The Vespiary

The Hive => Methods Discourse => Topic started by: humidbeing on June 15, 2002, 07:26:00 AM

Title: Dirty mdp2p cleanup by freezing out shit
Post by: humidbeing on June 15, 2002, 07:26:00 AM
Swim having real problems right now getting appropriate
solvent for H2so4 hydrolysis extraction.
Swim ha shit sitting in freezer, dirty, and some stuff is obviously more solid/viscous.
Would removal of solids at freezer temps be enough to
avoid washes which would normally be done while oil is
in a Np solution? IE to avoid nasty crap while ditilling?
 swim knows a nice soulution of MDP2P in enough np will
avoid emulsion, but can swim wash without the NP and
make it clean enough to distill without decomposition/
rearrangement?
   Hints, please swim has to act fast, and cannot find
pure DCM in this fucking hick town.
  Already went through so much shit to get the azeotrope
of the tolly out, but just need one green light from
a knowledgeble bee to go ahead.
Thanks!@
This is a hypothetical situation, as is all swims posts here.
CG I miss you sweety, I really do.
Title: Try bicarb.
Post by: terbium on June 15, 2002, 07:57:00 AM
Try a saturated solution of sodium bicarbonate (baking soda). Even if you do get an emulsion etc. at least you will have neutralized the strong acid and the product will keep better until you can get some solvent.
Title: use the toluene you have
Post by: goiterjoe on June 16, 2002, 08:01:00 AM
Toluene will work for the extraction of MDP2P from the sulfuric acid mix.  Ether would be better.  Remember to watch the layers, as the NP layer will more than likely be on top of the acid if using toluene instead of on the bottom like with DCM.
Title: thx
Post by: humidbeing on June 16, 2002, 08:58:00 AM
Thanks, but DCM it's gotta be unless you want that damn
azeotrope when there's glycol in there.
All turned out well though.
CG I miss you sweety, I really do.
Title: huh?
Post by: goiterjoe on June 16, 2002, 07:40:00 PM
there isn't any glycol in there if you hydrolyze it correctly.  I'm telling you from experience that toluene will work just fine for what you are doing.
Title: Ether isn't that great of a solvent for this ...
Post by: Osmium on June 16, 2002, 10:46:00 PM
Ether isn't that great of a solvent for this extraction. Ether solubility in plain water is somewhere around 7% if I recall correctly, and in acids it is even higher. This means you will lose a LOT of ether when you do this. You can reclaim it by distilling it out of the water, but unless you have a rotovap this is too tedious.
I'm not fat just horizontally disproportionate.
Title: ok
Post by: goiterjoe on June 16, 2002, 10:56:00 PM
I just said ether because that is the solvent shulgin used for this reaction. 

Ether is relatively cheap though.