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Metal-organic framework supported heteropoly acid catalyst for synthesizing glutaraldehyde and production method of metal-organic framework supported heteropoly acid catalyst

A technology of immobilized heteropolyacids and organic frameworks, applied in the field of catalysts for the heterogeneous catalytic oxidation of cyclopentene to synthesize glutaraldehyde, can solve the problem that the total production capacity is less than 500 tons, the yield of glutaraldehyde is not high, and there is no industrial value and other problems to achieve excellent catalytic performance, facilitate production control, and prevent loss

Inactive Publication Date: 2015-03-25
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is estimated that the current domestic demand for pure glutaraldehyde reaches 20,000 tons per year, and most of the glutaraldehyde used is imported. Only a few units such as Wuhan Organic Chemical Factory use acrolein to produce, and the total production capacity is less than 500 tons. tons / year
The catalysts in these reactions are very sensitive to water and need to be operated in an anhydrous system, and the yield of glutaraldehyde is not high (less than 50%); no industrial value

Method used

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  • Metal-organic framework supported heteropoly acid catalyst for synthesizing glutaraldehyde and production method of metal-organic framework supported heteropoly acid catalyst

Examples

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Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: A kind of metal-organic framework immobilized heteropolyacid catalyst for the synthesis of glutaraldehyde, its production method comprises the following steps:

[0023] Place the reactor in a water bath at 35°C, add 80 ml of DMF (N,N-dimethylformamide) to the reactor, and dissolve 2.0 g of terephthalic acid H 2 (BDC) and 2.8 g ZrCl 4 Dissolve in DMF, stir to dissolve, then add 1.5 ml of concentrated hydrochloric acid (concentration: 1.179g / ml), stir for 3 h, then add 0.497 g of phosphotungstic heteropoly acid, continue stirring for 2 h, mix the above reaction The raw material was transferred into a stainless steel reactor, crystallized at 120°C for 30 h, taken out, filtered, washed and dried, and the product was activated at a constant temperature of 180°C for 10 h in an air atmosphere to obtain 1# catalyst.

Embodiment 2

[0024] Example 2: A kind of metal-organic framework immobilized heteropolyacid catalyst for the synthesis of glutaraldehyde, its production method comprises the following steps:

[0025] Place the reactor in a water bath at 35°C, add 80 ml of DMF (N,N-dimethylformamide) to the reactor, and dissolve 2.0 g of terephthalic acid H 2 (BDC) and 2.8 g ZrCl 4 Dissolve in DMF, stir to dissolve, then add 1.5 ml concentrated hydrochloric acid to it, stir for 3 h, then add 0.745 g phosphotungstic heteropoly acid, continue stirring for 2 h, after mixing evenly, transfer the above reaction materials into a stainless steel reaction kettle , crystallized at 120°C for 30h, took it out, filtered, washed, dried, and activated at a constant temperature of 180°C in an air atmosphere for 10h to obtain 2# catalyst.

Embodiment 3

[0026] Example 3: A kind of metal-organic framework immobilized heteropolyacid catalyst for the synthesis of glutaraldehyde, its production method comprises the following steps:

[0027] Place the reactor in a water bath at 35°C, add 80 ml of DMF (N,N-dimethylformamide) to the reactor, and dissolve 2.0 g of terephthalic acid H 2 (BDC) and 2.8 g ZrCl 4 Dissolve in DMF, stir to dissolve, then add 1.5 ml concentrated hydrochloric acid to it, stir for 3 h, then add 0.994 g phosphotungstic heteropoly acid, continue stirring for 2 h, after mixing evenly, transfer the above reaction materials into a stainless steel reaction kettle , crystallized at 120°C for 30 h. Take it out, filter, wash and dry it, and activate it at 180°C for 10 h at a constant temperature in an air atmosphere to obtain 3# catalyst.

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Abstract

The invention relates to a metal-organic framework supported heteropoly acid catalyst for synthesizing glutaraldehyde and a production method of the metal-organic framework supported heteropoly acid catalyst. The catalyst is prepared by a one-step synthesis method, namely a heteropoly acid component with catalytic oxidation activity is introduced into a duct of a metal-organic framework material UiO-66 in the process of synthesizing the metal-organic framework material UiO-66. The catalyst has the characteristics that the catalyst has a crystal framework structure, the active component is highly dispersed, and the heteropoly acid is over-high in load. The catalyst is applied to catalytic selective oxidation reaction of cyclopentene, so that the selectivity and the yield of the glutaraldehyde is greatly improved; the numerical value is much higher than the reported homogeneous catalysis level; and the metal-organic framework supported heteropoly acid catalyst has important industrial application value.

Description

[0001] technical field [0002] The invention belongs to the technical field of chemical industry and relates to a catalyst for synthesizing glutaraldehyde, in particular to a catalyst for synthesizing glutaraldehyde by heterogeneous catalytic oxidation of cyclopentene and a production method thereof. Background technique [0003] Glutaraldehyde is a very important chemical product, which is widely used as a disinfectant, tanning agent for leather, fixative for tissue sections under optical and electron microscopes, cross-linking agent for proteins and polyhydroxy compounds, and micromicelle curing agent, etc. . It is estimated that the current domestic demand for pure glutaraldehyde reaches 20,000 tons per year, and most of the glutaraldehyde used is imported. Only a few units such as Wuhan Organic Chemical Factory use acrolein to produce, and the total production capacity is less than 500 tons. tons / year. Nowadays, acrolein two-step method is used to synthesize glutara...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C47/12C07C45/28
Inventor 杨新丽刘洋曹晓雨谢文磊李浩博戴维林
Owner HENAN UNIVERSITY OF TECHNOLOGY
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