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Method for preparing Pd/carbon catalyst for hydrofinishing of coarse isophthalic acid

A crude isophthalic acid, hydrogenation refining technology, applied in physical/chemical process catalysts, separation/purification of carboxylic acid compounds, chemical instruments and methods, etc., can solve the problem of low dispersion of metal Pd, low crystallite content, etc. problems, to achieve the effect of easy environmental protection, high microcrystalline content and high activity

Inactive Publication Date: 2009-01-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by this invention is that the dispersibility of metal Pd in ​​the catalyst that exists in the prior art is low, the problem that crystallite content is low, provide a kind of new palladium / Preparation method of carbon catalyst

Method used

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  • Method for preparing Pd/carbon catalyst for hydrofinishing of coarse isophthalic acid
  • Method for preparing Pd/carbon catalyst for hydrofinishing of coarse isophthalic acid
  • Method for preparing Pd/carbon catalyst for hydrofinishing of coarse isophthalic acid

Examples

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Embodiment 1

[0039] 100 grams of 4 to 8 mesh, specific surface 800 to 1200 meters 2 The coconut shell activated carbon per gram is washed with 0.1N 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 impregnation solution with a concentration of 0.2N is used to impregnate activated carbon with equal volume for 8 hours, and then dried at 80-120°C for 2-8 hours for later use.

[0040] Then prepare 40 milliliters of chloropalladium acid solution whose palladium weight content is 0.5%, adjust the pH value to between 4 and 6 with alkali, make it form palladium glue, stabilize it for 10 to 200 minutes, spray the palladium glue The catalyst precursor was obtained on the above treated activated carbon. After the catalyst precursor was aged overnight, 20 grams of 5% by weight sodium formate and 200 grams of pure water were used to prepare a reducing solution. The catalyst precursor was immersed in the re...

Embodiment 2

[0042] Activated carbon is washed with 5.0N nitric acid, and the washing temperature is 80°C, then washed with water until neutral, and all the other are the same as in Example 1.

Embodiment 3

[0044] Activated carbon is washed with 5.0N phosphoric acid, and the washing temperature is 80° C., then washed with water until neutral, and all the other are the same as in Example 1.

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Abstract

The invention relates to a preparation method of a Pd / C catalyst which is used for hydrogenation refining of crude isophthalic acid, and the preparation method is mainly used for solving the problems of low dispersion of metal Pd and low microcrystal content in the catalyst which is prepared by the prior art. The preparation method firstly carries out the pickling of activated carbon carrier, then uses water or alkali for washing till neutral nature and carries out the drying, water solution containing nitrite ions is further used for infiltration, wherein, the concentration of the nitrite ions is 0.01 to 0.5N, the using amount of infiltration liquid is 0.1 to 3.0 times of the saturated absorption amount of the activated carbon carrier, the infiltration time is 2 to 24 hours; the activated carbon is then used for removing water, Pd compound is impregnated, and a reducing agent is further used for carrying out the reduction to obtain a catalyst product; therefore, the technical proposal can better solve the problems and can be used in the industrial production for hydrogenation refining of the crude isophthalic acid.

Description

technical field [0001] The present invention relates to a kind of preparation method that is used for the palladium / charcoal catalyst of crude isophthalic acid hydrogenation refining, especially about the loaded palladium / carbon catalyst that is used for refining crude isophthalic acid by selective hydrogenation reaction Preparation. Background technique [0002] Supported palladium / carbon catalysts are mainly used for the selective hydrogenation of unsaturated organic compounds. The crude isophthalic acid obtained by the oxidation of m-xylene contains a certain amount of by-product impurities, and the existence of m-carboxybenzaldehyde (3-CBA for short) affects the quality and color of polyester, and it is difficult to use the usual crystallization method remove. However, after the selective hydrogenation of the supported palladium / carbon catalyst into m-toluic acid, it can be separated and purified by crystallization. Since the palladium / carbon catalyst usually uses a s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J21/18C07C63/24C07C51/42
Inventor 陈大伟畅延青姜瑞霞唐泓朱小丽张海涛穆宇飞
Owner CHINA PETROLEUM & CHEM CORP
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