Short Path Distillation

[Thomas@LRL]

We notice that the slower we increase the temp as we go, the lighter it is, batch sizes ranging from -500-900 grams.

Starting the mantle at 150c and then waiting until the reagent temp comes within 30c and then raise the mantle 10 degrees c through our run. PID controllers coming in a few weeks.

Do you stop to swap the contaminated glassware between 180 and 200c?

 

[flatslabs]

Is anyone noticing that small batch-feed sizes come out lighter, more pure, or less stinky than large ones?

Are you using a different sized kit for different sized batches, maybe getting better vac on the smaller kit?

 

[dj digigrow]

Bump*

Bump*

Boat loads of info on here.
Whats the best complete kit currently out at the moment for < $5K?
Or am i better off just piecing together my own?
Im gonna start from page one again and re-read lol..
Thanks guys. (I was gone from this site for years , should've never left for so long)

 

[Goldleaflabs]

Boat loads of info on here.
Whats the best complete kit currently out at the moment for < $5K?
Or am i better off just piecing together my own?
Im gonna start from page one again and re-read lol..
Thanks guys. (I was gone from this site for years , should've never left for so long)

go to the website and tell them you're from IGMAG. They got complete kits for good prices, fully supported, and will give a discount for ICMAG members

 

[EugeneOregon]

Hey guys,
I am looking to set up a short path distillation unit in my lab and I am unsure where to start. I don't want to purchase anything like the Kugelrhor or any other system, simply because I am unsure if the application is even worth pursuing. I currently have a Buchi rotary vap and a lot of various glassware and equipment, and hoping I can fab something for testing purposes. If you guys have any information on how to do this it is greatly appreciated, or if I'm a fool for not just purchasing the equipment let me know.

Thanks,
Sym

You don't need the kugelrohr oven, just the bulbs and a heating mantle.

https://www.youtube.com/watch?v=rD5tIdnDNl0

 

[davorint]

Hey EG, I am very interested about your setup, specifically the vacuum and pump connections, but all your vidz are down. Could you please upload them again?
Thanks in advance!

 

[BlackestofOps]

Yes, I am having the exact same problem. The heart tests out at 40% D9THC, with a large spike of some unknown chemical that elutes at the same time as CBC would, but it is not CBC. I am not using excessive heat, my boiling flask stays under 205C, and my vacuum level is below 0.01 mTorr. The tails are high in CBN, up to 5%. My input oil is between 60-70% D9THC and around 10% THCA.
I have had this occur in several batches now, all from the same grow site. I am starting to think it is some peculiarity with their grow regimen.

 

[mobin]

Yes, I am having the exact same problem. The heart tests out at 40% D9THC, with a large spike of some unknown chemical that elutes at the same time as CBC would, but it is not CBC. I am not using excessive heat, my boiling flask stays under 205C, and my vacuum level is below 0.01 mTorr. The tails are high in CBN, up to 5%. My input oil is between 60-70% D9THC and around 10% THCA.
I have had this occur in several batches now, all from the same grow site. I am starting to think it is some peculiarity with their grow regimen.

do your runs take a long time? esterfication/isomerization suspect. you have any sorbants in the boiling flask? too low of pH can ester-fy thc so anything acidic being played with in the workup? your vac level is suspiciously low, i take it thats at the pump inlet not at the reaction site. when cfm capeable pumps pull right through leaks you can get fun shit like this too.

 

[BlackestofOps]

do your runs take a long time? esterfication/isomerization suspect. you have any sorbants in the boiling flask? too low of pH can soaponify thc so anything acidic being played with in the workup? your vac level is suspiciously low, i take it thats at the pump inlet not at the reaction site. when cfm capeable pumps pull right through leaks you can get fun shit like this too.

My runs do take a long time. My production rate has been between 120 and 250 ml/hr when in the cannabinoid fraction. No sorbants in the boiling flask or used at all in the pre-process. The vac level is measured nearer the pump than the boiling flask, yes.

I don't think it is a vac leak, however. I re-distilled the 40% THC run, and no further degradation of THC occurred. To me, this seems like a possible pH issue or a heat driven reaction with another chemical that is present in the winterized oil. The decay in the first run would max out when the reactive compound is exhausted, and no further degradation would occur on subsequent re-distillations. Just my working theory for now. I am awaiting some supplies to pH test my winterized oil.

 

[G.O. Joe]

I have had this occur in several batches now, all from the same grow site. I am starting to think it is some peculiarity with their grow regimen.

Any sulfur for instance that makes it that far does bad things on heating. There is dihydrocannabinol in between THC and CBN, CBC from CBG and so on. GC/MS would be helpful but the big question is what is the other 20-30% and what in that is unusual.

 

[BlackestofOps]

Any sulfur for instance that makes it that far does bad things on heating. There is dihydrocannabinol in between THC and CBN, CBC from CBG and so on. GC/MS would be helpful but the big question is what is the other 20-30% and what in that is unusual.

Joe, very insightful, thanks. The grow is using sulfur in the veg phase as a spray on insecticide. Do you have more information on the interaction of sulfur and THCD9? I think you may be on to something. Although, the raw co2 extract and the winterized oil does not have a sulfur odor, something I've encountered processing 3rd party trim.

 

[G.O. Joe]

Elemental S is usually used for PM. How much is picked up depends on the solvent and temperature. If S is heated at 200-250 C with any high boiling organic that has hydrogen S can remove, H2S will form and for instance refluxing any of the isomeric THC's with enough S will give good yields of CBN. So, CBD can also be converted to CBN, after isomerization with acid. Once the S is gone though that's it. A little metal perhaps or strong acid on the other hand might do a lot of damage catalytically. Also, things like terpenes can become oxidized and then act as oxidants.

 

[BlackestofOps]

Elemental S is usually used for PM. How much is picked up depends on the solvent and temperature. If S is heated at 200-250 C with any high boiling organic that has hydrogen S can remove, H2S will form and for instance refluxing any of the isomeric THC's with enough S will give good yields of CBN. So, CBD can also be converted to CBN, after isomerization with acid. Once the S is gone though that's it. A little metal perhaps or strong acid on the other hand might do a lot of damage catalytically. Also, things like terpenes can become oxidized and then act as oxidants.

I can't wait to distill another batch, now. I went ahead and threw some pure copper into a 10:1 EtOH oil mix, and sure enough, the copper reacted blue. We have had up to 5% CBN in our distillation results, and D9THC as low as 40%. But when I redistilled, the THC would remain constant at 40%, which jives nicely with your theory of the free S being used up, and no further isomerization occurring. I am also awaiting pH test results to chase down that possibility.

Thanks for the great tip. I'll keep this thread updated when I am able to run the process again and get results back.

 

[technoforcesolu]

Thin Film Technology – Short Path Distillation
Short Path Distillation is a technique which involves distillate travelling a short distance done at a reduced pressure. Distillation means distillate from one glass bulb to another without need for separating two chambers. Short path evaporation complements thin film evaporation technology, allowing greater capability to provide right solution for separation problems.
The Technoforce thin film short path distillation system is bench scale system and designed for distillation of thermally sensitive products under vacuum system. This technique is excellent for heat processing and high boiling products. This can be used for compounds which are unstable at high temperature or to purify small amounts of compound.

The short path distillation system consists of cylindrical body, double mantled and filled with heating medium and condenser inside. Product is being spread through the thin film inner surface of evaporator by rotating wiper elements in glass. These wipers are processed to inner wall by centrifugal forces where they produce a thin film with distribution of liquid film. That condenser is arranged in center of glass of evaporator and cooled by a cooling thermostat.
Short path distillation is suited for evaporation, concentration and stripping of heat sensitive products as:
• Stripping of monomers from silicon oils and polymers
• Evaporation of oil and wax fractions
• Fractionating of waxes into hard and super hard waxes
• Stripping solvents and dimmers from resins
• Distillation of monoglycerides from triglycerides
• Evaporation of methylester
With more than 28 years of experience in the field of integrated manufacturing facility. Technoforce develops and designs carries out basic and detail engineering, distributes and carries out the maintenance for distillers under vacuum. We also carry out distillation tests with clients to obtain reliable data which to design or construct specific distiller for client’s applications.

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[G.O. Joe]

Someone else uses the term SPD to refer to perhaps mythical SPD gear, instead of ordinary glassware! If only unerased Indian spam could also refer to THCA in the face of the THCa sadness. Maybe it's India that wins Trump's trade war with China, but has anyone ever heard of these technoforce people?

I'll keep this thread updated when I am able to run the process again and get results back.

*tapping foot arms folded*

Yes dissolved sulfur is a bit reactive so there are several possibilities. Chromatography might be spiffiest.

Has distilling after a good cleaning taken CBG to CBC, and THC to CBN with mystery peaks (that I suspect are di- or hexahydrocannabinols, not THC isomers)? You know the old crap in crap out. Does yield increase if extract is cleaned to relatively pure cannabinoid acids before heating?