Synthesis of hydrazine sulfate

Preparation of hydrazine sulfate

Hydrazine sulfate is used to prepare hydrazine hydrate and anhydrous hydrazine.

Preparation of hydrazine sulfate from ammonia and sodium hypochlorite

Preparation of hydrazine sulfate from ammonia and sodium hypochlorite

Preparation of hydrazine sulfate from ammonia and sodium hypochlorite

Eight grams of sodium hydroxide pellets are dissolved in 50 ml of water and 50 g of crushed ice are added when the solution has cooled. The alkaline liquid is poured into a 250 ml suction flask fitted with a stopper and a gas inlet tube leading well into the mixture. A good current of chlorine is passed in while the flask is cooled in ice until the gain in weight is 6 g. As no excess of chlorine must be present this weight of chlorine is somewhat less than the theoretical amount required. Two grams of gelatin are dissolved in 15 ml of hot water diluted with cold water to 50 ml and mixed with 165 ml of concentrated aqueous ammonia contained in a one-liter Erlenmeyer flask. The prepared sodium hypochlo­rite solution is now added; the slight evolution of nitrogen soon ceases. The entire reaction mixture is immediately heated to the boiling point and then evaporated rapidly in a smaller vessel over a free flame until the volume is about 90 ml. The solution is cooled in ice while concentrated sul­furic acid is added dropwise from a separatory funnel until no more product crystallizes out. About 25 ml of acid are required. The mixture is allowed to stand in the cooling bath until the material has settled well (about 15 minutes), then suction-filtered, pressed well, washed first with 15 ml of 2M sulfuric acid and then with 25 ml of alcohol. It is dried in air. The yield of hydrazine sulfate 5-6 g.

Inorganic laboratory preparations, by G. G. Schlessinger, 74-76, 1962

Preparation of hydrazine sulfate is presented in the following video by Doug’s Lab.

Preparation of hydrazine sulfate from aminomethanedisulfonic acid

Preparation of hydrazine sulfate from aminomethanedisulfonic acid

Preparation of hydrazine sulfate from aminomethanedisulfonic acid

Twenty-three grams of the potassium aminomethanedisulfonic acid are stirred to a paste with 34 ml of water and mixed with a solution of 10 g of potassium nitrite in 6 ml of water. The mixture warms up to 40-50°C and within 10 to 15 minutes all the solid material has dissolved. The solution is made alkaline to litmus with 6N potassium hydroxide solution and cooled in ice. The orange-yellow crystals of potassium diazomethanedisulfonate are filtered off without washing. This moist product is dissolved in a solution of 18 g of sodium sulfite 7-hydrate in 12 ml of water, and the solution is made alkaline if necessary with dilute aqueous sodium carbonate, then warmed gently on the steam bath until the yellow color has disappeared. Ninety grams of 20 % sul­furic acid are now added to the warm liquid and the reaction mixture is heated until the odor of sulfur dioxide has gone. On cooling in ice, the hydrazine sulfate crystallizes out. The crystals are filtered, washed first with 2M sulfuric acid and then with alcohol. It is dried in air. The mother-liquor may be concentrated to yield of hydrazine sulfate. Total yield of hydrazine sulfate is about 7 g with melting point 254° C.

Inorganic laboratory preparations, by G. G. Schlessinger, 74-76, 1962

IUPAC Name

hydrazine;sulfuric acid

InChI

InChI=1S/H4N2.H2O4S/c1-2;1-5(2,3)4/h1-2H2;(H2,1,2,3,4)

InChI Key

ZGCHATBSUIJLRL-UHFFFAOYSA-N

Canonical SMILES

NN.OS(=O)(=O)O

MeSH Synonyms

hydrazine, hydrazine dihydrochloride, hydrazine hydrate, hydrazine monohydrate, hydrazine mononitrate, hydrazine nitrate, hydrazine phosphate (1:1), hydrazine phosphate (2:1), hydrazine sulfate, hydrazine sulfate (1:1) monosodium salt, hydrazine sulfate (2:1), hydrazine tartrate, segidrin

Depositor-Supplied Synonyms

Hydrazine sulfate, Hydrazine monosulfate, Hydrazine sulphate, Hydrazine, sulfate, 10034-93-2, Hydrazinium sulfate, Hydrazonium sulfate, Hydrazine sulfate (1:1), Hydrazine, sulfate (1:1), Segidrin, Sehydrin, Diamine sulfate, hydrazine; sulfuric acid, Siran hydrazinu, Idrazina solfato, Hydrazinium(2+) sulfate, Diamidogen sulfate, Hydrazine dihydrogen sulfate salt, HYDRAZINE HYDROGEN SULFATE, Siran hydrazinu [Czech], Hydrazine sulfate (VAN), Hydrazinium(2+) sulphate, Idrazina solfato [Italian], NSC-150014, CCRIS 336, UNII-1N369SAT01, HSDB 5086, EINECS 233-110-4, NSC150014, NSC 150014, NSC 215190, Hydrazine sulfate salt, AI3-18433, 1184-66-3, HS, WLN: ZZ &S-O4, hydrazinium bisulfate, diamine; sulfuric acid, PubChem15719, ACMC-20akr3, AC1L2NPQ, DSSTox_CID_703, Hydrazine dihydrogen sulfate, hydrazinium hydrogen sulfate, H4766_ALDRICH, DSSTox_RID_75745, DSSTox_GSID_20703, Idrazina solfato [Italian], KSC159Q6P, H4766_SIGMA, Hydrazine and hydrazine sulfate, 455865_ALDRICH, CHEMBL1981828, 53900_FLUKA, CTK0F9867, MolPort-003-927-920, ZGCHATBSUIJLRL-UHFFFAOYSA-N, 1N369SAT01, 53900_SIAL, 216046_SIAL, Tox21_302995, LS-318, NSC215190, AKOS015901874, NSC-215190, Hydrazinium sulfate, Hydrazonium sulfate, NCGC00256445-01, NCI60_001038, SC-65219, CAS-10034-93-2, DB-029899, RT-000235, FT-0624941, 3B4-4095, I14-13839, I14-60487, 95416-15-2

Removed Synonyms

Hydrazine hemisulfate salt, 302-01-2 (Parent), 1184-66-3 (sulfate), 10034-93-2 (Parent), CID24842, 13464-80-7 (sulfate[2:1]), 88491-70-7

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