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Method for preparing hydroxylamine

A hydroxylamine and hydrogen technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., can solve problems such as uneven distribution of feed hydrogen and obstruction of hydroxylamine concentration

Active Publication Date: 2007-10-10
CHINA PETROCHEM DEVMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the hydroxylamine reactor using this air intake method will produce uneven distribution of feed hydrogen, and then wall flow (wall flow), channeling (channeling) and other phenomena will occur in the reactor, which will seriously affect the gas, liquid, and gas in the reaction. The mass transfer between solids prevents the increase of hydroxylamine concentration

Method used

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  • Method for preparing hydroxylamine
  • Method for preparing hydroxylamine
  • Method for preparing hydroxylamine

Examples

Experimental program
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Embodiment 1

[0034] Using the reactor 10 as shown in Figure 2, through the pipeline 22 at 130M per hour 3 The aqueous reaction medium is fed to the hydroxylamine reactor at a flow rate of 0.04 mol / kg of hydroxylamine phosphate, 2.89 mol / kg of hydrogen ion, 2.46 mol / kg of phosphoric acid, and 0.26 mol / kg of free nitric acid. The circulating hydrogen system is introduced into the middle gas distributor 16 of the reactor 10 through the line 24, and the fresh hydrogen system is introduced into the bottom gas distributor 18 of the reactor 10 through the line 26. Under the conditions of a temperature of 53° C. and a hydrogen partial pressure of 55%, a 10% palladium / activated carbon catalyst is used for catalysis to synthesize hydroxylamine phosphate. In the phosphate inorganic treatment solution at the outlet of the hydroxylamine reactor, the synthesized hydroxylamine phosphate concentration is 1.15 mol / kg, the hydroxylamine selectivity is 85.5%, and the catalyst activity is 26.6 g hydroxylamine / hou...

Embodiment 2

[0036] Using the reactor 10 as shown in Figure 4, through the pipeline 22 at 130M per hour 3 The aqueous reaction medium is fed to the hydroxylamine reactor at a flow rate of 0.04 mol / kg of hydroxylamine phosphate, 2.89 mol / kg of hydrogen ion, 2.46 mol / kg of phosphoric acid, and 0.26 mol / kg of free nitric acid. The circulating hydrogen is introduced into the middle gas distributor 16 of the reactor 10 through the line 24, and the fresh hydrogen is introduced into the bottom gas distributor 18 and the upper gas distributor 20 of the reactor 10 through the lines 26 and 28. The bottom gas distributor 18 and the upper gas distributor 20 The ratio of fresh hydrogen in the gas distributor 20 is 2:1. Under the conditions of a temperature of 53° C. and a hydrogen partial pressure of 55%, a 10% palladium / activated carbon catalyst is used for catalysis to synthesize hydroxylamine phosphate. In the phosphate inorganic treatment solution at the outlet of the hydroxylamine reactor, the synthes...

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Abstract

This invention discloses a method for preparing hydroxylamine. The method comprises: feeding nitrate-containing aqueous reaction medium into a reactor, and catalytically reducing nitrate groups with hydrogen to obtain hydroxylamine. The reactor comprises: a hydroxylamine reaction region, a cooler at bottom, and a middle gas distributor and a bottom gas distributor set above and below the cooler, respectively, for introducing hydrogen, which can improve the uniformity of hydrogen distributed in the reactor. Therefore, the gas-liquid-solid mass transfer is effectively performed, thus the catalyst activity is improved, the reaction selectivity is improved, and high-concentration hydroxylamine is obtained.

Description

Technical field [0001] The present invention relates to a method for producing hydroxylamine. More specifically, it relates to a method for producing hydroxylamine by reducing nitrate ions with hydrogen. Background technique [0002] Caprolactam is an important raw material for the manufacture of polyamide (also known as nylon). The traditional method for preparing caprolactam is to use the hydroxylamine oxime process to oximize hydroxylamine and cyclohexanone to obtain cyclohexanone oxime, and then make cyclohexanone oxime be produced by Beckmann rearrangement. Caprolactam. Therefore, the preparation of hydroxylamine has become a key technology for the production of caprolactam. The reaction for producing hydroxylamine is mainly prepared by using monometallic palladium / carbon or bimetallic palladium-platinum / carbon as a catalyst, and using hydrogen to catalytically reduce nitrate in a phosphoric acid buffer solution. However, pure hydroxylamine is an unstable structure, which au...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C215/00
Inventor 杨树鸿罗守礼
Owner CHINA PETROCHEM DEVMENT