Method for preparing load type palladium/carbon catalyst

A carbon catalyst and supported palladium technology, which is applied in the field of preparation of supported palladium/carbon catalysts, can solve the problems of strong uncertain negative influence, difficulty in uniform distribution of supported activated carbon, influence on Pd dispersibility, etc., so as to increase the anchoring effect. Effect

Inactive Publication Date: 2005-12-21
CHINA PETROLEUM & CHEM CORP
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Problems solved by technology

However, because hydrogen peroxide itself is also oxidizing, it can oxidize the surface groups of activated carbon, which will change the surface physical and chemical properties of the support, that is, change the surface group structure of the support, which has a strong uncertain negative impact and will damage the catalyst. Other properties, such as palladium loading strength, catalyst life, selectivity, etc.
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

Method used

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  • Method for preparing load type palladium/carbon catalyst
  • Method for preparing load type palladium/carbon catalyst
  • Method for preparing load type palladium/carbon catalyst

Examples

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[0041] [Example 1]

[0042] Put 100 grams of 4~8 mesh with a specific surface area of ​​800~1800m 2 / g coconut shell activated carbon was washed with 0.4N nitric acid at a washing temperature of 80°C, and then washed with water to neutrality.

[0043] Prepare Br with potassium bromide and water - Soak the solution with a concentration of 0.01N, soak the activated carbon in an equal volume for 2-24 hours, and dry it at 80-120°C for 2-8 hours.

[0044]To prepare the Pd solution, take the required amount of chloropalladic acid solution containing 16wt% palladium, add deionized water to 40ml, and then add the required amount of ethylenediaminetetraacetic acid disodium 10wt% aqueous solution to it, and Add deionized water to prepare 60 ml of Pd solution. After the Pd solution is stable for 10 to 200 minutes, the treated activated carbon is immersed in the Pd solution for 3 hours to obtain a catalyst precursor. The catalyst precursor is aged for 24 hours, and 20 grams of 5wt% hydrazine ...

Example

[0045] [Examples 2-8]

[0046] Different halides are used to prepare the infiltration solution containing halogen ions, and the rest are the same as in Example 1. The specific halide and halide ion concentration of the infiltration solution are listed in Table 1.

Example

[0047] [Examples 9-23]

[0048] Different Pd-containing compounds and chelating agents are used to prepare the Pd solution, and the rest are the same as in Example 1.

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Abstract

This is the producing method of a kind of supported palladium/carbon catalyst. The catalyst makes grains or molding active carbon as carrier, the content of loading active component metal Pd is 0.2 - 4wt%. It orderly includes: have acid wash to carrier active carbon; wash carrier active carbon with water to neutral; have soakage with watery solution containing nitrite ion to carrier active carbon; dry carrier active carbon to get rid of water; prepare Pd solution with water-soluble Pd compound, a kind of chelateding agent and water to infuse or insufflate the carrier active carbon, the content of Pd compound in the Pd solution counted by Pd is 10 - 20wt%; the mol proportion of chelateding agent and Pd is (0.01 - 1) : 1, the chelateding agent is got from anyone of ethylene diamine tetraacetic acid (EDTA), ethylene diamine tetraacetic acid disodium (EDTAD), ethylene diamine tetraacetic acid tetrasodium (EDTAT), hydroxyethyl ethylenediamine triacetic acid (HEDTA), diethylene triamine pentaacetic acid (DTPA) or amine triacetic acid; after having deoxidizing treatment with reducing agent to get activator products.

Description

technical field [0001] The invention relates to a preparation method of a supported palladium / carbon catalyst for 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 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 catalys...

Claims

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Application Information

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IPC IPC(8): B01J23/44
Inventor 钱斌陈大伟畅延青吴征穆宇飞周茂俊
Owner CHINA PETROLEUM & CHEM CORP
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