Author Topic: Al/Hg nitromethane max. reaction size  (Read 3659 times)

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Dope_Amine

  • Guest
Al/Hg nitromethane max. reaction size
« on: October 26, 2000, 09:29:00 AM »
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.......

Antibody2

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #1 on: October 27, 2000, 09:11:00 PM »
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 explosion :o .

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

Osmium

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #2 on: October 28, 2000, 12:53:00 AM »
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.

Dope_Amine

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #3 on: October 28, 2000, 01:32:00 AM »
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.......


baalchemist

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #4 on: October 28, 2000, 09:22:00 AM »
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.

Vibrating_Lights

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #5 on: December 22, 2001, 12:26:00 AM »
Using .005 Al how much ketone MeNO2 could be proscessed in a 2l.

Chromic

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #6 on: December 22, 2001, 12:55:00 AM »
You could comfortably do 25g of MDP2P in a 2L flask.

PoohBear4Ever

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #7 on: December 22, 2001, 03:52:00 AM »
So, 40g in a 3L if equipted with sufficent reflux condensor?

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Goodtimes

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #8 on: December 22, 2001, 07:19:00 AM »
I have heard of 50gs posted before.........

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

someone may find out someday......  8)

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


Antibody2

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #9 on: December 22, 2001, 04:36:00 PM »
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.

LaBTop

  • Guest
Re: Al/Hg nitromethane max. reaction size
« Reply #10 on: December 23, 2001, 08:59:00 AM »
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/

WISDOMwillWIN