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Method for prepn. of high concentration hydroxymaline in the prodn. process of hexanolactam

A production process, caprolactam technology, applied in the fields of hydroxylamine, nitrogen and non-metallic compounds, organic chemistry, etc., can solve the problems of low production efficiency, achieve the effect of increased unit consumption, increased concentration of hydroxylamine, and reduced investment costs

Inactive Publication Date: 2004-10-06
中国石油化工股份有限公司巴陵分公司 +1
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Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide a method for preparing high-concentration hydroxylamine in the production process of caprolactam, so as to overcome the defects of low production efficiency in the prior art

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  • Method for prepn. of high concentration hydroxymaline in the prodn. process of hexanolactam
  • Method for prepn. of high concentration hydroxymaline in the prodn. process of hexanolactam

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Embodiment Construction

[0013] See figure 1 , The raw material inorganic liquid first enters the first reactor 1 from the middle and lower part of the first reactor 1, and reacts with the hydrogen entering the bottom of the first reactor 1 in the presence of a catalyst to generate hydroxylamine. The inorganic liquid containing hydroxylamine is reacted from the first reactor 1 After the top of the reactor 1 overflows, it enters the first gas-liquid separator 2. The inorganic liquid containing low concentration of hydroxylamine and a small amount of catalyst enters the first filter 3. The filtered catalyst is sent back to the first reactor 1. The liquid enters the mixer 4, is mixed with the supplementary nitric acid, and then enters the middle and lower part of the second reactor 5, and continues to react with the hydrogen entering the bottom of the second reactor 5 in the presence of a catalyst to make the hydroxylamine in the inorganic liquid The concentration increases from 0.7~0.85mol / kg to 1.3-1.35mol...

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Abstract

The method for preparing high-concentration hydroxylamine in the course of production of caprolactam adopts series-connection of two reactors, and adopts high superficial velocity, and adds a liquid-liquid quick mixer between two reactors to quicken micromixing of intermediate supplemental nitric acid and first reactor outlet inorganic liquid so as to obviously raise concentration of hydroxylamine and reduce circulation quantity of inorganic liquid, and can reduce operation cost, and can retain high reaction selectivity.

Description

Technical field [0001] The invention relates to a method for preparing high-concentration hydroxylamine, in particular to a method for generating hydroxylamine by hydrogenation and reduction of nitrate. Background technique [0002] Caprolactam is an important chemical raw material and a monomer for the synthesis of nylon 6 and engineering plastics. The cyclohexanone-hydroxylamine method is currently the main process for preparing caprolactam. Therefore, in the production process of caprolactam, the production of hydroxylamine will directly affect the production cost and output of caprolactam. The traditional production method of hydroxylamine is to carry out a dilute aqueous nitric acid solution (inorganic liquid for short) with ammonium hydrogen phosphate as a buffer and hydrogen in the presence of a bimetallic Pd+Pt / C or a single metal Pd / C catalyst in a single-tower reactor. Reaction, such as the technique reported in the literature Moesdijk, C. van de (1979), Thesis, THEindh...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/14C07D223/10
Inventor 顾雄毅熊烨杨立新沈瀛坪朱泽华张晖程立泉谯荣
Owner 中国石油化工股份有限公司巴陵分公司
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