Dope_Amine (Hive Bee / Eraser)
10-26-00 09:29
No 63485
      Al/Hg nitromethane max. reaction size  Bookmark   

I understand that one might need to worry about possible explosions when doing a big Al/Hg nitro rxn.  What would be the most ketone one could react in a 5 L and still be fairly safe?  Thanx.  I don't know shit about the nitro, but 80% yields are converting me.

something for your mind.......
(Hive Bee)
10-27-00 21:11
No 64034
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

Antibody had an idea, to set-up a continous nonstop nitro assembly line. It is a two pot idea.
You do a 2x in a 2l flask, after nitro  and ketone have been added and things simmer down switch the contents of flask to a 5gal pail sitting inside of a hotwater bath on another stirplate to finish. then start another 2x in a 2l flask and when it simmers down dump it in the 5gal pail. Keep going as long as you want.You could do several batchs a day like this. Stopping the 2nd pail every 2-3 batchs to do work-up and gassing

The bigger the rxnsthe greater the chance of a runaway.If they runaway they do it during the addition, not after they start cooling.

This way you never risk a loss of more than 1 batch.

BTW it is more a volcanoe to look out for than an explosionshocked.

Just an idea. Think also about the size of sepfunnel etc. you will need for work-up of a large scale-up. Little bites might digest better.

Jimi loves ya
(Stonium's / Changer)
10-28-00 00:53
No 64119
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

When doing such big reaction I really would look into using thicker Al. Much gentler, no runaway reaction, no explosion, much more efficient Al usage (less sludge to get rid of), all that.
But I'm repeating myself here.
You can aminate about 200-250g of ketone safely in a 5L flask when using MeNO2 and about 500g when using 40% aq. MeNH2. Easily.
(Hive Bee / Eraser)
10-28-00 01:32
No 64127
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

Thanks Os for answering my question!  Do ya think 50 g of Al/mole of ketone could be cut down for a 500 g'er using MeNH2?  Any suggestions on g:g ratio of HgCl to Al? Thanks! 

something for your mind.......

(Hive Bee / Eraser)
10-28-00 09:22
No 64257
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

SWIM uses 100mg HgCl2 on the 50g scale with the Al/Hg/Nitro. If it is added directly into reaction mix it doesnt take much, I would guess ~400-500mg tops on a 500g scale,if added directly to reaction.
(Hive Bee)
12-22-01 00:26
No 249650
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

Using .005 Al how much ketone MeNO2 could be proscessed in a 2l. 
(Hive Addict)
12-22-01 00:55
No 249658
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

You could comfortably do 25g of MDP2P in a 2L flask.
(Junior Service Representative)
12-22-01 03:52
No 249690
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

So, 40g in a 3L if equipted with sufficent reflux condensor?

(Hive Addict)
12-22-01 07:19
No 249710
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

I have heard of 50gs posted before.........

Seems that may be the max. or above.......

someone may find out someday...... cool

"The gods are too fond of a joke."  (Aristotle)

(Commodore "Mole Bouncer")
12-22-01 16:36
No 249809
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

Ritters original write up as appeared in TS2, called for 50g ketone w/ 55g Al in a 2l flask, but with a much slower addition than baal adherants might be acustomed to.
12-23-01 08:59
No 249999
      Re: Al/Hg nitromethane max. reaction size  Bookmark   

Ehh, am drunk again, got another idea:

Why not addept the idea of a railgun to make a railgunring around your flask/vessel/tank?
And throw in a stirrer bar to get slung around the SIDE? Details of making a railgun with numerous links ever given by me on the Couch. DO NOT DARE to patent this idea, or I will haunt you untill the next 10 generations of your greed infected offspring!!!

Any more drunks around? Let's go to the Couch.

Ahh, fuckit, better stay here, more sophisticated audience, why is everybody whining about stirringcapacity? Fuck, get a batterydriven drill, 100$, stick a paintstirrer in it from the next shelf (get a bottle of paintremover from theothershelf and get that ugly blue color off first or it will be eaten away by your ketones, making your dream, "hehe, atlastnobodytalksaboutdreaminganymore, fuckers", multicolored), smash the ketone in your face when you stick that dildo in the fluid.

1m3 NaOH, HCl, H2SO4 PTFEtanks secondhand 100$RHULE!

Afraid of initiaiting a fuckin explosion? Attach a thickwalled piece of vacuumtube to your paintstirrer and on the other end a convenient pin, stick the pin in your batterydrill, VOILA, stirring at remote distance! )Do not forget to stick a fittingtightly spiralled metal spring inside your vacuumtube, or the fuckin thing will strangle your skinny neck.)

Stick a long piece of stirrershaft through your refluxcondenser, fit in place by a oversized hole in a stopper on top of your condenser and hang the fuckin batterydrill on it, will move any kind of alu pices around, success guaranteed. Any vapours can pass through the oversized hole, blow them away with a hairdryer liberated from any innocent female hanging around in the vecinity.
Really worried inventors stick another oversized stopper at the bottom of their condensers, fuckin whinies, who gives a fuck about glassroadkill on the way to wisdom?

Up yours! EtOH RHULES! LäBTöp/