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Supported tungstic acid catalyst for synthesizing glutaraldehyde and its producing method

A technology for synthesizing glutaraldehyde and supporting type, applied in the chemical industry, can solve problems such as difficulty in separating homogeneous catalysts, and achieve the effects of many times of recycling, simple preparation and wide operating range.

Inactive Publication Date: 2003-06-25
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to propose a loaded tungstic acid catalyst and its preparation method for the heterogeneous catalytic oxidation of cyclopentene to synthesize glutaraldehyde, so as to fundamentally solve the problem of difficult separation of homogeneous catalysts

Method used

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  • Supported tungstic acid catalyst for synthesizing glutaraldehyde and its producing method

Examples

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Embodiment 1

[0016] Example 1: At room temperature, electromagnetic stirring, 12.5ml of 3MTiCl 4 The solution was dropped into 50ml of distilled water, stirred for 1h, 40g of urea was added, stirred for 20min, 5.0g of ammonium sulfate was added, stirred for 2h, 50ml of absolute ethanol was added, stirred for 4h. The resulting clear solution was transferred to a 200ml autoclave and sealed, crystallized at 80°C for 20h, and then taken out; filtered, washed with water, washed with ethanol, and dried under vacuum at 80°C for 24h. Available white TiO 2 Powder, marked as 1# carrier.

Embodiment 2

[0017] Example 2: At room temperature, electromagnetic stirring, 12.5ml of 3MTiCl 4 The solution was dropped into 50ml of distilled water, stirred for 1h, added 30g of urea, stirred for 20min, added 5.0g of ammonium sulfate, stirred for 2h, added 50ml of absolute ethanol, stirred for 4h. The resulting clear solution was transferred into a 200ml autoclave and sealed, crystallized at 100°C for 20h, and then taken out; filtered, washed with water, washed with ethanol, and dried under vacuum at 80°C for 24h. Available white TiO 2 Powder, marked as 2# carrier.

Embodiment 3

[0018] Example 3: In an oil bath at 95°C, weigh 0.054g of xanthosungstic acid in 15ml of deionized water, stir for 20min, add 0.89g of oxalic acid, and stir for 1h to obtain a clear solution; add 1g of carrier #1, stir and evaporate, 120 Bake at ℃ for 24h, treat at 500℃ for 3h, granulate, sieving through 40-60 mesh to obtain 3# catalyst.

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Abstract

The present invention belongs to the field of chemical technology, and is a kind of supported tungstic acid catalyst for multiphase catalytic oxidation and synthesis of glutar aldehyde from cyclopentene. The catalyst has TiO2 microball of unique structure synthesized through homogeneous alcohol-hydrothermal process as the carrier and WO3, prepared with ammonium tungstate / tungstic acid and assistant and through dissolving in water, adding TiO2 microball, evaporation, stoving, roasting, activating and other steps, on the TiO2 carrier. The WO3 / TiO2 catalyst has very high gluter aldehyde selectivity and yield and extremely high industrial application value.

Description

Technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of a supported tungstic acid catalyst for the heterogeneous catalytic oxidation of cyclopentene to synthesize glutaraldehyde. Background technique [0002] Glutaraldehyde is a very important chemical product. It is widely used as a disinfectant, leather tanning agent, fixative for optical and electron microscope tissue sections, protein and polyhydroxy compound crosslinking agent, and micromicelle curing agent, etc. . It is estimated that the current total domestic demand for pure glutaraldehyde will reach 20,000 tons / year, most of which rely on imports. Only the Wuhan No. 1 Organic Synthesis Chemical Plant uses acrolein method to produce it, with a total production capacity of less than 500 tons / year. Now the industry uses acrolein two-step method to synthesize glutaraldehyde (Japanese Patent Publication No. 59-108734). Because this method h...

Claims

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Application Information

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IPC IPC(8): B01J23/30B01J37/00C07C45/34C07C47/12
Inventor 郭昌文戴维林曹勇范康年
Owner FUDAN UNIV
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