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Process for preparing Pd/carbon catalyst of high activity

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

Active 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

[0006] The technical problem to be solved by the present invention is that there are problems of poor metal Pd dispersion, low crystallite content and poor thermal stability in the catalyst in the prior art, and a new preparation method of high-activity palladium / carbon catalyst is provided

Method used

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  • Process for preparing Pd/carbon catalyst of high activity
  • Process for preparing Pd/carbon catalyst of high activity
  • Process for preparing Pd/carbon catalyst of high activity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Put 100 grams of 4~8 mesh with a specific surface of 800~1800 meters 2 The coconut shell activated carbon per gram is washed with 0.4 mol / L nitric acid, then washed with water to neutrality, and dried at 120°C for 2-8 hours.

[0029] The above-mentioned treated activated carbon was impregnated with 44 g of Pd solution to obtain a catalyst precursor (Pd content of 0.51 g). The catalyst precursor is aged for 24 hours, reduced with 300 g of 3 wt% sodium formate reducing solution at room temperature for 0.5 hours, and then reduced with 500 g of 0.2 wt% sodium formate reducing solution at 70-100°C for 1 hour, and then washed with pure water The catalyst product is obtained after it is neutralized and dried.

Embodiment 2～12

[0031] Choose different reducing solution concentration, dosage and reduction time, different Pd content, and the rest are the same as in Example 1, see Table 1.

Embodiment 13

[0033] Select hydrazine hydrate as the reducing agent, and the rest are the same as in Example 1.

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Abstract

The invention relates to a preparation method of a high activity Pd / C catalyst, and the preparation method is mainly used for solving the problems of poor Pd dispersion in the catalyst, low microcrystal content and poor thermal stability of the prior art. The preparation method adopts activated carbon as a carrier and impregnates or sprays solution containing Pd on the activated carbon for preparing a precursor of the Pd / C catalyst, the precursor of the catalyst is carried out the step-by-step reduction treatment by using a reducing agent after the aging treatment, reduction fluid with the high concentration of 3 to 30 percent by weight is firstly used for carrying out the reduction for 0.1 to 24 hours at the normal temperature, then the reduction fluid with the low concentration of 0.1 to 2 percent by weight is then used for carrying out the reduction for 0.5 to 24 hours at 50 to 120 DEG C, and the Pd / C catalyst is obtained by water washing; therefore, the technical proposal can better solve the problems and can be used in the industrial production of para-toluic acid catalyst by using 4-carboxy benzaldehyde.

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 supported palladium / carbon catalyst used for selective hydrogenation reaction to refine crude terephthalic acid. Background technique [0002] The supported palladium / carbon catalyst is mainly used for the selective hydrogenation of unsaturated organics, especially for the purification of crude terephthalic acid. Impurities such as p-carboxybenzaldehyde (4-CBA) in crude terephthalic acid are added After the hydrogen is converted into other compounds, it can be separated and purified by crystallization. Since palladium / carbon catalysts usually use a single active component, the prior art has 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 performance of the catalyst. influences. [0003] Since the terephthalic acid hydrofining reaction proce...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J21/18C07C51/487C07C63/26
Inventor 唐泓畅延青
Owner CHINA PETROLEUM & CHEM CORP
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