Preparation method of solid hydroxylamine sulfate

A hydroxylamine sulfate and solid technology, applied in the field of preparation of solid hydroxylamine sulfate, can solve the problems of non-compliance with safety production and environmental protection requirements, complex process route, long process flow, etc., and achieves low production cost, short process flow, and improved adsorption effect. Effect

Active Publication Date: 2020-06-16
ZHEJIANG JINHUA NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The yields provided by the above technologies and existing patents are low, and there are disadvantages such as complex process routes, long proces...

Method used

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  • Preparation method of solid hydroxylamine sulfate

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Effect test

Embodiment 1

[0023] A preparation method of solid hydroxylamine sulfate, its operation steps are:

[0024] Add 20Kg of concentrated sulfuric acid into the mixing kettle, then add pure water to dilute the sulfuric acid concentration to 20%, stir and mix evenly, add 38Kg of butanone oxime into the mixing kettle, after stirring and mixing, add the feed liquid into the reactor, the reactor Use forced circulation heating, temperature control at 70°C, and reaction time of 5 hours to generate hydroxylamine sulfate and butanone; after the reaction is completed, control the vacuum degree to 0.06MPa, distill the butanone under reduced pressure, and then put the remaining reaction liquid into the separator for stratification. Coarsely separate the organic and inorganic phases, put the obtained lower inorganic phase (hydroxylamine sulfate solution) into the organic matter removal tower, remove the remaining organic matter, and then heat and concentrate the obtained hydroxylamine sulfate mother liquor t...

Embodiment 2

[0032] A preparation method of solid hydroxylamine sulfate, its operation steps are:

[0033] Add 30Kg of concentrated sulfuric acid into the mixing tank, then add pure water to dilute the concentration of sulfuric acid to 30%, stir and mix evenly, add 80Kg of butanone oxime into the mixing tank, after stirring and mixing, add the feed liquid into the reactor, the reactor Use forced circulation heating, temperature control at 85°C, and reaction time of 8 hours to generate hydroxylamine sulfate and butanone; after completing the reaction, control the vacuum degree to 0.08MPa, distill the butanone under reduced pressure, and then put the remaining reaction liquid into the separator for stratification. Coarsely divide the organic and inorganic phases, and enter the obtained lower inorganic phase (hydroxylamine sulfate solution) into the organic matter removal tower to remove the remaining organic matter, and then heat and concentrate the obtained hydroxylamine sulfate mother liquo...

Embodiment 3

[0041] A preparation method of solid hydroxylamine sulfate, its operation steps are:

[0042] Add 40Kg of concentrated sulfuric acid into the mixing kettle, then add pure water to dilute the sulfuric acid concentration to 40%, stir and mix evenly, add 150Kg of butanone oxime into the mixing kettle, after stirring and mixing, add the feed liquid into the reactor, the reactor Use forced circulation heating, temperature control at 95°C, and reaction time of 10 hours to generate hydroxylamine sulfate and butanone; after the reaction is completed, control the vacuum degree to 0.1MPa, distill the butanone under reduced pressure, and then put the remaining reaction liquid into the separator for stratification. Coarsely divide the organic and inorganic phases, and enter the obtained lower inorganic phase (hydroxylamine sulfate solution) into the organic matter removal tower to remove the remaining organic matter, and then heat and concentrate the obtained hydroxylamine sulfate mother l...

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Abstract

The invention relates to the field of chemical engineering, and in particular, relates to a preparation method of solid hydroxylamine sulfate. According to the preparation method of the solid hydroxylamine sulfate through the reaction of sulfuric acid and diacetylmonoxime, conventional reagents are used in the method, no toxic raw material is used, the reaction process conditions are mild, the technological process is short, the production cost is low, a byproduct butanone can be generated, and the method is economical and environmentally friendly; the recyclable metal-doped graphene adsorbingmaterial is adopted, organic residues in a hydroxylamine sulfate solution can be efficiently adsorbed by utilizing a strong complexing effect between metal ions and diacetylmonoxime, and the method has the advantages of energy conservation, environmental protection and high utilization rate.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of solid hydroxylamine sulfate. Background technique [0002] Hydroxylamine sulfate is often used as analytical reagent, reducing agent, film, photofinishing medicine, and also used in organic synthesis. It has a wide range of uses. The traditional preparation methods of hydroxylamine sulfate mainly include nitromethane method, acetone oxime method, nitric oxide reduction method, ammonium disulfonate hydrolysis method, etc. [0003] 201710912030.3 discloses a preparation method of hydroxylamine sulfate, which includes the following steps: 1), after uniformly mixing the acid solution and oxime as raw materials, enter the reactive distillation tower for rectification, and get hydroxylamine sulfate and unreacted oxime and A mixed solution of acid; 2), the mixed solution obtained in the tower kettle is partially transported to a stripping tower with a pump to re...

Claims

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Application Information

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IPC IPC(8): C01B21/14B01J20/22C07C45/65C07C45/82C07C49/10
CPCC01B21/1454C01B21/1481B01J20/22B01J20/20C07C45/65C07C45/82C01P2006/80C07C49/10Y02P20/10
Inventor 段仲刚周强张军良王雄张则瑜
Owner ZHEJIANG JINHUA NEW MATERIALS
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