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Selective hydrogenation catalyst for unsaturated ketone and preparation method and application thereof

A hydrogenation catalyst and selective technology, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of poor catalytic stability of hydrogenation catalysts, and achieve excellent catalytic performance and stability , high catalytic activity and strong sustainability

Inactive Publication Date: 2018-12-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The hydrogenation catalysts disclosed in these two patent applications have poor catalytic stability

Method used

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  • Selective hydrogenation catalyst for unsaturated ketone and preparation method and application thereof
  • Selective hydrogenation catalyst for unsaturated ketone and preparation method and application thereof
  • Selective hydrogenation catalyst for unsaturated ketone and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Weigh 1g of carboxymethyl chitin and disperse in 50ml of water, add 1g of F127 and stir well. Then add 1g of cerium nitrate hexahydrate and 1ml of nitric acid, mix well, and stir until dry at 80°C; then, transfer to a 30ml crucible, and perform calcination in a nitrogen furnace. The specific calcination process is: heat up to 1000°C at 5°C / min , calcined at 1000 ° C for 1 h; then, naturally cooled to room temperature. The calcined mixture is pulverized to obtain a highly dispersed cerium oxide composite nitrogen-doped carbon material. Weigh 1 g of the above material, add it to 60 mL of deionized water, slowly add 1 mL of PdCl with a concentration of 10 mg / mL 2 solution, stirred at 50°C for 12h, dried in an oven at 70°C for 24h, calcined in air at 300°C for 1h, and reduced with hydrogen at 300°C for 1h (hydrogen flow rate 50mL / min, heating rate 5°C / min) to obtain unsaturated ketone Selective hydrogenation catalyst.

[0046] figure 1 with image 3 The transmission el...

Embodiment 2

[0048] Weigh 1g of carboxymethyl chitosan and disperse it in 50ml of water, add 1g of F127 and stir evenly. Then add 1g of cerium nitrate hexahydrate and 1ml of nitric acid, mix well, and stir until dry at 80°C; then, transfer to a 30ml crucible, and perform calcination in a nitrogen furnace. The specific calcination process is: heat up to 1000°C at 5°C / min , calcined at 1000 ° C for 1 h; then, naturally cooled to room temperature. The calcined mixture is pulverized to obtain a highly dispersed cerium oxide composite nitrogen-doped carbon material. Weigh 1 g of the above material, add it to 60 mL of deionized water, slowly add 1 mL of 10 mg / mL PdCl 2 solution, stirred at 50°C for 12h, dried in an oven at 70°C for 24h, calcined in air at 300°C for 1h, and reduced with hydrogen at 300°C for 1h (hydrogen flow rate: 50mL / min, heating rate: 5°C / min) to obtain unsaturated ketone Selective hydrogenation catalyst. The dispersion of Pd measured by CO titration is 81%, and the specif...

Embodiment 3

[0050] Weigh 1g of carboxymethyl chitin and dissolve in 50ml of water, add 1g of F127 and stir well. Then add 1g of zirconium nitrate pentahydrate and 1ml of nitric acid and mix evenly, stir until dry at 80°C; then, transfer to a 30ml crucible and calcinate in a nitrogen furnace. The specific calcining process is: heat up to 1000 ℃, calcined at 1000℃ for 1h; then, cool down to room temperature naturally. The calcined mixture is pulverized to obtain a highly dispersed zirconia composite nitrogen-doped carbon material. Weigh 1 g of the above material, add it to 60 mL of deionized water, slowly add 1 mL of 10 mg / mL PdCl 2 solution, stirred at 50°C for 12h, dried in an oven at 70°C for 24h, calcined in air at 300°C for 1h, and reduced with hydrogen at 300°C for 1h (hydrogen flow rate: 50mL / min, heating rate: 5°C / min) to obtain unsaturated ketone Selective hydrogenation catalyst. The dispersion of Pd measured by CO titration is 79%, and the specific surface area of ​​the catalys...

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Abstract

The invention discloses a selective hydrogenation catalyst for unsaturated ketone. By taking a highly dispersed metal oxide compounded nitrogen doped porous carbon material as a carrier, noble metal particles are attached to the nitrogen doped porous carbon material, wherein the noble metal particles is 0.1-20% with respect to the mass content of the nitrogen doped porous carbon material. The invention also discloses a preparation method and an application of the catalyst. The metal oxide in the catalyst is uniformly distributed in and compactly combined with the nitrogen doped porous carbon material. The nano noble metal particles are dispersed highly. The experimental method is simple. The raw materials are very wide in source and high in sustainability, so that scaled production can beachieved. The catalyst shows excellent catalytic activity and stability in selective hydrogenation reaction of carbon-carbon double bonds of a key intermediate in a vitamin industrial chain.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for selective hydrogenation of unsaturated ketones, a preparation method thereof, and an application in the selective hydrogenation reaction of carbon-carbon double bonds of key intermediates in the vitamin industry chain. Background technique [0002] More than 80% of all kinds of chemicals used in life are produced through specific catalytic processes. At the heart of the catalytic process is the catalyst. However, heterogeneous catalysts have attracted extensive attention due to their ease of operation. As an important representative of heterogeneous catalysts, supported metal nanocatalysts have a wide range of applications. Dispersing the active metal on a carrier can greatly reduce the amount of metal used while achieving the same catalytic effect. Carbon material is an ideal catalyst carrier because of its high thermal and electrical conductivity...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/10C07C45/62C07C49/04
CPCC07C45/62B01J27/24B01J35/615C07C49/04
Inventor 王勇王哲陈益庆
Owner ZHEJIANG UNIV
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