SU64567A1 - Hydroxylamine release method - Google Patents

Description

One of the conventional methods for producing hydroxylamine is the Raschig-Semon method, which consists of the following steps:

1) reduction of sodium nitrite with sodium bisulfite;

2) hydrolysis of the resulting disulfide} hydroxylamine zone in mono: ulfonate;

4) obtaining the oxime and its distillation;

4) conversion of the oxime to the hydroxylamine salt; isolation and purification of the resulting salt.

The disadvantage of the Raschig-Semon method is the difficulty of purifying the obtained hydroxylamine from ammonia salts formed in the first and second stages of the production process.

The method proposed by the authors eliminates this drawback, thereby increasing the yield of the product and making it possible to obtain reactive varieties of hydroxylamine (p.a. and pure) without further purification.

The difference of the proposed method from those described in the literature and applied in practice lies in the fact that non-acetone dissolved in water in all proportions is used to obtain oxime.

and giving water-soluble oxime, and higher ketones, insoluble in water and forming oximes that are very little soluble in water. The very low solubility of the higher ketone oximes in water makes it possible to wash them with ammonia impurity with water when teaching reactive varieties of hydroxylamine;

The proposed method can be applied to isolate hydroxylamine in all methods for its preparation, as well as from production wastes.

Example 1. To a mixture of 324 g of sodium nitrite and 1200 g of ice, 2250 g of liquid sodium bisphosphate are added, preventing the temperature of the reaction mixture from rising above minus I. After 30 minutes, about 300 ml of sulfuric acid are added to the sodium disulfonate hydroxylamine obtained. . weight 1.37 to an acidic reaction to a piece of paper congo. 585 g of methyl butyl ketone is then added to the solution; after stirring for three hours, the resulting mixture was poured into 5% sodium hydroxide solution (500 ml) and distilled, taking an excess of methyl butyl ketone and the resulting methyl butyl ketoxime.

The product obtained is purified from ammonia by four times washing with water and treated at the boil with a mixture of 1240 ml of distilled water, 390 ml of h. A. hydrochloric acid (sp. in. 1.18) and 5 g of activated carbon, selecting the fraction of methyl butyl ketone at a temperature of 85-99 °. The residue in the flask is filtered, evaporated, and then the hydrochloride hydroxylamine is obtained by suction.

Output hd a and After washing with ethyl alcohol it is about 120 g.

Example 2. Production was carried out as described in Example 1, including the preparation of an oxime, and then instead of stripping, the oxime was separated as an oily layer. Further processing is done.

as indicated in Example I. The resulting product qualifies as technical.

Example 3. In the preparation of oxime, as indicated in examples 1 and 2, a purified fraction of ketones derived from waste from the production of acetone and woody methanol is used.

Subject invention

Claims (2)

1. A method of separating hydroxylamine from an aqueous solution by transferring it to ketoxime, then separating it and decomposing acidic, characterized in that ketones (or their mixtures separated from waste of various derivatives) are used to form ketoxime, whose oximes are slightly soluble in water. 2. A method according to claim 1, characterized in that the oximes obtained are purified from ammonium salts by washing with water.