i have a questions about crystallization of 4mmc*hbr(!! not hcl) so i used to work with scales about 15kg in one pot
my yields in bromination is 96-100% of theory, amination give me 86% of FB (it is theory almost max, you cant move further balance of reaction) and acidification with
diluted hbr in totalness to make 1g mmc to 2.5ml o water. So, even without washing i have this after acidification -
clean,needles matt like fiber glass (room temp +8) but allexcess water inside this matt, and this is problem.First time i try to melt it, place in +22c 35% humidity, and after 4 days i have this -
some are okay, some not. So the problem is something inside is oxidizing or simple condensed to trash point where it osibviously bad.
DCM is bad in washing aquos solution of 4mmc, he only wash some trash which is nonpolar. So it can help but a very little.
My question is - how to extract clean 4mmcHbr fron not so clean brine h2o.
First i thought. thay if a lot of mmc precipitated at +8c, maybe it`s much more simple in comparison with 4mmcHcl to make a cold extraction, so i try 500ml h2o +40g mmc, and place in friedge for 12h, no result, how is it?!
overall i have a few ways - try salt\acetone extraction
try to crush this glass like matt and rinse with ipa\acetone
or ...a lof of or.... So i need a man with expirience with 4mmc*Hbr (i`m a pro on hcl, but this situation is slightly different)
on all photos here - same mef in h2o, and sorry for my eng