Method for preparing high-selectivity Pd/TiO2-C hydrogenation catalyst

A hydrogenation catalyst and high-selectivity technology, applied in the field of selective hydrogenation, can solve the problems of difficult to increase the active component Pd loading, low selectivity of the hydrogenation catalyst, etc., and achieve easy separation, hydrogenation conversion rate and High selectivity and cost saving effect

Active Publication Date: 2011-07-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] For Pd / TiO in the prior art 2 The selectivity of hydrogenation catalyst is low, and the shortcoming that the load capacity of active component Pd is difficult to improve, the object of the present invention is to provide a kind of method that adopts pH swing to be in TiO 2 -C powder loaded with high content of noble metal Pd to prepare highly selective Pd / TiO 2 -C hydrogenation catalyst method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) the hydrochloric acid solution containing palladium chloride that the preparation pH value is 2, and the sodium hydroxide solution that the pH value is 12;

[0032] (2) Under stirring conditions, the mass content of C is 7%, the particle size is 200 mesh, and the specific surface area is 200m 2 / g, pore volume 0.6cm 3 / g, TiO with a pore volume of less than 2nm and a percentage of the total pore volume of 3% 2 -C powder is dispersed in 10 times the mass of deionized water to prepare TiO 2 -C powder suspension solution, the temperature of the suspension solution is controlled at 50°C;

[0033] (3) the hydrochloric acid solution containing palladium chloride prepared by step (1) is added dropwise to the TiO of step (2) 2 In the suspension solution of -C powder, adjust the pH value of the suspension to 3, stop feeding, and stay for 0.2h. Then add sodium hydroxide solution until the pH value reaches 10, stop feeding, and stay for 0.2h. Then add the hydrochloric aci...

Embodiment 2

[0037] (1) the hydrochloric acid solution containing palladium chloride that the preparation pH value is 1, and the sodium hydroxide solution that the pH value is 9;

[0038] (2) Under stirring conditions, the mass content of C is 7%, the particle size is 200 mesh, and the specific surface area is 200m 2 / g, pore volume 0.6cm 3 / g, TiO with a pore volume of less than 2nm and a percentage of the total pore volume of 3% 2 -C powder is dispersed in 10 times the mass of deionized water to prepare TiO 2 -C powder suspension solution, the temperature of the suspension solution is controlled at 5°C;

[0039] (3) the hydrochloric acid solution containing palladium chloride prepared by step (1) is added dropwise to the TiO of step (2) 2 In the suspension solution of -C powder, adjust the pH value of the suspension to 2, stop feeding, and stay for 0.2h. Then add sodium hydroxide solution until the pH value reaches 8, stop feeding, and stay for 0.2h. Then add the hydrochloric acid s...

Embodiment 3

[0043] (1) the hydrochloric acid solution containing palladium chloride that the preparation pH value is 3, and the sodium hydroxide solution that the pH value is 13;

[0044] (2) Under stirring conditions, the mass content of C is 7%, the particle size is 200 mesh, and the specific surface area is 200m 2 / g, pore volume 0.6cm 3 / g, TiO with a pore volume of less than 2nm and a percentage of the total pore volume of 3% 2 -C powder is dispersed in 10 times the mass of deionized water to prepare TiO 2 -C powder suspension solution, the temperature of the suspension solution is controlled at 95°C;

[0045] (3) the hydrochloric acid solution containing palladium chloride prepared by step (1) is added dropwise to the TiO of step (2) 2 In the suspension solution of -C powder, adjust the pH value of the suspension to 4, stop feeding, and stay for 1 hour. Then add sodium hydroxide solution until the pH value reaches 12, stop feeding, and stay for 1h. Then add the hydrochloric aci...

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Abstract

The invention provides a method for preparing a high-selectivity Pd/TiO2-C hydrogenation catalyst, which comprises the following steps of: preparing an inorganic acid solution of a Pd-containing compound, and preparing an inorganic base solution of the Pd-containing compound; preparing a suspension solution of TiO2-C powder; adding the inorganic acid solution of the Pd-containing compound into the suspension solution of TiO2-C powder, regulating the pH value of the suspension to be 2-4, and standing for 0.01-1 hour; adding the inorganic base solution until the pH value reaches 8-12, and standing for 0.01-1 hour; adding the inorganic acid solution of the Pd-containing compound, regulating the pH value of the suspension to be 2-4, and standing for 0.01-1 hour, thereby finishing one PH swing; repeating the processes for 1-10 times; and then, reducing the suspension by a reducer to obtain the Pd/TiO2-C hydrogenation catalyst in which the Pd content is 1.1-20%. The Pd/TiO2-C hydrogenation catalyst prepared by the method provided by the invention has high hydrogenation conversion rate and high selectivity.

Description

technical field [0001] The present invention relates to a kind of highly selective Pd / TiO 2 -C hydrogenation catalyst preparation method, the catalyst can be used for catalytic hydrogenation of various unsaturated organic compounds in petrochemical, pharmaceutical, dyestuff, pesticide and other industries, especially for the selection of nitro, alkyne, ketone, aldehyde, etc. Sexual hydrogenation. Background technique [0002] Supported noble metal catalysts have good hydrogenation performance, and are used in the catalytic hydrogenation of various unsaturated organic compounds in petrochemical, pharmaceutical, dyestuff, pesticide and other industries, especially the selective addition of nitro, alkynes, ketones, aldehydes, etc. Hydrogen plays an extremely important role. The properties of the catalyst are not only determined by the composition and content, but also closely related to the preparation method and process conditions of the catalyst. The same raw material, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07B35/02
Inventor 王继元曾崇余堵文斌许建文卞伯同陈韶辉柏基业朱庆奋庞焱
Owner CHINA PETROLEUM & CHEM CORP
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