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Technological route for synthesizing medical glutaraldehyde

A process route and a technology for glutaraldehyde are applied in the field of process routes for synthesizing medical glutaraldehyde, and can solve the problems of unguaranteed transportation and storage, poor stability of high-purity glutaraldehyde, low yield, etc. The effect of increasing the number, keeping the color number stable, and high product purity

Active Publication Date: 2016-06-01
宁夏荆洪生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The high-purity glutaraldehyde produced by this method has poor stability, transportation and storage cannot be guaranteed, and the yield is low due to multi-stage distillation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In a three-necked flask equipped with a vacuum water tank, a rectifying head and a tower section, add crude dihydropyranyl methyl ether and 0.2% mol of hydroquinone, heat at 95-105°C, and control the reflux ratio to 2:1, Adjust the reflux ratio according to the sampling results, collect more than 99.5% of dihydropyranyl methyl ether, and the external standard content is 98.2%.

[0017] In the three-necked flask, add 400mL (1mol) of water, and when the vacuum pressure of the system is 0.2MPa, heat the water to boiling (remove the dissolved oxygen in the water), then add the high-purity dihydropyranyl methyl ether (1mol ) and 0.2mol / L disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution at a temperature of 85-89°C. After the reaction, crude glutaraldehyde (with a content of about 47%) was obtained.

[0018] Add hydroquinone (0.2% mol) into a three-necked flask equipped with a vacuum water tank, a rectifying head, and a tower section, and continuously ad...

Embodiment 2

[0020] In a three-necked flask equipped with a vacuum water tank, a rectifying head, and a tower section, add crude dihydropyranyl ethyl ether and 0.4% mol p-benzoquinone, heat at 95-105°C, and control the reflux ratio to 2:1, according to The sampling results were adjusted to the reflux ratio, and more than 99.5% of the dihydropyranyl ethyl ether was collected, and the external standard content was 98.6%.

[0021] In the three-necked flask, add 800mL (2mol) of water, when the vacuum pressure of the system is 0.2MPa, heat the water to boiling (remove the dissolved oxygen in the water), then add the high-purity dihydropyranyl ethyl ether (1mol ) and 0.1mol / L disodium hydrogen phosphate-citric acid buffer solution at a temperature of 85-89°C. After the reaction, crude glutaraldehyde (with a content of about 30%) was obtained.

[0022] In a three-neck flask equipped with a vacuum water tank, a rectifying head and a tower section, add p-benzoquinone (0.4% mol), and continuously ad...

Embodiment 3

[0024] In a three-necked flask equipped with a vacuum water tank, a rectifying head, and a tower section, add crude dihydropyranyl isopropyl ether and 0.5% mol of 2,6-di-tert-butyl-4-methylphenol, and heat for 95- 105°C, control the reflux ratio to 2:1, adjust the reflux ratio according to the sampling results, collect more than 99.5% of dihydropyranyl isopropyl ether, and the external standard content is 98.4%.

[0025] In the three-necked flask, add 400mL (1mol) of water, and when the vacuum pressure of the system is 0.2MPa, heat the water to boiling (remove the dissolved oxygen in the water), and then add the high-purity dihydropyranyl isopropyl ether ( 1mol) and 0.05mol / L glycine-hydrochloric acid buffer solution at a temperature of 85-89°C. After the reaction, the crude glutaraldehyde (with a content of about 45%) was obtained.

[0026] In a three-necked flask equipped with a vacuum water tank, a rectifying head and a tower section, add 2,6-di-tert-butyl-4-methylphenol (0...

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Abstract

The invention discloses a technological route for synthesizing medical glutaraldehyde. Dihydropyran alkyl ether is used for separating high-boiling-point substances by means of decompression rectification, and dihydropyran alkyl ether refined products are acquired. A buffering solution serves as a catalyst, water is added for hydrolysis, hydrolysis reaction liquid is subjected to continuous decompression rectification, and high-purity medical glutaraldehyde is acquired. The route is stable in technology, high in yield and stable in color number, and the products have competitive advantages.

Description

technical field [0001] The invention relates to a process route for synthesizing medical glutaraldehyde, which belongs to the technical field of organic synthesis. Background technique [0002] Medical glutaraldehyde has been widely used in medical and health care, microbial industry, sterilization of breeding sites, microcapsule curing, hardening agent for electron microscopes and color picture tubes, protein chemistry, biological enzymes and immobilization of cells. [0003] The method in the prior art mainly adopts the first reaction to prepare glutaraldehyde with conventional content, and then removes low boiling and high boiling glutaraldehyde by multi-stage distillation to finally obtain more than 99% glutaraldehyde. The high-purity glutaraldehyde produced by this method has poor stability, transportation and storage cannot be guaranteed, and the yield is low due to multi-stage distillation. Contents of the invention [0004] In order to overcome the deficiencies of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/12C07C45/60C07C45/82
CPCC07C45/60C07C45/82C07C47/12
Inventor 陈雷韩连成朱美山杨辉
Owner 宁夏荆洪生物科技股份有限公司
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