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Molecular sieve catalyst containing pores in tungsten media utilized for synthesizing glutaraldehyde and its preparation method

A technology for synthesizing glutaraldehyde and mesoporous molecular sieve, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the difficulty of separating catalysts from products, the production capacity is less than 500 tons, and the yield of glutaraldehyde is less than 500 tons. It can achieve the effect of excellent catalytic performance, insensitive reaction parameters, and easy production control.

Inactive Publication Date: 2003-10-08
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the glutaraldehyde currently used in China is imported, and only a few units such as Wuhan Organic Chemical Factory use the acrolein method to produce it, with a total production capacity of less than 500 tons per year.
These catalysts are all very sensitive to water, need to operate in anhydrous system, and the yield of glutaraldehyde is all not high (less than 50%)
And because it involves anhydrous hydrogen peroxide, the operation is extremely dangerous and basically has no industrial value
The homogeneous tungstic acid catalyst reported by Jiang Anren et al. obtained the results of cyclopentene conversion rate of 100% and glutaraldehyde yield > 70% (ZL 89 1 09401.6), but due to the difficulty in separating the catalyst from the product, there is still certain difficulty

Method used

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  • Molecular sieve catalyst containing pores in tungsten media utilized for synthesizing glutaraldehyde and its preparation method
  • Molecular sieve catalyst containing pores in tungsten media utilized for synthesizing glutaraldehyde and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Example 1: 40°C oil bath, electromagnetic stirring, 60 mL of concentrated hydrochloric acid was added into 312 mL of deionized water containing 0.3 g of template agent P123 (molecular weight: 5800), and stirred for 4 hours. Add 25.6 g of ethyl orthosilicate, stir for 1 hour, add 10 mL of aqueous solution containing 0.495 g of phosphotungstic acid, and continue stirring for 24 hours. Transfer the obtained colloid into a 1000mL autoclave and seal it, and take it out after crystallization at 100°C for 72 hours; filter, wash with water, and bake at 100°C for 24 hours. Calcined in an oxygen atmosphere at 700°C for more than 6 hours, granulated, sieved with 40-60 meshes, and activated at 800°C for 3 hours to obtain catalyst #1.

Embodiment 2

[0023] Example 2: In an oil bath at 35°C, with mechanical stirring, 90 mL of concentrated hydrochloric acid was added into 468 mL of deionized water containing 0.5 g of template agent P123 (molecular weight: 5800), and stirred for 6 hours. Add 25.6g ethyl orthosilicate, stir for 2 hours, add 10mL aqueous solution containing 1.05g ammonium tungstate, and continue stirring for 36 hours. Transfer the obtained colloid into a 1000mL autoclave and seal it, and take it out after crystallization at 100°C for 48 hours; the remainder is the same as in Example 1 to obtain 2# catalyst.

Embodiment 3

[0024] Example 3: 50° C. oil bath, electromagnetic stirring, 45 mL of concentrated hydrochloric acid was added into 208 mL of deionized water containing 0.4 g of template agent P123 (molecular weight: 5800), and stirred for 3 hours. Add 25.6g ethyl orthosilicate, stir for 1.5 hours, add 10mL aqueous solution containing 2.15g sodium tungstate, and continue stirring for 48 hours. Transfer the obtained colloid into a 500mL autoclave and seal it, and take it out after crystallization at 100°C for 96 hours; the remainder is the same as in Example 1 to obtain 3# catalyst.

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Abstract

A novel multi-phase W-contained catalyst for preparing glutaraldehyde by using the aqueous solution of hydrogen peroxide as oxidizing agent to selectively oxidize cyclopentene is prepared through in-situ introducing tungsten oxide in the process for synthesizing SBA-1.5 full-silicon mesoporous molecular sieve. Its advantages are high dispersity of active component, ultrahigh load capacity of tungesten oxide, and high selectivity.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a tungsten-containing mesoporous molecular sieve catalyst used for heterogeneous catalytic oxidation of cyclopentene to synthesize glutaraldehyde and a manufacturing method thereof. Background technique [0002] Glutaraldehyde is a very important chemical product, which is widely used as a disinfectant, a leather tanning agent, a fixative for optical and electron microscope tissue sections, a cross-linking agent for proteins and polyhydroxy compounds, and a micromicelle curing agent, etc. . It is estimated that the total domestic demand for pure glutaraldehyde will reach 20,000 tons / year. Most of the glutaraldehyde currently used in China is imported, and only a few units such as Wuhan Organic Chemical Factory use acrolein to produce it, with a total production capacity of less than 500 tons per year. All adopt acrolein two-step method synthetic glutaraldehyde (patent o...

Claims

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Application Information

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IPC IPC(8): B01J29/00C07C45/28C07C47/12
Inventor 郭昌文戴维林曹勇范康年
Owner FUDAN UNIV
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