Continuous reactive distillation equipment for synthesising methoxylamine hydrochloride and process thereof

A technology of methoxyamine hydrochloride and reactive distillation, which is applied in the field of continuous reactive distillation, can solve the problems of low equipment production capacity, large consumption of process raw materials, long production cycle, etc., and achieve stable product quality, good product quality, The effect of reducing production energy consumption and material consumption

Inactive Publication Date: 2013-05-22
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process route is a batch process, with large consumption of process raw materials, long production cycle, and low equipment production capacity; at the same time, as a batch reaction process, the residence time of materials in the reactor is long, and there are many potential side reactions

Method used

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  • Continuous reactive distillation equipment for synthesising methoxylamine hydrochloride and process thereof
  • Continuous reactive distillation equipment for synthesising methoxylamine hydrochloride and process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Attached figure 1 The schematic diagram of the equipment structure is shown. After the raw material oxime methyl ether is preheated, the temperature is 50°C, the flow rate is 300kg / h, and it enters the lower part of the reaction section of the reactive distillation dividing wall tower; the raw material hydrochloric acid with a mass concentration of 30% has a temperature of 25°C, the flow rate is 336kg / h, and it enters the reactive rectification dividing wall tower from the upper part of the reaction section; the molar ratio of hydrogen chloride and methyl oximide in hydrochloric acid is 0.8:1, and the two raw materials undergo acidic hydrolysis reaction of methyl oximide in the reaction section and Carry out vapor-liquid mass transfer separation and realize the process of continuous reactive distillation.

[0041] The material of the reactive distillation dividing wall tower is carbon steel lined with enamel. The reaction section of the reactive distillation dividing wa...

Embodiment 2

[0044] Attached figure 1 The schematic diagram of the equipment structure is shown. After the raw material oxime methyl ether is preheated, the temperature is 40°C, the flow rate is 240kg / h, and it enters the lower part of the reaction section of the reactive distillation dividing wall column; the raw material hydrochloric acid with a mass concentration of 30% has a temperature of 25°C, the flow rate is 638kg / h, it enters the reactive rectification dividing wall tower from the upper part of the reaction section; the molar ratio of hydrogen chloride and methyl oximide in hydrochloric acid is 1.9:1, and the two raw materials undergo acidic hydrolysis reaction of methyl oximide in the reaction section and Carry out vapor-liquid mass transfer separation and realize the process of continuous reactive distillation.

[0045] The material of the reactive distillation dividing wall tower is carbon steel lined with enamel. The reaction section of the reactive distillation dividing w...

Embodiment 3

[0048] Attached figure 1 The schematic diagram of the equipment structure is shown. After the raw material oxime methyl ether is preheated, the temperature is 50°C, the flow rate is 300kg / h, and it enters the lower part of the reaction section of the reactive distillation dividing wall column; the raw material hydrochloric acid with a mass concentration of 20% has a temperature of 25°C, the flow rate is 755kg / h, it enters the reactive rectification dividing wall tower from the upper part of the reaction section; the molar ratio of hydrogen chloride and methyl oximide in hydrochloric acid is 1.2:1, and the two raw materials undergo acidic hydrolysis reaction of methyl oximide in the reaction section and Carry out vapor-liquid mass transfer separation and realize the process of continuous reactive distillation.

[0049] The material of the reactive distillation dividing wall tower is carbon steel lined with enamel. The reaction section of the reactive distillation dividing wall ...

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Abstract

The invention provides continuous reactive distillation equipment for synthesising methoxylamine hydrochloride by taking oxime methyl ether and hydrochloric acid as raw materials, and a process thereof, wherein a vertical clapboard is arranged in a reactive distillation dividing-wall column in the continuous reactive distillation equipment provided by the invention, and used for dividing the column into four areas, namely, a common distillation section, a reaction section, a stripping section and a lateral stripping section; and oxime methyl ether and hydrochloric acid solution enter from the upper part and the lower part of the reactive distillation section respectively, hydrolysis reaction for oxime methyl ether is performed in the reaction section, the generated methoxylamine hydrochloride is discharged from the bottom of the reactive distillation section, the generated by-product, namely, the mixture of acetone and oxime methyl ether, enters in the common distillation section in the form of a gaseous phase to be separated, more than 95% acetone is obtained on the top of the column, and the separated oxime methyl ether is recycled. According to the continuous reactive distillation equipment and the process provided by the invention, the dividing-wall column is combined with reactive distillation, and hydrolysis reaction and product separation are intensively performed in one column, thus effectively reducing energy consumption and equipment investment cost.

Description

technical field [0001] The invention belongs to the technical field of continuous reactive distillation, and more specifically relates to a new equipment and a new process for continuously producing methoxyamine hydrochloride by using a reactive distillation dividing wall tower with oxime methyl ether and hydrochloric acid as raw materials. Background technique [0002] Methoxyamine hydrochloride is a white crystal powder, soluble in water, soluble in alcohol, insoluble in ether and toluene, etc.; the solution is acidic and has certain hygroscopicity. Methoxyamine hydrochloride is a salt of strong acid and weak base. It is an important fine chemical intermediate and is widely used in the synthesis of functional dyes, low-toxicity pesticides, new herbicides and medicines. In terms of medicine, it is mainly used in the production of antibiotics such as sulfamethoxazole, cefuroxime acid (ester), and hydroxyurea; in terms of pesticides, it is mainly used in the production of phe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C239/20C07C49/08C07C45/42
CPCY02P20/10
Inventor 黄智贤王红星叶长燊邱挺李玲况晨辉
Owner FUZHOU UNIV
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