guyincognito (Stranger)
07-18-01 14:16
No 191578
      Recovering MD-P2P Question  Bookmark   

Swim runs a 600 gram md-p2p sodium cyano run and recovers some md in dcm.  when swim tries to recover by distilling off the dcm them distilling over the md-p2p - it comes over at like 4 different boiling points then turn before even 3/4 way done it turn black and smokes - all done under good aspirator vacuum (same one I use to successfully distill md the first time to use)

Is the md bad? 

Is it not md-p2p anymore?

Is there some way swim could have screwed up and made some % md in the performic reaction and the other % is some kind of md -like substance?

Does the md need to be washed with water or something before recovering?
07-20-01 13:04
No 192209
      Re: Recovering MD-P2P Question  Bookmark   

when swim pulls over the md the first time - it comes over under vac at up to 240 and still gets product in later step -

when doing the recovery - something comes over at 100 - then like 140 - then it goes up - starts smoking and turn black - maybe even in the few days before it degraded into other things that hate heat?
07-20-01 14:27
No 192238
      Re: Recovering MD-P2P Question  Bookmark   

That's way too high, 240 C. A good aspirator reaches easily 12 mbar with cold water feed.
You have a leaking destillation setup or your aspirator is damaged by strong acids or alkalics.
Test your whole setup first with water, and report back what temp in C the water boiled at full vacuum.
Is the tap water pressure for the aspirator high enough, is it cold enough(15 C or less?)
MDP2P with a good functioning aspirator will fully boil at 165 C. It starts slowly boiling at 155 C.

I would not attempt to recover MDP2P with the means you have in your posession, without TLC or a gaschromatograph it's pretty useless after all the messy byproducts you created. LT/

07-22-01 18:51
No 198201
      Re: Recovering MD-P2P Question  Bookmark   

swim thought it was way too high, but the aspirator seems to be fine - may be hose is wrecked - will do water boil test to see what it pulls.

Swim is going to build vacuum station using water pump to get better flow rate - even though local pressure is pretty good.

swim used to pull over md at 190-200 with exact same setup - maybe it has been damaged as you say.