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Method for improving quality of oxammonium hydrochloride

A hydroxylamine hydrochloride, quality technology, applied in the directions of hydroxylamine, nitrogen and non-metallic compounds, can solve the problems of difficulty in meeting the quality standards of pharmaceutical grade hydroxylamine hydrochloride, strict quality requirements of hydroxylamine hydrochloride, and difficulty in cleaning, etc., so as to improve hydroxylamine hydrochloride The effect of quality, improving economic efficiency and simple operation process

Inactive Publication Date: 2010-03-03
SHANDONG XINGHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These impurities are difficult to remove before the product is packaged; in addition, during the storage of the product, due to the presence of impurities, the product will turn yellow to varying degrees
As the raw material of pharmaceutical intermediate products, customers have extremely strict requirements on the quality of hydroxylamine hydrochloride, and it is difficult for industrial products of hydroxylamine hydrochloride produced by the existing technology to meet the quality standards of pharmaceutical grade hydroxylamine hydrochloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The filter is made of polypropylene material with a filter area of ​​4M 2 ; Use polyester filter cloth with a filtration accuracy of 0.074mm; control the vacuum degree -0.05Mpa-0.1Mpa, and the temperature is 80°C-120°C, pass the hydrolyzed hydroxylamine hydrochloride hydrolyzate through the filter, pump it into the concentration tank, and enter the next step craft.

[0021] The obtained product has no black spots and impurities, and does not change color within 2 years of storage.

Embodiment 2

[0023] According to the method and steps of embodiment 1, the difference is that the NYB-4 type high-efficiency plate-type sealed filter is adopted, and the filtration accuracy is 0.15mm; the obtained product has no black spot impurities, and the product is preserved for 2 years without changing color.

Embodiment 3

[0025] According to the method and steps of Example 1, the difference is that the ZX series self-cleaning filter element filter is adopted, and the filter area is 4M 2 ; The obtained product has no black spots and impurities, and the product does not change color after being stored for 2 years.

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PUM

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Abstract

The invention relates to a method for improving the quality of oxammonium hydrochloride, which belongs to preparation of hydroxylamine compounds, in particular to a method for improving the quality ofproducts in the process of preparing the oxammonium hydrochloride. The method is characterized in that: in the conventional oxammonium hydrochloride production technology process, at least one filtering device is added, so that oxammonium hydrochloride solution generated by acidifying and hydrolyzing nitromethane through hydrochloric acid is filtered by the filtering device and then enters a condensation working section. The invention provides a method, which has less investment and simple operation process, eliminates black spots in the products, ensures that products cannot turn yellow in the storage life and obviously improves the quality of the oxammonium hydrochloride. The products have no black spots and impurities and cannot change color after being stored for two years. The invention not only suitable for process improvement on preparing the oxammonium hydrochloride by acidifying and hydrolyzing the nitromethane through the hydrochloric acid, but also suitable for purifying industrial oxammonium hydrochloride products the quality index of which do not reach the reagent level; the industrial oxammonium hydrochloride products are dissolved, filtered and recrystallized according to the conventional recrystallization process to reach the quality standard of the reagent level oxammonium hydrochloride products.

Description

technical field [0001] The invention is a method for improving the quality of hydroxylamine hydrochloride. The invention belongs to the preparation of hydroxylamine compounds, and particularly relates to a method for improving product quality in the preparation process of hydroxylamine hydrochloride. Background technique [0002] Hydroxylamine hydrochloride, colorless needle crystal, is an important chemical raw material for organic synthesis. It is mainly used as a pharmaceutical intermediate in the pharmaceutical industry. In the prior art, the production process of nitromethane and hydrochloric acid hydrolysis is adopted. In the process of hydrolysis, there are many kinds of by-products, as well as impurities that enter with the raw materials, which are difficult to remove. For example, obvious black oil-soluble spots, colorless metallic contamination, etc. These impurities are difficult to remove before the product is packaged; in addition, during the storage of the p...

Claims

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Application Information

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IPC IPC(8): C01B21/14
Inventor 高庆辉侯诗东韩己强
Owner SHANDONG XINGHUI CHEM
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