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
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[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...
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[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...
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[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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