Hi guyz, we are extracting cbda and cbga from wet biomass by the bioherbolysis process, a process that uses water to extract cannabinoids , sunflower oil is then added and the acidic cannabinoids are then extracted into the sunflower oil.
From this stage, the sunflower oil with acidic cannabinoids is then mixed with alkaline water, the acidic cannabinoids are then extracted from the sunflower oil into the alkaline water. This alkaline water is then reacted with phosphoric acid stripping the acidic cannabinoids and concentrating them and we get acidic cannabinoids concentrated in the form brownish granules.
The problem now is one of our potential client is saying that our product is not clean, it has got residual acid and terpenes.
My question is, how best can we wash this product to remove residual acidity and some other impurities?
I also want to know the best method we can use to fully decarboxylate this product and then process it to clean isolates.
Well, it depends on how your facility is set up and if you are able to operate in an explosion proof environment. Pentane is great for crystallization but has a lower BP and higher vapor pressure than Hexane which is 3x more neurotoxic. I would suggest reading into some crystallization methods that are posted here publicly in order to familiarize yourself with the process and required equipment/materials.
You might take a gander at this thread where they are using Heptane:
This seems to be a solution to this problem, would you mind giving a list/sop of the whole proces that you are using so that i can apply the same. From those pictures the crude isolate is very clean.
The SOP is listed as a downloadable link in that link I posted. Download it and become VERY familiar with it before you attempt. If you aren’t using alkanes or any other explosive solvents, you better make damn sure you know what you are doing, your equipment is safe and capable (all seals alkane rated, all motors, pumps, switches, controllers rated, proper ventilation and PPE, all MSDS in hand and completely understood). Start small scale in a beaker with <1L and slowly and methodically work up to larger batch sizes. Understand that you will be working with something as energetic as gasoline. Not only will it kill you, it will hurt the entire time you and your team are dying. Understand what you are working with before getting in balls deep. Not trying to scare you as it is a fairly straightforward process if strict safety protocols are adhered to. I just don’t want to encourage you to take actions callously and you wind up getting hurt, or worse yet, someone else.
Actually, heptane is significantly more dangerous than pump gasoline.
Octane rating is a measurement of how resistant to pre-ignition (knock) a fuel is. Most pump gasses are rated at 87 to 94, with higher numbers meaning you can lean on the fuel more before it goes kaboom on its own.
Heptane is the zero point on the octane scale.
You have to try to ignite gasoline. Heptane WANTS to go kaboom.
It can be perfectly safe to work with if you take the right precautions. Ventilation to mitigate vapour pooling. Ground and bond everything you’re working with, including the staff. Anti-static clothes and lab coats. Work under inert atmospheres.
We use heptane daily in our facility, in very large quantities. We have not yet had any safety indicents with it. But we’ve been very careful and also on at least one occasion lucky.
It’s not something I would be comfortable recommending to the average person who doesn’t know what they’re doing.
Very small bench top quantities? Sure. Production? Not without a ton of safeties in place.
And safety seems to be the last thing that everyone wants to do because “it’s too expensive.”
Thanks for that. Having had my fair share of redneck fires, it truly amazed me how quick hexane went up in comparison to gasoline. I couldn’t imagine a fuge or reactor getting spicy with decent quantity.
As you and I have both stated, if this is a method that @dan1 decides to try, they should definitely work on benchtop scale for a while before deciding to fill up a reactor. If your method works in a beaker, and is repeatable, chances are it will work at larger scale providing the equipment is up to snuff. This is certainly not something that you want to throw caution in the wind.
Thank you so much for assisting me to tackle this problem. I will not definately not jump into handling those dangerous solvents as per your advice.
Here is what i intent to start working on, provided my bosses gives me the resources.
I intent to perform LLE, whereby i will dissolve my full spectrum cbda into heptane. Mix this with water in a separating funnel, shake gentley to wash impurities like Na, Phosphorous, residual acidity, heavy metals.
I will then have my clean cbda full spectrum in heptane.
But still need this to be decarboxylated to cbd. Now is it advisable to take this liquor into a rota vapour distill off heptane at the same time decarboxylating cbda.
Or i can start the crystallisation of cbda right away before decarboxylation?
You may require multiple washes to completely remove whatever compounds you’re trying to remove.
Those washes may need to be modified with various additives to adjust the pH or other parameters.
If you remove the heptane in a roto you will have minimal to no decarb happen by the time it’s done as alkanes are not (significant) decarb catalysts.
So if you want to decarb, which is necessary for crystallization, you’ll need to either do it under pressure so you don’t boil off the heptane, or boil off the heptane, decarb, then re-introduce heptane for crystallization.
If be shocked if the resulting post-decarb crude crystallized nicely with acceptable yield. I’d imagine that depending on what other crap is in there, you’ll need to apply at least one or two other processing steps to get to a product that you’re happy with.
Once you do get to a crystallizable crude, you need to work out your crystallization parameters.
This is a very deep rabbit hole. Good luck.
Don’t be discouraged if you spend a month working on this and still don’t have acceptable product at the end of it.
Zimbabwe is a bit out of reach at the moment but send me a phone number and I think that we can sort this quick with some video calls if possible
Are you able to buy reagents ( locally or order internationally?
I can send you some but that will only be enough for proof of concept
Thank you so much Lincoln20XX, have seen that set up on a certain Thread here. I think i can apply this setup after washing the product, for the next stage of decarboxylation. Is it so.
but send me a phone number and I think that we can sort this quick with some video calls if possible