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Author Topic: methylamine from gallium/aluminum reduction of nitromethane  (Read 260 times)

overunity33

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methylamine from gallium/aluminum reduction of nitromethane
« on: April 18, 2011, 02:59:55 AM »
Im surprised I haven't seen an al/hg writeup that utilises al/gallium alloy... Its safe, easier (no shredding foil) and way more OTC...
My interest in it is generating methylamine gas on demand... Apparently from someone on SM you can drop a chunk of al/ga alloy into hobby grade nitromethane (60%+ MeOH), it will generate hydrogen and methylamine, which you can pipe through an HCl solution to recover the salt.  Another option is dropping it into pure nitromethane and piping it into alcohol to be used in a further reaction... I am kind of hesitant to do this because of the heat generated, you don't want that nitromethane igniting, shooting flames into your explosive gas saturated alcohol...

What do you guys think? Has anyone here had any experience with al/ga?  Apparently much more vigorous reaction for the surface area then al/hg..

Sedit

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #1 on: April 18, 2011, 03:08:42 AM »
I think you should scan thru a thread of mine known as Sedits random experiments.... its mostly junk information from years ago but you will find that your overthinking this and a simple Zn/HCl will generate your desired results. Drip this onto NaOH and gas into HCl for a good workup.

This is a TRUE dissolving metal reduction... A birch reaction commonly known as a dissolving metal reduction has no resemblence to a real dissolving metal reduction at all.
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Shake

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #2 on: April 18, 2011, 03:38:00 AM »
you can just use naoh and aluminium with nitro.. i dont know what the auto ignition tempreture of nitro is but if it ignites in the vessel it will go off like tnt, with zero oxygen shortage to fuel the explosion

psychexplorer

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #3 on: April 25, 2011, 01:36:17 AM »
If it autoignites from heat, it will deflagrate, not detonate. Getting NM to detonate requires either extreme pressure or another HE.

Although NM is somewhat oxygen starved itself, the resulting fire is still no joke.

Tungsten.

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #4 on: May 03, 2011, 02:01:13 AM »
Quote from: Sedit on April 18, 2011, 03:08:42 AM
I think you should scan thru a thread of mine known as Sedits random experiments.... its mostly junk information from years ago but you will find that your overthinking this and a simple Zn/HCl will generate your desired results. Drip this onto NaOH and gas into HCl for a good workup.

This is a TRUE dissolving metal reduction... A birch reaction commonly known as a dissolving metal reduction has no resemblence to a real dissolving metal reduction at all.


I just searched and the thread didn't come up. :(

Either it got deleted, or I'm too stupid to use the search function properly (both are equally possible.)
-W

Sedit

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #5 on: May 03, 2011, 02:47:19 AM »
http://127.0.0.1/talk/index.php/topic,195.40.html

The entire thread is full of half assed experiments. Last page I made a few post about it. I believe something in the castor oil that contaminates commercial Nitromethane could possibly be reducing the Nitromethane in the presence of alkoxides...

There is also short mention of Acidic dissolving metals but that thread was mostly designed for failers so not much discussion went into it ;D . Its a simple reduction of a Nitrogroup using dissolving metals in mineral acids.

Here this will help, http://www.sciencemadness.org/talk/viewthread.php?tid=227
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Tsathoggua

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #6 on: May 03, 2011, 11:08:55 AM »
Using NaOH is NOT a good idea, where nitro is concerned. It forms nitronate salts with the alkali metal hydroxides, and carbonates, it may also do with group II ones.

Shock-sensitive primaries, the corresponding dinitroalkane alkali metal salts have been reported to blow when they are wet.

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Sedit

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #7 on: May 03, 2011, 12:54:38 PM »
So I heard,  ;D . After the fact that is. But nothing blew up so ill be ok. This is why everything is done in test tubes and not 10kg reactor vessles.
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fractal

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #8 on: May 03, 2011, 02:24:38 PM »
Quote from: shroomedalice
oh and dont piss on the salt that is left as acid makes the sodium salt of nitromethane explode.

Reminded me of this post lmao

Shake

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #9 on: May 03, 2011, 11:36:52 PM »
Hey can someone clear something up for me?

 methylamine gas + Hcl = methylamine hydrochloride right?

So would you bubble methylamine gas into acidic solution then evaporate and dry to get the hcl?

sounds almost too easy hmmm..

if you have a very basic solution of 2L NaOH and H2O say 30% in a 2 neck RBF then add 60mLs Nitromethane and set to stir, then in an addion funnel either aluminium dust in a solution or maybe anti perspirant deodourant which is 18% aluminium chlorohydrate drip it in slowly and gas it into a solution with a gas dispurser in the end of the tube..
weigh the solution before and after to make sure it has been absorbed, then HCL gas that solution to get crystals to fall out?

just an idea, i havnt checked what has already been done with this..

« Last Edit: May 03, 2011, 11:46:06 PM by Shake »

psychexplorer

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Re: methylamine from gallium/aluminum reduction of nitromethane
« Reply #10 on: May 04, 2011, 12:57:37 AM »
Shake,

Correct on the first count. You'll find that reaction handy for both preparing MeAm in a solid form for handling or storage, as well as capturing MeAm(g) so it doesn't have to be vented anywhere. That odor is not one you want blowing towards your neighbors.

I'm not quite sure what you're doing with aluminum dust and deodorant. You need amalgamated aluminum metal, not just anything with an Al in it. For this, use the heavy duty foil, cut into tiny bits, and balled up with a coffee grinder. Also, you need to pay attention to the order in which you add your NaOH. Basification is needed post-reduction.
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