Alternative to Rotovap Distillation

SnapsProvolone

SnapsProvolone

Well-Known Member
Ok, so we know that with apparatus such as a rotovap using vacuum and heat one can relatively selectively boil off terpenes, thus fractionally distilling a concentrate.

What say we flip this upside down.

We go to cryo temps of -170f, hypothetically locking up all / most compounds, then each column wash would take place at an incrementally higher temp pulling the compounds released by that temperature.

My idea, a properly sized cryo mech cold head stuck on top of a column could possibly provide this temperature regulation, perhaps two stage, one precooling the solvent, the next maintaining the column itself.

Thoughts?
 
SnapsProvolone

SnapsProvolone

Well-Known Member
For example, Limonene would predictably wash above -101f. Once the sweet spots for each terpene to be extracted is determined, its just a matter of choosing wash points based on goals...
 
Fadedawg

Fadedawg

Well-Known Member
SnapsProvolone said:
Let me guess, you're ordering one to play with or already have something performing this function?
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Giggling with glee to see your fertile mind working! One of my greatest joys is watching where synergism takes the minds of others, and the new ideas they come up with.

Alas, I wish I had unlimited time and funds to pursue everything that looks promising and exciting, but sadly in this case copied the link for further study when I have at least more time.

I am currently researching using a molecular still to separate out the oleo-resins individual components.

http://www.popeinc.com/still-products/wiped-film-stills-evaporators
 
CashCrops

CashCrops

Well-Known Member
Good stuff snaps, I for see an unlimited future of newly focused medical uses once all the red tape clears from our useless gov. I can only imagine what certain colleges have to work with in this area alone.
 
stems&seeds

stems&seeds

Active Member
How does one selectively concentrate Terpenes alone without also taking some THC, CB, etc with it? Forgive me for what seems like a stupid question. From what I understand many of the terpenes have similar if not higher boiling points than many of the active ingredients from which we are trying to seperate.
With regards to solvents such as ethanol/alcohol how would one fractionally distill and or separate these components?
Reason I ask if we've been using a rotovap, and have made many extractions but have had little luck with further separation of components as mentioned above. That said, the extractions are far more aromatic and flavorful as compared to butane. We've most lately been trying to mix "highly terpy" etoh extractions with winterized butane extractions to add terpenes to an otherwise minimally flavorful concentrate.
 
SnapsProvolone

SnapsProvolone

Well-Known Member
stems&seeds said:
How does one selectively concentrate Terpenes alone without also taking some THC, CB, etc with it? ...
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I hypothesize that each compound has a "freezing" point.

That stated, I hypothesized that selective wash temps, each sequentially warmer, can gather specific compounds in a relatively selective manner.
 
stems&seeds

stems&seeds

Active Member
While I agree that each compound has a freezing point, how can we be certain that whatever solvent we choose will not simply "wash" away everything? Meaning how can we be sure that freezing will in fact "lock" that compound within the column?
To counter what I just said. Observing the many etoh extractions we've done, it's become apparent that the colder the wash, the less terpenes it seemed to extract. By the same token, the colder the wash, the less unwanted materials are extracted as well obviously. When observing warm, or room temp extractions, we've noticed more terpenes are preserved. However more "unwanted" materials are also extracted such as chlorophyll, waxes, etc.
Point being your hypothesis may not be too far off.
In practice however wouldn't it be far easier to simply fractionally distill? This is already being done on a semi successful basis as we speak if I'm not mistaken.
 
SnapsProvolone

SnapsProvolone

Well-Known Member
stems&seeds said:
While I agree that each compound has a freezing point, how can we be certain that whatever solvent we choose will not simply "wash" away everything? Meaning how can we be sure that freezing will in fact "lock" that compound within the column?
To counter what I just said. Observing the many etoh extractions we've done, it's become apparent that the colder the wash, the less terpenes it seemed to extract. By the same token, the colder the wash, the less unwanted materials are extracted as well obviously. When observing warm, or room temp extractions, we've noticed more terpenes are preserved. However more "unwanted" materials are also extracted such as chlorophyll, waxes, etc.
Point being your hypothesis may not be too far off.
In practice however wouldn't it be far easier to simply fractionally distill? This is already being done on a semi successful basis as we speak if I'm not mistaken.
Click to expand...
I'm trying to find cold extraction "sweet spots" & "sour spots" so as to avoid heat decomposition of my terps. IMO heat need not be involved, nor decarboxylation or free radicals.
 
stems&seeds

stems&seeds

Active Member
Which is why I believe ethanol coupled with rotary evaporation can be some of the most "terpene rich" extracts I have personally come across. I have read elsewhere that ethanol as a polar solvent has the ability to extract more components than a non-polar solvent such as butane. While this is both good and bad, bad as it extracts more unwanted materials(chlorophyll, starch, etc.), however good in the fact that it can supposedly extract more terpenes. We've all collectively determined through cold extraction, we can minimize the "unwanted's."
We then can distill the ethanol solution with a rotary evaporator with little to no heat at all, instead using vacuum. Which is why I believe it is possible to make a potent extract while preserving most if not more terpenes than many other forms of extractions widely used today.
 
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stems&seeds

stems&seeds

Active Member
I'm still curious as to how exactly those are going about fractionally distilling terpenes. Maybe I'm just not understanding this concept correctly, and that's certainly a possibility! I cannot however understand how one would be able to separate the terpenes without also taking with it the active ingredients(THC, CB's, etc)
The boiling points of some terpenes fall below those of the THC, CB's, etc., while many other terpenes have boiling points that are higher. Considering the majority of terpenes have higher boiling points than those active ingredients mentioned above, how would one extract simply those terpenes without at the same time the active ingredients? Further complicating this question is how would we attain this with solvents that have a boiling point that is lower than all of the components mentioned above?
I feel there is something I am simply not grasping
 
SnapsProvolone

SnapsProvolone

Well-Known Member
The variation in boiling points allows for us to freeze up various compounds while staying just warm enough to extract a group of compounds that remain unfrozen at that temperature. Then we warm the system up a little bit and grab the next batch, and so forth. Obviously we would require the solvent have a boiling point lower than -170 or what we determine to be the ideal temp for the coldest wash.

With practice one could determine specific wash points that pull groups of desirable compounds and points where we may selectively pull undesirable compounds.
 
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