We have separate goals sedit, that's why my methods seem to be more expensive or more involved.  4kg of Formaldehyde and 2kg of ammonium chloride give about 500g of pure methylamine hydrochloride.  Not to mention, the workup is a pain, it's a mess, it's frustrating - I don't have an air-conditioned lab, so hygroscopic materials piss me off.  I'd prefer not to deal with the HCl salt at all.  I think that is my main attraction to these methods; not dealing with salts, and going from one phase to another and purifying with filtering.  My most recent experiences with methylamine HCl have shown me that filtering is very unpredictable.  Maybe it was a few ml below the typical volume I filter, but the crystals were unfilterable.  It plugged my vacuum filtration up so much that it completely stopped dripping on full vacuum.  I lost much of my yield, and much of my hexamine that time.  And yes, I tried it with gravity filtration too, even worse. 

With the two methods I've been interested in, Al/Hg & Nitro or H2 & Nitro, I don't have to deal with any hygroscopic salts, I don't have to filter a hygroscopic salt, and they're both quite clean reactions.  Al/Hg & nitro just requires hobby fuel, aluminum, and small amounts of mercury.  All of which I can get no problem.  H2 & nitro makes up for it's harder to obtain chemicals by being so much more awesome.  I have no problem building a hydrogenating apparatus once I have the tank.  That's fun to me.  Plus, I only have to build it once, then it just works.  After that, I just prepare the catalyst, load the container, pressurize it, and turn it on.  (It's a little more involved than that obviously).  Once it's done, I filter out the catalyst, and I've got my desired methylamine solution.  Probably 3-4 hours depending on the catalyst used, as opposed to the day it took me to make methylamine*HCl.  If I've got a slow day, I regenerate the catalyst, then load the machine up again.  Rinse and repeat.  Plus, In the container I'm looking at, I could probably do a 1L reduction at a time.  If I supersize it, then even more.  Perhaps one of those kegs would be up for the job.

"We have separate goals sedit, that's why my methods seem to be more expensive or more involved.  4kg of Formaldehyde and 2kg of ammonium chloride give about 500g of pure methylamine hydrochloride. "

You are right we do. I was using it for reductive amination and you only need methylamine pure. The amalgum is uneeded for this. I would not be to shocked if plan old HCl/Al with no amalgum didn't accomplish what you need.

.... Then don't use Formaldehyde and ammonium chloride. The reaction I posted reduces MeNO2 thru the Fe/HCl route. Yeilds damn near theoretical. I think your mistaken in that you think the dissolving metal reductions are for Formaldehydr but they are indeed dont to generate the PUREST form of methylamine one can get thru the reduction of MeNO2. Same Idea as the amalgum its just the amalgum is not needed as the potential the amalgum is made for is to reduce imines but MeNO2 can be reduced much easyer. No salt to deal with no filtering unreacted products just run the reaction Condense the solution and the base it and feed the vapors into the solvent of choice.

To each is own I guess but if its because of a misunderstanding of the reaction believe the Fe/HCl is the cleanest and most cost effective time wise and montary.

Small fireX that I have are tested at 565PSI Im not to sure but that should be enough for hydronation.

Yeah Pd/C requires 80psi, so pressure I'm not too worried about.  The only thing I don't like about the Fe/HCl method is that it requires Fe and HCl in addition to MeNO2.  Haha, I know it seems weird, but not only does Hydrogenation seem easier to me, it seems more fun to use, and to build hahaha.  To be honest, I'm not quite sure that I'm exactly doing this just to make the methylamine, I think hydrogenations would be fun haha.

I priced out an 80cu ft bottle of H2 (the big ass bottles you see), and it's 250 bucks for the tank, then 26 bucks for a full recharge.  80cu ft of H2 pressurized to 1atm is 50mol.  I know for a fact, that H2 is pressurized to well over 15psi however, so just multiply 50 by however many atmospheres of pressure is in there.  For example, if it were pressurized to 500psi with hydrogen, thats 1667 moles of H2.  This is enough to generate roughly 35,000 liters of 40% methylamine solution (assuming ~80% yeild from hydrogenation).  The catalyst can be regenerated and loss is only from mechanical.  Once you buy the 26 bucks worth of hydrogen, the only price is occaisonal repurchasing PdCl2, nitromethane, and solvent. 

Bio posted a lot of information on using various forms of aluminum including powder many years ago, before the Wasp's Nest was available    The most critical factor affecting amalgamation is the purity of the aluminum, which is most easily tested using nitromethane in methanol    A lot of aluminum simply isn't pure enough, which causes the reduction to fail 

Bio posted that aluminum powder surprisingly wasn't nearly as reactive as foil  One should always do a test amalgamation in a test tube before anything else is done, that's the only way to know if the aluminum is pure enough 

poisoninthestain said:

Run aluminum foil through a paper shredder for incredible surface area. Never had a single amalgam fail in my personal experience with either acid or basic reductions.

Very true, a most excellent tip as poisoninthestain point's out. Paper shredder gives hundreds of little aluminum rectangles, and they work great scientifically, no need to cut out individual squares. Just buy a paper shredder, it works great. Also try heating up the solution of hg and meoh (stirring for 1/2 hour previously) to about 120 F degree then about 5 minutes or more minutes after dropping in the foil it "should be" ready....most of the shiny surface goes away and pieces of foil begin to rise to the top, and the bubbling grows more intense, and the bubbles a bit larger. then turn off the heat from the stir mantel for the rest of the process...don't even stir the foil while it sits in the meoh, that way it is easier to monitor the foil for when it begins to float, and easier to monitor the exact point when the small bubbles start to turn into much larger bubbles rising from the bottom of the solution to the top...these 3 things, bigger bubbles, shiny appearance goes away, some pieces start to float...are all key indicators to begin the additoion...in other words, once the foil is added, turn off the external 120 degree F heat....you will notice that if the reaction is progressing it will create lots of heat on it's own, be turbulent, slow motion bubbling moving up from the bottom to the top, volcanic like bubbling on the surface, and even 20 to 30 minutes later when the stir plate is room temp to the touch, the reaction flask will be incredibly hot due to the heat it creates on its own. try generic heavy duty foil and can even scrub it a bit on front and back with steel wool to scratch it up a bit, may or may not make a difference. 9 times out of 10 it works great, but there is always that 1 time out of 10 that it doesn't get off to a great start as expected, the trickiest part of the whole process.

Overhead stirring eliminates having to swirl by hand during heaviest part of reaction. Drill or burr a seperate hole into rubber stopper, feed stir rod thru hole, wrap plumbers tape around area where stir rod feeds thru rubber hole so that the hole area is nearly air tight, then put a tiny bit of petroleum jelly around the plumbers tape, this will allow the stir rod to turn easily at any speed without any air/gas leaks.

Use a glass, or stainless steel sleeve, lubricate with vacuum grease or petroleum jelly. Look at picture below...