Sure I am
And this is how you do it:
You need a overhead stirrer, a simple one from an old battery drill works great + PTFE stir-rod + blades off Aliexpress - 10 USD or so.
But you can use iron/steel in this reaction without any problems too. Vessel, Stirrer, etc.
60 g P2P need less then 25 g Aluminium as granules or shavings if any possible 99,999..% - no powder! Ebay or whatever, not watched not expensive. Do not use foil! The less Al the less mess in the workup.
40 g Methylamine Base thats 100 g of 40% aqueous solution, you can use MeNH2 in alcohol too or you can make the base in situ from the hydrochloride.
Solvent: EtOH or IPA or methanol. If you use Ethanol denaturated you should remove any MEK or other Ketone used for denaturation.
When using MeNH2.HCl or MeNH2 in alcohol you can process 400 g P2P in a 4 liter flask, when using it as watery solution not so much as you need more alcohol to compensate for the shitload of water in the reaction.
General outline of the reaction: Make half of the Al to Amalgam by using Hg salt in warm water/alcohol mix Just enough to cover the Al. Decant this and put Al in the reaction flask. Add methylamine and half of the alcohol, the other half is used to dilute the P2P. Start stirring, warm up to 40 °C - cut off heating, prepare a cooling bath with water at room temperature and start adding P2P slowly. A dropping funnel comes handy for anything bigger. Use the cooling bath to keep temperature below 50 °C. No refluxing! This would just drive all the methylamine out - which you need in and the stink....
Use a thermocouple/thermometer IN the flask for measuring.
Takes time when done remove cooling bath (do NOT use ice-water or you might kill the reaction off whats bad.
Add the rest of the Al (what you amalgamate using the same Hg/water as before) in two portions according to the P2P addition, say one portion when half of the P2P is in and the rest when 90% are in. Bigger amounts processed take longer and you divide into more portions, common sense.
No problem if it gets to 70 °C but it starts stinking. Do not cool below 40 °C or it may die.
After everything is in and the temp drops, start heating it mildly to keep at about 50 °C
Best over night.
Next day you cool it down, add ice-cold NaOH solution, and steamdistill directly from the pot or after an extraction depending on your setup and equipment. Before steaming out the meth you distill off the alcohol which is loaded with methylamine and gets re-used next time and then you can cut the amount of methylamine used to half.
for 100 ml of P2P:
40g of Al 99,9999..% pure as shavings or granules
70 g of methylamine, this equals 155 g of methylamine hydrochloride + 90 g NaOH (first time. Later when using the methylamine loaded alcohol cut amounts by half)
Now the question of water. Water is needed but too much is not good.
I recommend to use methylamine in alcohol or to make it from the HCl salt and NaOH what can be done in the same pot, the formed salt does not hurt (if you use an overhead stirrer of course). In this case you add three times 25 ml of water to the reaction. One portion at the beginning, one portion when about half of the P2P was added and the rest later say when 2/3 of P2P are in? You get the drift.
Anybody who knows where in EU I can get some BMK, like 2 kg or so, for a reasonable price, please PM me.
thx
