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Glutaraldehyde preparing method by cyclopentene heterogeneous catalytic oxidation

A technology of heterogeneous catalytic oxidation and glutaraldehyde, which is applied in the directions of oxidative preparation of carbonyl compounds, etc., can solve the problems of complex process flow, the yield is not further improved, and the total output is less than 2000 tons/year, and the yield is obvious. , the effect of simplified post-processing process and low cost

Inactive Publication Date: 2006-12-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

But at present, there are only a few manufacturers in China, and the total output is less than 2,000 tons per year, which is far from meeting the needs of domestic production, and most of them rely on imports.
This method solves the recovery problem of the catalyst, but makes the technological process complicated, and the yield has not been further improved
[0006] Deng Jingfa of Fudan University (Chemstry Letters 1999, 371) used the conventional impregnation method to load ammonium tungstate on silica, and further roasted to obtain WO 3 / SiO 2 , using this catalyst to oxidize cyclopentene to synthesize glutaraldehyde, the solvent is tert-butanol, and 50% hydrogen peroxide is used. Although the catalyst can be reused, the highest yield is only 60%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In a 50mL round bottom flask equipped with a stirrer and a reflux condenser, add 1g of 20% WO 3 / SiO 2 , 13.78 g 10% H 2 o 2 Tributyl phosphate solution, drop 1.30g cyclopentene. Normal pressure, reaction temperature 30°C. The reaction stopped after 7 hours. filter catalyst. The yield of glutaraldehyde was quantitatively analyzed by gas chromatography. The yield is 90%.

Embodiment 2

[0019] In a 50mL round bottom flask equipped with a stirrer and a reflux condenser, add 1g of 20% WO 3 / SiO 2 , 13.78 g 10% H 2 o 2 butyl acetate solution, drop 1.30g cyclopentene. Normal pressure, reaction temperature 30°C. The reaction stopped after 7 hours. filter catalyst. The yield of glutaraldehyde was quantitatively analyzed by gas chromatography. The yield was 82%.

Embodiment 3

[0021] In a 50mL round bottom flask equipped with a stirrer and a reflux condenser, add 1g of 20% WO 3 / Zeolite, 13.78g 10% H 2 o 2 Tributyl phosphate solution, drop 1.30g cyclopentene. Normal pressure, reaction temperature 30°C. The reaction stopped after 7 hours. filter catalyst. The yield of glutaraldehyde was quantitatively analyzed by gas chromatography. The yield is 80%.

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Abstract

A process for preparing glutaraldehyde from cyclopentene by multi-phase catalytic oxidizing features that the cyclopentene is used as raw material, the solution of tributyl phosphorate in H2O2 is used as oxidant, its catalyst is the carried one with WO3 as active component, its reaction temp is 30-40 deg.C and its output rate is 90%.

Description

technical field [0001] The invention relates to the preparation of glutaraldehyde, in particular to a method for preparing glutaraldehyde through heterogeneous catalytic oxidation of cyclopentene with high yield. Background technique [0002] Glutaraldehyde is mainly used in biomedical engineering, immunochemistry, leather chemistry, food microbiology industry, petroleum exploration, environmental protection and many other aspects. Due to its excellent properties and wide range of applications, glutaraldehyde has attracted much attention from all over the world. But at present, there are only a few manufacturers in China, and the total output is less than 2,000 tons per year, which is far from meeting the needs of domestic production, and most of them rely on imports. People have been looking for an industrial production method with simple process route and low cost. [0003] At present, large foreign companies mainly use the pyran method, but the catalysts used are differ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/12C07C45/28
Inventor 李德才刘菁徐杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI