From Crude to CBD Isolate

Hello!

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?

Thank you very much!

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you the man! :man_scientist:

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.

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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

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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?

In any case thanks a lot!

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.

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For final washes…Ever try a water wash and/or 80/20 methanol/h20 flush? I like it, but havent heard much from others experience…

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Thank you for the info.

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?

Thank you!

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.

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You do not need heat or pressure but you can give it a go if youd like. My suggestion would be toggling with positive pressure. This is termed as a method for forced crystallization and is used widely in chemical processing. However please be careful putting volatile solvents under positive pressure, this is also referred to dramatically as a bomb…

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This seems almost on topic: ran across the following statements that I’m hoping the brain trust here can either confirm or deny.

When using ethanol as the extraction solvent, the temperature can somewhat determine whether THC or CBD are extracted more heavily.

Supercritical CO2 is the most customizable method, allowing for individualized extraction methods. At a specific temperature and pressure—around 80°F and 1100 PSI4—CBD is the only compound that will be drawn away from the plant material by the CO2solvent.

@Jonaaronbray? @photon_noir?

Edit: on the fence about providing the attribution. pretty sure y’all can figure it out if you care.

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I don’t think the statement about ethanol is true at all. Ethanol extracts more CBD than non-polar solvents, and it is always going to prefer CBD, no matter the temperature, but it still extracts THC just fine.

CO2 is customizable, but it is always non-polar and it’s actually a rather poor solvent for cannabinoid acids in general. That temperature and pressure would extract THC and CBD based on the presence of terpenes acting as cosolvents. So that, too, is false.

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Will this process work with dewaxed crude testing above 60%, or have you found distillation to be a necessary step?

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Hey hey, I’m working with several farmers growing cbd here in western Kentucky, I am also in possession of two large stainless stills was hoping to start up a lab in the the next6 months. Can you help?

Yes, message me

Hey guys, had a small question.

From time to time when I isolate CBD from distillate, the whole solution will sugar up (pictures below).
No proper seperation. What is it due to?

Is it because the cooling is going too fast and isn’t allowing proper seperation?

!

Not fully dewaxed?

try more solvent, looks like you formed small crystals.

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I already tried adding more solvent and the same things happens. I honestly think it’s because I’m cooling it too fast.

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image

The less super saturation, the larger the crystal. Add more solvent. Don’t cool so fast if you’re worried. Take your time. Big crystals take a lil longer unless you’ve really honed your process.

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