2. Notes

In the preparation of the sodium hypochlorite solution it is quite

necessary that the mixture be kept cold and be alkaline to red

litmus paper at the end of the reaction, if good yields of hydrazine

are to be obtained.

Since iron is an anti-catalyzer, it is necesssary{sic} to use

distilled water throughout the process.

As a viscolizer, a substance such as starch, glycerol, glue or

gelatine may be used; the last, however, gives by far the

most satisfactory results.

In order to obtain a pure white hydrazine sulfate as the

first precipitate, it is necessary to cool the hydrazine solution

thoroughly and filter it twice before the sulfuric acid is added.

Moreover, the sulfuric acid must be added slowly and with stirring.

If these conditions are not followed, material containing

brown particles results.

The mother liquor obtained from the crystallized hydrazine

sulfate contains a small amount of hydrazine. If 200 g.

of copper sulfate are dissolved in water and added to 10 l.

of the filtrates from the above processes, a light-blue crystalline

precipitate of the double salt of copper sulfate and hydrazine

sulfate will be formed after ten hours. This salt, when suspended

in ten times its weight of distilled water and treated with hydrogen

sulfide, decomposes into copper sulfide and hydrazine sulfate.

After the copper salt has been filtered off, the solution

is concentrated until the hydrazine sulfate crystallizes.

The yield of product is small, so that it is hardly advisable

to undertake this recovery in the laboratory.

It is possible for one man, simultaneously evaporating six dishes

of the hydrazine mixture, to turn out from 20 to 25 runs in nine hours.

The time for the evaporation of a solution, such as is mentioned

in the experimental part, with a four-flame Bunsen burner, is two to

three hours; if the evaporation is carried out more slowly than this,

the yield of product is distinctly diminished.

Organic Syntheses An Annual Publication of Satisfactory Methods for the Preparation of Organic Chemicals · 第 51 / 135 题