Mesoporous carbon microsphere supported composite catalyst as well as preparation method and application of mesoporous carbon microsphere supported composite catalyst

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: 2017-12-01
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

Method used

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  • Mesoporous carbon microsphere supported composite catalyst as well as preparation method and application of mesoporous carbon microsphere supported composite catalyst
  • Mesoporous carbon microsphere supported composite catalyst as well as preparation method and application of mesoporous carbon microsphere supported composite catalyst
  • Mesoporous carbon microsphere supported composite catalyst as well as preparation method and application of mesoporous carbon microsphere supported composite catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Measure 0.8mL of 25-28% ammonia water, 1.5g F127, 64mL of ethanol, and 160mL of deionized water, stir the three fully, then add 1.6g of resorcinol, stir until all is dissolved, and then slowly drop Add 2.24 mL of an aqueous formaldehyde solution with a mass concentration of 37-40%, stir at 20°C for 12 hours, transfer to a hydrothermal reaction kettle and keep at 80°C for 12 hours, and then centrifuge and wash to obtain a red-brown polymer solid powder.

[0045] Weigh 3g of alanine and dissolve it in 30mL of deionized water, add 1.12mL of ethylenediamine, stir evenly, transfer the mixture to the reactor at 100°C for 5 hours, then transfer the reaction solution to a molecular weight cutoff of 1000 The dialysis bag is subjected to dialysis for 12 hours; then the dialysate is freeze-dried with a relative vacuum of -0.099~-0.05MPa and a temperature of -10°C for 10 hours to obtain carbon quantum dot solid powder.

[0046] Take 20 mL of chloropalladium alcohol aqueous solution with...

Embodiment 2

[0049] Measure 0.8 mL of 25-28% ammonia water, 0.5 g F127, 96 mL of ethanol, and 120 mL of deionized water, stir the three fully, then add 1.6 g of resorcinol, stir until all is dissolved, and then slowly drop Add 3 mL of an aqueous formaldehyde solution with a mass concentration of 37-40%, stir at 25°C for 20 hours, transfer to a hydrothermal reaction kettle and keep at 100°C for 15 hours, and then centrifuge and wash to obtain a red-brown polymer solid powder.

[0050] Weigh 3.4g of alanine and dissolve it in 31mL of deionized water, add 1.15mL of ethylenediamine, stir evenly, transfer the mixture to the reactor at 100°C for 5 hours, then transfer the reaction solution to a molecular weight cutoff of Perform dialysis on a 9000 dialysis bag for 12 hours; then freeze-dry the dialysate with a relative vacuum of -0.099~-0.05MPa and a temperature of -10°C for 10 hours to obtain a solid quantum dot powder.

[0051] Take 60 mL of ammonium tetrachloropalladate alcohol solution with a pal...

Embodiment 3

[0054] Measure 0.8mL of 25-28% ammonia water, 2.0gF127, 64mL of ethanol, and 180mL of deionized water. Stir the three fully, then add 1.6g of resorcinol, stir until all is dissolved, and then slowly drip Add 4 mL of an aqueous formaldehyde solution with a mass concentration of 37-40%, stir at 10°C for 30 hours, transfer it to a hydrothermal reactor and keep it at 35°C for 18 hours, and then centrifuge and wash to obtain a red-brown polymer solid powder.

[0055] Weigh 3g of alanine and dissolve it in 30mL of deionized water, add 2mL of ethylenediamine, stir evenly, transfer the mixture to the reactor at 120°C for 5 hours, then transfer the reaction solution to a molecular weight cutoff of 1000 The dialysis bag is subjected to dialysis for 24 hours; then the dialysate is dried at a relative vacuum degree of -0.099 to -0.05 MPa, a temperature of 50° C., and freeze-dried for 5 hours to obtain a solid quantum dot powder.

[0056] Take 38.25mL of ethylenediamine palladium chloride alcoh...

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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

(1) Technical field [0001] 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 the catalytic hydrogenation reduction reaction of chloronitrobenzene compounds. (2) Technical background [0002] The process of reducing chloronitrobenzene to chloroaniline is an important basic organic synthesis reaction. The product chloroaniline is a very versatile organic chemical intermediate and occupies a pivotal position in the field of fine chemicals. The traditional iron powder and sodium sulfide reduction processes are forced to be eliminated by the state due to their shortcomings such as high pollution, low efficiency, and high labor intensity. It is replaced by a green, friendly and efficient catalytic hydrogenation process. However, this method has a side reaction of dehydrochlorination and hydrogenolysis, which generates aromatic amines and hydrochloric acid, which ...

Claims

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Application Information

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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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