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A kind of supported highly dispersed nano-gold catalyst and its preparation method and application

A high-dispersion, nano-gold technology, applied in the direction of catalyst activation/preparation, carbon-based compound preparation, chemical instruments and methods, etc., can solve problems such as many steps, difficult control of particle size and dispersion, complicated separation and purification processes, etc.

Active Publication Date: 2022-05-03
YUNNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] ① Precious metal catalysts need multi-step preparation. Generally, alkaline reagents are used as precipitants to prepare carrier metal oxides, and then gold particles are loaded on the metal oxide carriers step by step. This process has many steps and many other reagents are introduced. The amount of reagents needs to be precisely controlled, the reagents need to be removed, and surfactants are needed to make the gold particles evenly distributed and the particle size uniform, and the steps are complicated
[0015] ②Active center gold shows high activity at zero valence. Chlorauric acid is used in the traditional method of preparation. Gold is first combined with tetravalent gold and metal oxide carrier, and then the tetravalent gold is reduced by reducing agents such as sodium borohydride or hydrogen. Reduction to zero-valent gold, the process has many steps and high cost, and the amount of reducing agent needs to be precisely controlled, and gold is easy to agglomerate during the reduction process, the particle size and dispersion are difficult to control, and the cost is high
[0016] ③At present, most of the reaction conditions used in the industrial production of vanillin need to add acid or alkali additives, and accompanied by toxic oxidants, the synthesis process is complicated, and the reaction yield is not high
Moreover, the preparation reaction of vanillin is difficult to control and only the product vanillin is obtained, and over-oxidized vanillic acid and even p-benzoquinone are often generated. There are many by-products in the reaction, and the process of separation and purification is relatively complicated.

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  • A kind of supported highly dispersed nano-gold catalyst and its preparation method and application

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preparation example Construction

[0037] The invention provides a preparation method of a loaded highly dispersed Au / ZnO nano-gold catalyst, comprising the following steps:

[0038] 2-Methylimidazole is mixed with chloroauric acid solution to obtain a mixed solution;

[0039] Adding the zinc salt solution dropwise to the mixed solution for precipitation to obtain a precursor;

[0040] The precursor is calcined to obtain a supported highly dispersed Au / ZnO nano-gold catalyst.

[0041] In the present invention, unless otherwise specified, the required preparation materials are commercially available products well known to those skilled in the art.

[0042] In the invention, 2-methylimidazole is mixed with chloroauric acid solution to obtain a mixed solution. In the present invention, the mass ratio of the 2-methylimidazole to the chloroauric acid solution in the chloroauric acid solution is preferably (100-5000):1, more preferably 1000:1.

[0043] In the present invention, the preparation process of the chlor...

Embodiment 1

[0069] Add 1 mL of chloroauric acid aqueous solution (5 mg / mL) to 100 mL of methanol to obtain a chloroauric acid solution (concentration is 50 μg / mL);

[0070] Weigh 5g of 2-methylimidazole, and dissolve 2-methylimidazole in the chloroauric acid solution under stirring conditions (rotating speed 600rpm), and continue stirring for 10min after it is completely dissolved to obtain a mixed solution;

[0071]Weigh 1.84g of zinc nitrate hexahydrate solid and dissolve it in 100mL of methanol, put the obtained zinc nitrate solution into a decompression funnel, add it dropwise to the mixed solution, let stand for 24h, and precipitate, and centrifuge the obtained material, The obtained solid material was dried in an oven at 80°C, and after grinding, the precursor was obtained;

[0072] The precursor was placed in a muffle furnace and calcined at 500° C. for 4 h, and the heating rate was 2° C. / min to obtain a supported highly dispersed Au / ZnO nano-gold catalyst.

Embodiment 2

[0074] Add 1 mL of chloroauric acid aqueous solution (5 mg / mL) to 100 mL of methanol to obtain a chloroauric acid solution (concentration is 50 μg / mL);

[0075] Weigh 5g of 2-methylimidazole, and dissolve 2-methylimidazole in the chloroauric acid solution under stirring conditions (rotating speed 600rpm), and continue stirring for 10min after it is completely dissolved to obtain a mixed solution;

[0076] Weigh 1.14g of zinc acetate solid and dissolve it in 100mL of methanol, put the resulting zinc nitrate solution into a decompression funnel, add it dropwise to the mixed solution, let stand for 24h, and precipitate, centrifuge the resulting material, and The solid material is dried in an oven at 80°C, and after grinding, the precursor is obtained;

[0077] The precursor was placed in a muffle furnace and calcined at 500° C. for 4 h, and the heating rate was 2° C. / min to obtain a supported highly dispersed Au / ZnO nano-gold catalyst.

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Abstract

The invention provides a supported high-dispersion nano-gold catalyst, a preparation method and application thereof, and belongs to the technical field of nano-gold catalysts. In the present invention, 2-methylimidazole is used to promote the precipitation of zinc salt and chloroauric acid, and at the same time, 2-methylimidazole is used as a stabilizer and a template, so that the gold nanoparticles are highly dispersed and the particle size is uniform and controllable, and zinc oxide has six The special shape of the edge shape, the self-reduction of gold occurs during the roasting process, and the ionic gold precursor is reduced to zero-valent gold. Only one-pot method can be used to synthesize gold particles with small, uniform and controllable particle size distribution, high dispersion, and special The morphology of the Au / ZnO catalyst avoids the disadvantages of the traditional synthesis method, such as the introduction of many reagents, complicated steps, and difficult control of particle size distribution. In the Au / ZnO nano-gold catalyst prepared by the invention, the nano-gold particles are small and uniform in particle size (average particle size is 3±0.2 nm), which can achieve 100% conversion rate of vanillin and 100% conversion rate of vanillin. Optional.

Description

technical field [0001] The invention relates to the technical field of nano-gold catalysts, in particular to a supported highly dispersed nano-gold catalyst and its preparation method and application. Background technique [0002] Vanillin, also known as vanillin, chemical name 3-methoxy-4-hydroxybenzaldehyde, is the most important biomass fragrance in modern society. In nature, vanillin exists in the seeds of vanilla pods and has a strong milky aroma. Nowadays, vanillin is widely used in various aspects, such as in the food field: in cakes, syrups, barbecues, chocolates, drinks and other foods as a food additive to increase flavor; in the field of fine chemicals, it can also be used in cosmetics, Health products, etc.; in the synthesis of polymers, it is also used in the preparation of plastics and rubber. Over the past century, the industrial synthesis of vanillin has gradually matured, and many methods for the synthesis and preparation of vanillin have been reported, bu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/66B01J37/03B01J37/08C07C45/38C07C47/58B01J35/02B82Y30/00B82Y40/00B01J35/00
CPCB01J23/66B01J37/0018B01J37/031B01J37/082C07C45/38B82Y30/00B82Y40/00B01J35/394B01J35/23B01J35/40B01J35/50C07C47/58
Inventor 方文浩林鹏曹秋娥
Owner YUNNAN UNIV