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Tungsten-containing mesoporous titanium dioxide nano tube catalyst and preparation thereof

A technology of mesoporous titanium dioxide and nanotubes, applied in the chemical industry, can solve problems such as difficulty in separating catalysts from products, production capacity of less than 500 tons, and low yield of glutaraldehyde, etc., achieve excellent catalytic performance, improve efficiency, and facilitate production control Effect

Inactive Publication Date: 2008-09-10
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 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 Anren et al. has obtained the result that the conversion rate of cyclopentene is 100% and the yield of glutaraldehyde is greater than 70% (ZL89109401.6). Difficulties

Method used

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  • Tungsten-containing mesoporous titanium dioxide nano tube catalyst and preparation thereof
  • Tungsten-containing mesoporous titanium dioxide nano tube catalyst and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Weigh 2.0g of titanium dioxide powder P25, place it in a hydrothermal kettle filled with 300mL 10mol / L NaOH, stir in an oil bath at 120°C for 48h, take out the hydrothermal kettle, cool to room temperature, pour out solution, wash the precipitate with distilled water to neutrality, disperse into 0.1mol / L dilute hydrochloric acid solution, ultrasonicate for 10min, stir at room temperature for 4h, continue to wash with distilled water until neutrality, filter and dry to obtain titanium dioxide nanotubes (titania nanotube, TiO 2 (NT)) is denoted as 1# carrier. The reaction conditions used were 1.0 mL cyclopentene, 1.4 mL 50% H 2 o 2 , 10mL tert-butanol, T=308K, the reaction time is 24h.

Embodiment 2

[0023] Example 2: In an oil bath at 95°C, weigh 0.108g of yellow tungstic acid and dissolve it in 15ml of deionized water, stir for 20min, add 1.78g of oxalic acid, stir for 1h to obtain a clear solution; add 1g of 1# carrier, stir and evaporate, 120 It was baked at ℃ for 24 hours, treated at 500℃ for 3 hours, granulated, and sieved with 40-60 mesh to obtain 2# catalyst. The reaction conditions are as example 1.

Embodiment 3

[0024] Example 3: In a 95°C oil bath, weigh 0.215g of yellow tungstic acid and dissolve in 15ml of deionized water, stir for 20min, add 3.548g of oxalic acid, stir for 1h to obtain a clear solution; add 1g of 1# carrier, stir and evaporate. Remaining with example 2, be recorded as 3# catalyst. The reaction conditions are as example 1.

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Abstract

The invention belongs to the technical field of the chemical industry, in particular to a tungsten containing mesoporous titanium dioxide nanometer tube catalyst and a preparation method thereof. The catalyst takes the mesoporous titanium dioxide material with a tubular structure as a carrier and tungstenic acid as an active component; the mol ratio of the titanium dioxide to the active component is 1.9 to 55.1. The measured ammonium tungstate or yellow tungstenic acid and a latent solvent are dissolved in hot water; then the mesoporous TiO2 nanometer tube carrier is added; the WO3 / TiO2 nanometer tube catalyst is prepared by the steps of vaporizing, drying, baking and activating, etc. The mesoporous TiO2 nanometer tube improves the loading threshold value of the tungstenic acid; the prepared WO3 / TiO2 nanometer tube catalyst shows higher selectivity and yield during the reaction of catalyzing cyclopentene to selectively oxidize to prepare glutaric dialdehyde, the selectivity and yield is higher than the that of a homogeneous tungstenic acid catalyst, the defects of hard separation and recycling of homogeneous tungstenic acid are overcome and the catalyst has important industrial application values.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a catalyst for synthesizing glutaraldehyde by heterogeneous catalytic oxidation of cyclopentene and a preparation method thereof. Background technique [0002] Glutaraldehyde (Glutaraldehyde, OHC (CH 2 ) 3 CHO) is a very important chemical product. Its two aldehyde groups are very active and can undergo various reactions, especially the effect of crosslinking and solidifying proteins. Therefore, it is widely used as a disinfectant and leather tanning agent. , Fixatives for tissue sections under optical and electron microscopes, cross-linking agents for proteins and polyhydroxy compounds, and micromicelle curing agents, etc. With the development of economy and the change of environment, infectious viruses such as AIDS (HIVs), hepatitis B, sexually transmitted diseases, tuberculosis, and SARS have aroused widespread concern of people. The number of hepatiti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/30B01J21/06C07C45/28C07C47/12
Inventor 戴维林杨新丽高瑞华范康年
Owner FUDAN UNIV
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