Preparation method and application of an in-situ supported metal mesoporous carbon microsphere catalyst

A technology for supporting metals and catalysts, which is applied in the preparation and application field of in-situ supported metal mesoporous carbon microsphere catalysts, can solve the problems of reducing catalyst selectivity, product purity, unfavorable product separation and purification, etc., and achieves easy reuse and shortens the preparation time Effects of Time, Strong Industrialization Prospects

Active Publication Date: 2021-07-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are excessive hydrogenation side reactions in this method, which will generate corresponding alcohols, which reduces the selectivity of the catalyst and the purity of the product, which is not conducive to the separation and purification of the product.

Method used

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  • Preparation method and application of an in-situ supported metal mesoporous carbon microsphere catalyst
  • Preparation method and application of an in-situ supported metal mesoporous carbon microsphere catalyst
  • Preparation method and application of an in-situ supported metal mesoporous carbon microsphere catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Measure 0.2ml of 0.04g / mL Pd(NH 3 ) 4 Cl 2 Aqueous solution, 0.2mL of ammonia water with a mass concentration of 25% to 28%, 40mL of ethanol, and 100mL of deionized water are fully stirred, and then 1.8g of resorcinol is added, stirred until completely dissolved, and then slowly added dropwise with 0.8mL Formaldehyde aqueous solution with a mass concentration of 37-40% was stirred at 20°C for 12 hours, then transferred to a hydrothermal reaction kettle and kept at 100°C for 30h, and then centrifuged and washed to obtain a reddish-brown polymer solid powder. Dry at 45°C for 24 hours at a relative vacuum of -0.099~-0.05MPa.

[0037] Then the solid obtained above was reduced with hydrogen-argon mixed gas (hydrogen gas fraction is 10%), the process was kept at 200°C for 2 hours, at 600°C for 3 hours, and at 800°C for 4 hours, (wherein the heating program was: 1°C / min from room temperature to 200°C, 5°C / min from 200°C to 600°C, 10°C / min from 600°C to 800°C, space velocity...

Embodiment 2

[0039] Measure 0.2ml of 0.04g / mLPd(NH 3 ) 4 Cl 2 Aqueous solution, 0.5mL of ammonia water with a mass concentration of 25% to 28%, 50mL of ethanol, and 150mL of deionized water are fully stirred, and then 1.5g of resorcinol is added, and after stirring until completely dissolved, slowly add 0.5mL of Formaldehyde aqueous solution with a mass concentration of 37-40% was stirred at 25°C for 15 hours, then transferred to a hydrothermal reaction kettle at 150°C for 20 hours, and then centrifuged to obtain a reddish-brown polymer solid powder. Dry at 90°C for 12 hours at a relative vacuum of -0.099 to -0.05MPa.

[0040] Then the solid obtained above was reduced with hydrogen-argon mixed gas (hydrogen gas fraction is 10%), the process was kept at 200°C for 1 hour, at 600°C for 3 hours, and at 800°C for 4 hours, (wherein the heating program was: 1°C / min from room temperature to 200°C, 5°C / min from 200°C to 600°C, 10°C / min from 600°C to 800°C, space velocity not less than 30h -1 ) ...

Embodiment 3

[0042] Measure 0.2ml of 0.04g / mLPd(NH 3 ) 4 Cl 2 Aqueous solution, 0.3mL of ammonia water with a mass concentration of 25% to 28%, 30mL of ethanol, and 60mL of deionized water were fully stirred, then 2.9g of resorcinol was added, and after stirring until completely dissolved, 2mL of Formaldehyde aqueous solution with a mass concentration of 37-40% was stirred at 30°C for 20 hours, then transferred to a hydrothermal reaction kettle at 100°C for 12 hours, and then centrifuged and washed to obtain a reddish-brown polymer solid powder. Dry at 80°C for 16 hours at a relative vacuum of -0.099 to -0.05MPa.

[0043] Then the solid obtained above was reduced with hydrogen-argon mixed gas (hydrogen gas fraction is 10%), the process was kept at 200°C for 2 hours, at 600°C for 3 hours, and at 800°C for 4 hours, (wherein the heating program was: 1°C / min from room temperature to 200°C, 5°C / min from 200°C to 600°C, 10°C / min from 600°C to 800°C, space velocity not less than 30h -1 ) to o...

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Abstract

A preparation method and application of an in-situ supported metal mesoporous carbon microsphere catalyst, the preparation method comprising: 1) dissolving a metal precursor in ammonia water to prepare a metal ammonia complex solution; 2) taking the metal ammonia complex Solution, ammonia solution, ethanol and deionized water are thoroughly mixed, then resorcinol is added, and formaldehyde solution is slowly added dropwise, and after stirring at 10-50°C for 12-48 hours, the hydrothermal reaction is carried out at 50-200°C for 12 hours. ~36 hours, then centrifuged and washed to obtain a reddish-brown polymer solid powder, and then dried; 3) The polymer solid obtained in step 2) is roasted in a reducing atmosphere containing hydrogen to obtain in-situ supported metal mesoporous carbon microsphere catalyst. The invention provides the application of the catalyst in the selective catalytic hydrogenation of substituted phenols represented by formula (I) to synthesize substituted cyclohexanones represented by formula (II), which has high conversion rate, high catalytic activity, Features of high stability.

Description

[0001] (1) Technical field [0002] The invention relates to a preparation method and application of an in-situ supported metal mesoporous carbon microsphere catalyst. The catalyst can be used to catalyze hydrogenation of phenolic substances to generate ketone compounds. [0003] (2) Technical background [0004] Ketones are organic chemical intermediates with a wide range of uses. They are widely used in the fields of medicine, pesticides, and dyes. They are very important types of fine chemical products. At present, there are mainly two synthesis methods: oxidation method and catalytic hydrogenation method. The oxidation method is to obtain the corresponding ketone compounds under certain conditions and the action of an oxidizing agent. However, these oxidation reactions need to be carried out under high temperature and pressure, and the selectivity of products is relatively low, the requirements for industrialization are relatively high, and the prospects are limited. Cata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J23/42B01J23/46B01J35/08B01J37/10B01J37/18C07C49/517C07C45/00
CPCB01J23/42B01J23/44B01J23/46B01J35/08B01J37/10B01J37/18C07C45/006C07C49/517
Inventor 卢春山张雪洁冯振龙丰枫马磊张群峰许孝良李小年
Owner ZHEJIANG UNIV OF TECH
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