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Synthesis of methylamine hcl from formaldehyde (large scale)

William Dampier

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1. 10 kg of 40% formaldehyde and 5 kg of ammonium chloride were mixed in a reactor with a distillation head.
2. The mixture was stirred with gradual heating, distilling primary products at 50 *C.
3. When the distillate stopped and removed the mixture was heated to 110 *C.
4. Heating the mixture was continued for 6 hours under stirring.
5. The vacuum was pumped into the reactor and the water was distilled as much as possible.
6. It was added 10 liters of n-butyl alcohol, heated to 100 *C and stirred until the precipitate decreased.
7. The mixture was filtered through a nutsche-filter to separate from an insoluble precipitate (ammonium chloride) and the alcohol solution was returned to the reactor.
8. The alcohol was as distilled as possible under vacuum, the obtained crystals were dried about vacuum and packaged in vacuum packaging in order to avoid hydration. Yield: ~3 kg.
 
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