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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 directions of hydroxylamine, nitrogen and non-metallic compounds, organic chemistry, etc., can solve problems such as low production efficiency, and achieve the effects of increasing unit consumption, reducing circulation, and reducing investment costs

Inactive Publication Date: 2003-05-21
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

[0004] 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

Method used

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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 1

[0021] The composition and content of the raw material inorganic liquid are H 3 PO 4 (20wt%), NH 3 OHH 2 PO 4 (0.75wt%), NH 4 NO 3 20wt%), HNO 3 (2.5wt%), H 2 O (55 wt%).

[0022] 90,000 kg / h of raw material inorganic liquid first enters the first reactor 1 from the middle and lower part of the reactor 1, and reacts with the hydrogen entering the bottom of the first reactor 1 in the presence of a catalyst to generate hydroxylamine with a concentration of 0.8mol / kg, the inorganic liquid containing hydroxylamine overflows from the top of the first reactor 1 and enters the first gas-liquid separator 2, the inorganic liquid containing low concentration hydroxylamine and a small amount of catalyst enters the first filter 3, and the filtered catalyst is sent back to the first filter In the first reactor 1, the inorganic liquid containing low-concentration hydroxylamine enters the mixer 4, mixes with the nitric acid that is supplemented, and then enters the middle and lower ...

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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 through 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 use ammonium hydrogen phosphate as a buffer solution of dilute nitric acid aqueous solution (abbreviated as inorganic liquid) and hydrogen in the presence of bimetallic Pd+Pt / C or monometallic Pd / C catalysts in a single-tower reactor. Reaction, such as the technique reported in literature Moesdijk, C. van de (1979), Thesis,...

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Application Information

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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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