Method for preparing supported palladium/carbon catalyst

A carbon catalyst and supported palladium technology, applied in the field of preparation of supported palladium/carbon catalysts, can solve the problems of low crystallite content, low conversion rate, low Pd dispersion and the like, and achieve high crystallite content, simple steps, Long service life effect

Inactive Publication Date: 2008-02-13
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 dispersion, low crystallite content, and

Method used

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  • Method for preparing supported palladium/carbon catalyst
  • Method for preparing supported palladium/carbon catalyst
  • Method for preparing supported palladium/carbon catalyst

Examples

Experimental program
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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 palladium-containing 16% by weight of chloropalladium acid solution, add deionized water to 40 milliliters, then add 2.16 grams of 10% by weight of additive A aqueous solution, and add deionized water to prepare Pd solution 60 ml. Alkali was added to adjust the pH of the palladium solution to 7, and after the Pd solution was stable for 180 minutes, the above-mentioned treated activated carbon was 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 was immersed in the red...

Embodiment 2～24

[0056] Select different Pd-containing compounds and additives to prepare the Pd solution, and the rest are the same as in Example 1. For the specific Pd-containing compound, the content of the Pd-containing compound in the Pd solution (calculated as Pd), the specific additive and the molar ratio of the additive and Pd, see Listed in Table 1.

Embodiment 25～31

[0058] According to the various steps and conditions of Example 1, different Pd-containing compounds and additives are selected to prepare the Pd solution. After the Pd solution is stable for 180 minutes, the Pd solution is sprayed on the activated carbon to obtain a catalyst precursor. In addition, the type of inorganic acid, inorganic acid Concentration, pickling time, drying time, temperature, pH value of additive and Pd compound solution, reducing agent type, reduction treatment temperature and reduction treatment time, all the other are the same as Example 1, and the changed conditions are shown in Table 2.

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Abstract

The present invention relates to a loaded-type palladium/carbon catalyst preparation method, which mainly solves the problems in prior art that in the prepared Pd/C catalyst, the dispersibility of metal Pd is low; a crystallite content of which is low; the thermal stability is bad, and the transformation rate towards carboxyl benzaldehyde is low. The present invention solves the problems well by a technical proposal that activated carbon is adopted as a carrier; the Pd solution is used to soak or spray on the activated carbon to make the activated carbon into palladium/carbon, in which the Pd solution is added with R1, R2 or R3, which are all selected from one of H, CH3, NH2, OH or COOH, and n or m, which are all selected from an integer from 0 to 5. The present invention can be used for the industrial production of the catalyst towards methyl benzoic acid, which is prepared by a selective hydrogenation reaction towards the carboxyl benzaldehyde.

Description

technical field [0001] The invention relates to a preparation method of a supported palladium / carbon catalyst, in particular to a preparation method of a supported 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. [00...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J21/18C07C63/26C07B35/02
CPCB01J35/008B01J37/0203B01J35/006B01J37/10B01J37/0207B01J21/18B01J35/0013B82Y40/00B01J23/44B82Y30/00B01J37/16B01J35/0066B01J37/02C07C55/22
Inventor 钱斌畅延青陈大伟杨为民唐泓朱小莉肖忠斌
Owner CHINA PETROLEUM & CHEM CORP
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