Solvent:Biomass ratio therefore flow rate is by far the most important specification for CO2 extraction equipment. Nobody is running too fast for cannabis extraction even though some systems have poorly designed extraction vessels (aspect ratios). Nobody ever says - that’s too efficient or that’s too fast. The only application where this can come into play is in very low solvent:feed applications like defatting soy, canola or varios terpenes. Those solvent:feed ratios are more like 8:1 or 12:1 vs cannabis solvent:feed ratios of 50:1 or 90:1. Total Cost of Ownership is what all major companies use to measure an investment in production equipment. Most CO2 manufacturers, despite all of the natural advantages of the green solvent, have not kept up with the speed of ethanol and hydrocarbons on a per hour basis. This has lead to a graveyard of systems throughout the world.

[JonaaronbrayAzoth]

How about you run your extraction at the perimeters that you dewax with?

Have you not proven that you can extract cannabinoids without wax using Co2?

Why are you extracting all of that wax in the first place if you’re just going to run lower pressures Co2 over it to extract the cannabinoids?

It baffles me why anyone uses supercritical Co2 for the extraction of cannabinoids when near critical or sub critical can extract much cleaner cannabinoid fractions.

[GreenMill]

What we have proven is that our Real-Time Winterization module de-waxes during the supercritical extraction of cannabinoids, adding absolutely no time to the run cycle. These are normal ScCO2 extractions that produce fully de-waxed oleoresin with full retention of the THC/a or CBD/a.

Yes, it has been possible all along to “de-wax with CO2,” but the equipment of the time could not make it viable for business purposes.

Here, you extract for a few hours and you’re done. (Unless you want to go straight into distillation.)

[TharProcess]

I think that’s what so interesting about CO2. You can automate the run to extract into one separator for 17 min at lower pressure (sub or super) and then increase the pressure/temp of the run in a gradient and get the rest of what you require. Running low pressure is time consuming. Plus, we now know that lower pressure CO2 machines lack the safety considerations high pressure systems have. They have doors that open sideways and have caused debilitating injury and have been rejected by some companies because of the way their doors open toward the user.

Our normal operating runs call for terps first at 65 - 75 bar, then an automated ramp up to 175, 200 or 250 bar - depending on customer preference. Some products can go into the terp collector, others into the medium pressure separator (which could be isolated if you like) and others into the lower pressure recycled separator. Everything seems easy until you get to scale.

Pretty soon, hops extraction will follow this path. In fact, most of the total tonnage of US extraction of hops will go through Thar Process machines in the NW and Midwest by the end of '22. These systems are scaled to 6 tonnes / day of biomass depending on how much time they want to spend on terpenes vs. alpha acids. Regarding lab scale amounts of waxes…yawn.

The small labs will disappear - this game is going to be about scale over the next 5 years:

I’m glad that we are all having this discussion, but we are at risk of just becoming an echo chamber. So I think its important that we are talking to EtOH users rather than ourselves…

[JonaaronbrayAzoth]

“Plus, we now know that lower pressure CO2 machines lack the safety considerations high pressure systems have. They have doors that open sideways and have caused debilitating injury and have been rejected by some companies because of the way their doors open toward the user.”

I find this statement to be suspect, have you ever even operate a pig launcher? Be it a German or American pig launcher, they both have a two stage operation which makes it impossible to open the door fully without full depressurization.

I find “pipe machines” (machines which use pipe for vessels as opposed to a custom manufactured vessel) to be unsafe because they are never rated to below -20f. Any Co2 extraction system with vessels not rated down to -40f is dangerous because it’s a matter of time before a vessel holding liquid Co2 will reach sub -20f temperatures.

The insistence of “SFE” engineers not to have any experience running their equipment on the marketed botanicals before “training” the customer is maddening. The blind leading the blind…

Why would a “SFE engineer” develop a system that wasn’t capable of extracting the main target of the market (THC-a) effectively?

If there was a more effective way to extract clean target fractions why wouldn’t you engineer your system to extract quickly using these more selective set points?

Everyone manufacturing Co2 equipment should look at themselves for the failure of the technology (myself included).

The simple fact is that Co2 systems don’t make marketable cannabiniod products without a second solvent.

Until there is complete refinement of the targets in the system, Co2 systems will be a novelty.

Full inline winterization with solvent recovery with a CXE injection will give you a marketable product from the extraction system. This is the only thing that can save Co2 from obscurity.

I have retrofit kits that allow injection and refinement but I haven’t been able to finish a system that integrates the second solvent recovery.

If someone with the funds wishes to see this system come to life please reach out to me, there are two 700 liter CXE skids waiting for instruments and pumps in Tulsa.

[AlexSiegel]

Has the terpene debate been settled in CO2 vs hydrocarbon extraction?

I’m inexperienced with CO2. I’ve never compared extracting with cold hydrocarbon to an optimal CO2 extraction when it comes to terpenes. The same material into both systems does the hydrocarbon or the CO2 have a better terpene profile?

Then there’s the non terpene flavors that could come over as well

[AlexSiegel]

I’m also wondering if there’s anyone who has developed a reasonable amount of data around the possibility of pressure and heat causing degradation to the many plant compounds in weed.

Similar to a synthetic chemist who should identify the possible contaminants, should CO2 extraction be held to a higher standard than something like hydrocarbon extraction where there’s much less opportunity for chemistry to happen