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Preparation method of hydroxylamine sulfate

A technology of hydroxylamine sulfate and sulfuric acid, which is applied in the chemical industry, can solve the problems of excessive acid in reactants, high energy consumption of distilled water, waste of raw materials, etc., and achieve the effects of avoiding side reactions, increasing the utilization rate of raw materials, and improving the total yield

Active Publication Date: 2017-07-14
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

[0006] Although the above two Chinese patent applications all disclose the method for preparing hydroxylamine sulfate by reactive distillation, the acid oxime in the whole preparation process is relatively large, and the reactant acid is excessive, resulting in waste of raw materials, and the energy consumption of distilling water is relatively large. The crystallization of hydroxylamine sulfate needs to be cooled down, and the energy consumption of the rectification and crystallization process is relatively high

Method used

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  • Preparation method of hydroxylamine sulfate

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Effect test

Embodiment 1

[0034] Butanone oxime, 50wt% sulfuric acid aqueous solution according to butanone oxime and H 2 SO 4 The molar ratio is 1:0.5 (the molar ratio of butanone oxime and the aqueous sulfuric acid solution is 0.367:1). Weigh 435.6g and 490g respectively, add them to the reaction kettle for reactive distillation, and control the pressure of the reactive distillation system in the reactor to 0.028-0.055MPa, the temperature of the tower bottom is 80-85°C, the top reflux ratio is 0-6, and the butanone distilled from the top of the rectification tower is removed in time. After four hours of reactive distillation, take a sample from the tower kettle periodically (for example, every hour), and titrate the concentrations of sulfuric acid and hydroxylamine sulfate therein. After reacting for seven hours, when the hydroxylamine sulfate concentration was 5mol / L, the reaction solution was transferred to a crystallization tank for crystallization. The crystals were filtered twice, and the crys...

Embodiment 2

[0036] Butanone oxime, 55wt% sulfuric acid aqueous solution according to butanone oxime and H 2 SO 4 The molar ratio is 1:0.5 (the molar ratio of butanone oxime and sulfuric acid aqueous solution is 0.449:1). Weigh 348.48g and 356.36g respectively, add them to the reaction kettle for reactive distillation, and control the pressure of the reactive distillation system in the tower reactor 0.030-0.055MPa, the temperature of the tower bottom is 80-85°C, the top reflux ratio is 0-6, and the butanone distilled from the top of the rectification tower is removed in time. After four hours of reactive distillation, take a sample from the tower kettle periodically (for example, every hour), and titrate the concentrations of sulfuric acid and hydroxylamine sulfate therein. After seven hours of reaction, when the concentration of hydroxylamine sulfate was 5 mol / L, the temperature of the reaction system was lowered to 50° C. and the reaction solution was transferred to a crystallization ta...

Embodiment 3

[0038] Butanone oxime, 60wt% sulfuric acid aqueous solution according to butanone oxime and H 2 SO 4 The molar ratio is 1:0.5 (the molar ratio of butanone oxime and sulfuric acid aqueous solution is 0.551:1). Weigh 435.6g and 408.33g respectively, add them to the reaction kettle for reactive distillation, and control the pressure of the reaction distillation system in the tower reactor 0.025 ~ 0.055MPa, the temperature of the tower bottom is 80 ~ 90 ° C, the top reflux ratio is 0 ~ 6, and the butanone distilled from the top of the rectification tower is removed in time. After four hours of reactive distillation, take a sample from the tower kettle periodically (for example, every hour), and titrate the concentrations of sulfuric acid and hydroxylamine sulfate therein. After reacting for seven hours, when the hydroxylamine sulfate concentration was 4mol / L, the reaction solution was transferred to a crystallization tank for crystallization. The crystals were filtered twice, an...

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Abstract

The invention belongs to the field of chemical engineering and relates to a preparation method of hydroxylamine sulfate. In the preparation method, sulfuric acid and ketoxime are employed as raw materials for producing the hydroxylamine sulfate in a reactive rectification system. The preparation method includes the steps of: (1) adding a sulfuric acid solution and ketoxime to the reactive rectification system to perform reactive rectification; (2) successively withdrawing a distillate from the column top of the reactive rectification system, when concentration of the hydroxylamine sulfate in the reaction liquid reaches 2-8.5 mol / L, performing crystallization and filtration at the same time; and (3) reducing the temperature of the reaction liquid and performing crystallization and filtration. The method for producing the hydroxylamine sulfate is greatly reduced in production energy consumption and achieves zero-emission of process wastewater.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a preparation method of hydroxylamine sulfate. Background technique [0002] Hydroxylamine sulfate is a chemical product with a wide range of uses, which can be used to synthesize pesticide raw materials, pharmaceutical raw materials, rubber additive raw materials, natural rubber stabilizers, metal treatment agents, fiber modifiers, developers, reducing agents and polymer catalysts, etc. . [0003] The traditional preparation methods of hydroxylamine sulfate mainly include nitromethane method, natural gas (methane) nitration method, nitric oxide reduction method, ammonium disulfonate hydrolysis method and the like. However, the product yield of the nitromethane method is low, there are many types of by-products, and the investment in separation equipment is large; although the production process of the ammonium disulfonate hydrolysis method is mature, it is only suitable for large-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
CPCC01B21/1409C01P2006/80Y02P20/10
Inventor 张卫东刘乐乐杜昕洋龙波
Owner BEIJING UNIV OF CHEM TECH
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