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Expansion of THP Method for Extraction

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amor_fati

amor_fati

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SWIM got to thinking lately about how he hates to manually filter or decant anything and about how handy the THP method is for foregoing this. SWIM also has some MHRB powder on hand and was considering using a combination of drytek extraction and THP methods to extract from it.

Due to the use of acetone, he'd have to construct the percolator from HDPE or aluminum, and he just so happened to have an HDPE vinegar bottle handy. Something along the lines of this:

hdpe_32oz_caraffe_28-400_28-410%202008-08-15.jpg


SWIM's quite certain that the acetone won't melt this plastic, as he's tested it and knows acetone is often sold in HDPE bottles.

SWIM's proposal is to:
-load the MHRB material on top of the cotton rag stuck in the neck (with the bottle upside down)
-place a second cloth on top of the material to keep it from floating up
-pour acetone through the percolator and collect in a jar for disposal in order to defat the material
-after the defat, remove the top cloth and mix in sodium carbonate
-slowly add water to the material to moisten it while lightly stirring to ensure total moisturization
-allow to react for about one hour
-mix in anhydrous magnesium sulfate to chemically dry the material while stirring to ensure total dryness
-replace the top rag
-pour fresh acetone through the percolator and collect in a jar
-precipitate product out of the collected solvent by FASA method

SWIM would use the bottom that he cut off the bottle to protect the acetone from evaporating or collecting ambient moisture.

It's quite likely that considering the success he's had and seen reported with maximized dissolution of product by THP, that this method will turn out more effective than methods requiring decanting and filtering.

Some sort of a plunger could even be implemented within this to force more solvent out of the cloth filters, like an aeropress.
 
i dont think you need to do the defat on this...the FASA will take care of that...just freebase and then run it through the THP..collect acetone and add FASA

since FASA is basically a defatting step
 
SWIM's acetone comes in hdpe, so yes that should be fine

btw, is there any way to skip the magnesium sulfate part? SWIM can only find it in 20% solution, small bottles and very expensive.. could sun dry or fan dry or something of the kind work? supposedly it becomes a paste, so could SWIM do that in a glass baking dish and leave it drying? How much would a little water interfere with the end result?
 
endlessness said:
[snip...]

btw, is there any way to skip the magnesium sulfate part? SWIM can only find it in 20% solution, small bottles and very expensive.. could sun dry or fan dry or something of the kind work? supposedly it becomes a paste, so could SWIM do that in a glass baking dish and leave it drying? How much would a little water interfere with the end result?
Click to expand...

SWIM found solid magnesium sulph(/f)ate crystals in a garden store. It was very cheap but would require recrystallisation to remove the bits of grit:x . After crystallising from solution, cover the pyrex dish with foil and roast in an oven, preferably electric rather than gas, at 220degC for about 4-6 hours depending how much you have in the dish. A thin layer works better. Thick layers tend to turn into a big hard crust of a lump.
 
Some observations thus far:
-The amount of filtering material and acetone used should be in proper proportion to the amount of plant material, otherwise it will require an impractical amount of acetone.
-No defatting needs to be performed, as the solvent will come out murky after basification anyway.
-Basification and drying of material should occur in a separate container, the material should be scooped into the percolator, any remaining material should be washed acetone, and that acetone should be poured through the percolator.

SWIM used a very small amount of material and possibly neglected to let the plant material soak and basify for long enough. The yield after FASA was quite brown and unlike fumarates he's precipitated out of xylene and toulene. However, SWIM is going to basify the material to determine the outcome. Next time, he will heed the observations stated above.

If performed in a practical manner, this method should work for any drytek extraction to include extraction from Trichocereus and Anadenanthera.
 
Problems encountered:
-Material solidifies, causing the acetone to seep around it rather than through it.
-Some solvent remains in the cloth filter.

Proposed solutions:
-DO NOT PACK the material into THP.
-Use a size of bottle that allows for the material to remain unpacked (SWIM used a small vinegar bottle).
-or use a material that may not solidify so much when dried (perhaps foliage, rather than bark).

SWIM's product seems to be retrievable, as he seems to have the expected yeild in a fumarate form. He will basify to confirm.
 
this is really good idea with the cebil seeds...may save a lot of time...and with better yields..SWIM may try this on some chaliponga sometime
 
Eh, too many false positives to tell. SWIM's methods of experimentation require some refinement. SWIM isn't too hopeful for using this method with MHRB, but he did at least find a more efficient filtration method (bottle as the funnel, cloth as the filter). It seemed to work well for alcohol extractions of trichocereus, however, so maybe it's just an issue of the consistency of the material. Anyway SWIM's still hopeful but isn't holding out for MHRB. However, cebil, trichocereus, and possibly chaliponga still look promising.
 
sure they do...after you extract with acidic water solution...freebase the water..pull with a solvent..and drop out with FASA
 
True, SWIM misspoke, but he doesn't happen to be using any NPS and feels separatory methods require an unnecessary amount of materials, equipment and work. SWIM's in the process of phasing such equipment and has already phased such materials out of his kit. He's focusing on helping develop dry-techniques, rather than reverting back to separatory techniques.

But yes, if one is inclined to using aqueous extractions, THP is actually made for such extractions, and as long as SWIY can get the product out of aqueous and into an NPS, FASA can almost always be used. SWIM was considering using it for syrian-rue as the first step of obtaining either freebase harmaloids or synthesizing THH.
 
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