Hydrochloric Acid → HCID 178513185, compound

Participants

Reaction Conditions

Reaction Steps

Hydrazine hydrate (64% hydrazine, 20 lbs, 0.4-mole) was charged to a 30-gal glass-lined reactor and hydrochloric acid (32.1%, 45.4 lbs, 0.4 lb-mole) was added to it with stirring and cooling over 30 min. The resulting hydrazine hydrochloride solution was heated to 80° C. and cyanamide (50%, 36 lbs, 0.43 lb-mole) was metered in over ~30 min in 5-lb increments while maintaining the reaction temperature at ~85° C. Reaction is exothermic; introduction of an initial 7-lb charge of H2NCN caused a temperature excursion from 80° to 103° C. during the first minute. Thereafter, with full reactor cooling, the temperature was maintained at 80°-85° C. range during remainder of addition. The mixture was stirred at 85° C. for 2 hrs, then cooled to 25° C. and the pH measured, which showed a value of 7.6. A slurry of sodium bicarbonate (35 lbs, 0.42 lb-mole) in 65 lbs of water was added all at once and the reaction was stirred overnight. The white solid product was isolated by centrifugation, washed with water (4 gal), then returned to the reactor and resuspended with 150 lbs fresh water. A final centrifugation gave 82 lbs of wet-cake which was dried in a vacuum oven at ~35° C. and 29 in Hg. Assay of the dried material showed 99% AGB, for an overall yield of 96% based on hydrazine charged.

Provenance & Evidence