DE2343052A1 - Aluminium salt of N-nitroso-N-cyclohexyl-hydroxylamine prodn. - by reaction between corresp. alkali salt and aluminium salt of strong acid - Google Patents

Abstract

Prodn. of aluminium salt of N-nitroso-N-cyclohexyl-hydroxylamine by exchange reaction between an alkali salt of N-nitroso-N-cyclohexylhydroxylamine and an aluminium sal of a mineral acid, in soln. is improved in that a neutral soln. of the alkali salt and a strongly acidic soln. of the aluminium salt are mixed together. Under these conditions the formative of a by-prod. contg. a polyaluminate ion (as in the conventional process) is avoided.

Description

BASB ¹ Aktiengesellschaft

Our reference: O.Z. ^ O 072 Sws / Wil 6700 Ludwigshafen, 23-8.1975

Process for the preparation of the aluminum salt of N-Nitroso-N-

cyclohexylhydroxylamine ^

The present invention relates to a valuable new process for the preparation of the aluminum salt of N-nitroso-N-cyclohexylhydroxylamine under control of the pH.

It is known that from the aqueous solution of the N-nitroso-N-cyclohexylhydroxylamine potassium salt by double reaction with aluminum salts of mineral acids, for example aluminum chloride or aluminum sulfate, the N-Nltroso-N-cyclohexylhydroxylamine alurainium salt receives.

The procedure is that a dilute aqueous solution of the potassium salt is ^{cooled to 0} ° C., the potassium hydroxide solution present in the solution is neutralized and an aqueous solution of an aluminum salt of a mineral acid is added.

The resulting precipitate is separated off, washed with water and dried at low temperature.

It was found that in this precipitation of the M-nitroso-N-cyclohexylhydroxylamine aluminum salt, it creates a by-product having a melting point of about 36O ⁰ C.

It is assumed that the alurainate ion Al (OHK ¹ (similar to the silication) condenses to polyaluminants with the escape of water, including one mole of N-nitroso-N-cyclohexylhydroxylamine

/ "AI (OH) ₃ -O-AI (OH) ₂ -O-AI (OH) ₂ -O-AI (Oh) ₃ J ⁷ ". ^{1 f}

It has been found that this by-product does not occur if an approximately neutral solution of the above is used for the reaction Alkali salt and a strongly acidic solution of the aluminum salt are used. Among the alkali salt is the potassium or sodium

509813/1054

- dd - O.Z. 30 072

to understand salt or their mongrel. The potassium salt is preferred. The mineral acid is to be understood as meaning hydrochloric acid, sulfuric acid or nitric acid. Sulfuric acid is preferred.

A roughly neutral solution is a solution with a pH of 6.5 to 8. The pH range 7 to 8 is preferred. A strongly acidic solution is a solution with a pH of 1 to 2.5 » the pH range 1.5 to 2 is preferred.

example

30 parts (parts by weight) of a 30% (percent by weight) aqueous solution of the N-nitroso-N-cyclohexylhydroxylamine potassium salt are diluted with 30 parts of water and adjusted to a pH of 7 to 8 by adding dilute sulfuric acid (50%) set. The solution is cooled to ⁰ ° C. and a solution of 11.1 parts of Al ₂ (SO ₁ ^) ^ χ 18 H ₃ O and 25 parts of water is brought to pH with dilute sulfuric acid (50%) from 1.5 to 2 has been set to run rapidly. The resulting precipitate is filtered off after stirring for one hour, free of sulfate gewasohen with water and dried at 6O ⁰ C to 65.

7.5 parts of N-nitroso-N-cyclohexylhydroxylamine aluminum salt are obtained, which is free from the above-mentioned by-product.

/ 3 509813/1 054

Claims (1)

- 1 - O.Z. 30 072 Claim Process for the preparation of the aluminum salt of N-nitroso-N-cyclohexylhydroxylamine by double reaction of an aqueous solution of an alkali metal salt of N-nitroso-N-cyclohexylhydroxylamine with the aqueous solution of an alurainium salt of a mineral acid, characterized in that an approximately neutral solution is used for the reaction of the above-mentioned alkali salt and a strongly acidic solution of the aluminum salt are used. BASF Aktiengesellschaft. Stsj 509813/1054