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A kind of refining method of methoxyamine hydrochloride

A kind of technology of methoxyamine hydrochloride and refining method, applied in the refining field of methoxyamine hydrochloride, can solve problems such as affecting product quality

Active Publication Date: 2022-05-27
ZHEJIANG JINHUA NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The method of producing methoxyamine hydrochloride by hydrolysis under hydrochloric acid conditions after etherification of oxime compounds is a relatively advanced method at present. This method can avoid the use of toxic substances such as sulfur dioxide and sodium nitrite, reduce the emission of nitrogen oxide waste gas, and react The advantages of mild conditions and low investment cost, but the method of purifying methoxyamine hydrochloride mostly adopts the method of enriching and crystallizing, and inorganic salts will be generated during the preparation process of this method, and the conventional purification methods are easy to bring inorganic salts into Into the product, affecting product quality

Method used

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  • A kind of refining method of methoxyamine hydrochloride
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  • A kind of refining method of methoxyamine hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0028] A kind of purification method of methoxyamine hydrochloride, its scheme is:

[0029] The reaction solution in the 100kg reaction tower still is pumped into the reboiler through the reaction tower pump and heated and circulated to 50 ° C, and then enters the rectification tower 1 to carry out the vacuum rectification reaction, and the distillate flows into the reaction tower distillation tank through the secondary condensation at the top of the tower. , the distillation tower still liquid is pumped into the tower still liquid separator for stratification, and the lower layer is the methoxyamine hydrochloride solution; then the lower layer methoxyamine hydrochloride solution is pumped into the concentration tower, and after the concentration The tower circulating pump and the reboiler of the concentration tower are circulated and heated to 60 °C and concentrated to 40%, then add 80 kg of organic solvent, stir and mix evenly, and then cool down to 30 °C through a heat excha...

Embodiment 2

[0038] A kind of purification method of methoxyamine hydrochloride, its scheme is:

[0039]The reaction liquid in the 200kg reaction tower still is pumped into the reboiler through the reaction tower pump and heated and circulated to 60 ° C, then enters the rectification tower 1 to carry out the vacuum rectification reaction, and the distillate flows into the reaction tower distillation tank through the secondary condensation at the top of the tower. , the distillation tower still liquid is pumped into the tower still liquid separator for stratification, and the lower layer is the methoxyamine hydrochloride solution; then the lower layer methoxyamine hydrochloride solution is pumped into the concentration tower, and after the concentration The tower circulating pump and the reboiler of the concentration tower are circulated and heated to 70 ℃ and concentrated to 50%, then add 100 kg of organic solvent, stir and mix evenly, and then cool down to 35 ℃ through a heat exchanger, an...

Embodiment 3

[0048] A kind of purification method of methoxyamine hydrochloride, its scheme is:

[0049] The reaction liquid in the 300kg reaction tower still is pumped into the reboiler through the reaction tower pump to be heated and circulated to 80 ° C, and then enters the rectification tower 1 to carry out the vacuum rectification reaction, and the distillate flows into the reaction tower distillation tank through the secondary condensation at the top of the tower. , the distillation tower still liquid is pumped into the tower still liquid separator for stratification, and the lower layer is the methoxyamine hydrochloride solution; then the lower layer methoxyamine hydrochloride solution is pumped into the concentration tower, and after the concentration The tower circulating pump and the reboiler of the concentration tower are circulated and heated to 80 °C and concentrated to 60%, then add 160 kg of organic solvent, stir and mix evenly, and then cool down to 40 °C through a heat exch...

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Abstract

The present invention relates to the field of chemical industry. The present invention is a method for refining methoxyamine hydrochloride. First, the volatile organic matter and reaction raw materials in the reaction liquid are rectified and removed by rectification, and then concentrated by a concentration tower and then added The organic solvent causes the inorganic salt to precipitate, and the inorganic salt in the kettle liquid is removed by filtration; what this method uses is a kind of hydrophilic polysulfone microporous filtration membrane, which has good filtration effect and filtration efficiency, and does not affect the process of the whole process. Continuity; the present invention uses the principle of the different solubility of methoxyamine hydrochloride and inorganic salts in organic solvents to precipitate inorganic salts by adding organic solvents, and then achieve the purpose of removing inorganic salts; organic solvents of the present invention can be recycled , do not increase the material cost of production, do not increase the treatment capacity of the three wastes, and the methoxyamine hydrochloride purified by the method of the present invention has higher purity, which improves product quality and market competitiveness.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for purifying methoxyamine hydrochloride. Background technique [0002] Methoxamine hydrochloride is an important pharmaceutical and chemical intermediate, mainly used in the production of medicines and pesticides. [0003] CN112125822A discloses a method for preparing methoxyamine, which at least comprises: contacting a raw material gas containing methyl nitrite and a reducing agent with a reduction reaction catalyst in a reactor to perform a reduction reaction to obtain methoxyamine. The method can fully utilize methyl nitrite, an important intermediate in the coal-to-ethylene glycol process, and the methyl nitrite conversion rate is high. The present application also provides a method for preparing methoxyamine hydrochloride using the above method to obtain methoxyamine as a raw material. [0004] CN105859575B relates to a method for co-producing methoxyamine hydroc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C239/20B01D67/00B01D69/02B01D71/68B01D61/14
CPCC07C239/20B01D67/0081B01D69/02B01D71/68B01D61/147B01D2325/36
Inventor 周黎旸周强段仲刚徐碧涛张军良张超群
Owner ZHEJIANG JINHUA NEW MATERIALS
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