Acid base extraction issues
I am using standard Acid base extraction procedures, I have done this a few times with tea and coffee to get whitish yellow needle-like crystals. I am doing this on ground mimosa rootbark.
let powder sit in a cool 500 ethanol/methanol slurry for 3 days with a bit of dilute HCL to make any remaining freebase a salt
Filtered 450 ml obtained of a milky yellow fluid
I then added 75 ml toluene to the mix, and let it sit on a stirring plate for 30 minutes
I was going to add the NaOH to basify it but it appeared that the two fluids were completely miscible creating a homogeneous, clear, yellow fluid upon the addition of the NaOH ethanol mixture, maybe 1 gram in 15 ml, the fluid became instantly milky and cloudy like the first solution but lighter.
I was worried at this point because that is not what nonpolar solvents are supposed to do, but i let it sit and I saw 2 layers form after 2 hours, one clear very faint yellow one, and a milky white one
The next morning I siphoned off the bottom aqueous layer and added the (hopefully) nonpolar layer. I let it sit for 3 hours and noticed a few mm thick intensely yellow layer of clear fluid develop above the milky one.
My theory is that for some crazy reason the methanol/ethanol solvated the tolouene and when a base was added it fell out of solution in very small micro-particals, which then combined at the very top and were lighter than the toluene bubles inside of ethanol so the pure toluene floated up.
I stirred it gently with a stirring rod which seemed to increase the amount in the solid tolouene layer and decrease the amount in the white milky layer, while adding a very small layer of ethanol at the very bottom.
It has been 2 days and I am about 1/2 through the milky layer
Has anyone has experience with this or tolouene based extractions, How could I clear up this problem faster? I want to get some tetrachloromethane, or even better pentane(nonpolar, mostly nontoxic, boiling point is around 93 F), I would kill for some.
