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A kind of preparation method of hydroxylamine salt

The technology of a hydroxylamine salt and a rectifying column is applied in the field of preparation of hydroxylamine salt, which can solve the problems of low acid utilization rate, inability to prepare high-quality hydroxylamine sulfate, inability to reuse, etc., and achieves high conversion rate, overcoming organic residues, and reaction rate. quick effect

Active Publication Date: 2016-04-06
ZHEJIANG SAINON CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of using this technology is simple, but this method cannot prepare high-quality hydroxylamine sulfate, and the obtained hydroxylamine salt contains organic residues, and the excess acid in the system has a low utilization rate and cannot be reused.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] According to the molar ratio of oxime and 10% sulfuric acid as 1:0.5, weigh 73.2 grams of acetone oxime with a purity of 99.9%, and 490 grams of 10% sulfuric acid, and use the dropping funnel to add it to the rectifying tower from the middle at a speed of 2ml / s. Medium distillation, control the temperature at 50~60°C, the absolute pressure at 0.09MPa, and control the top reflux ratio to 100 (that is, total reflux). After 15 minutes, adjust the top reflux ratio to 1 and the bottom reflux ratio to 5. Part of the still liquid is returned to the rectification section of the rectification tower, circulated for hydrolysis, collected separately, and sampled for analysis. The pH of the tower top liquid was measured to be 7, and the content of the oxime in the organic phase was analyzed to be 0.1% after the tower bottom liquid was extracted with absolute ethanol. Finally, the still liquid was concentrated, crystallized, filtered, and dried to obtain 160 grams of solid hydroxylam...

Embodiment 2

[0029] According to the molar ratio of oxime and 10% sulfuric acid as 1:0.5, weigh 73.2 grams of acetone oxime with a purity of 99.9%, and 490 grams of 10% sulfuric acid, and use the dropping funnel to add it to the rectifying tower from the middle at a speed of 2ml / s. Medium distillation, control the temperature at 50~60°C, the absolute pressure at 0.09MPa, control the top reflux ratio to 100 (that is, total reflux), after 15 minutes, adjust the top reflux ratio to 1, and the tower bottom reflux ratio to 0 ( That is, no circulation), collected separately, and sampled for analysis. The pH of the tower top liquid was measured to be 7, and the content of the oxime in the organic phase was analyzed to be 2.8% after the tower bottom liquid was extracted with absolute ethanol. Finally, the still liquid was concentrated, and after cooling, crystallization, filtration and drying, 151.2 grams of solid hydroxylamine sulfate were obtained. The yield was 97%, and the conversion rate was...

Embodiment 3

[0031] According to the molar ratio of oxime and 20% hydrochloric acid as 1:1, weigh 73.2 grams of acetone oxime with a purity of 99.9%, and 365 grams of 20% hydrochloric acid, and use the dropping funnel to add it to the rectifying tower from the middle at a speed of 2ml / s. Medium distillation, control the temperature at 50~60°C, the absolute pressure at 0.09MPa, control the top reflux ratio to 100 (that is, total reflux), after 15 minutes, adjust the top reflux ratio to 0.5, and the tower bottom reflux ratio to 8, Part of the still liquid is returned to the rectification section of the rectification tower, circulated for hydrolysis, collected separately, and sampled for analysis. The pH of the tower top liquid was measured to be 6.5, and the content of the oxime in the organic phase was analyzed to be 0.3% after the tower bottom liquid was extracted with absolute ethanol. Finally, the still liquid was concentrated, cooled, crystallized, filtered, and dried to obtain 66.6 gra...

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Abstract

The invention relates to a preparation method of a hydroxylamine salt. The existing preparation process of the hydroxylamine salt is complex, the production safety needs to be enhanced and the product stability is poorer. The invention adopts the following technical scheme: firstly well preparing an appropriate amount of acid solution and oxime according to the molar ratio that C=NOH: H is 1: (1-1.3), wherein the mass fraction of the acid solution is 10%-35%; and adding the solution which is well prepared in the first step into a rectifying tower, controlling the absolute pressure of the rectifying tower at 0.095-0.1MPa and keeping the temperature of a tower kettle at 20-130 DEG C to perform distillation, controlling the tower top reflux ratio at 0-4, timely separating fractions, controlling the reflux ratio of the tower kettle at 0-100, circulating part of kettle liquid, and finally concentrating, crystallizing, filtering and drying a product to get the high-quality solid hydroxylamine salt. According to the preparation method disclosed by the invention, the efficiency of the rectifying tower is improved, the reaction rate is promoted, the using quantity of the raw materials is saved, the quality of a crude finished product is optimized, and the organic residues are overcome; and the process flow is short, the raw materials are saved, the yield is high, the product quality is stable, the post-treatment is simple, and the preparation method is environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a preparation method of hydroxylamine salt. Background technique [0002] Hydroxylamine salt is a very versatile chemical product. Hydroxylamine sulfate and hydroxylamine phosphate are mainly used in the production of caprolactam, pesticides, etc.; hydroxylamine hydrochloride is mainly used as raw materials for synthetic industries such as pharmaceuticals, spices, and dyes. [0003] At present, the methods for preparing hydroxylamine sulfate mainly include nitric oxide reduction method, acetone oxime method, hydrolysis, etc.; the methods for preparing hydroxylamine phosphate mainly include hydrogenation catalytic reduction method and hydrolysis method; the methods for preparing hydroxylamine hydrochloride mainly include nitromethane water solution, acetone oxime method, ammonium disulfonate hydrolysis method, etc. Such methods generally have disadvan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/14
Inventor 徐书群
Owner ZHEJIANG SAINON CHEM
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