Hydrochloric Acid → HCID 178513185, compound

Temperature

25 °C

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.

1. temperaturecooling over 30 min
2. customwas metered in over ~30 min in 5-lb increments
3. temperaturewhile maintaining the reaction temperature at ~85° C
4. customReaction
5. customfrom 80° to 103° C.
6. temperatureThereafter, with full reactor cooling
7. temperaturethe temperature was maintained at 80°-85° C. range
8. additionduring remainder of addition
9. stirringThe mixture was stirred at 85° C. for 2 hrs
10. stirringwas stirred overnight
11. customThe white solid product was isolated by centrifugation
12. washwashed with water (4 gal)
13. customA final centrifugation gave 82 lbs of wet-cake which
14. customwas dried in a vacuum oven at ~35° C.
15. additioncharged

ORD record

ord-e1b9678464814daaa71620a359f23662

Source dataset

uspto-grants-1986_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04565014