Ruthenium/carbon catalyst with activated carbon subjected to supercritical CO2 treatment as carrier and method for preparing catalyst

A ruthenium-carbon catalyst and activated carbon technology are applied in the field of ruthenium-carbon catalyst and its preparation, which can solve the problems of increased surface functional groups, different stability, and more adsorption of catalytically active components, and achieve the effects of mild supercritical conditions and low price.

Inactive Publication Date: 2012-06-13
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The acid-base treatment, liquid-phase oxidation treatment, and gas-phase oxidation treatment of activated carbon are used to increase the oxygen-containing functional groups on the surface of activated carbon. The increase in oxygen-containing functional groups can lead to more adsorption of catalytically active components, which may improve catalyst performance.
However, some researchers gave different results, thinking that the increase of surface functional groups is not conducive to the activity of catalysts.
[0007] Relevant experimental results prove that although the oxygen-containing functional groups on the surface of activated carbon are conduc

Method used

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  • Ruthenium/carbon catalyst with activated carbon subjected to supercritical CO2 treatment as carrier and method for preparing catalyst
  • Ruthenium/carbon catalyst with activated carbon subjected to supercritical CO2 treatment as carrier and method for preparing catalyst
  • Ruthenium/carbon catalyst with activated carbon subjected to supercritical CO2 treatment as carrier and method for preparing catalyst

Examples

Experimental program
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Effect test

example 1

[0044] Put 10.0g (40-60 mesh) activated carbon into a 150ml reactor, seal the reactor, and use a high-pressure syringe pump to pump CO 2 Fill until the pressure reaches 8.0 MPa, then use the temperature program to raise the reactor to 60 °C, maintain the supercritical condition for 2 hours, lower the temperature, release the pressure, and unload the reactor to obtain the modified activated carbon. Take 6g of the above-mentioned activated carbon, and use RuCl with a concentration of 0.05g / ml 3 (In which the ruthenium content is 37%) solution 20mL impregnated for 4 hours, then dried at 120°C, the dried sample was placed in the quartz tube of the tubular heating furnace, reduced with hydrogen, reduced at 200°C for 2h, 300h°C for 1h, stop heating, When continuing to cool to room temperature through hydrogen, the ruthenium carbon catalyst sample was obtained. The activity assay result was 46.41 mmol·min -1 g -1 Ru.

example 2

[0046] Put 10.0g (40-60 mesh) activated carbon into a 150ml reactor, seal the reactor, and use a high-pressure syringe pump to pump CO 2 Fill until the pressure reaches 8.0 MPa, then use the temperature program to raise the reactor to 80 °C, maintain the supercritical condition for 2 hours, lower the temperature, release the pressure, and unload the reactor to obtain the modified activated carbon. Take 6g of the above-mentioned activated carbon, and use RuCl with a concentration of 0.05g / ml 3 Immerse 20mL of aqueous solution (the ruthenium content is the same as Example 1) for 4 hours, then dry at 120°C, put the dried sample into the quartz tube of the tubular heating furnace, reduce with hydrogen, reduce at 200°C for 2h, and at 300h°C for 1h, stop heating, When continuing to cool to room temperature through hydrogen, the ruthenium carbon catalyst sample was obtained. Activity assay result 49.92 mmol·min -1 g -1 Ru.

example 3

[0048] Put 10.0g (40-60 mesh) activated carbon into a 150ml reactor, seal the reactor, and use a high-pressure syringe pump to pump CO 2 Fill until the pressure reaches 8.0 MPa, then use the temperature program to raise the reactor to 100 °C, maintain the supercritical condition for 2 hours, lower the temperature, release the pressure, and unload the reactor to obtain the modified activated carbon. Take 6g of the above-mentioned activated carbon, and use RuCl with a concentration of 0.05g / ml 3 Immerse in 20mL of aqueous solution (the content of ruthenium is the same as in Example 1) for 4 hours, then dry at 120°C, put the dried sample into the quartz tube of the tubular heating furnace, reduce it with hydrogen, reduce at 200°C for 2h, and at 300h°C for 1h, stop heating, When continuing to cool to room temperature through hydrogen, the ruthenium carbon catalyst sample was obtained. Activity assay result 47.78 mmol·min -1 g -1 Ru.

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Abstract

The invention relates to a ruthenium/carbon catalyst with activated carbon subjected to supercritical CO2 treatment as a carrier and a method for preparing the catalyst. The method comprises the following steps of: (1) putting a certain amount of activated carbon into a reaction kettle, and introducing CO2 by using a high-pressure injection pump to reach the pressure of 8.0 to 14.0MPa; (2) raising the temperature of the reaction kettle to be between 60 and 100 DEG C; (3) keeping the supercritical condition for 2 to 6 hours, reducing the temperature, and relieving the pressure to obtain modified activated carbon; and (4) impregnating a certain amount of modified activated carbon into a RuCl3 aqueous solution for 4 hours, drying at the temperature of 120 DEG C, putting the dried sample intoa quartz tube of a tube-type heating furnace, reducing by using hydrogen at the temperature of 200 DEG C for 2 hours and at the temperature of 300 DEG C for 1 hour, closing a temperature controller, cooling to room temperature, and thus obtaining the ruthenium/carbon catalyst. The activity of the ruthenium/carbon catalyst prepared by the method is obviously improved due to the action of supercritical treatment, and the defect of a supercritical organic medium is overcome.

Description

technical field [0001] The present invention relates to the ruthenium carbon catalyst that is used for the synthesis of ammonia, the hydrogenation of glucose to sorbitol, the hydrogenation of compounds containing benzene ring etc., especially a kind of ruthenium carbon catalyst with supercritical CO 2 The treated activated carbon is a carrier ruthenium carbon catalyst and a preparation method thereof. Background technique [0002] Supported ruthenium on carbon catalyst is an important catalyst, which is widely used in the synthesis of ammonia, the hydrogenation of glucose to sorbitol, and the hydrogenation of compounds containing benzene rings. Catalytic hydrogenation of glucose to prepare sorbitol is currently the main way to prepare sorbitol. Sorbitol is a polyol widely used in food, medicine, cosmetics and industrial production. Under high pressure conditions, batch reactor or circulating fluidized bed is used as reactor, 50% glucose solution is used as raw material, a...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J37/00C07C31/26C07C29/132
CPCY02P20/54
Inventor 李利民徐三魁郭楠楠王晓栋张朋
Owner ZHENGZHOU UNIV
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