Wondering if anyone has any tips on how to improve the concentration of cannabinoids in their final distillate?
My expectation would be that the colder the extraction and finer the filtration you would remove/prevent more undesirables from making it into your crude and ending up in your distillate.
Currently we’re producing a distillate around 85% THC and just under 90% (900 mg/g) of total cannabinoid content while extracting (EtOH) between -25 and -40C and filtering down to 1micron.
My assumption is that the remaining 100mg/g are undesirable compounds like lipids or starches but curious if anyone filters down lower (eg. 0.5u, 0.1u, or smaller) and if that has proven to improve final concentration.
you’re distilling. which is going from liquid to vapor and back to liquid again.
can you offer any explanation for how removing solids would affect the final composition of the distillate?
you’re doing a fractional distillation. what might be going on here that could be improved?
you can certainly get ahead of the game by deliberately targeting specific non-target molecules, but simply filtering for the sake of filtration is not going to get you very far until you get down into the range of things that might legitimately co-distill or interfere with your distillation. things in the kiloDalton range… Your target is about 1/3 of a kDa.
KD, or kD is the abbreviation for kiloDalton and is equal to 1,000 Molecular Weight Cut-> Of(MWCO). A solution having a molecular weight
of 1,000,000 would be equivalent to 1,000 KD. The table listed below gives a general relationship between kiloDalton to Microns
(micrometers), Nanometers, and Angstroms:
Run your heads at the highest temp you can without distilling thc, and leave it at this temperature for longer (until you see 0 drops after 5 minutes), distill on the lower end of your distillation temperatures (you still want a good rate) and leave it at this temperature for longer. You can try using a spinning band, but I don’t think it helps more than a percent. Redistilling helps a little more, but it isn’t more than like a few percent. Activating under a vacuum helps a few percent since you get less conversion to other cannabinoids. Winterizing makes the whole process easier, but doesn’t always help increase potency and is a waste of time.
Frankly not. I have done comparative testing using membranes in the 10,000 Da range (Like 0.002um = 2nm or so). You don’t really start seeing any benefit to distillate potency until you’re really getting down in the sub-1000 Da range. At that level you’re beginning to remove compounds that are actually small enough to volatilize and go to the distillate side.
You will see less mass in the distillate residue, since like you said, you’re removing starches etc, but those things wouldn’t have distilled over anyway.
I like @DrWHY420 head procedure. I had some distillate out of a wiper with heads that hadn’t been stripped enough. Bad tasting distillate is a shame. I just short path it out but it’s only necessary for edibles in my opinion. As someone who makes edibles, I wouldn’t buy that distillate for that purpose. This would coincidentally increase your potency as well as improve your quality.
I think a LLE should be almost mandatory if you extract with ethanol. Unless you’re a proof nazi, residual water is going to pull sugars/starch. This stuff dehydrates and chars at 160c and turns into aldehydes and crap. It comes out after a second pass I think but the compounds generated from that reaction are so wide there’s lots of ? . Just do an LLE, you gotta be tricky to scale it well, but it’s worth it. Give it a try on the bench top to confirm tho, in case I’m wrong . And if not sugars, trace cations and metals. Those isomerizing pricks.
-25 may not be cold enough if you’re not spraying fast enough. If so you’ll get waxes and starches.
Also, there’s some stuff that’s really hard to get rid of even with good processes and distillation. Free fatty acids don’t come out easy. Magsil does it, but it kinda takes the soul out in my opinion. 90 is quite good, you may just need to tune your process to run better which will get you the next 5%
If you want 99%, trash your ethanol system, get into hydrocarbon extraction, recrystallize THCa twice , decarb.
My apologies, I’ve been away dealing with some things over the last couple days and haven’t had a chance to respond to all of the great discussion and advice.
My thought process was more in the vein of the lipids and waxes which might have gotten extracted but were solid/semi solid enough to be able to be filtered out at very fine levels.
Thanks so much for this advice, I look forward to testing it out! Although the biomass we were using for this past run tested well (20%), it’s age and color (more brown than green) were suspect and I’m figuring that this could also have had an impact on the final composition if the distillate.
Still very new to the distilling game so definitely going to make mistakes and try and learn from them and all of you
Push heads forward, then back off in temp. Then when doing tails do similar. It’s all about the cut off points.
I was having a difficult time a while back finding a solution like this. I ended up called @spdking at summit and he gave me a free sop to solve two issues I was having. Most people don’t know, but if you have a issue you can call them and they will hold your hand and walk you through it. I only talk to Elliot when I have issues, he really cares about others success. He can redo your sop in real time and solve your issues at no charge. When I say quick results I mean quick results.
Also keep your condenser above 100c or else you will not bounce out impurities and they will booger up and collect in the distillate.
One of the tricks of the trade is to run your condenser arm hot.
Which is distinct from mere “filtration”, and some leave till after first pass distillation.
Do you winterize? How and when make a difference.
Filtering the miscella to better than 20um before it is allowed to get above extraction temp can be helpful for preventing continued extraction (except if you’re already extracting at rm temp…)
They are also on point re: proofing. Even 180 changes the extraction profile…
@Lightbulb once again sounds like Elliot , and is referencing “hot condenser”, and the fact that you are performing a fractional distillation here.
Which brings me back to
…I’m assuming (as is @Lightbulb) that you’re using what folks in this industry refer to as an SPD, but nothing you said so far excludes a wiper. The differences are enough that telling us what you’re running is gonna get you further (than just filtering to hell and back )
The majority of distillers like hot condensing effect and benefits. The only people who don’t practice it are the ones with the inability to perform it. E.g. like lesser functional chiller units.
The problem with most preprocessing is the issue with cutting corners to make the day easier. This should be intolerable to distillers as it creates a lacking product. I cannot stand any idea of cutting corners. The most valuable advice you will ever get is to create a streamline process that is a know process with steps to pre process properly.
Winterization. It’s extremely important to use 200 proof and no watered down solvents as the winterization process and next step rely on the solvent purity.
Carbon scrub and do it fast and quick. This will prevent any unwanted compounds from really being present that are most commonly held between fractions.
Rotovap hot. The hotter the better.
Distill and push each fraction further, if you are unsure push even further.
First pass should never ever be done as a refinement pass. Only if you have removed the misc compounds. The first pass should always be done as fast as possible, but managed temps. This is the most important part of being able to push a second pass out with higher potency, and clearer colors. If you have a cat 3 or remediated product you can run a refined first pass. The goal is to shave off all misc compounds in the first pass and prevent isomerization. Removing it as fast as possible prevents degradation and excessive recirc of the compounds. The second pass can shave hairlike fractions this way as the bulk of compounds that would have been evaporating are now gone.
. And if not sugars, trace cations and metals. Those isomerizing pricks.
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