• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Extracting acacia using entirely local materials (just rainwater, bark ashes, limes)

Migrated topic.
Stochastic

Stochastic

Esteemed member
I've recently been thinking again of water-only extractions using 100% locally harvested materials (i.e. rainwater, ashes, and limes).

The main component of an acacia bark brew is tannins, which can supposedly constitute up to 40% of the dry weight of the bark. You can confirm this by tasting a bark brew, which will dry your mouth and close your throat immediately.

Aside from that, the brew would contain alkaloids, minerals, carbohydrates, phenolics (mainly proanthocyanidins), and trace amounts of protein.

Of these, the carbohydrates are neutral, the phenolics are weakly acidic, and the proteins could be variable.

Here's my thought:

1. brew the bark. This will make an acidic solution, perhaps around pH 4-5.
2. add ashes (from burning the bark). This will add raise the pH and add a lot of calcium.
3. filter out the precipitate, which will consist almost entirely of calcium tannate and freebase alkaloids.
4. add acid (lime juice) to dissolve the freebase alkaloids. The highly stable and insoluble calcium tannate crystals would not re-dissolve.
5. filter out the calcium tannate
6. basify the solution with more ashes
7. filter out the freebase

Any reasons why this might not work? Anyone tried something like this?
 
A couple more thoughts & questions:
multiple short boils would seem likely to extract more alkaloid and fewer tannins, which have a much higher molecular weight and are probably bound more tightly in the plant matrix.
& I've used CaOH boil to rapidly precipitate tannins in acorns, but not in this kind of process. Does anyone have experience precipitating tannins?

Would love to hear from anyone on why this wouldn't (or would) work. I haven't read of this kind of extraction being attempted, but if it works it would seem to be a game-changer.
 
I like your idea. I have a an acacia madenii tree. Acacia Madenii isn't native where I live yet perhaps one day I might use your inspiration to do something like you describe with it and what my land give me.
 
Cool idea Stochastic.. I've been trying to come up with something similar. You can also make your own lye out of ash easily... I have been making lye out of the ash of Acacia Decurrens and various Eucalypts and it works very well.

If you were able to distill you could also use something like eucalyptus or tea tree oil as a carrier for FB alkaloids I suspect.. although it would probably be wrought with "impurities". Would you consider ethanol if you made it yourself? Its very useful :)

You could also use vinegar in place of lime juice.. apple cider vinegar is really effective for extraction and you can easily make it from apples... chop apples.. store in a sterilized jar and cover with water. Leave for several weeks.. Filter solids. keep liquid. Boom.

I guess the question here is.. at what point does something cross the threshold and cease being "natural"

Limonene oil can also be easily extracted from orange peels if you have a good amount.. food for thought (literally).. all these things are also easily available but I feel you on the DIY thing. Hardware stores may not be around forever :)

I will come back to this .. I must go for now though
 
Well, here's another thread that I missed while away during the summer! These kinds of ideas are aligned exactly with the things I've been learning for practically my whole life. Your scheme more or less follows in the footsteps of some of the alchemists.

What local materials do you have? How far are you willing to travel in order to gather them? What will you permit as a source of heat? Do you intend to do it all yourself - making charcoal, burning lime from limestone or shells, preparing acids and solvents of various kinds, making apparatus out of earthenware or glass - I could go on and on but the list generally makes me a tiny bit more happy, as a somewhat lazy and unmotivated person, that we live in a technologically advanced civilisation 😁

I think the best method of removing tannins is to extract the plant material with hot 40% ethanol - export strength vodka - at 60°C and then precipitate as calcium tannate with Ca(OH)₂. The alkaloids should remain in solution in the alcohol.

There's a bit of a knack to adding the lime at the correct rate but if you get that right it precipitates quite cleanly and can be decanted and filtered easily. Adding an excess of lime should be avoided, and it's also easier to add the lime as a slurry made with a little more of the vodka.

I'm also not entirely sure whether the acacia tannins are wholly precipitated by this method - different kinds of tannin exist - so a I'd be grateful for a definitive practical confirmation. In that respect, I can confirm that it works for acorns.

That may have been the easy bit of the process though, since you still need to recover them from a fairly dilute solution in a mixed aqueous solvent. Both distillation and chromatography might prove rather tedious, so this set me thinking - what about using a solid, acidic adsorbent? I can't guarantee that you'd be able to source the exact material locally, but something like the clinoptilolite that THanoC used for their recent CBD conversion seems like it might fit the bill. This particular zeolite is known for its ability to absorb ammonia, so perhaps it might work for amines too? The amines should - with any luck - be recoverable with an acid wash, and both of these processes could be expedited by having the adsorbent in a column (so much for avoiding chromatography, eh? :lol: )

Once you've evaporated the acid washings (yes, use a volatile acid that evaporates cleanly!) it should be a simple matter of making a paste with a base - lye ash or lime - and pulling the freebase alkaloids with a little alcohol or acetone. And yes, you can make your own acetone relatively easily from local materials. Dry distillation of calcium acetate is the classic method.

Hope this all helps, I'm looking forward to hearing of people's efforts, and of course I'm more than happy to discuss troubleshooting, method development and further technical matters.
 
Thanks heaps for that info downwardsfromzero .. i hope soon to try something like this

Also, i missed in the OP the part about the materials being local .. so i guess that rules out oranges and apples as allies depending on your location
 
acacian said:
Cool idea Stochastic.. I've been trying to come up with something similar. You can also make your own lye out of ash easily... I have been making lye out of the ash of Acacia Decurrens and various Eucalypts and it works very well.

If you were able to distill you could also use something like eucalyptus or tea tree oil as a carrier for FB alkaloids I suspect.. although it would probably be wrought with "impurities". Would you consider ethanol if you made it yourself? Its very useful :)

You could also use vinegar in place of lime juice.. apple cider vinegar is really effective for extraction and you can easily make it from apples... chop apples.. store in a sterilized jar and cover with water. Leave for several weeks.. Filter solids. keep liquid. Boom.

I guess the question here is.. at what point does something cross the threshold and cease being "natural"

Limonene oil can also be easily extracted from orange peels if you have a good amount.. food for thought (literally).. all these things are also easily available but I feel you on the DIY thing. Hardware stores may not be around forever :)

I will come back to this .. I must go for now though
Click to expand...

In the tropics, citrus is much more common than apples. If I was going to distill a solvent, I'd soak orange peels in ashes to pre-treat them and then distill the limonene. Oranges are the best source of limonene, and when pre-treated by soaking in K2CO3, they give up to 6% limonene at 99% purity. But I'm curious to try without any nonpolar solvent.

"conventional" extractions are perfect, everything is perfect - and, there's another layer of perfection in doing an extraction as gently and minimally as possible, where all of the materials have been personally procured and prepared. That's my interest.
 
downwardsfromzero said:
Well, here's another thread that I missed while away during the summer! These kinds of ideas are aligned exactly with the things I've been learning for practically my whole life. Your scheme more or less follows in the footsteps of some of the alchemists.

What local materials do you have? How far are you willing to travel in order to gather them? What will you permit as a source of heat? Do you intend to do it all yourself - making charcoal, burning lime from limestone or shells, preparing acids and solvents of various kinds, making apparatus out of earthenware or glass - I could go on and on but the list generally makes me a tiny bit more happy, as a somewhat lazy and unmotivated person, that we live in a technologically advanced civilisation 😁

I think the best method of removing tannins is to extract the plant material with hot 40% ethanol - export strength vodka - at 60°C and then precipitate as calcium tannate with Ca(OH)₂. The alkaloids should remain in solution in the alcohol.

There's a bit of a knack to adding the lime at the correct rate but if you get that right it precipitates quite cleanly and can be decanted and filtered easily. Adding an excess of lime should be avoided, and it's also easier to add the lime as a slurry made with a little more of the vodka.

I'm also not entirely sure whether the acacia tannins are wholly precipitated by this method - different kinds of tannin exist - so a I'd be grateful for a definitive practical confirmation. In that respect, I can confirm that it works for acorns.

That may have been the easy bit of the process though, since you still need to recover them from a fairly dilute solution in a mixed aqueous solvent. Both distillation and chromatography might prove rather tedious, so this set me thinking - what about using a solid, acidic adsorbent? I can't guarantee that you'd be able to source the exact material locally, but something like the clinoptilolite that THanoC used for their recent CBD conversion seems like it might fit the bill. This particular zeolite is known for its ability to absorb ammonia, so perhaps it might work for amines too? The amines should - with any luck - be recoverable with an acid wash, and both of these processes could be expedited by having the adsorbent in a column (so much for avoiding chromatography, eh? :lol: )

Once you've evaporated the acid washings (yes, use a volatile acid that evaporates cleanly!) it should be a simple matter of making a paste with a base - lye ash or lime - and pulling the freebase alkaloids with a little alcohol or acetone. And yes, you can make your own acetone relatively easily from local materials. Dry distillation of calcium acetate is the classic method.

Hope this all helps, I'm looking forward to hearing of people's efforts, and of course I'm more than happy to discuss troubleshooting, method development and further technical matters.
Click to expand...

Thank you, I appreciate your insights and time.

I'm open to using a steel pot, but if I can find a bottle gourd grown nearby I'd use that as a vessel and drop in hot stones to boil. I'd also be open to using filter paper until/unless I figure out a suitable alternative I can produce. While it'd be nice for all of the tools to be locally procured, my primary interest is the substances.

The tannins in Confusa are condensed tannins (flavonoid polymers), and the root extract was found to contain 28% tannins. https://www.sciencedirect.com/science/article/pii/S2225411018301044

I don't have a still handy, and I haven't looked into simple ways to concentrate alcohol, so I may not go that route this time.

To recover the precipitated alkaloids + tannins, I thought to simply allow the solution to settle until it was clear and decant the liquid from the precipitate.

However, biochar could work as an adsorbent for the alkaloids if need be. Adding the char to the first alkaline solution, shaking it up, straining it out, and then releasing the alkaloids with acids. But in that case I'd just try treating the precipitate with acid first.

As for a volatile acid - it seems that it would take me fermenting and distilling vinegar. I figured it wouldn't make a huge difference if I just used some fermented lime juice to dissolve the alkaloids from the first precipitate, filter out the remaining tannins, and add more ash lye to once again precipitate the alkaloids (this time tannin-free). Let them settle, decant, and finally filter and/or evaporate. Do you not think this would work?
 
I would say you would be best to concentrate on separating the subtle from the gross at every stage, as well as treating yourself to the use of some industrially manufactured vessels. You would want to have at least one batch of more highly purified potash for the final precipitation.

Repurposed domestic and hardware store items will get most of the task done, although some kind of distillation apparatus would likely improve your outcomes whether you use it for water, vinegar, alcohol, limonene or acetone. For the purification of lye ash, a sturdy cast iron pan would be a massive help.

I'm not convinced that fermented lime juice counts as a volatile acid and thus I can't help thinking you might at least want to try fashioning an earthenware retort for the distillation of vinegar. Once you get that done, alcohol and acetone aren't too far out of reach.

Filtration can be carried out through ordinary printer paper if you lay it on top of something absorbent like kitchen towels, where the capillary effect of the latter helps to draw the liquid through the less porous upper paper layer. This video shows the technique and is also worth watching for, among other reasons, the way it demonstrates method development. Link should go direct to the bit about filtration but if not, it starts at 25'55":
[youtube]

One more thing I'm not entirely convinced about is the use of biochar to collect the alkaloids, both in terms of efficiency in absorbing (adsorbing) them, and the subsequent recovery process. Is this something for which you've seen a precedent? Then again, biochar is noted for its ion-exchange capacity so I would think acid-rinsed biochar might be worth experimenting with for alkaloid recovery.
 
If I persist with my original plan, of dissolving the freebase + Ca-Tannate in lemon juice to dissolve the alkaloids and then adding more lye to precipitate the freebase followed by filtration and washing, I wouldn't need to use a volatile acid.

Do you think the freebase would not be recoverable through settling / decanting / filtration?
 
Every time you use lemon juice in the process you introduce impurities. By all means go ahead with the experiment as you envisage it if you think it will work. I'd suggest ensuring that at least your lye ash solution is relatively pure and conduct small-scale tests on test tube sized amounts.

Reports of collecting solid freebase by adding base to a solution of a DMT salt always involved relatively pure materials, as far as I recall. Is there a specific report of recovering alkaloids from a crude mixture that you have been using as a reference?
 
Every acid-base extraction adds lye to a heterogenous solution to release freebase. In the crude acid solution, Alkaloid-H+ is in solution with a variety of other cations (K+, Ca+, Na+, Amino+, etc) and a variety of anions (Cl-, HCO3-, Carboxyl-, Alkoxyl-, etc). This of course does not prevent it from precipitating at a sufficiently high pH, which is the basis of all of the extractions on this website. Or perhaps I'm missing something from your question?


As I see it, boiling the bark extracts only the substances that are soluble at ~pH 5.
Adding lye to precipitate alkaloids and tannins, filtering the solids, and washing them with lyewater leaves only the substances that become insoluble during the transition between pH 5 and pH ~10.
Adding acid to the precipitate and discarding leaves only the substances that do not form stable crystals (i.e, only the alkaloids), and adds impurities from the source of the acid.
Adding lye again, filtering the precipitate, and washing with lyewater extracts only the alkaloids again (there are no alkaloids in lemon juice).
 
Wood ashes were collected from the stove and boiled. The lyewater was poured off and boiled down to concentrate it several-fold.

Finely shredded acacia bark was boiled 3 times with a bit of lemon juice, the 3 boils were combined and reduced slightly. They will be allowed to settle overnight in a jar and the clear liquid will be decanted and filtered to remove particulates.

Tomorrow the lyewater will be added to the clarified brew.
 
Back
Top Bottom