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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: 2021-07-30
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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  • Refining method of methoxyamine hydrochloride
  • Refining method of methoxyamine hydrochloride
  • Refining method of methoxyamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

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

Embodiment 2

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

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

Embodiment 3

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

[0049] Pump the reaction liquid in the reactor of 300kg reaction tower to the reboiler for heating and circulation to 80°C through the reaction tower pump, then enter the rectification tower 1 for vacuum rectification reaction, and the distillate flows into the distillation tank of the reaction tower through secondary condensation at the top of the tower , the rectification tower still liquid is pumped into the tower still liquid separator for stratification, the lower layer is methoxyamine hydrochloride solution; then the lower layer methoxyamine hydrochloride solution is pumped into the concentration tower, after concentration The tower circulation pump and the concentration tower reboiler are heated to 80°C and concentrated to 60%, then add 160kg of organic solvent, stir and mix evenly, then cool down to 40°C through a heat exchanger, and then filter through a microporous membrane filter. The o...

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Abstract

The invention relates to the field of chemical industry, in particular to a refining method of methoxyamine hydrochloride. The refining method comprises the steps of rectifying and removing volatile organic matters and reaction raw materials in reaction liquid by using a rectification method, concentrating by using a concentration tower, adding an organic solvent to separate out inorganic salt, and removing the inorganic salt in kettle liquid by filtering. The hydrophilic polysulfone microporous filtration membrane used in the method has good filtration effect and filtration efficiency, and does not affect the continuity of the whole process; according to the principle that methoxyamine hydrochloride and inorganic salt have different solubility in an organic solvent, the inorganic salt is separated out by adding the organic solvent, and then the purpose of removing the inorganic salt is achieved; and the organic solvent can be recycled, the material cost of production is not increased, the treatment capacity of three wastes is not increased, the methoxyamine hydrochloride obtained through purification by the method has higher purity, and the product quality and the market competitiveness are improved.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for refining methoxyamine hydrochloride. Background technique [0002] Methoxyamine hydrochloride is an important pharmaceutical and chemical intermediate, mainly used in the production of pharmaceuticals and pesticides. [0003] CN112125822A discloses a method for preparing methoxyamine, which at least includes: 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 the important intermediate methyl nitrite in the coal-to-ethylene glycol process, and the conversion rate of the methyl nitrite is high. The present application also provides a preparation method of methoxyamine hydrochloride obtained by the above method as raw material. [0004] CN105859575B relates to a method for co-producing methoxyamine hydrochlorid...

Claims

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Application Information

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Patent Type & Authority Applications(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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