So, as I have mentioned before, I’m in a non-legal state…but hemp legislation just passed. Yay.
I’m interested in EtOH extraction, to be followed by cold-temperature EtOH winterization. We’ll call this semi-refined crude.
Now, what are my next steps to get to pure CBD crystal isolate?
Do I remove all solvent and then short path?
What do I do between crude extract and CBD crystal? Is it near-identical to THC-A crystal mining or is there another component that I’m totally missing?
Help, additional questions, general direction all appreciated.
I am also interested in this process. I have read that it could be possible using d-limonene. Also curious about the possible use of isopropanol due to it being fairly non-polar.
I recently had a minion accidentally crystallize a kg or so of CBD at about 60% purity out of ethanol. without winterization.
If she had done a de-colour beforehand, and/or extracted 30C colder, we might have had a suitable substrate for recrystallization out of ethanol.
I can’t see any good way of getting from the chunks in green/black slime in the jar to finely divided white crystals without using an alkane, and saline washes, but it does seem like there is a route to clean isolate that doesn’t require distillation.
I am also curious if anyone has any info about making the crystals for what a lot of places are calling terpsolate, as well as how/when they reintroduce the terps and at what percent. Also I’d like to know what the difference is in making the powder isolate vs the crystals/isolate are they just very finely ground after the crystals have formed or is this another process.
My home state just passed Hemp legalization too I think they’re the 39th state to do so! They are awaiting the rules from the dept. of ag to be put out so hopefully next year can be utilized. If so I’d love to start a lab down there, land/housing is so cheap. Life would be good.
Do you have any advice on seperation of CDB from THCA in crude? I am interested in trying to make some CBD isolate but do not have access to high CBD hemp and hence will have to remove other canabinoids. My thoughts are to remove as many contaminents as possible from canabinoids through winterisations and then distill to seperate.
First thing, CBD crystallizes much more readily than CBDa. I’ve
had the best consistent results crystallizing with distilled material testing at least 60% CBD.
Measure distillate weight
Heat distillate to within 5-10c of solvent (Pentane preferably)(36c)
Measure out half the weight of the distillate in solvent (1g pentane : 2g distillate)
Heat solvent to within 5c of BP (ideally in glass reactor w/ reflux attachment)
Combine distillate and solvent, fully mix (supersaturation)
Cool to room temp
Cool to 0c (precipitation)
When happy with crystallization pour off liquid
Use 0c solvent to wash crystals to purity over filter paper
I was curious about CBD crystallization, especially about the difference between powder isolate and crystals/isolate (just like @Griffin.Labs was) and was wondering if it would be possible to talk more about it?
Powder will be more quickly formed crystals in general. Would be probable they could be forced to crystallize for timesake or efficiency. Crystals or shards are usually grown. Controlling the cooling process more slowly will allow more pure, larger crystals/shards while the powder many times is formed from a quicker method of precipitation.
if you follow the procedure I outlined you will most likely achieve a chunky powder. Be sure to smash it to a smooth powder for proper drying.
If you wish to grow larger crystals, take some of this powder and reintroduce a little in between step 6 and 7, and like @QGA said, slow down the cooling process (up to several weeks) to 0c
So what is different for precipitation? If larger crystals need more time and a slower cooling process, then precipitation requires less time and an extremely fast cooling process?
Both processes can be referred to as precipitation. Rate at which it occurs effects granularity. Check out the THCA ppt thread to find explanations from multiple perspectives at a variety of levels.
When you say slow down the cooling process, do you mean gradually decreasing the temperature day by day
(ex: start at room temp and decrease the temperature by 1c everyday until reaching 0c?).
I’m just really intrigued by the powder.
I’ve been able to grow crystals by mixing distillate with a mixture of Hexane+Ethyl acetate, then passing through columns. I then rotovap what comes out and mix it with cold pentane and put it in the freezer.
Any thought on this process?
But I’m really intrigued by the powder and quicker form of precipitation. Should there be heat and pressure applied to force the CBD to precipitate quicker, and in smaller particles?
No because that solution has valuable cannabinoids and I do not want to take the time nor effort to remove methanol/water mix from that mother liquor. Cold hydrocarbon solvent works wonderfully and can wash many many times without any loss of cbd crystal.
