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Short Path Distillation

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
 

Gray Wolf

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The Bucci rotary union and joints are unlikely to hold low enough vacuum levels to be a roaring success short path distilling cannabis oleoresin.
 
Thank you for the response Gray Wolf. Do you have any advise on a pre-fab'd unit that I can purchase that will be able to do the task? I can't seem to find any other info on setting up my own unit, and I'm not keen on trying to "wing it".
 

Gray Wolf

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An Aldrich Krugelrohr is the cheaper way to do it.

Molecular stills like the Meyers or Pope are higher volume and more expensive.
 

HG23

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Hey GW,

Speaking of the Keugelrohr, did you guys get a chance to hijack the heating element controls in yours?
 

Gray Wolf

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Hey GW,

Speaking of the Keugelrohr, did you guys get a chance to hijack the heating element controls in yours?

No reply from the factory yet and once we got a gauge on the system we realized that we had a vacuum leak in the pumping system.

After repairs, Joe was able to distill Clear at least 10 degrees below the 220C limit.
 

Gray Wolf

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A6 Grower

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Thin film short path fractional distillation works better than a simple boiling flask.

Yes but simple boiling flasks with a heating mantle and stirrer is almost as good and only costs ~$1000.... Thin film is like buying a small piece of property(25k and up). I have a few quotes for systems. Probably going with the centrifugal myers instead of the pope look alikes. But that for when processing volume is needed. Unless your processing more than 100g a day a simple boiling flask setup or two is just fine.

Key with this setup is keeping the whole top condenser warm, i find 110F or more is good and keeps things moving towards the receiving flask. The receiving flask is in DI/ISO. Also just ordered some 2 neck flasks and am going to start only pulling a vacuum on my receiving flask instead of the whole cow. Hopefully that way any vapors condense on the flask before getting sucked out by the vacuum... still need a cold trap on it lol, my poor vacuum...
 
A6 what is your reasoning for Meyer over Pope? Do you have some technical experience that has swayed your decision in one direction or another? We recently spoke with both of them as well. Both parties were clearly confident that they could produce a solid product.

GW do have an opinion about which design is more suited for producing high quality distillate?
 

G.O. Joe

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Both parties were clearly confident that they could produce a solid product.

How much product? Do they think a nitrogen-agitated multi-tap contraption with significant output could get welded together for less, with the savings going towards vacuum upgrades?
 

Permacultuure

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A6 what is your reasoning for Meyer over Pope? Do you have some technical experience that has swayed your decision in one direction or another? We recently spoke with both of them as well. Both parties were clearly confident that they could produce a solid product.

GW do have an opinion about which design is more suited for producing high quality distillate?

I think it plays into how far you want to go. Just make clear? or do molecular distillations of each compound, many of which we don't know much about.

On another note, we've noticed that near every pesticide, myclobutanil being the most prevalent, carries over with the cannabinoids during distillation. Most of these distillation process are not only purifying cannabinoids but increasing pesticide potency as well.

More often than not a mass produced "clear" has tested positive for pesticides when taken randomly off the shelf. This is a serious issue that needs to be addressed and discussed. CLEAR DOES NOT MEAN CLEAN
 

Gray Wolf

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A6 what is your reasoning for Meyer over Pope? Do you have some technical experience that has swayed your decision in one direction or another? We recently spoke with both of them as well. Both parties were clearly confident that they could produce a solid product.

GW do have an opinion about which design is more suited for producing high quality distillate?

I haven't used either one, but I know Lebermuth, one of the worlds largest essential oil suppliers, uses the Meyer's system for molecular distillation of their essential oils. That is who turned me on to them back when.

Meyers produces a thin film using a spinning disc, while Pope uses a wiped thin film. They make from small lab models, to things the size of a house for the food industry.

To A-6's point, Eden Labs produces one made from a large glass globe with a spinning magnetic stir bar to produce a thin film. It started out as an alcohol reclaim device and was expanded using higher vacuum. (Picture attached)

I haven't seen a comparison of the three's speed and efficiency in our application.

All are simple processes, albeit handsomely priced, so we are investigating building our own continuous process system, with the money it cost for the existing offerings. More if we come up with tangible results..........
 

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How much product? Do they think a nitrogen-agitated multi-tap contraption with significant output could get welded together for less, with the savings going towards vacuum upgrades?

I cant speak on a nitrogen agitated contraption but they both claim around 1000 mL per hr throughput depending on your feed time. The crux being the faster feed times equate to a less pristine product. So for the comparable bench top models I don’t think throughput is a distinguishing factor. They are both clearly above any of the other methods in speed already.

I agree with a6 bc a centrifuge seems to have more potential. Being that it can separate by weight more accurately.

What makes you say that? Being that they both only use “one theoretical plate” as it was, they are not very good at separating compounds less than ten degrees in separation of BP as per the reps. However, if you have personal experience that places one over the other I would appreciate the input, I certainly do not.

I think it plays into how far you want to go. Just make clear? or do molecular distillations of each compound, many of which we don't know much about.

On another note, we've noticed that near every pesticide, myclobutanil being the most prevalent, carries over with the cannabinoids during distillation. Most of these distillation process are not only purifying cannabinoids but increasing pesticide potency as well.

More often than not a mass produced "clear" has tested positive for pesticides when taken randomly off the shelf. This is a serious issue that needs to be addressed and discussed. CLEAR DOES NOT MEAN CLEAN

Even if pesticides are moved over, and they clearly can be, they are only what was already in the oil going into the machine so I don’t see this as a knock on distillation. They quantity of pesticide is not changing by turning it into distillate. It may be more concentrated due to less other stuff to dilute it but the overall quantity present in the oil is unchanged. So if there is a pesticide problem is needs to be addressed in the original extraction or the plants that are being grown. Not to say I don’t agree with you that these testing results don’t need to be addressed but it does not have play in the validity of molecular distillation as a process in my opinion either. We are only interested in producing clean products for our consumers so if the pesticide issue has to be handled further up the chain it will be.

I haven't used either one, but I know Lebermuth, one of the worlds largest essential oil suppliers, uses the Meyer's system for molecular distillation of their essential oils. That is who turned me on to them back when.

Meyers produces a thin film using a spinning disc, while Pope uses a wiped thin film. They make from small lab models, to things the size of a house for the food industry.

To A-6's point, Eden Labs produces one made from a large glass globe with a spinning magnetic stir bar to produce a thin film. It started out as an alcohol reclaim device and was expanded using higher vacuum. (Picture attached)

I haven't seen a comparison of the three's speed and efficiency in our application.

All are simple processes, albeit handsomely priced, so we are investigating building our own continuous process system, with the money it cost for the existing offerings. More if we come up with tangible results..........

If that happens I am always eager to listen to any advices GW. I would say that while the theory is the same, after looking at the specs and speaking with reps from these companies Eden labs machine seems crude by comparison. I assume that by continuous process system you mean a machine that is using a feed rate to keep constant amounts of homogenous starting material in contact with the distillation apparatus of your choosing? Obviously the Eden doesn’t fall into this category by design.
 

Gray Wolf

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Even if pesticides are moved over, and they clearly can be, they are only what was already in the oil going into the machine so I don’t see this as a knock on distillation.

If that happens I am always eager to listen to any advices GW. I would say that while the theory is the same, after looking at the specs and speaking with reps from these companies Eden labs machine seems crude by comparison. I assume that by continuous process system you mean a machine that is using a feed rate to keep constant amounts of homogenous starting material in contact with the distillation apparatus of your choosing? Obviously the Eden doesn’t fall into this category by design.

Pesticide contamination was recently shown by the Oregonian investigation to be a major issue, so not to be taken lightly, as we do concentrate those residues as well.

Tis true that it isn't caused by distillation but never the less one of the land mines we distillers have to contend with.

Getting it out is far more difficult, if even possible in all cases, than using material without pesticide residue as feed stock.

Please definitely put/keep this on your radar, due to the magnitude the problem was shown to be locally.

Yes continuous feed as opposed to processing a discreet batch at a time. Something for the big boys that don't care if the strains get mixed, or have so much of one strain that the point is moot.

Yeah, Eden didn't even design it as a molecular still, but an alcohol recovery still.

After playing with it at high vacuum levels, they discovered that it will also fractionate at least closely enough to separate the mono and sesquiterpenes from the diterpene cannabinoids, and the longer chain molecules like the chlorophyll, anthro cyanins, and plant waxes.

Fritz says it is successful enough that they may offer it in stainless, instead of glass.
 
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