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Preparation method of palladium carbon catalyst

A palladium-carbon catalyst and catalyst technology, applied in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high metal palladium crystallite content, good dispersibility, and low metal palladium dispersion performance , to achieve high hydrogenation performance, good dispersion, and eliminate the effect of strong reduction centers

Active Publication Date: 2012-08-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In view of the shortcomings of the unsatisfactory control method and low dispersion performance of the metal palladium crystallite content in the crude terephthalic acid hydrotreating Pd / C catalyst, the purpose of the present invention is to provide a preparation method for the palladium carbon catalyst. Invented catalyst with high palladium crystallite content and good dispersibility

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take 10 g of particles with a particle size of 4-8 mesh and a specific surface area of ​​1050 m 2 / g of granular coconut shell carbon was put into deionized water, set the speed at 500 r / min, and stirred continuously for 5 h to remove the dust adsorbed on the surface of the activated carbon and the loose parts on the surface, and dried at 120 °C for 5 h for later use. The pretreated activated carbon was impregnated in a cyclohexane solvent containing titanium tetrachloride for 1 h, and then purged with nitrogen at a flow rate of 500 ml / min and a humidity of 50% for 2 h after filtration. Finally, it was dried at 120°C for 5 h, then impregnated with a solution containing palladium chloride, and then reduced with a sodium formate solution at room temperature for 2 h. After the reduction, it was washed until neutral to obtain the palladium-carbon catalyst of this example.

[0037] The palladium-carbon catalyst obtained in this embodiment has the following properties: the co...

Embodiment 2

[0040] Take 10 g of particles with a particle size of 4-8 mesh and a specific surface area of ​​1050 m 2 / g shaped coconut shell carbon was put into deionized water, set the speed at 500 r / min, and stirred continuously for 5 h to remove the dust adsorbed on the surface of the activated carbon and the loose parts on the surface, and dried at 120 °C for 5 h for later use. The pretreated activated carbon was sprayed with light naphtha solvent containing titanium tetrachloride for 0.1 h, and after filtration, it was purged with nitrogen gas at a flow rate of 1000 ml / min and a humidity of 90% for 1 h. Finally, after drying at 120°C for 5 h, impregnated with a solution containing palladium acetate, and then reduced with sodium formate solution at room temperature for 2 h, and washed until neutral after reduction to obtain the palladium-carbon catalyst of this example.

[0041] The palladium-carbon catalyst obtained in this embodiment has the following properties: the content of meta...

Embodiment 3

[0044] Take 10 g of particles with a particle size of 4-8 mesh and a specific surface area of ​​1050 m 2 / g of granular coconut shell carbon was put into deionized water, set the speed at 500 r / min, and stirred continuously for 5 h to remove the dust adsorbed on the surface of the activated carbon and the loose parts on the surface, and dried at 120 °C for 5 h for later use. The pretreated activated carbon was impregnated in a xylene solvent containing tetrabutyl titanate for 10 h, and after filtration, it was purged with nitrogen gas at a flow rate of 10 ml / min and a humidity of 10% for 10 h. Finally, it was dried at 120°C for 5 h, then impregnated with a solution containing palladium nitrate, and then treated with sodium formate solution at room temperature for 2 h. After the reduction, it was washed until neutral to obtain the palladium-carbon catalyst of this example.

[0045] The palladium-carbon catalyst that present embodiment obtains has following properties: the conte...

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Abstract

The invention discloses a preparation method of a palladium carbon catalyst for hydrorefining of terephthalic acid. The method is characterized by employing the following steps of: exposing pretreated particles or molding activated carbon to light hydrocarbon solvent of titanium-containing compounds; filtering and purging with nitrogen gas; drying and impregnating the mixture into a solution of palladium-containing compound; reducing and washing the mixture to neutral, so as to obtain the palladium carbon catalyst. Compared with the prior art, the invention is characterized in that, first, grafted titanium dioxide and its cluster are firmly connected with activated carbon carrier, thereby effectively eliminating a strong reduction center on the activated carbon surface; second, the palladium carbon catalyst has high microcrystal content of metal palladium, good dispersion and high activity of catalyst. and third, the preparation method of the catalyst is simple.

Description

technical field [0001] The invention relates to a preparation method of a palladium-carbon catalyst, in particular to a preparation method of a palladium-carbon catalyst used for hydrogenation purification of aromatic aldehydes such as crude terephthalic acid or p-carboxybenzaldehyde. [0002] Background technique [0003] Purified terephthalic acid (PTA) is a very important organic chemical raw material, and its downstream processing products are mainly polyester fibers, polyester films, packaging bottles and PET engineering plastics. In the crude terephthalic acid (CTA) produced by the liquid-phase oxidation of p-xylene (PX), it generally contains 2000-3000 μg / g of p-carboxybenzaldehyde (4-CBA), the main impurity, because its aldehyde group is relatively active , which will affect the color of polyester fiber, it is necessary to convert 4-CBA into p-toluic acid, which is easily soluble in hot water, by hydrogenation and refining at a high temperature of 270-285 ° C. The r...

Claims

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Application Information

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IPC IPC(8): B01J23/44C07C51/487C07C63/26
Inventor 堵文斌王继元许建文卞伯同陈韶辉杨爱武柏基业朱庆奋庞焱
Owner CHINA PETROLEUM & CHEM CORP
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