I need some help.
Recently started making distillate. This site has been extremely helpful. So thank you everyone for contributing.
I have an issue I haven’t been able to find any solid answers to. Hoping someone has experienced this before.
I have what appears to be oil droplets/bubbles in my distillate. At first I thought they were air bubbles, but on closer examination I realized that it was oil. (Picture at bottom of post)
Now I see that all my crude from this batch of biomass, has small oil specks floating on top, and the consistency is kind of runny (this is post winterization). I speculate that the material was sprayed with some kind of vegetable or petroleum oil based pesticide. Considering the results (see pic) does this sound plausible?
I have done some searching around the forum and haven’t found any definitive answers to this problem. Here is the information I have found:
@ScoobyDoobie posted the following in
In both cases i just dissolved the extracts in hexane, chilled with dry ice and filtered the solution… Followed by brine washes. Green cleaner was harder to remove due to the goddamn sodium laureth sulfate…
Scooby also posted this
Green cleaner is primarily made up of sodium lareth sulfate and soybean oil which would be easy enough to remove it from an extract solution with the addition of potassium hydroxide to react with the soy ran oil followed by mixing with attapulgite clay for subsequent filtration.
I don’t know if I am following this correctly, but it sounds like: dissolve oleo in non polar solvent and do a brine wash with a high enough pH to saponify the vegetable/petroleum oil?
These triglycerides, we can saponify them with alkali and wash them out when doing a saline scrub, right?
@Future Nah, saponification is probably something you want to avoid, since that would cause your cannabinoids to be micelle-soluble in polar solvents like water… and conditions that caustic should be avoided for other chemical reasons.
The above leads me to believe a high pH brine wash is not the right tool for the job.
I also found these bits of gold from Photon referencing MgO in response to a question posted by Square Root:
I have not left it in for any WFE processes. It can be partitioned into water from non-polar solution of the crude, which also helps saponify and wash out vegetable oils… oops! I let another hint slip!
Understand that saponification is the creation of soap, a strong emulsifying agent, from fatty acids. That means partitioning non-polar resin solution with water can cause issues with the partition. It helps to use fairly briny salt water for the first wash or two.
Also know that the heat processing of the oleoresin causes oils to break down into smaller chains of more similar sizes. This actually could be beneficial,sincethe soaps would be more water soluble and less non-polar (cannabinoids, but not necessarily the solvent) emulsifying.
So I am starting to think: dissolve first pass in 1:1 (?) heptane add MgO (<=5mL per 1000g of oleo) to oleo/heptane solution. Mix at high temp (?) for 20 to 30 minutes. Add saturated brine solution, agitate, allow to seperate and filter. Repeat until water comes off clear. Wash with DI water to remove any remain MgO. Do I need to worry about the pH of MgO? Recover heptane. Second pass.
Edit: Maybe add the MgO dry so more heat can be applied? Then dissolve in Heptane and wash?
Any insight on either of these processes would be greatly appreciated, or just a wink and a nod if I am on the right track.