Preparation method for functionalized graphene loaded noble metal nano-crystalline composite catalyst

A noble metal nanocrystal and composite catalyst technology, which is applied in the preparation of organic compounds, the preparation of amino hydroxy compounds, and metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of uneven distribution of oxygen-containing groups and rapid aggregation. , uneven distribution of nanoparticles, etc., to achieve the effect of excellent catalytic performance

Inactive Publication Date: 2014-09-17
HENAN AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the existing technologies use graphite oxide as a carrier, and use the oxygen-containing groups and defect positions on the surface of graphite oxide to bind and immobilize nanoparticles. However, due to the surface defects, graphite oxide completely loses its electrical conductivity compared with graphene. The electrons cannot move freely in the layer, and the thermal conductivity is also greatly affected.
Therefore, using this as a carrier to catalyze organic reactions only takes advantage of its large specific surface area. It is difficult to exert the excellent electron transport performance and thermal conductivity of graphene. At the same time, the defects and oxygen-containing groups caused by oxidation are distributed on the s

Method used

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  • Preparation method for functionalized graphene loaded noble metal nano-crystalline composite catalyst
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  • Preparation method for functionalized graphene loaded noble metal nano-crystalline composite catalyst

Examples

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Example Embodiment

[0021] Example 1

[0022] (1) The preparation of graphite oxide, add 1g of graphite powder into the reactor, add 100g of concentrated sulfuric acid under ice-salt bath conditions to make the graphite evenly dispersed, then add 1g of sodium nitrate and 5g of potassium permanganate under stirring. Remove the ice-salt bath after reacting for 2h, then put the reactor in an oil bath and gradually heat to 80℃ to continue the reaction for 6h, stop heating, cool to room temperature, add hydrogen peroxide with a mass concentration of 30% until no gas is released, then filter the product , Washed with hydrochloric acid and deionized water, redispersed, centrifuged, freeze-dried to obtain graphite oxide;

[0023] (2) The surface of graphite oxide is modified with benzene sulfonic acid. Add 100 mg of graphite oxide and 3 g of p-aminobenzene sulfonic acid to 100 g of deionized water, sonicate for 20 minutes, and then add 0.5 g of sodium nitrite catalyst under nitrogen protection, and heat to 8...

Example Embodiment

[0025] Example 2

[0026] (1) Preparation of graphite oxide, add 3g of graphite powder into the reactor, add 80g of concentrated sulfuric acid under ice-salt bath conditions to make the graphite evenly dispersed, then add 2g of sodium nitrate and 9g of permanganic acid under stirring Potassium, after 2h reaction, remove the ice salt bath, then put the reactor in the oil bath and gradually heat to 80℃ to continue the reaction for 6h, stop heating, after cooling to room temperature, add 30% hydrogen peroxide until no gas is released, and then The product is filtered, washed with hydrochloric acid and deionized water, redispersed, centrifuged, and freeze-dried to obtain graphite oxide;

[0027] (2) Benzenesulfonic acid modification on the graphite oxide surface, add 150mg of graphite oxide to 150g of deionized water, sonicate for 50min, then add 1.5g of isoamyl nitrite catalyst under the protection of nitrogen, heat to 80℃, stir and reflux 18h, stop the reaction, centrifuge, wash, fi...

Example Embodiment

[0029] Example 3

[0030] (1) Preparation of graphite oxide, add 2g of graphite powder into the reactor, add 90g of concentrated sulfuric acid under ice-salt bath conditions to make the graphite uniformly dispersed, then add 1.5g of sodium nitrate and 7g of high manganese under stirring After 2 hours of reaction, remove the ice salt bath, then put the reactor in an oil bath and gradually heat it to 80°C to continue the reaction for 6 hours, stop heating, cool to room temperature, add hydrogen peroxide with a mass concentration of 30% until no gas is released, then The product is filtered, washed with hydrochloric acid and deionized water, redispersed, centrifuged, and freeze-dried to obtain graphite oxide;

[0031] (2) Benzenesulfonic acid modification on the graphite oxide surface, add 120mg of graphite oxide to 120g of deionized water, ultrasonic for 30min, then add 1g of sodium nitrite catalyst under the protection of nitrogen, heat to 80℃, stir and reflux for 18h, stop Reactio...

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Abstract

The invention discloses a preparation method for a functionalized graphene loaded noble metal nano-crystalline composite catalyst, which synchronously realizes reduction of a noble metal precursor and graphite oxide to obtain the composite catalyst in a structure that grapheme with surface modified by sulfonic acid is uniformly loaded with noble metal nano-crystalline. The method comprises the following steps: 1, preparing the graphite oxide; 2, carrying out covalent modification on the graphite oxide by benzenesulfonic acid; and 3, synchronously reducing the noble metal precursor and the graphite oxide and stabilizing noble metal nano particles by utilizing a coordination effect between a sulfonic acid group and the noble metal. Meanwhile, the surface sulfonic acid group has the hydrophilcity so that the catalyst can be uniformly dispersed in a water solution. A result shows that the noble metal nano particles with narrow size distribution can be uniformly distributed on the surface of graphene to form the efficient catalyst which has good dispersion in the water solution. Catalytic reduction reaction of p-nitrophenol proves that the catalyst has a very excellent catalysis performance; the catalyst still keeps the previous activity after being recycled and reutilized for five times.

Description

technical field [0001] The invention relates to the technical field of chemical catalysis, in particular to a method for preparing a functionalized graphene-supported noble metal nanocrystal composite catalyst. Background technique [0002] Noble metal nanocrystalline homogeneous catalysts stabilized by ligands have important applications in catalytic organic reactions due to their fast reaction rate, good selectivity, and high catalytic yield. However, homogeneous catalysts are difficult to purify for recycling after catalysis, so their applications are greatly limited. The development of a highly dispersed noble metal nanocrystal composite catalytic system supported by a carrier can effectively solve the above-mentioned shortcomings of homogeneous catalysts, and has broad prospects in practical applications. [0003] Graphene is very suitable for the support of noble metal nanocatalysts due to its large specific surface area, high thermal and electrical conductivity, and ...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J23/52B01J23/50B01J23/42B01J23/44C07C215/76C07C213/02
Inventor 王志敏徐翠莲高光芹李鑫
Owner HENAN AGRICULTURAL UNIVERSITY
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