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A kind of palladium catalyst and its preparation method and application

A palladium catalyst and reaction technology, applied in the field of catalysis, can solve the problems of low catalysis efficiency, low reactant conversion rate and product selectivity, etc., and achieve the effect of improving catalysis efficiency

Active Publication Date: 2018-06-26
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, with the rise in the price of precious metals, more and more research has focused on the efficient utilization of supported noble metal catalysts. However, in the prior art, there is still the problem of low catalytic efficiency of supported noble metal catalysts. When applied to catalytic reactions, the conversion rate of reactants and the selectivity of products are low

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  • A kind of palladium catalyst and its preparation method and application
  • A kind of palladium catalyst and its preparation method and application
  • A kind of palladium catalyst and its preparation method and application

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preparation example Construction

[0033] The invention provides the preparation method of described palladium catalyst, comprises the following steps:

[0034] (1) Mix palladium source, zirconium source and solvent, react the obtained mixed solution under microwave heating, obtain colloid;

[0035] (2) Drying, calcining and reducing the colloid obtained in the step (1) in sequence to obtain the palladium catalyst.

[0036] The invention mixes the palladium source, the zirconium source and the solvent, reacts under microwave heating, and obtains the colloid. In the present invention, the solvent preferably includes alcohol and water; the alcohol preferably includes one or more of methanol, ethanol and propanol. In order to fully mix the palladium source and the zirconium source in the solvent, the present invention preferably provides a zirconium source solution and a palladium source solution first, and then mixes the zirconium source solution and the palladium source solution to obtain a mixed solution.

[...

Embodiment 1

[0062] (1) 0.006mol zirconyl nitrate is mixed with 80ml ethanol to obtain zirconyl nitrate solution; 2 PdCl 4 Mix with water to prepare 0.04mol / L K 2 PdCl 4 solution.

[0063] (2) Accounting for 0.1wt% of the palladium catalyst by active metal palladium particles, the zirconium oxynitrate solution in step (1) is mixed with K 2 PdCl 4 The solutions were mixed, stirred at 600 rpm for 30 min at room temperature, placed the obtained mixed solution in a microwave reactor, and reacted with microwave heating for 15 min under stirring at 600 rpm to obtain a colloid; wherein, the microwave heating power was 400W, and the microwave heating temperature was 120°C.

[0064] (3) Dry the colloid obtained in step (2) in a vacuum oven with a vacuum degree of 7Pa at 60°C for 10h, move it into a muffle furnace after drying, calcinate at 250°C for 6h, and then grind it to 100-200 mesh; The material obtained after grinding was placed in a tube furnace, and was reduced at 200°C for 6 hours in ...

Embodiment 2

[0072] Mix 0.4g of the palladium catalyst prepared in Example 1, 0.2g of succinic acid and 40ml of 1,4-dioxane, and stir and react at 800rpm at 180°C for 4h in an atmosphere with a hydrogen pressure of 3MPa to obtain γ- Butyrolactone.

[0073] The conversion rate of succinic acid was 98.2%, and the selectivity to γ-butyrolactone was 97.3%.

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Abstract

The invention provides a palladium catalyst, which includes active metal palladium particles and a zirconium oxide carrier, wherein the active metal palladium particles with a particle size less than 0.3 nm account for 55.7% to 96.2% of the total number of active metal palladium particles. The invention also provides a preparation method of the palladium catalyst. The palladium source, the zirconium source and the solvent are mixed, and the obtained mixed solution is reacted under microwave heating to obtain a colloid; the obtained colloid is sequentially dried, calcined and reduced. , to obtain the palladium catalyst. The palladium catalyst provided by the invention is used to catalyze the preparation of γ-butyrolactone from succinic acid. The conversion rate of succinic acid is as high as 99.5%, and the selectivity of γ-butyrolactone is as high as 99.3%, which is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of catalysis, and in particular relates to a palladium catalyst and its preparation method and application. Background technique [0002] γ-butyrolactone is an important chemical intermediate. In my country, γ-butyrolactone is mainly used to produce γ-pyrrolidone, methylpyrrolidone, polyvinylpyrrolidone, and a small part is used to produce pesticides, pharmaceutical intermediates, Electrolyte solutions and solvents. In recent years, the domestic market for downstream products of γ-butyrolactone and its derivatives has expanded rapidly, and the supply of γ-butyrolactone and its downstream products is in short supply. In the prior art, γ-butyrolactone can be prepared from 1,4-butanediol, maleic anhydride, C4 carboxylate, maleic anhydride or dimethyl succinate as raw materials, but the common raw materials are relatively expensive. Expensive, harsh reaction conditions, complex process and difficult to purify components....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07D307/33
CPCC07D307/33B01J23/44B01J35/396B01J35/40
Inventor 陈立芳漆志文张弛
Owner EAST CHINA UNIV OF SCI & TECH