humidbeing (Can't SWIM)
06-15-02 07:26
No 321546
      Dirty mdp2p cleanup by freezing out shit  Bookmark   

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/
   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.
This is a hypothetical situation, as is all swims posts here.

CG I miss you sweety, I really do.
(Old P2P Cook)
06-15-02 07:57
No 321559
      Try bicarb.  Bookmark   

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 on BackOrder)
06-16-02 08:01
No 321976
      use the toluene you have  Bookmark   

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.
(Can't SWIM)
06-16-02 08:58
No 321989
      thx  Bookmark   

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 on BackOrder)
06-16-02 19:40
No 322109
      huh?  Bookmark   

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.
(Stoni's sexual toy)
06-16-02 22:46
No 322177
      Ether isn't that great of a solvent for this ...  Bookmark   

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 on BackOrder)
06-16-02 22:56
No 322179
      ok  Bookmark   

I just said ether because that is the solvent shulgin used for this reaction. 

Ether is relatively cheap though.