Tungsten-contained mesic porous molecular sieve catalyst for synthesis of glutaral dehyde and its preparation

A technology for synthesizing glutaraldehyde and mesoporous molecular sieve, applied in molecular sieve catalysts, chemical instruments and methods, catalysts for physical/chemical processes, etc. It can achieve the effects of insensitive reaction parameters, excellent catalytic performance, and easy production control.

Inactive Publication Date: 2005-10-12
FUDAN UNIV
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  • Application Information

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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 acrolein 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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  • Tungsten-contained mesic porous molecular sieve catalyst for synthesis of glutaral dehyde and its preparation
  • Tungsten-contained mesic porous molecular sieve catalyst for synthesis of glutaral dehyde and its preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Dissolve 1.92g NaOH in 100ml deionized water at room temperature, add 10mL aqueous solution containing 1.468g sodium tungstate and 17.5g surfactant CTAB, dissolve with hot water, and stir for 1h. 20.8 g of TEOS was added dropwise to this solution under vigorous electric stirring to obtain a white gummy mixture, and stirring was continued for 2 h. Then sealed and crystallized at 100°C for 24h. Take it out, cool it, adjust the pH value to 0 with concentrated hydrochloric acid, re-seal and crystallize at 100°C for 24 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. The electron micrograph of typical W-MCM-48 catalyst is attached figure 1 And attached figure 2 .

Embodiment 2

[0023] Example 2: In a 35°C oil bath, dissolve 10.6g NaOH in 420ml deionized water, add 10mL aqueous solution containing 0.853g tungstic acid and 18.7g surfactant CTAB, dissolve with hot water, and stir for 1 hour. 20.8 g of TEOS was added dropwise to this solution under vigorous electric stirring to obtain a white gummy mixture, and stirring was continued for 3 h. Then sealed and crystallized at 80°C for 36h. Take it out, cool it, adjust the pH value to ~1 with concentrated hydrochloric acid, re-seal and crystallize at 80°C for 12 hours, filter, wash with water, and bake at 120°C for 24 hours. Calcination temperature is 200 DEG C, remaining is the same as embodiment 1, obtains 2# catalyst.

Embodiment 3

[0024] Example 3: In a 50°C oil bath, dissolve 0.2g NaOH in 20ml deionized water, add 10mL aqueous solution containing 1.75g ​​silicotungstic acid and 10.4g surfactant CTAB, dissolve with hot water, and stir for 5 hours. 20.8 g of TEOS was added dropwise to this solution under vigorous electric stirring to obtain a white gummy mixture, and stirring was continued for 4 h. Then sealed and crystallized at 110°C for 30h. Take it out, cool it, adjust the pH value to ~7 with concentrated hydrochloric acid, re-seal and crystallize at 110°C for 18h, filter, wash with water, and bake at 110°C for 24 hours at 1300°C, as in Example 1 to obtain 3# catalyst.

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Abstract

A multi-phase W-contained catalyst for preparing glutaraldehyde from cyclopentene through selective oxidizing by the aqueous solution of hydrogen peroxide is prepared through synthesizing the meso-porous MCM-48 all-silicon molecular sieve while adding the tungstic acid precursor to introduce the tungsten oxide with high catalytic oxidizing activity to the skeleton of MCM-48 molecular sieve. Its advantage is high selectivity and output rate of glutaraldehyde.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular 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. . At present, because glutaraldehyde is widely used in secondary oil recovery water injection fungicides in oilfields, the demand for glutaraldehyde has risen sharply. 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/00C07C45/28C07C47/12
Inventor 戴维林杨新丽陈慧曹勇范康年
Owner FUDAN UNIV
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