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Preparation method for in-situ loaded metal mesoporous carbon microsphere catalyst and application

A technology for supporting metals and mesoporous carbons, which is applied in catalyst activation/preparation, carbon-based compound preparation, organic compound preparation, etc., can solve problems such as separation and purification of unfavorable products, reduce catalyst selectivity and product purity, and achieve easy reuse. , the effect of shortening the preparation time and strengthening the prospect of industrialization

Active Publication Date: 2018-12-14
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 for in-situ loaded metal mesoporous carbon microsphere catalyst and application
  • Preparation method for in-situ loaded metal mesoporous carbon microsphere catalyst and application
  • Preparation method for in-situ loaded metal mesoporous carbon microsphere catalyst and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 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, then 1.8g of resorcinol is added, and after stirring until completely dissolved, slowly add 0.8mL of 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 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.

[0032] 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 )...

Embodiment 2

[0034]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.

[0035] 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 ) t...

Embodiment 3

[0037] 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.

[0038] 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

The invention discloses a preparation method for an in-situ loaded metal mesoporous carbon microsphere catalyst and application. The preparation method comprises the following steps: 1) dissolving a metal precursor into ammonia water so as to obtain a metal ammonia complex solution; 2) sufficiently mixing the metal ammonia complex solution, an ammonia water solution, ethanol and deionized water, further adding resorcinol, slowly dropping a formaldehyde solution, stirring for 12-48 hours at 10-50 DEG C, carrying out a hydrothermal reaction for 12-36 hours at 50-200 DEG C, carrying out centrifugal washing so as to obtain red brown polymer solid powder, and drying; 3) roasting the polymer solid obtained in the step 2) in a reduction atmosphere with hydrogen, thereby obtaining the in-situ loaded metal mesoporous carbon microsphere catalyst. The invention further provides application of the catalyst in reactions for synthesizing substituted cyclohexanone of formula (II) as shown in the specification through selective catalytic hydrogenation of substituted phenol of formula (I) as shown in the specification. The preparation method has the characteristics of being high in conversion rate,high in catalysis activity and high in stability.

Description

(1) Technical field [0001] 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. (2) Technical background [0002] 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. Catalytic hydrogena...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J23/42B01J23/46B01J35/08B01J37/10B01J37/18C07C49/517C07C45/00
CPCC07C45/006B01J23/42B01J23/44B01J23/46B01J37/10B01J37/18B01J35/51C07C49/517
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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