Method for preparing palladium/carbon catalyzer by hydrogenising and refining crude terephthalic acid

A technology of crude terephthalic acid and carbon catalyst, which is applied in the preparation of organic compounds, catalysts for physical/chemical processes, preparation of carboxylate, etc. Easy eco-friendly disposal, long service life, simple steps effect

Inactive Publication Date: 2005-01-19
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the stability of the impregnation solution containing Pd compounds is very poor, which relatively increases the requirements of the catalyst preparation process.
U.S. Patent No. 4,476,242 proposes to use organic solvents such as methanol or pyridine to prepare impregnation solutions containing Pd compounds. It is said that this is also very effective in preventing the migration of Pd and grain growth, but the production process uses methanol or pyridine. Harmful organic compounds to the human body are unfavorable in terms of environmental protection or labor protection

Method used

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  • Method for preparing palladium/carbon catalyzer by hydrogenising and refining crude terephthalic acid
  • Method for preparing palladium/carbon catalyzer by hydrogenising and refining crude terephthalic acid
  • Method for preparing palladium/carbon catalyzer by hydrogenising and refining crude terephthalic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0038] 100 grams of 4-8 mesh, specific surface 800-1200m 2 / g coconut shell activated carbon is washed with 0.4N nitric acid at 80°C, then washed with water until neutral, and dried at 120°C for 2 to 8 hours. Prepare NO with sodium nitrite and water 2 - The impregnating solution with a concentration of 0.01N is used to impregnate the activated carbon with an equal volume for 2 to 24 hours, and to dry at 80 to 120°C for 2 to 8 hours before use.

[0039] Then prepare 40 milliliters of chloropalladium acid solution whose palladium content is 0.5wt%, add about 1.0 milliliters of tartaric acid of 2wt% therein, then adjust the pH value to between 4~6 with alkali, make it form palladium glue, stable After 10 to 200 minutes, the palladium colloid solution is sprayed on the above-mentioned treated activated carbon to obtain a catalyst precursor. After aging the catalyst precursor overnight, use 20 grams of 5wt% sodium formate and 200 grams of pure water to prepare a reducing solutio...

Embodiment 2

[0041] Prepare NO with sodium nitrite and water 2 - Concentration of 0.05N immersion solution, equal volume impregnation of activated carbon for 2 to 24 hours, the rest is the same as in Example 1.

Embodiment 3

[0043] Prepare NO with sodium nitrite and water 2 - Concentration of 0.2N immersion solution, equal volume impregnation of activated carbon for 2 to 24 hours, the rest is the same as in Example 1.

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Abstract

A method for preparing Pd / C catalyst for selective hydrogenation is provided. The content of Pd in catalyst is 0.2 to 5% by weight. The preparing process includes the following steps: active carbon carrier is washed by 0.1 to 5N concentration of acid washing liquid selected from hydrochloric acid, nitric acid or phosphoric acid; active carbon carrier is washed to neutrality by water and dried; the active carbon carrier is soaked in nitrite ion containing solution for 2 to 24 hours and dried; the Pd compound is sprayed on the active carbon carrier to form catalyst precursor, after aging and reduction process, the catalyst product is obtained. Metal Pd in catalyst has higher dispersion degree and the content of crystallite is very high.

Description

technical field [0001] The invention relates to a preparation method of a supported palladium / carbon catalyst for selective hydrogenation reaction, in particular to a preparation method of a supported palladium / carbon catalyst 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 refining process of crude terephthalic acid, where impurities such as p-carboxybenzaldehyde (4-CBA) in crude terephthalic acid are passed through After hydrogenation, it can be transformed into other compounds, which can be separated and purified by crystallization. Since palladium / carbon catalysts usually use a single active component, the research on its improvement has been focused on the structure of the support and the distribution of metal Pd on the support, which will indeed have a great impact on the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07C51/487C07C63/26
Inventor 钱斌吴征陈大伟许红兵
Owner CHINA PETROLEUM & CHEM CORP
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