Non-loading type nano-scale composite carbon-noble metal catalyst as well as preparation method and application thereof

A noble metal catalyst and nano-sized technology, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of incomplete exposure of active sites, low utilization of precious metals, and uneven distribution of precious metals. Hydrogen and thermal energy loss, dechlorination suppression effect is remarkable, and the synthesis method is simple

Active Publication Date: 2018-12-21
ZHEJIANG UNIV OF TECH
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  • Abstract
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Problems solved by technology

However, during the catalytic hydrogenation reduction of chloronitrobenzene to chloroaniline, dechlorinated by-products will be generated, which will cause equipment damage and product quality decline. Therefore, the most efficient and stable catalyst for research is catalytic hydrogenation A key step in the reduction method
[0003] In the existing reports, researchers have used the following methods to construct new hydrogenation catalyst structures and active sites to achieve the purpose of inhibiting dechlorination: 1) Enhance the strong interaction between the metal and the support [ACS Catalysis, 2013, 3(6):1386-1396]; 2) Doping heteroelements on the surface of the carrier, such as nitrogen [New Carbon Materials, 2016, 31(3):287-292]; 3) Constructing dual / multi-component catalysts, Such as Pt / C(Fe)[J.Applied CatalysisA:General,2012,429:17-23], etc., this type of catalyst has the characteristics of high activity and strong practical production applicability, but its selectivity and stability need to be improved , and they all use the method of loading precious metals on the carrier, which often leads to uneven distribution of precious metals and incomplete exposure of active sites, resulting in low utilization of precious metals and unsatisfactory catalytic performance. Higher activity is still urgently needed in industrial applications. , selectivity and stability of industrial catalysts

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  • Non-loading type nano-scale composite carbon-noble metal catalyst as well as preparation method and application thereof
  • Non-loading type nano-scale composite carbon-noble metal catalyst as well as preparation method and application thereof
  • Non-loading type nano-scale composite carbon-noble metal catalyst as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0057] A 0.001g / mL chloropalladium acid solution and a 0.001g / mL chloroplatinic acid solution were prepared using a conventional noble metal salt dissolution method. Mix 1 g of citric acid solid powder, 5 ml of chloropalladium acid solution, and 5 ml of chloroplatinic acid solution, set the temperature of the water bath at 30 ° C, start magnetic stirring for 3 hours, and after the stirring is completed, dry the mixed solution in a low-temperature vacuum (the low-temperature vacuum drying condition is a relative vacuum Degree -0.099MPa, temperature is -10 ℃, drying time 10h) to obtain the complex solid powder of citric acid and noble metal; ℃ / min to raise the temperature to 200°C, and keep it at 200°C for 0.5h. After the pyrolysis process is completed and the temperature is lowered to room temperature, slowly add 50ml of deionized water dropwise, and start magnetic stirring until the solid is completely dissolved. Finally, the solution is vacuum-dried at low temperature ( Low-t...

Embodiment 2

[0059] A 0.03 g / mL chloropalladium acid solution and a 0.03 g / mL palladium nitrate solution were prepared using a conventional noble metal salt dissolution method. Mix 2g of citric acid solid powder, 5ml of chloropalladium acid solution and 5ml of palladium nitrate solution, set the temperature of the water bath at 50°C, start magnetic stirring for 6 hours, and after the stirring is completed, dry the mixed solution under low-temperature vacuum drying to obtain a complex of citric acid and noble metal Solid powder (low temperature vacuum drying condition is relative vacuum degree -0.05MPa, temperature is 0°C, drying time is 24h); then, put the complex mixed solid powder in a round bottom flask, heat up to melting, and then dry at 5°C / min to raise the temperature to 300°C, and keep it at 300°C for 2 hours. After the pyrolysis process is completed and the temperature is lowered to room temperature, slowly add 50ml of deionized water dropwise, and start magnetic stirring until th...

Embodiment 3

[0061]A 0.001g / mL palladium nitrate solution and a 0.001g / mL rhodium dichloride solution were prepared using a conventional noble metal salt dissolution method. Mix 3g of citric acid solid powder, 5ml of palladium nitrate solution and 5ml of rhodium dichloride solution, set the temperature of the water bath to 40°C, start magnetic stirring for 4 hours, and after the stirring is completed, dry the mixed solution under low-temperature vacuum drying to obtain complexation of citric acid and precious metals solid powder (low temperature vacuum drying condition is relative vacuum degree -0.05MPa, temperature is -10°C, drying time is 24h); then, put this complex mixed solid powder in a round bottom flask, heat up to melting, and then Raise the temperature to 300°C at 5°C / min and keep it at 300°C for 2 hours. After the pyrolysis process is completed and the temperature is lowered to room temperature, slowly add 50ml of deionized water dropwise, and start magnetic stirring until the so...

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Abstract

The invention discloses a non-loading type nano-scale composite carbon-noble metal catalyst as well as a preparation method and application thereof. The catalyst is granular and the particle size is not greater than 20nm; each particle is formed by compounding one noble metal particle and one carbon dot; the average size of the carbon dots is 1 to 10nm and the average size of the noble metal particles is 1 to 10nm; noble metal is one of platinum, palladium, iridium, ruthenium and rhodium; the mass ratio of the noble metal to carbon is (0.01 to 0.3) to (0.5 to 2.5). The non-loading type nano-scale composite carbon-noble metal catalyst provided by the invention is applied to reaction of synthesizing chloroaniline through photo-thermal catalysis and hydrogenation via chloronitrobenzene, and has the characteristics of high conversion rate, high catalytic activity, high reaction speed and high stability.

Description

(1) Technical field [0001] The invention relates to a non-loaded nano-sized composite carbon-noble metal catalyst and a preparation method thereof, as well as the application of the catalyst in the photothermal catalysis of selective hydrogenation reaction of chloronitrobenzene. (2) Technical background [0002] Chloroaniline is an important organic chemical raw material and intermediate widely used in fine chemical fields such as medicine, pesticides, dyes, etc. It occupies a very important position in the production of fine chemicals at home and abroad. For the production of chloroaniline , as a traditional industrial production method: reduction methods such as iron powder reduction method, alkali sulfide reduction method and electrochemical reduction method, due to the problems of large energy consumption and serious pollution, the traditional reduction method is gradually abandoned at home and abroad to prepare halogenated anilines. The hydrogenation reduction method ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J35/02C07C209/36C07C211/52
CPCC07C209/365B01J23/44B01J35/004B01J35/023C07C211/52Y02P20/584
Inventor 卢春山季豪克张雪洁王昊朱倩文周烨彬岑亚青李小年
Owner ZHEJIANG UNIV OF TECH
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