So whats the crystaline stuff on the bottom is it Methylamine HCL or is it Ammonium Cholride.Most likely Ammonium Chloride.
Does swim need to evaporated the top layer to get the methylamine or what. I'm confused.Filter the lower crystals and place them aside. take the Meoh mixture and place it in a beaker in the freezer. Methylamine flakes should precipitate.
You have chosen a peculiar and innefficient way to make Methylamine. Choose another way and read more up on the subject.
.......or you could try this
What you will need (scale to suit your needs)
1 x 3 litre 3 neck flask
1 x 2 litre R.B.F.
1 x 1 litre R.B.F.
1 x still head
1 x condenser
1 x vacuum adaptor
1 x thermometer (a good quality one with single degree measurements)
1 x hotplate stirrer
1 x egg shaped stir bar
1 x Buchner funnel
1 x vacuum flask
1 x beaker (or suitable alternative)
1 x vacuum source (aspirator is sufficient)
vari0us stoppers
560 grams Hexamine(4 moles)
1950 mls of 30% Hydrochloric acid (16 moles)
400 mls DH2O
1. In a 3 litre 3 neck flask, set up for standard distillation in an oil bath, upon a hotplate/stirrer, was placed 560 grams of crushed Hexamine, 1950 mls 30% HCl and 400 mls DH2O, with the 2 litre R.B.F. as the recieving flask.
2. In One of the side necks was placed a thermometer that was immersed well into the mixture and the other side neck was sealed up. The still head was also sealed with a stopper.
3. The hotplate stirrer was turned on and stirring and heating was commenced.
4. The temperature was closely watched on the thermometer, as it was raised over a period of 2-3 hours to 103-104 C and held at that temperature for a further 6 hours.
5. After the 6 hour period the amber colored fluid was QUICKLY poured into a large beaker and allowed to cool to room temp.
6. When room temp was achieved, the beaker was noted to have a large amount of precipitated NH4CL. This was quickly filtered offf via Buchner and the remaining distillate was returned to the standard distillation rig. The NH4CL can be placed aside for future use.
7. The heat on the distillation rig was raised and half the liquid volume was distilled off.
8. The contents of the 3 litre 3 neck flask were again QUICKLY poured into a beaker and allowed to cool to room temp, and the distillate was discarded.
9. Upon reaching room temp the contents of the beaker had again precipitated a good amount of NH4Cl. This was again vacuum filtered via buchner and the NH4CL placed aside.
10. The remaining distillate was placed into the 2 litre R.B.F. and the 1 litre R.B.F. was set up to recieve.
11. Standard distillation was again commenced and a third to a half of the volume of the amber liquid is distilled Off until a skin has been noted forming. Then turn off the heat.
12. The contents of the 2 litre flask were QUICKLY poured into a beaker that was sealed with cling wrap. The contents of the 1 Litre recieving flask were discarded.
13. The beaker was allowed to sit for a few hours until room temp was achieved and then moved into the refrigerator.
14. After several hours the beaker was removed to the freezer and left overnight.
15. Next morning, vacuum filter crystals.
16. Dry vacuumed crystals are then covered in DRY acetone and swirled for several minutes and then Vacuum filtered again.
This step may not be necessary if temperature was correctly held at 103-104 for recommended time. Weight of crystals has never altered after acetone washes. 17. Store in a tightly sealed container.
Never less than 330 grams of Methylamine Hydrochloride (~4.9 moles, enough to aminate 290-300 grams MDP2P ), from 560 grams Hexamine, achieved with this method