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Preparation method of heterogeneous catalyst of organic coordination compounds of mesoporous structure metals

A technology of coordination compounds and heterogeneous catalysts, applied in organic compound/hydride/coordination complex catalysts, catalyst activation/preparation, physical/chemical process catalysts, etc. The changes of the central microenvironment and the increase of steric hindrance can achieve the effect of high-efficiency and long-lasting catalytic activity, increase the speed of chemical reaction, and improve product quality.

Inactive Publication Date: 2010-08-04
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But its shortcoming is: 1, the design or improvement of catalyst is difficult
2. Due to the heterogeneity of the surface, the utilization rate of surface active components is limited
3. The direction of the catalytic reaction is not easy to control, and the activity and selectivity cannot achieve the best effect
This method usually brings some problems such as catalyst instability; uneven distribution of active sites on the support; increased steric hindrance, and changes in the microenvironment of the catalytic active center by ligands, etc.

Method used

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  • Preparation method of heterogeneous catalyst of organic coordination compounds of mesoporous structure metals
  • Preparation method of heterogeneous catalyst of organic coordination compounds of mesoporous structure metals
  • Preparation method of heterogeneous catalyst of organic coordination compounds of mesoporous structure metals

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Experimental program
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Effect test

Embodiment 1

[0034] The preparation method of mesoporous metal-organic coordination compound heterogeneous catalyst:

[0035] 0.33g ZrCl 4 Dissolved in 6ml DMF; 0.20g H 2 BDC was dissolved in 6ml of DMF; the two solutions were mixed and stirred at 25°C for 0.5h. Then the mixed solution was transferred to MDS-6 polytetrafluoroethylene microwave reactor, and reacted for 4mins under the condition of 400W. The reactor was taken out and naturally cooled to room temperature, then filtered and washed with DMF; dried in a vacuum oven at 160°C for 24 hours; a white solid catalyst Zr-MOF was obtained.

[0036] The structural parameters of the Zr-MOF catalyst determined by the BET method are listed in the following table:

[0037] S BET (m 2 / g)

[0038] The catalyst Zr-MOF is applied to the formation reaction process of flavonoids under solvent-free conditions as follows:

[0039] Add 1.0mmol phlorotriphenol, 1.2mmol ethyl acetoacetate, 0.05g catalyst Zr-MOF to a 10ml round bottom ...

Embodiment 2

[0043] 0.66g ZrCl 4 Dissolved in 12ml DMF; 0.40g H 2 BDC was dissolved in 12 ml DMF; the two solutions were mixed. Stir at 25°C for 0.5h, then transfer the mixed solution to a polytetrafluoroethylene MDS-6 microwave reactor, and react at 400W for 4mins. The reactor was taken out and naturally cooled to room temperature, then filtered, washed with DMF, and dried in a vacuum oven at 160°C for 24 hours to obtain a white solid catalyst Zr-MOF. The structural parameters of the Zr-MOF catalyst determined by the BET method are listed in the following table:

[0044] S BET (m 2 / g)

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Abstract

The invention relates to a preparation method of a heterogeneous catalyst of organic coordination compounds of mesoporous structure metals, belonging to a preparation method of heterogeneous catalysts. Theterogeneous catalyst prepared by the prior art has the defects that the utilization ratio of surface active composition is limited, the direction of catalytic reaction can not be controlled easily, and the activity and the selectivity can not reach the optimal effect. In the invention, the preparation method of the heterogeneous catalyst of organic coordination compounds of mesoporous structure metals comprises the following steps of: mixing zirconium tetrachloride, 1,4-terephthalic acid and N,N-dimethylformamide solvent under the condition of microwaves, and stirring the mixture at room temperature until the solution is clear; adding the solution into a microwave reactor for microwave heating, removing the supernatant solution, and washing the residual solid matters with the N,N-dimethylformamide solvent; and drying the washed matters in a vacuum mode to obtain the heterogeneous catalyst. The invention has the advantages of simple process and easy operation; the prepared heterogeneous catalyst has efficient catalytic activity; and the catalyst can be recycled, thereby reducing the production cost and decreasing the environment pollution.

Description

technical field [0001] The invention relates to a method for preparing a heterogeneous catalyst, in particular to a method for preparing a heterogeneous catalyst of a mesoporous metal organic coordination compound. technical background [0002] Catalyst is an important material in chemical industry production, which plays a decisive role in the benefit of chemical production. According to the form of catalyst in the chemical reaction, it can be divided into heterogeneous catalyst and homogeneous catalyst. Most commercial catalysts in the prior art are heterogeneous catalysts. The advantages of heterogeneous catalysts are that the active components of the catalyst can be widely varied; the temperature range used is wide; the catalyst is easily separated from the product; and it is easy to realize industrialization. But its disadvantages are: 1. It is difficult to design or improve the catalyst. 2. Due to the heterogeneity of the surface, the utilization rate of the surface...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J37/34C07D311/30
CPCY02P20/50Y02P20/584
Inventor 黄建林朱凤霞杨旭石张昉李和兴
Owner SHANGHAI NORMAL UNIVERSITY
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