Frost bitten, ice encapsulated resin glands: rotovap lyophilization

Freezer burn had me down. I thought things might be hopeless and I’d be forced to make distillate with this flower.
Then I realized I had all of the components required to create a system capable of sublimating the ice: my rotovap, more vac, @Killa12345’s cold traps, dry ice, acetone.


Filling the bath with acetone and ice (and a dash of dry ice occasionally depending on temps) kept the ice crystalline,
Packing the traps with dry ice then filling all the way with acetone keeps them cold enough to condense.
Spin slow and maintain the freezing bath until desired dryness.
Bomb live extract still possible!

It’s also possible to shell flash freeze like this and lyophilize sensitive powders at a lab scale.

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Why is the rotovape flask brown, did you add oil too?

The flask is an amber glass

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Oh ok. Well super cool tech! Did a lot of trichomes fall off from all the agitation while frozen?

Surprisingly there wasn’t much that came off! I didn’t fully vac these down to be extremely dry; I was mainly trying to expose the goods. I think a lot would break off if it was vacuumed to the point of brittleness. Spinning at 7 rpm was pretty gentle

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What mbar did you get to when desired dry, may be good to add for parameters for others, I do see you set to 0 but it’s sitting at 237

Great idea, well done. Gonna save someone’s ass big time. Definitely tricks of the trade status

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I got to zero eventually, but the rotovap gauge only goes to zero so I also had a secondary vac gauge that got to 200 micron roughly. The minimum vac one must achieve to sublimate the water is 10 mbar when the water temp is at zero C. Lowering the bath temp further will require colder cold traps, so I was trying to sit right at freezing and maintain that temp.

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Thank you for the excellent write up!

@SidViscous has mentioned this strategy a couple or three times, but a how-to with pictures makes it way more accessible…

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The process I outlined above was a proof of concept that allowed me to purchase a used freeze dryer (lyostar) when I got the used unit it was non functioning because it did not have a correct pc and they do not sell one that is older software. The cost to refurbish was over 100k.
I decided to gut the beast and hook up my own chillers and vac. It’s working like a charm!



This thing has been pumping out kilos of freeze dried products no problem, so I scooped a second unit for 2k I’m about to demo and daisy chain the two for double throughput.

If you have a tight budget this is a viable way to get good throughput if you’ve got supporting ancillary equipment.
If you’ve got a huge budget call up Parker freeze drying and go hard!

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Great work! This looks like a fun project to work on, thanks for the nudge. Now I’m off to find me a deal!

How cold are you running the chillers and how deep of vacuum?

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Did you by anychance measure the water content on that bad boy? Before and after?

That lovely piece of amber honey in glass was made with hydrocarbons I persume?

Agreed with @Concentrated_humbold post yourself in tricks of the trade…

Would love to try that jar my friend… Looks delicious…

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This could be an option with some capacity. A door would be an easy enough fix. Note there does seem to be some damage in the picture on the right side.

Hard to want to pull the trigger on this stuff without more info.

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OH MY!! great find, thanks for sharing!

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edit:unfortunately no great deals

It was a super fun project. I have the Huber running the lower coil down to -50 C if I have an opportunity to upgrade that to -80 I will. The shelves run from -20-40C so it doubles as a vac oven for secondary drying. The vacuum I change depending on the application, I keep my ice sublimation chart handy! For flower I use as minimal as possible but for nanoemulsions or other powders I drop it as low as my coil will allow without sublimating there.

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I made that last year and it was :fire:.

I made it with pentane. Unfortunately, I didn’t measure the water but the flower seemed extremely dry and brittle after!

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That means… Under 9(000)!

Kidding my guess eith that description is under 20% w.c.

Well played sir!