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Method for preparing glutaraldehyde

A technology of glutaraldehyde and dihydropyran, which is applied in the field of glutaraldehyde preparation, can solve the problems of multiple side reactions, low yield, high anti-corrosion requirements, etc., and achieve reduced production costs, high product purity, and good selectivity Effect

Inactive Publication Date: 2010-12-29
浙江巨邦高新技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high requirements on the anticorrosion of equipment, and has many side reactions, poor selectivity, low yield, and poor environmental protection.
[0006] CN1137034, CN200410017890 have reported the method for preparing glutaraldehyde using microporous crystalline aluminosilicate and heteropolyacid as catalyst, which has good selectivity and is environmentally friendly, but the number of times the catalyst is used mechanically is low and the corresponding cost is relatively high
[0007] Others have many patents again, such as CN00812098, US6559346, CN1371348, etc., have introduced the method for continuous hydrolysis distillation to prepare glutaraldehyde, wherein mainly made a lot of designs to the continuous scheme of process, but all do not involve to reaction catalyst

Method used

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  • Method for preparing glutaraldehyde
  • Method for preparing glutaraldehyde
  • Method for preparing glutaraldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 128.0g (1.0mol) of 2-ethoxy-3,4-dihydropyran, 180.0g (10.0mol) of water, 3.5g (0.02mol) of [Hmin][HSO 4 ] and 0.01g of hydroquinone were added to a 500ml autoclave and heated to 80°C under rapid stirring. The temperature was maintained at 80° C. for 4 hours and then the reaction was stopped. Cool down and take out the reaction solution, put it into a three-necked flask, install a rectification column, and collect the ethanol solution (66.5 grams) by distillation at 50°C under -0.08MPa, then increase the vacuum to -0.099MPa, and gradually heat up to 100°C. A small amount (15 grams) of the transitional fraction was applied mechanically to the next batch of hydrolysis, and 271.7g of fractions at 100-105°C were collected, with a concentration of 33.7%, a yield of 91.6%, and an organic content (purity) of 99.5%. The conversion rate of 2-ethoxy-3,4-dihydropyran was 98.7%, and the selectivity of glutaraldehyde was 97.2%.

Embodiment 2

[0031] 114.0g (1.0mol) of 2-methoxy-3,4-dihydropyran, 180.0g (10.0mol) of water, 7.1g (0.04mol) of [C 2 mim][HSO 3 ] and 0.01g of hydroquinone were added to a 500ml autoclave and heated to 100°C under rapid stirring. The temperature was maintained at 100°C for 2 hours and then the reaction was stopped. Cool down and take out the reaction solution, put it into a three-necked flask, install a rectification column, collect methanol solution (71.7 g) by distillation at 50°C under -0.08MPa, raise the vacuum to -0.099MPa, and gradually heat up to 100°C. A small amount of (13.3 grams) transitional fraction was applied mechanically to the next batch of hydrolysis, collecting 100-105 ° C fraction 268.1g, concentration 31.5%, yield 85.5%, organic content (purity) 99.5%. The conversion rate of 2-ethoxy-3,4-dihydropyran was 95.5%, and the selectivity of glutaraldehyde was 98.1%.

Embodiment 3

[0033] 114.0g (1.0mol) of 2-methoxy-3,4-dihydropyran, 270.0g (15.0mol) of water, 5.0g (0.02mol) of [(C 2 H5N) 3 ][CF 3 o 3 S] and 0.01g of hydroquinone were added to a 500ml autoclave and heated to 80°C under rapid stirring. The temperature was maintained at 80°C for 2 hours and then the reaction was stopped. Cool down and take out the reaction solution, put it into a three-necked flask, install a rectification column, and collect methanol solution (58.8 grams) by distillation at 50°C under -0.08MPa, then raise the vacuum to -0.099MPa, and gradually heat up to 100°C. A small amount of (17.7 grams) transitional fraction was applied mechanically to the next batch of hydrolysis, and 298.9g of cuts at 100-105°C were collected, with a concentration of 30.1%, a yield of 89.97%, and an organic content (purity) of 99.3%. The conversion rate of 2-ethoxy-3,4-dihydropyran was 94.6%, and the selectivity of glutaraldehyde was 98.6%.

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Abstract

The invention provides a method for preparing glutaraldehyde with high conversion rate, high product purity, simple operation, environmental protection and suitability for small-scale intermittent production and large-scale continuous operation. The method for preparing the glutaraldehyde comprises the following steps of: adding an ion acid catalyst into 2-alkoxy-3,4-dihydropyrane and water, wherein the molar ratio of the 2-alkoxy-3,4-dihydropyrane, the water and the ion acid catalyst is (1-100): (2-300):1; performing hydrolysis reaction under the conditions that the reaction temperature is 20 to 150 DEG C, the reaction time is 1 to 20 hours and the reaction pressure is 0.01MPa to 0.1MPa; and obtaining the glutaraldehyde by negative pressure distillation, wherein the ion acid catalyst can be recycled.

Description

technical field [0001] The invention relates to a preparation method of glutaraldehyde. Background technique [0002] Glutaraldehyde is an extremely important chemical raw material, which is widely used in biomedical engineering, cellular immunology, biochemistry, leather chemistry, histochemistry and food, microbial industry, medical and health, environmental protection and other fields. At present, the main synthetic method is to carry out Diels-Alder addition reaction of vinyl ether and acrolein to generate 2-alkoxy-3,4-dihydropyran, and then hydrolyze it under an acidic catalyst to obtain glutaraldehyde and the corresponding alcohol. [0003] There have been many known methods for the hydrolysis of 2-alkoxy-3,4-dihydropyrans to glutaraldehyde for a long time. As described in US Pat. No. 4,489,205, glutaraldehyde is prepared by continuous hydrolysis using acidic diatomaceous earth, strongly acidic cation exchange resin, etc. as immobilized catalysts. Wherein the proces...

Claims

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Application Information

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IPC IPC(8): C07C47/12C07C45/60B01J31/02
CPCY02P20/584
Inventor 吴建平杨晓光王从敏徐林祥
Owner 浙江巨邦高新技术有限公司