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A kind of method for co-production of biurea and hydroxylamine sulfate

A technology of hydroxylamine sulfate and biuret, applied in chemical instruments and methods, hydroxylamine, nitrogen and non-metallic compounds, etc., can solve the problems of easy thermal decomposition, difficult separation, and difficult comprehensive utilization of hydroxylamine, and achieve the effect of maximizing benefits

Active Publication Date: 2018-10-02
ZHEJIANG HAIHONG HLDG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The process conditions in this process are milder than US24526, but the reaction of hydrogenation of nitrourea to form hydroxylamine salt and semicarbazide salt is a competing reaction, both of which are easily soluble in water, and hydroxylamine is easily decomposed by heat, which makes subsequent separation difficult and difficult. Comprehensive utilization

Method used

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  • A kind of method for co-production of biurea and hydroxylamine sulfate
  • A kind of method for co-production of biurea and hydroxylamine sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 10.5g of nitrourea, 20mL of water, 10mL of sulfuric acid with a concentration of 60% and 0.1g of a Pt / C catalyst with a loading capacity of 5% into the hydrogenation reactor in sequence, and start stirring. Raise the reaction temperature to 20°C and keep the pressure at 0.5Mpa. After the reaction is over, release the pressure, centrifuge and separate the catalyst, neutralize to a sulfuric acid concentration of 10%, and then slowly add sodium cyanate solution dropwise, wherein the sodium cyanate The content was 6.6g, and the resulting white precipitate was filtered, washed, dried and weighed. The filtrate was concentrated and crystallized, and the resulting white crystalline substance was filtered, washed, dried and weighed.

Embodiment 2

[0027] Add 10.5g of nitrourea, 20mL of water, 10mL of 80% sulfuric acid and 0.1g of Pd / C catalyst with a loading capacity of 5% into the hydrogenation reactor in sequence, and start stirring. Raise the reaction temperature to 50°C and keep the pressure at 0.5Mpa. After the reaction is over, release the pressure, centrifuge and separate the catalyst, neutralize to a sulfuric acid concentration of 10%, and then slowly add the sodium cyanate solution dropwise, wherein the sodium cyanate The content was 7.92g, and the resulting white precipitate was filtered, washed, dried and weighed. The filtrate was concentrated and crystallized, and the resulting white crystalline substance was filtered, washed, dried and weighed.

Embodiment 3

[0029] Add 10.5g of nitrourea, 20mL of water, 20mL of sulfuric acid with a concentration of 80% and 0.1g of Pd / Al with a loading capacity of 10% in the hydrogenation reactor 2 o 3 Catalyst, start stirring. Raise the reaction temperature to 50°C and keep the pressure at 1.0Mpa. After the reaction is over, release the pressure, centrifuge and separate the catalyst, neutralize to a sulfuric acid concentration of 10%, and then slowly add the sodium cyanate solution dropwise, wherein the sodium cyanate The content was 7.92g, and the resulting white precipitate was filtered, washed, dried, and its melting point was measured and weighed. The filtrate was concentrated and crystallized, and the resulting white crystalline substance was filtered, washed, dried, and its melting point was measured and weighed.

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Abstract

The invention discloses a method for coproducing biurea and hydroxylamine sulfate. The method comprises the following steps: adding nitrourea, sulfuric acid and a catalyst into a hydrogenation reaction kettle, carrying out reaction while controlling the material proportion, reaction temperature and reaction pressure so as to generate hydroxylamine salt and aminourea salt, carrying out centrifugal separation to remove the catalyst, neutralizing until the system has higher acidity than cyanic acid, and slowly and dropwisely adding a cyanate-containing solution, wherein the aminourea salt and cyanate directly react to generate the solid biurea in the acidic system, and the hydroxylamine salt is converted into hydroxylamine sulfate in the presence of sulfuric acid. The biurea can be used for producing an ADC (azodicarbonamide) foaming agent; and the hydroxylamine sulfate can be used as an analytical reagent and reducer, and can also be used in organic synthesis. The nitrourea is hydrogenated to synthesize the hydroxylamine salt and aminourea salt, and the cyanate is directly added without separating the intermediate product to coproduce the solid biurea and hydroxylamine sulfate, thereby maximizing the benefits.

Description

technical field [0001] The invention relates to the production field of biurea, and mainly relates to a method for co-producing biurea and hydroxylamine sulfate. Background technique [0002] Biurea is an important fine chemical intermediate, mainly used in the production of ADC foaming agent (azodicarbonamide), and can also be used as flame retardant and smoke suppressant, anti-slip agent, fireproof and antimelt of high-grade cables, etc. [0003] At present, the method of producing biurea is mainly formed by condensation of hydrazine hydrate and urea under acidic or acid-free conditions. The patent (application number: 201510149075.0) introduces a new process for synthesizing biurea with semicarbazide. And cyanate solids are added to water, the temperature is controlled, and then acid is slowly added to obtain biurea solids. The process can be operated under normal temperature and pressure, and the yield can reach 100%, while the by-product is sodium salt, which has no po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C281/06C01B21/14
CPCC01B21/1454C07C281/06
Inventor 陈海贤徐智锋董梅
Owner ZHEJIANG HAIHONG HLDG