I have been reading around the forums quite a bit, and am stuck in this rabbit hole because there is such a treasure trove of information to help me improve upon!
I had a few quick questions to make sure my brain is on the right path to helping make a higher quality crude oil extract, not only for just crude, but to expand upon with distillation down the road as well.
Currently, our lab is producing crude oil at a small rate (~2000g/mo), however its hard to use in many products because it always has a burnt fishy type smell to it from the decarb, and carries some nasty looking particulate in after decarb as well.
My goal is to really improve the methods currently in place, and Ive seen and read many threads regarding decolorization and clarifying with celite and AC to really refine the process. My question is, will either of these methods help with the issues I seem to be experiencing?
Our cold EtOH will be refined soon as well, but currently using a cascading bucket tek system that leaves much of the liquid phase either a dark brown, or green depending on where in the process it was filtered with 100 micron filters. The end product is coffee black even after winterization, which goes thru a qualitative filter.
I was thinking of doing some small R&D on a test batch, with a celite and AC scrub to clarify and improve upon the color immensely. My question is, what size micron filter works best for this process? I only have two ceramic buchner funnels to work with at his point, and a shit vacuum pump.
Any advice helps! I have read thru what feels like a ton of information and still making my way thru it all, but would love some feedback.
Lots of good things on this site for you. you can just search the key terms to see more in depth discussions about each topic.
Cold and fast ethanol extraction- This will be probably your best bet for increasing crude quality. keeping the contact time low and quickly filtering out all plant material while the ethanol is still cold will give you lighter colored, more potent crude. Doing the extraction cold leaves behind lots of undesirables.
Filtration media- There are many options here. Celite and Diatamaceous Earth (DE) are primarily filter aids, meaning they will retain very fine plant particulate.
-Bentonite - an activated bentonite clay does a good job of adsorbing water soluble molecules, this will help clarity, and remove any particles that you find in your roto after ethanol removal, or after decarb. Bentonite will slightly remove orange/red color, but this is not its best use in ethanol.
Activated Carbon- Good at removing the green color from extracts, look out though, using this while not doing a very cold very quick wash can cause your extract to turn a deep red, in my and many others experience.
I would start here, search around using key terms and i’m sure you’ll find some other useful stuff i didnt mention.
Our ethanol extraction process definitely brings over some green due to me realizing the process in place where the ethanol is pre-chilled, however not with the dry ice prior to the introduction of the plant material. After reading a bit on here I see there would be a much higher advantage to introduce both the ethanol and dry ice together to cool it to cryo temps, before introducing plant material to it.
Is there a specific micron filter size that is prefered when using a non-fritted buchner funnel to ensure carbon and celite do not pass thru into the filtered material?
Appreciate the insight, I will be starting to search more and see if I can find the answers that I am looking for more in-depth!
Things to look out for, be careful when it comes to adding dry ice directly to the ethanol, the CO2 can dissolve in the ethanol and leave you with a more acidic crude. this can affect the quality of your distillation.
The finest filter that I use is a whatman 4, which if I recall is somewhere around 70 microns. To filter finer things, I build a filter of DE, celite or bentonite on top of the whatman 4 filter. Mix the powder you choose (AC should not be on the bottom, choose DE, celite or bentonite) with an equal part of ethanol. Set the filter paper onto the buchner with vacuum on by wetting the paper and gently running your finger around the edges to seal any bumps. Then, keeping the powder mixture stirring, pour it into the buchner so it forms a nice layer over the bottom. Some powder will make it through, so take the same ethanol and re pour it into the buchner. keep doing this till you feel like the powder isnt coming through, normally the third time i pour it through no more powder comes out. rinse your flask so any powder in it will be removed. pour fresh ethanol into the buchner, and check for powder making it through. Once no more comes through, the filter is set and you dont have to worry about it anymore. The matrix of celite, de, or bentonite will catch all plant matter.
Try winterizing before decarbing as well. I have had decent results with just doing a -50c extraction (keeping the ethanol no warmer than -50c), but by far my best results came from winterizing crude that was likely extracted with warm ethanol (I say likely because I bought that crude already made and did not extract myself) with methanol. I’m going to try a methanol winterization with a cold extracted ethanol crude next and I’ll be sure to post my results. For details on winterizing with methanol, just type “methanol winterization” into the search bar.
In regards to winterization, if you do your extraction cold enough, you will not extract the plant fats that you are trying to remove by winterizing. (otherwise, you are going to have quite a bit of fats to crash out)
I am thinking of putting a small proposal together for the owners to have me observe any changes regarding coloration and final product outcome from even just doing a simple filtering process with the celite and AC. Im looking at one of our reaction buckets now and the ethanol is completely green.
I assume these byproducts being left inside are partially why there is this burnt sediment material that I have to filter out after our decarb?
coppertop, thank you for your input as well! We do have a winterization step with our oil, once we have removed a majority of our ethanol from the crude oil, we re-introduce a small amount just to make the product more fluid to remove easily from our 20L rotovap, then simply throw that into a container in a freezer overnight. Once this happens we filter with a buchner funnel on qualitative paper and coffee filters, but there is a TON of byproduct left over (140-200g of byproduct from 3lbs of starting material). They have mentioned to me that they lab tested this byproduct material and still had some 20-30% THCA content, which makes me wonder why we throw it away.
Once this filtration is completed it gets thru our smaller 5L rotovap to remove the remainder of the alcohol then a decarb on a hot plate.
That’s debatable. I’ll have to look for who is was that was saying this, but they claim that they’re still pulling a bunch of fats by winterizing after a cold ethanol wash. Which is why I want to see if I can reproduce his claim.
The burnt sediment is most likely water solubles, in my experience. To test, try to gather a bunch of the sediment, and then let warm water run over (you can just hold it in your hand). Most likely it will seem to “melt” away, as it dissolves into the water. It also shouldnt dissolve well in ethanol, making it much harder to clean. Bentonite will take care of this. you can simply use it in your filter. Had the same issue when I started.
I have a decarb process coming up later this week and will definitely test the theory!
I have noticed it makes the crude smell horrible, almost fishy from burning it. We usually collect it in a sieve when we are pouring our decarbed oil into a smaller beaker, so it will be easy to gather it up and check out.
Two days as a member on this forum and I am already learning more than I did in 2 months being around the crew here…
This is true, methanol is the best alcohol for winterization. I wouldnt be too surprised if you are right and there is a bit more to pull out. My lab cant use methanol though, so I only know the limits of ethanol. I frequently try winterizing after condensing the oil a bit, but i think the way I wash (cold <60C and fast 10min total contact time) avoids the majority of fats.
Grade 44: 3 ÎĽm (slow to medium filter paper)
Thin version of Grade 42 retaining very fine particles but with lower ash weight per sample and almost twice the flow rate of Grade 42. Is what I use, and like coppertop I keep everything at -50 below. Rent dry ice chest they keep it filled at a great price . I my color is always golden 45 min wash.
The previous manager had this set as a “high and fast” decarb process, near 315*C. I have had my thoughts on this, thinking it is also lending to this overly burnt aroma to the oil…
I have measured our temperatures once the Dry Ice and Ethanol are mixed together with trim, and I know it takes a few to reach cryo temps but I always hit -60…we are doing 3 washes with dry ice and ethanol.
Holy shit! Sounds like you’re degrading terpenes. That sounds similar to the smell of head fractions in distillation. Is it even under vac at that temp??
Dude, its nuts, it smells like piss when its decarbing big time. If this is what distillation smells like, Im halfway there lol. Its not under vac at all, open vessel on a hotplate until we hit ~300F on the oil and co2 generation stops.
Yea man, that’s your problem right there. At 150c it doesn’t take long at all to decarb. At those temps though you’re definitely wrecking your crude.
Fix your decarb process. If the material isnt going for distillation yet, you should decarb more in the 100C to 125C range, it will take longer, but boy, you are definitely breaking down some terps and maybe cannabinoids as well at that temperature. If you are doing it under vacuum, you can get that temp up to 150C.
Just saw you were using Fahrenheit, not as bad, but at 300F you probably want to be decarbing under vacuum. 240F is more reasonable for no vac.
Im pretty sure you mean Fahrenheit, 300 C is nearing 600F lol, your cannabinoids are gunna start boiling
I would love to try a low and slow decarb, because my god I opened a beaker last week and it smelled like used fry oil.
To clarify, the decarb that was set previously by the manager was 315C on the hotplate, and while decarbing we stir and check the temperature with a temp gun, until the oil reaches a temperature of 150C.
Keeping things consistent on temperatures, hopefully that makes sense. I havent seen any breakdown products, minimal CBN (~0.5% and not much of else).
So you would recommend a lower hotplate setting, say 125C, until the oil reaches this temperature?