Preparation of hydrazine hydrate
Preparation of hydrazine hydrate from hydrazine sulfate and potassium hydroxide
To a copper or silver retort a well mixed mixture of 100 g of dry hydrazine sulfate and 100 g of powdered potassium hydroxide and 5 ml of distilled water were placed (distillation flask made of glass also could be used, but molten potassium hydroxide aggressively acts upon glass).
The reaction mixture starts to distill and initially, the heating is unnecessary, but by the end of the reaction for the completion the mixture must be heated. Hydrazine hydrate, in which still contained water, was purified by fractional distillation. Pure hydrazine hydrate was distilled in the range of 117-119° C.
Руководство по препаративной неорганической химии, Г. Брауэра, 236, 1956 (Guide to preparative inorganic chemistry, H. Brauer, 236, 1956)
Preparation of hydrazine hydrate from hydrazine sulfate and sodium hydroxide
In a 750 ml copper flask (A glass flasks cannot be used because of the high temperature required in the distillation.), fitted with a reflux condenser, are placed 200 grams of hydrazine sulfate and 160 grams of sodium hydroxide. 75 ml of water (if less water is used, the yield is lowered, while more water dilutes the hydrazine hydrate without increasing the yield) are added gradually during about 5 minutes through the condenser; the reaction becomes fairly vigorous and care should be taken that none of the vapours· escape from the condenser. The mixture is refluxed for 1.5 hours. The reflux condenser is removed and the the flask is arranged for downward distillation. The product is distilled by heating the flask with a free flame; strong heating is required towards the end in order to drive over the last traces of hydrazine hydrate. The distillate is a clear liquid weighing 175 grams (the hydrazine hydrate is sometimes contaminated with silicic acid from the glass of the condonser, which could be removed by filtration), and contains 40-45% of hydrazine hydrate as shown by titration with standard acid. Hydrazine hydrate may be titrated with standard acid using methyl orange as indicator or about 0.1 gram, accurately weighed, of the hydrazine hydrate solution is diluted with about 100 ml of water, few drops of starch indicator added, and immediately before titration 5 grams of sodium bicarbonate are introduced.
The 40-45% hydrazine hydrate solution may be concentrated as follows. A mixture of 150 grams (or 144 ml) of the hydrazine hydrate solution solution and 230 ml of xylene are distilled using efficient fractionating column. All the xylene passes over with about 85 ml of water and upon distillation of the hydrazine hydrate, about 50 grams of 90-95% hydrazine hydrate are obtained.
Hydrazine hydrate is a strong light-refracting fuming in the air liquid; It has a peculiar smell, unlike the smell of ammonia. With water and alcohol is mixed; not miscible with ether, chloroform and benzene. Boiling point 118.7 ° C / 739.5 mm Hg.
A text book of practical organic chemistry, by A. I. Vogel, 190, 1974
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Hydrazine hydrate, Hydrazine monohydrate, Hydrazinium hydroxide, 7803-57-8, Hydrazine hydroxide, 10217-52-4, HYDRAZINE, MONOHYDRATE, Idrazina idrata [Italian], CCRIS 7739, Hydrazine, hydrate (6CI,7CI), Hydrazine hydrate solution, diamine hydrate, diazane hydrate, Idrazina idrata, hydrazin hydrate, hydrate hydrazine, hydrazine H2O, Hydrazine, hydrate, hydraziniumhydroxide, hydrazine-monohydrate, hydrazine mono hydrate, hydrazine mono-hydrate, mono hydrazine hydrate, PubChem21005, ACMC-1BEVD, hydrazine–water (1/1), AC1L2NL5, KSC182I0B, UNII-KYD297831P, 15622_RIEDEL, 18412_RIEDEL, 225819_ALDRICH, 53847_FLUKA, CHEBI:35511, CTK0I2400, IKDUDTNKRLTJSI-UHFFFAOYSA-N, MolPort-003-926-880, 15622_SIAL, 18412_SIAL, 53847_SIAL, KYD297831P, LTBB002570, 207942_SIAL, 225819_SIAL, STR00022, ANW-37146, AKOS015855338, RL00109, RTR-025027, AK124356, LS-76818, LS-76919, AB0062816, AB1003634, TR-025027, FT-0627110, A839316, I14-13408, Hydrazine hydrate solution 35% in water (22% hydrazine), Hydrazine hydrate solution 55% in water (35% hydrazine), 65209-65-6, 65492-74-2, 79785-97-0
HYDRAZINE, 302-01-2 (Parent), CID24654, 302-01-2