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Method for preparing high-activity palladium/carbon catalyst

A carbon catalyst and high-activity technology, which is applied in the preparation of organic compounds, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of low Pd dispersion, poor thermal stability, and low crystallite content. Effects of long life, high thermal stability, and high crystallite content

Inactive Publication Date: 2010-02-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is that the Pd / C catalyst prepared in the prior art has low Pd dispersity, low crystallite content, poor thermal stability, and low conversion rate of raw materials to carboxyformaldehyde (4-CBA). A new method for the preparation of highly active palladium / carbon catalysts for hydrogenation

Method used

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  • Method for preparing high-activity palladium/carbon catalyst
  • Method for preparing high-activity palladium/carbon catalyst
  • Method for preparing high-activity palladium/carbon catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] 100 grams of 4 to 8 mesh, specific surface 800 to 1800 meters 2 The coconut shell activated carbon per gram was washed with 0.4 mol / liter of nitric acid, then washed with water until neutral, and dried at 120°C for 6 hours for later use.

[0054] The preparation of Pd solution, get 3.2 grams of the chloropalladium acid solution containing palladium 16% by weight, add deionized water to 40 milliliters, then add 0.42 milliliters of additive A of 10 weight percent therein 1 aqueous solution, and added deionized water to prepare 60 ml of Pd solution. Alkali is added to adjust the pH of the palladium solution to 7, and after the Pd solution is stable for 180 minutes, the above-mentioned treated activated carbon is impregnated with the Pd solution for 3 hours to obtain a catalyst precursor. The catalyst precursor was aged for 24 hours, and the reducing solution was formulated with 20 grams of 5% by weight hydrazine hydrate and 200 grams of pure water. The catalyst precursor ...

Embodiment 2～48

[0056] Select different Pd-containing compounds and additives to prepare the Pd solution, and the rest are the same as [Example 1], the specific Pd-containing compound, the content of the Pd-containing compound in the Pd solution (calculated as Pd), the specific additive and the mole of the additive and Pd See Table 1 for comparison.

Embodiment 49～54

[0058] Different Pd-containing compounds and additives were selected to prepare the Pd solution. After the Pd solution was stable for 10-200 minutes, the Pd solution was sprayed on activated carbon to obtain a catalyst precursor, and the rest were the same as [Example 1].

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Abstract

The invention relates to a method for preparing a high-activity palladium / carbon catalyst and mainly aims to solve the problem that the prepared Pd / C catalyst in the prior art has the drawbacks of lowmetal Pd dispersity, low micro crystal content, poor thermal stability and low 4-carboxybenzaldehyde conversion rate. In the method, active carbon serving as a carrier is impregnated or sprayed witha solution containing Pd to form the palladium / carbon, wherein the solution containing Pd is added with an additive (represented by a formula); and in the formula, n or m is an integer selected from arange from 0 to 5, R1 and R2 may be H, CH3, NH2, OH or COOH, R3 may be H or R4-(CH2)l-CHCOOH, I is an integer selected from a range from 0 to 5, and R4 may be H, CH3, NH2, OH or COOH. Therefore, theproblems can be better solved by the technical scheme. The method can also be applied to the industrialized production of the p-toluic acid catalyst which is prepared by selective hydrogenation of the4-carboxybenzaldehyde.

Description

technical field [0001] The invention relates to a preparation method of a high-activity palladium / carbon catalyst, in particular to a preparation method of a high-activity palladium / carbon catalyst used for refining crude terephthalic acid through selective hydrogenation reaction. Background technique [0002] The supported palladium / carbon catalyst is mainly used for the selective hydrogenation of unsaturated organic matter, especially for the purification of crude terephthalic acid. Impurities such as p-carboxybenzaldehyde (4-CBA) in crude terephthalic acid are After the hydrogen is transformed into other compounds, it can be separated and purified by crystallization. Because the palladium / carbon catalyst usually adopts a single active component, its improvement research has always focused on the structure of the support and the distribution of metal Pd on the support in the prior art, and this will indeed have a great impact on the performance of the catalyst. influences...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07C63/26C07C51/487C07C51/42B01J21/16
Inventor 钱斌畅延青陈大伟唐泓朱小莉肖忠斌
Owner CHINA PETROLEUM & CHEM CORP
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