Preparation of hydrazine hydrate

Preparation of hydrazine hydrate from hydrazine sulfate and potassium

hydroxide

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).

A glass apparatus for the preparation of hydrazine hydrate

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

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.