Method for generating hydroxylamine by cyclohexanone-oxime through hydrolyzing

Abstract

The invention relates to a method for generating hydroxylamine by cyclohexanone-oxime through hydrolyzing. The method comprises the following steps of adding cyclohexanone-oxime, a catalyst and deionized water into a reactor, stirring, refluxing, condensing, and reacting for 0.5 to 2h at the temperature of 15 to 25 DEG C, so as to obtain the hydroxylamine; adding an methylbenzene extracting agent into the reactor, extracting at the reaction temperature, extracting an organic phase from a reaction liquid, and extracting a water phase, so as to obtain a product, namely a hydroxylamine water solution, wherein the catalyst is HZSM-5, silicotungstic acid, phosphotungstic acid or phosphomolybdic acid with a ratio of silicon to aluminum (silicon dioxide / aluminum oxide)) is 25 to 50. The method has the advantages that the reaction conditions are moderate, the operation is simple, the energy consumption is decreased, the environment-friendly and economical meanings are realized, and the environment-friendly catalyzing reaction process is performed.

Description

technical field [0001] The invention relates to a method for producing hydroxylamine (aqueous solution), in particular to a process for preparing hydroxylamine (aqueous solution) through hydrolysis of cyclohexanone oxime catalyzed by a solid acid. Background technique [0002] Hydroxylamine is a reducing agent in organic synthesis, which condenses with carbonyl compounds to form oximes. The molecular formula for hydroxylamine is NH 2 OH, can be seen as NH 3 A derivative formed by replacing one of the protons with a hydroxyl group is an unstable white crystal at room temperature, easy to deliquescence, and often exists in the form of aqueous solution. Hydroxylamine has two isomers, cis and trans. It is trans in the solid state, and may be a mixture of cis and trans in the gaseous state (Chinese patent, 201310082379.0). Hydroxylamine is an important chemical intermediate, which is widely used in the manufacture of nylon 66, ink, pigment, drug, pesticide, etc. At present, t...

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Problems solved by technology

[0008] Aiming at the difficulties in the continuous production of the above-mentioned liquid acids, the corrosion of equipment, the difficulty in recycling waste acid, the pollution of the environment by discharge, and the difficulty in separating catalysts from products, the present invention provides a method for preparing hydroxylamine by hydrolysis of cyclohexanone oxime. method

The invention solves the problems of corrosion of equipment and separation from products when liquid acids such as sulfuric acid, hydrochloric acid, and nitric acid are used as catalysts. The reaction conditions are mild, the operation is simple, and energy consumption is saved. The solid acid catalyst has good stability. and reusability, with environmental protection and economic significance, is an environmentally friendly catalytic reaction process

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