The preparation methods
[Method 1]
The preparation method is to add water into the reactor, add sodium nitrite under agitation, add sodium metabisulfite, and then acidify with sulfuric acid. The acidified material was fed into the hydrolysis kettle, acetone was added, and then neutralized with liquid alkali, and the neutralized liquid was distilled to obtain acetone oxime. Acetone oxime and hydrochloric acid were added into the salt kettle to react to form hydroxylamine hydrochloride and acetone. Acetone recovery and use; Hydroxylamine hydrochloride through concentration, cooling crystallization, centrifugal separation, drying, can be finished. Reaction equation: NaNO2[NaHSO3]→[H2SO4]HON(SO3Na)2[(CH3)2CH]→HON=C(CH3)2[HCl]→NH2OH·HCl
Another method of production is the nitromethane process. Hydroxylamine hydrochloride was prepared by reaction of nitromethane with hydrochloric acid. Reaction equation: CH3NO2[HCl]→[H2O]NH2OH·HCl
[Method 2]
The oximation method first adds a certain amount of water, a certain amount of sodium nitrite under agitation, and a certain amount of sodium metabisulfite, and then acidifies with sulfuric acid. After acidification, the material liquid was fed into the hydrolytic kettle, a certain amount of acetone was added, and then the liquid alkali was added for neutralization. The neutralizing liquid is drawn into the distillation kettle to distill acetone oxime. Acetone oxime and hydrochloric acid of a certain ratio were added into the salt concentration kettle for reaction to produce hydroxylamine hydrochloride and acetone. Acetone recovery for water supply. Hydroxylamine hydrochloride was concentrated, cooled, crystallized, centrifuged and dried to produce hydroxylamine hydrochloride finished products. its
Nahso3 Na2S2O5 + H2O - > 2
NaNO2 + 2 nahs3 - HON (SO3Na) 2 + NaOH
NaOH + - H2SO4 - NaHSO4 + H2O
HON (SO3Na) 2 + co + H2O (CH3) 2 - (CH3) 2 cnoh nahso4 + 2
(CH3) 2 cnoh + HCl + H2O and NH2OH · HCl + (CH3) 2 co
[Method 3]
1. Sodium nitrite synthesis (oximation method) Add water to the reactor, add sodium nitrite under agitation, add sodium pyrosulfite in stages, and then acidify with sulfuric acid. The acidified material was fed into the hydrolysis kettle, acetone was added, and then neutralized with liquid alkali, and the neutralized liquid was distilled to obtain acetone oxime. Acetone oxime and hydrochloric acid were added into the salt kettle to react to form hydroxylamine hydrochloride and acetone. Acetone recovery and use; Hydroxylamine hydrochloride through concentration, cooling crystallization, centrifugal separation, drying, can be finished. Raw material consumption norm: sodium nitrite (95%) 1970kg/t, sodium metabisulfite (64% SO2) 5418kg/t, acetone (98%) 1175kg/t. 2. Nitromethane process nitromethane interacts with hydrochloric acid and water to produce hydroxylamine hydrochloride. According to HGB3044-76, hydroxylamine hydrochloride product is white crystal, the content of grade 2 product ≥98.5, the content of grade 3 product ≥97%. Raw material consumption quota: nitromethane 1200kg/t, hydrochloric acid (30%) 1500kg/t.