Method for preparing hydroxylamine or hydroxylamine salt from ketone, ammonia and hydrogen peroxide

A hydrogen peroxide and hydroxylamine salt technology, applied in the direction of hydroxylamine, nitrogen and non-metallic compounds, etc., can solve the problems of high energy consumption, low conversion rate of ketoxime equilibrium, complex process, etc.

Active Publication Date: 2014-11-05
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is a pity that this method also has two problems: firstly, most of the ketoximes in industry are produced by oximating ketones with hydroxylamine, that is, the production of ketoxime needs to consume equimolar amounts of hydroxylamine, which makes the The hydrolysis method of ketoxime to produce hydroxylamine or hydroxylamine salt is meaningless; secondly, the equilibrium conversion rate of hydrolysis reaction of ketoxime is generally low, thus seriously affecting the energy consumption and production efficiency of the hydrolysis process
This method also has a common weakness, that is, the process is complicated and the energy consumption is large.

Method used

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  • Method for preparing hydroxylamine or hydroxylamine salt from ketone, ammonia and hydrogen peroxide
  • Method for preparing hydroxylamine or hydroxylamine salt from ketone, ammonia and hydrogen peroxide
  • Method for preparing hydroxylamine or hydroxylamine salt from ketone, ammonia and hydrogen peroxide

Examples

Experimental program
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Effect test

Embodiment 1

[0090] Example 1: Cyclohexanone-cyclohexane solution, hydrogen peroxide, and circulating water containing titanium-silicon molecular sieves were respectively continuously added to a 1000ml reactor equipped with a mechanical stirring and condensing reflux device through a double plunger micropump. The flow meter is added continuously; the concentration of hydrogen peroxide is 27.5%, the flow rate is 68.0g / h, the mass concentration of cyclohexanone solution is 37.5%, the flow rate is 130.8g / h, the flow rate of circulating water is 285.6g / h, and the flow rate of ammonia gas is 18.7g / h; The temperature is 69°C, and the pressure is maintained at normal pressure; the product overflows out of the reactor, and after separation by decantation, the catalyst is reused with the water phase, and the cyclohexane solution containing cyclohexanone oxime is sent to the storage tank for standby, and is determined by gas chromatography. It is sent into the countercurrent hydrolysis-centrifugal ex...

Embodiment 2

[0091] Embodiment 2: Reaction steps such as embodiment 1, the difference is that the ketoxime in the reaction is butanone oxime. Among them, the conversion rate of butanone oxime is 61.8%, and the selectivity of hydroxylamine sulfate is 99.5%.

Embodiment 3

[0092] Embodiment 3: The reaction steps are as in embodiment 1, the difference is that the inorganic acid in the reaction is hydrochloric acid. The conversion rate of cyclohexanone oxime was 57.2%, and the selectivity of hydroxylamine hydrochloride was 98.9%.

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Abstract

The invention relates to a method for preparing hydroxylamine salt / hydroxylamine from ketone, ammonia and hydrogen peroxide. The method has the following basic characteristics: ketone is used as a cyclic reaction medium, and an organic solvent insoluble or slightly soluble in water is used as a circulating solvent medium; the heterogeneous catalytic ammoximation technology and hydrolysis-extraction coupling technology are integrated to realize hydroxylamine and / or hydroxylamine salt preparation from basic raw materials of ammonia, hydrogen peroxide and inorganic acid.

Description

technical field [0001] The present invention relates to a method for preparing hydroxylamine and / or hydroxylamine salt from ketone, ammonia and hydrogen peroxide. Background technique [0002] The molecular formula of hydroxylamine is NH 2 OH is an unstable white crystal at room temperature and is easy to deliquescence; some studies have shown that divalent or ferric iron salts can catalyze the decomposition of 50% hydroxylamine solution; therefore, hydroxylamine is usually stored, transported and used in the form of aqueous solution or salt. Hydroxylamine salts mainly include hydroxylamine hydrochloride, hydroxylamine sulfate, hydroxylamine phosphate, and hydroxylamine nitrate. Hydroxylamine hydrochloride, hydroxylammonium sulfate and hydroxylamine phosphate are mainly used as intermediates in synthetic industries such as pharmaceuticals, spices, rubber chemicals, dyes, and engineering materials; hydroxylamine nitrate is mainly used in military and nuclear industries, such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
Inventor 罗和安游奎一赵方方彭超谭珊吴剑刘平乐
Owner XIANGTAN UNIV
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