Limonene extraction failure

[stimoceiver]

Hi,

SWIM was trying the limonene extraction. SWIM sliced some Trichocereus Bridgessi like a cucumber as a whole cactus and the pieces were dehydrated at 100F. No attempt was made to separate the cactus core etc. When they finished drying SWIM then ground up the dried slices to a very, very fine powder. So fine that SWIM's opening the blender caused smoke-like clouds of dust to go wafting.

Now SWIM is in between steps 2 and 3 and cannot perform step 3. The cactus/lime/water/limonene mix would barely blend, SWIM could smell the brushes cooking on the blender SWIM was using. Even after sitting for several days the mix has the appearance of a homogenized green colored mixture or colloid with no appreciable settling or layering. It is thick and sludgy like mud.

SWIM tried pouring some of this mixture into a coffee press to press the liquid and most of the cactus solids just go right thru the screen due to how fine SWIM ground the cactus.

SWIM tried adding a little more limonene to the mix but to no avail. To give you an idea of the thickness of this mixture, a spatuala inserted vertically in the sludge stays vertical. So there is no way to "pour off" the limonene.

Perhaps someone can suggest an arrangement of household objects SWIM might construct where SWIM could place a coffee filter to allow this sludge to filter by gravity? Experiments with a coffee filter have the sludge just sitting on top of the filter with very little seepage after 5 minutes.

Can anyone offer some suggestions that I could pass on to SWIM as to what SWIM might have done wrong or how SWIM might recover this mess to continue the extraction?

Best,

stimoceiver

 

[soulfood]

Adding more limonene was a bad idea... but all is not lost.

When I have this jelly mistake I use a potato masher, gravity and much patience. If you hold the mix back with the potato masher, but not push down on it and tip the vessel as much as you can without the goo coming out, then leave it for a little while the limonene should be running to the bottom.

Squeazing won't realy help until you have most of the limonene out, but if you apply very slight pressure on the potato masher after it's been tipped over for a few minutes you'll see some liquid come out of it. Using this method it took me about an hour to get 50ml out. So patience.

 

[SuperRad]

Not coring the cactus is sadly a serious error as it adds so much bulk with no goods. Not peeling the waxy skin is also a no-no as it will encourage emulsions while salting the mescaline.

My question: what was the consistency of the cactus after adding the water but before adding the limonene. When I did my extract, I truly used as little water as possible to get the whole thing damp, and then mixed like CRAZY. For more than 5 minutes like 69ron suggests, it was more like 10-15 minutes. The mixture was very thick and rubbery. I added the d-limo almost immediately after. The cactus remained thick and rubbery for about 24 hours, but as the CaOH continued to break the cactus down, it went to a cottage cheesy texture, and eventually became a homogenous sludge that was very soft.

 

[stimoceiver]

Soulfood & SuperRad,

Thanks for your reply. SWIM still has the mix sitting here in some containers and SWIM is ready to try some experiments at separating this seeming colloid.

SWIM's primary error appears to have been that SWIM sliced the cactus into flat discs like a cucumber or okra.

SWIM next stuck those in a dehydrator. Once dried, SWIM used a blender that pulverized those down to dust in a matter of 15 minutes.

To answer your questions, SWIM mixed with water and then added CaOH and continued trying to mix. The same blender that pulverized the dried cactus was now having a serious difficulty mixing the resulting sludge. On and off SWIM mixed for around a half hour before waiting eight hours for any separation to occur.

When it did not, SWIM tried using a coffee press and a metal spatula, but SWIM was unable to press any significant amount of limonene free of the mass. At this point SWIM tried adding more limonene and mixed and let sit.

When this didn't seem to help much SWIM read your message SuperRad and tried adding more CaOH, and mixing another hour or so.

After waiting for another eight hours for it to settle. SWIM reports that no visible separation of oil has occurred, and the material is quite sludgy. It is stored in a cylindrical plastic (vertical) container and SWIM notes that if one removes the cap and tilts the container horizontally, it barely even moves from its alignment parallel to the top of the cylinder, it would take probably five minutes for the sludge to move enough to pour out without helping it by giving the container a mechanical thud on the end. So SWIM thinks perhaps some oil may have separated underneath the sludge and/or in a thin layer between the sludge and the walls of the container, but if so it is minimal.

Perhaps someone knows of a mechanical setup that SWIM could use to place the bulk of the mass atop a filter? Maybe SWIM can retrofit the french press to use a paper filter. SWIM will give it another go but loses some each time SWIM transfers the goo.

SWIM was hoping someone with a better knowledge of chemistry could suggest something SWIM could add to this to allow it to separate out? More water? Perhaps something that de-emulsifies? If anyone can offer suggestions SWIM would greatly appreciate it as SWIM has nothing to lose to try a suggestion on a small batch.

 

[SuperRad]

OK I've reread what you wrote and it think I've found the biggest errors:

First the only think you should be using a blender for is to powderize the cactus. THEN put the podwer in the bowl and mix with the CaOH. This is very important, you want the lime and cactus to be mixed BEFORE you add the water.

Now slowly add the water, splash by splash, mixing by hand with a spoon. Once you stop seeing dry powder, stop adding water. Keep mixing the cactus sludge by hand (or with a kitchen mixer, not blender) for at least ten minutes, breaking apart all the clumps you have. Then pour the d-limo on top. Every hour or so, use a spoon to break the cactus sludge apart, allowing limonene to flow everywhere. Continue to break up all hard chunks. I let my limo soak for 24 hours (I do this twice with fresh limonene). After about 36 hours after mixing in the water, you should notice that the cactus mass has gotten alot "looser," and most of the hard rubbery chunks have just turned into 'cottage cheese.' The after another 24hrs, the cactus mass should be like a thick sticky slurry and should be a lot paler green (at this point there's almost no mesc left in that so you should just toss it or use it for composting).


The reason adding CaOH before the water is crucial is that the CaOH keeps the cactus from turning into an absorbent snot. By adding water in a controlled fashion, the cactus mass will remain solid and rubbery, and it will not absorb much liquid. I find that the cactus mass absorbs ~100ml limonene the first time, and then is "full" for the rest of the extraction (good luck ever getting much of that 100ml back).