fats…
anyone got a decent solution for dewing with magic dirt?
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With magic dirt? Technically, yes, any hydrated silica should be helpful in removal of fatty acids. However, FFAs are not your main target in crude cannabinoid resin solutions.
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Yes.
Fats/waxes/triglycerides… that which one might more traditionally bring down with a secondary solvent.
So dont bake the dirt?!?
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What about a jacketed reactor and just do it scrubbing style, then dump the whole thing into a centrifuge with filter bags? Get some misting wands in the centrifuge to flush the media while its being filtered.
Then dump the spent media into a giant french press with water in it, to get the remaining heptane to float to the top for complete solvent recovery?
Maybe add some ultra sonicators on the jacketed reactor?
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did u try lowering the amount of crude?
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I’ve been starting to reconsider this one. I want to try staging B80 with the driest upstream moving to more wet at the bottom. I’m thinking that the clay scrubs polar “junk” more effectively up to a point with a bit of water in the pores. Obviously steps to dry the solvent later are necessary (maybe even a bed of MgSO4 underneath).
I’m sure @Dr_Jebril is the right dirt genius to ask
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There are various experiments to be investigated there. 
In fact with “dry” clay powders (unbaked) there is not much water in the pores (large spaces between particles or agregates). All the water is actually right at the surfaces of clay platelets. It is solvating the cations which are adsorbed on the negatively charged clay platelets.
Polar solvents can replace water.
Actually I don’t know to what extent clay can hold water in large volumes of dry non polar hydrocarbon. Can the hydrocarbon dry the clay ? Or would a baked clay rather dry the hydrocarbon ?
Also what people doing crc finally prefer finaly ? Baked or unbaked ?
I’m learning those thing with you here.
I can ask many clay experrts I know, they would not have a clue since we mainly focused on acqueous chemistry.
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I’m officially putting it on my list of “things to test when I get my GCMS running”.
Here’s the lazy experimental plan:
Prep 1kg of B80 in a vacuum oven until it stops losing weight (never actually checked to see how long that takes)
Divide into 5 portions
Keep one portion aside and store in dessicator. Place other portions into airtight containers with varying amounts of water inside (probably place in a cup on top of the clay) and allow water to evaporate and be adsorbed. Probably try 0.5%, 1%, 2.5%, 5%, 10% w/w.
Separately, extract some crude from FF using heptane. Dry thoroughly with MgSO4.
Sample micelle and then divide into 5 lots
Filter through column of each clay sample
Wash column with equal amounts of dried heptane
Dilute first sample equivalent amount with dry heptane
Test 6 samples and see what gets stuck and what doesn’t.
Only concern is if the excess fat from the heptane extraction will compromise the results
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Depends on the geometry, and oven
In a ventilated oven, it takes between 24 and 48 hours at 105c.
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We run around 200C under ~100mtorr for about 2 hours which I have to imagine is massive overkill. I also wonder if it has the ability to damage the surface structure
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Yes it is a bit rough. Clays resist well up to above 400c. Still, above 150c you may promote some collapsus of the interlayer space (between clay sheets). This should be reversible (with rehydration), but may alter clay properties by decreasing the surface area.
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As @SidViscous alluded to, and which we have discussed before, @cyclopath , baking does NOT remove intercalated waters of hydration from clays… only furnace level calcining temperatures and conditions can do that. I am of the belief, in agreement with @SidViscous , that the waters of hydration remaining deep inside the clay/zeolite particles actually help activate the outer porous structure… especially when the superficial waters are removed through typical vacuum baking conditions! I think of it as a sort of metamaterial “polarity gradient” to explain it succinctly.
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And YES, @Dr_Jebril ! Superficial water repels any hydrocarbons carrying color bodies and other impurities, so it is essential to bake off that “lipophobic coating” to achieve sufficient pore-interaction and chemisorption!
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Are the removed compound ionic ? Cationic/anionic ? or rather simply polar ?
Various form of sorption are possible. If this is taking place right at clay surface, this would be cationic exchange. The hydrocarbon would have to hold cations… is this actually possible ? Or limited to protons only ? Or is held by little amounbts of water present in the solvent ?
I start to understand that the mechanism happening may rather be a “secondary sorption”, similar to what people are doing by intercalating clay with organics and making them lipophilic. This happens mainly through H-bonding with the clay, or with cations sorbed at the surface of the clay.
Baking above 105c for sufficient time removes the water which is present in the interlayers spacing, at the surface of clay platelets. The cations remains still.
Calcining the clay will remove the hydroxyle (OH) groups which are part of the octahedral layer (sandwiched between two tetrahedral layers in the smectite structure). They leave as the form of water molecule. But the structure then is irreversibly changed, at such level.
https://www.sciencedirect.com/topics/chemistry/dehydroxylation
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You people are miles ahead of my understanding of the technical vocabulary. But here I go.
I use b80 most of the time up until recent weeks. I now dry outside in a microwave, 6 minutes for 3 cups.
I almost ruined a vac ovens plumbing because I put a big deep stock pot full of b80 in it. No good!
It was like a mini Mont Versuvius! That was the first and last time, over a year ago
I did that. I quickly realized baking sheets worked fine without incident.
I measure powders by the cup and I’ve noticed if the powder holds shape onto/in sheet/bowl it’s too wet to used. Every time the powders are damp I get a red or purplish color extract no matter what strains.
I didn’t want to take the time one day to dry em out in the oven so I used the microwave. After figuring out how much time and amount I noticed the clumps were gone and it was like silky powder, like water in a bowl. I know it saves time and energy and I think it was very effective.
But we only get red extract during the short rain season. The rest of the season here is very dry and we have a lot more control and get light shades of yellow or clear.
I’ve seen other ops say they use microwave ovens to dry out powders. Does anyone have research or opinion on using microwaves?
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@Drink , here is some information on drying molecular sieves that can be applied to clean (very low iron) clays and the like:
EDIT: Be sure to read through the article comments section, below, too.
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@Photon_noir I could be wrong but I remember reading that water is how they swell the clays and that drying the bleaching clays could reduce the bleaching power because it collapses the structure thus resulting in less surface area. However most biomass will have lots of water already in it so I don’t know if this is true in our scenario
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@waxplug I believe this to be true and I’m not sure that the water in the biomass will “rehydrate” and/or regenerate the surface area. Seems like some clays can take alot more heat when drying meaning they are either stronger leaving pores open or they have different strengths in bonds with the moisture to help.
Maybe someone can confirm scientifically though as I’m shit without visuals and dry powder wet powder looks the same.
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Yes, @Waxplug1 , laminar clay structures are naturally hydrated and swollen with water. The only way to remove the so-called “intercalated” water of hydration is by a high temperature process called “calcination”. This process may slightly shrink individual particles of clay, but that actually increases the bulk surface area ratio. You see, the inter-laminar hydrated spaces or water-layers in between the layers of solid aluminosilicate are generally inaccessible to anything external except some natural cations (+)… so the surface area within those layers is not counted when it comes to chemisorption of things like color bodies. Only the external faces and rough edges of the clay particles are considered for our purposes in the surface area calculations. As such, smaller particles have more external surface area in ratio to volume than larger particles do.
This is also why simple baking, vacuum baking, or microwave baking are important for our purposes, to remove superficial or external water of hydration from that external surface area of our particles. When water is on the surface and clogging the external pores of the clay, our non-polar solvents and hydrophobic compounds are naturally repelled away from the particles. Quite simply, oil and water do not mix. You can think of the superficially wet clay particles as water droplets when they are surrounded by non-polar solvent and lipophiles.
@Greenz , It is only by removing that outer coating of water and boiling it out of the surface pores that our non-polar materials can access the active chemisorption sites of the clay particles.
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If you don’t bake w1 you can crash a lot of gunk just by reaching 0 psi (evaporative cooling/ 0c)
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