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Preparation method of high-activity palladium-carbon catalyst

A palladium-carbon catalyst, high-activity technology, applied in catalyst activation/preparation, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of poor catalyst activity, metal migration, small pore size, etc. uniform effect

Inactive Publication Date: 2013-11-20
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, coconut shell activated carbon contains less impurities and has high mechanical strength, but the price is relatively expensive and the pore size is small. It is generally more suitable for loading precious metals.
Keith et al describe in the US3138560 patent that there are some reducing groups on the surface of activated carbon such as aldehyde groups, free electrons and some impurity elements or ions. If the activated carbon is not treated, these reducing groups will directly reduce the palladium salt to form Shiny metal palladium film, causing metal migration and grain growth, resulting in poor catalyst activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Activated carbon pretreatment: use 10% H 2 o 2 and 2%HClO 4 The mixed solution was mixed with 97g of 200-325 mesh coconut shell charcoal activated carbon, the solid-to-liquid ratio was 5:1, stirred at 50°C for 2h, washed with distilled water until neutral, and set aside.

[0027] (2) Loading of palladium precursor: put 97g of treated activated carbon into a 2L flask, beat with 500ml of distilled water, and raise the temperature to 50°C. Add the prepared palladium chloride solution (3g palladium content) at a rate of 20ml / min under stirring, and place the reaction vessel in a 400W ultrasonic device for 30min, continue to stir for 2h and then let it stand overnight.

[0028] (3) Reduction: Slowly add 5% NaOH solution at a rate of 10ml / min until the pH is 9-10, raise the temperature to 80°C, add 6ml of 37% formaldehyde while stirring, reduce for 3 hours, and control the system by adding NaOH The pH is maintained at 8-9. Cool and filter.

[0029] (4) Washing and dr...

Embodiment 2

[0032] With the HClO described in embodiment 1 step (1) 4 Change to CH 3 COOOH, change the palladium chloride described in step (2) into palladium acetate, and other conditions remain unchanged.

Embodiment 3

[0034] The formaldehyde described in the embodiment 1 step (3) is replaced with 4.5ml80% hydrazine hydrate, and other conditions are unchanged.

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PUM

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Abstract

The invention discloses a preparation method of a high-activity palladium-carbon catalyst. The preparation method comprises the following steps of: (1) treating active carbon by using a compound oxidizing agent mixed solution; (2) slowly adding a palladium-chloride solution into the treated active carbon to obtain a mixed solution, and carrying out ultrasonic dispersion on the mixed solution; (3) adding alkali metal hydroxide or carbonate into the mixed solution ultrasonically dispersed to precipitate palladium ions, then adding a reducing agent, washing and drying to obtain a solid catalyst; and (4) carrying out plasma treatment on the solid catalyst to obtain a finished palladium-carbon catalyst. The preparation method disclosed by the invention has the advantages that compared with the traditional nitric acid, the high-activity palladium-carbon catalyst is environment-friendly and low-pollution; due to utilization of ultrasonic treatment, the dispersion of the catalyst is more uniform; and final plasma treatment is carried out on the catalyst, so that the activity of the catalyst is further improved.

Description

technical field [0001] The invention belongs to the field of supported noble metal catalysts, and in particular relates to a preparation method of a highly active palladium-carbon catalyst. The palladium-carbon catalyst is suitable for general hydrogenation reaction systems, and is particularly suitable for the hydrogenation of disproportionated rosin and cinnamaldehyde in the disproportionation of rosin. application. Background technique [0002] As we all know, palladium-carbon catalysts are widely used in medicine and chemical industry, especially in the hydrogenation of terephthalic acid, hydrogenation of unsaturated aldehydes and disproportionation of rosin. The present invention is mainly aimed at the improvement of the palladium-carbon catalyst preparation process, improves the dispersibility and stability of palladium in the pretreatment mode of activated carbon, ultrasonic-plasma technology, etc., and greatly improves the catalytic activity and Palladium utilizatio...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J37/00B01J37/34C07C61/29C07C51/00C07C33/32C07C29/141
Inventor 范丽丽李一平
Owner HOHAI UNIV
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