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A kind of mesoporous carbon microsphere-supported composite material catalyst and its preparation method and application

A technology of composite materials and catalysts, which is applied in the direction of catalyst activation/preparation, preparation of amino compounds, chemical instruments and methods, etc. It can solve problems such as large difference in properties, influence of catalyst performance on catalytic reaction, etc., achieve strong transfer ability and inhibit dechlorination The effect of high performance, catalytic activity and selectivity

Active Publication Date: 2019-12-24
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the activated carbon carrier used in the catalyst has a great impact on the performance of the catalyst and its catalytic reaction due to the large differences in the properties of different manufacturers and different carbon sources.

Method used

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  • A kind of mesoporous carbon microsphere-supported composite material catalyst and its preparation method and application
  • A kind of mesoporous carbon microsphere-supported composite material catalyst and its preparation method and application
  • A kind of mesoporous carbon microsphere-supported composite material catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Measure 0.8mL of ammonia water with a mass concentration of 25% to 28%, 1.5g of F127, 64mL of ethanol, and 160mL of deionized water, and stir the three thoroughly, then add 1.6g of resorcinol, stir until completely dissolved, and slowly drop Add 2.24 mL of formaldehyde solution with a mass concentration of 37-40%, stir at 20°C for 12 hours, transfer to a hydrothermal reaction kettle at 80°C for 12 hours, and then centrifuge and wash to obtain a reddish-brown polymer solid powder.

[0050] Weigh 3g of alanine and dissolve it in 30mL of deionized water, add 1.12mL of ethylenediamine, stir evenly, transfer the mixture to a reaction kettle at 100°C for 5 hours, then transfer the reaction solution to a molecular weight cut-off of 1000 The dialysis bag was dialyzed for 12 hours; then the dialysate was freeze-dried at a relative vacuum of -0.099 to -0.05MPa and a temperature of -10°C for 10 hours to obtain a carbon quantum dot solid powder.

[0051] Get 20mL of palladium metal...

Embodiment 2

[0054] Measure 0.8mL of ammonia water with a mass concentration of 25% to 28%, 0.5gF127, 96mL of ethanol, and 120mL of deionized water and stir the three thoroughly, then add 1.6g of resorcinol, stir until completely dissolved, and slowly drop Add 3 mL of formaldehyde solution with a mass concentration of 37-40%, stir at 25°C for 20 hours, transfer to a hydrothermal reaction kettle at 100°C for 15 hours, and then centrifuge and wash to obtain a reddish-brown polymer solid powder.

[0055] Weigh 3.4g of alanine and dissolve it in 31mL of deionized water, add 1.15mL of ethylenediamine, stir evenly, transfer the mixture to a reaction kettle at 100°C for 5 hours, then transfer the reaction solution to The 9000 dialysis bag was dialyzed for 12 hours; then the dialysate was freeze-dried at a relative vacuum of -0.099 to -0.05MPa and a temperature of -10°C for 10 hours to obtain a quantum dot solid powder.

[0056] Take 60mL of the palladium metal concentration of 0.001g / mL ammonium ...

Embodiment 3

[0059] Measure 0.8mL of ammonia water with a mass concentration of 25% to 28%, 2.0g of F127, 64mL of ethanol, and 180mL of deionized water, and stir the three thoroughly, then add 1.6g of resorcinol, stir until completely dissolved, and slowly drop Add 4 mL of formaldehyde solution with a mass concentration of 37-40%, stir at 10°C for 30 hours, transfer to a hydrothermal reaction kettle at 35°C for 18 hours, and then centrifuge and wash to obtain a reddish-brown polymer solid powder.

[0060] Weigh 3g of alanine and dissolve it in 30mL of deionized water, add 2mL of ethylenediamine, stir evenly, transfer the mixed solution to a reaction kettle at 120°C for 5 hours, then transfer the reaction solution to a reactor with a molecular weight cut-off of 1000 The dialysis bag was dialyzed for 24 hours; then the dialysate was dried at a relative vacuum of -0.099 to -0.05 MPa at a temperature of 50° C. and freeze-dried for 5 hours to obtain solid powder of quantum dots.

[0061] Get 38...

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Abstract

The invention discloses a mesoporous carbon microsphere supported composite catalyst as well as a preparation method and application of the mesoporous carbon microsphere supported composite catalyst. The catalyst is composed of a mesoporous carbon microsphere as well as an active component and a carbon quantum dot which are supported on the mesoporous carbon microsphere; the particle size of the catalyst ranges from 100nm to 1000nm; the active component is one or a combination of several of platinum, palladium, iridium, ruthenium and rhodium; the loads of metals in the active component are as follows: 0wt%-10.0wt% of palladium, 0wt%-10.0wt% of platinum, 0wt%-10.0wt% of iridium, 0wt%-10.0wt% of ruthenium and 0wt%-10.0wt% of rhodium, and not all the loads of palladium, platinum and rhodium are equal to zero; the total load of the active component is 1.0-20%; and the load of the carbon quantum dot is not higher than 30.0wt%. The invention provides the application of the mesoporous carbon microsphere supported composite catalyst to reaction for synthesizing chloroaniline shown as a formula (II) by carrying out selective catalytic hydrogenation on chloronitrobenzene shown as a formula (I) to show that the mesoporous carbon microsphere supported composite catalyst has the characteristics of high conversion rate, high catalytic activity and high stability.

Description

[0001] (1) Technical field [0002] The invention relates to a mesoporous carbon microsphere-supported composite material catalyst and a preparation method and application thereof. The catalyst can be used for catalytic hydrogenation reduction reactions of chloronitrobenzene compounds. [0003] (2) Technical background [0004] The reduction of chloronitrobenzene to chloroaniline is an important basic organic synthesis reaction. The product, chloroaniline, is a widely used organic chemical intermediate and occupies a pivotal position in the field of fine chemicals. The traditional iron powder and sodium sulfide reduction process has been forced to be eliminated by the state due to its shortcomings such as large pollution, low efficiency, and high labor intensity. Instead, it is a green, friendly and efficient catalytic hydrogenation process. However, there are dechlorination hydrogenolysis side reactions in this method, which will generate aromatic amines and hydrochloric acid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J23/42B01J23/46B01J37/03B01J37/08B01J37/18B01J35/08C07C209/36C07C211/52
CPCB01J23/42B01J23/44B01J23/462B01J23/464B01J35/0013B01J35/006B01J35/08B01J37/035B01J37/084B01J37/088B01J37/18C07C209/365C07C211/52
Inventor 卢春山冯振龙齐亚妮王梦君张群峰丰枫马磊李小年
Owner ZHEJIANG UNIV OF TECH
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