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Preparation method for nanocrystalline palladium-carbon catalyst with high activity

A technology of palladium carbon catalyst and nano crystallite, which is applied in the field of preparation of highly active nano palladium carbon catalyst, can solve the problems of poor dispersibility of active palladium particles, low yield of hydrogenation products, and few times of repeated application, and achieve small dispersion, The effect of good batch reproducibility and high number of repeated applications

Inactive Publication Date: 2016-07-20
SHAANXI KENUOHUA CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation of a highly active nano-microcrystalline palladium carbon catalyst for the shortcomings of poor dispersibility of active palladium particles in the traditional palladium carbon catalyst production process, few times of repeated application, low hydrogenation product yield and high by-products. method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Preparation of palladium complex: 8.4gPdCl 2 Add to 100ml ethanol water (volume ratio 2:1) mixed solvent, stir at 20°C for 45min, then add 20ml choline chloride, urea, ethylene glycol mixture (the mass of choline chloride, urea, ethylene glycol The ratio is 2:1:1), ultrasonic oscillation for 35min.

[0020] (2) Adsorption of the palladium complex: Add the palladium complex obtained above under a nitrogen atmosphere by stirring and dropping, impregnating and adsorbing on 95g of pre-treated carbon carrier, the dropping rate is 2ml / min, and the stirring speed is 800rpm, The adsorption temperature is 40°C, and the adsorption time is 2h.

[0021] (3) Reduction: Add 60ml of a mixed reducing agent with a concentration of 1mol / L (the molar ratio of formaldehyde and hydrazine hydrate is 2:1) at a rate of 1ml / min, and control the pH of the reaction solution by adding 5% NaOH aqueous solution=6- 9. After reacting for 100 minutes, cool and filter;

[0022] (4) Washing and dr...

Embodiment 2

[0024] (1) Preparation of palladium complex: 1.68gPdCl 2 Add to 25ml ethanol water (volume ratio 1:1) mixed solvent, stir at 25°C for 30min, then add 5ml choline chloride, urea, ethylene glycol mixture (the mass of choline chloride, urea, ethylene glycol Ratio of 1:1:1), ultrasonic oscillation for 25min.

[0025] (2) Adsorption of the palladium complex: Add the palladium complex obtained above under a nitrogen atmosphere by stirring and dropping, impregnating and adsorbing on 99g of pre-treated carbon carrier, the dropping speed is 5ml / min, and the stirring speed is 600rpm, The adsorption temperature is 30°C, and the adsorption time is 4h.

[0026] (3) Reduction: Add 10ml of a mixed reducing agent with a concentration of 0.5mol / L (the molar ratio of formaldehyde and sodium formate is 1:1) at a rate of 2ml / min, and control the pH of the reaction solution by adding 5% NaOH aqueous solution=4- 9. After reacting for 60 minutes, cool and filter;

[0027] (4) Washing and drying: ...

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Abstract

The invention discloses a preparation method for a nanocrystalline palladium-carbon catalyst with high activity. The preparation method comprises the following steps: preparation of a palladium complex; adsorption and adhesion of the palladium complex; preparation of a reducing agent; ultrasonic-assisted reduction and drying; etc. The nanocrystalline palladium-carbon catalyst with high activity prepared in the invention mainly overcomes the problems of difficulty in effective control of granularity and dispersity of palladium in palladium-carbon catalysts produced by traditional precipitation methods and impregnation methods, poor repeatability of batch production of the catalysts, large particle sizes, wide distribution range, low dispersity and poor stability of prepared active palladium particles, contamination of products caused by shedding of nanometer palladium particles, low repeated usage frequencies, etc. The nanocrystalline palladium-carbon catalyst with high activity prepared in the invention has the advantages of small sizes and smaller dispersity of active palladium particles, and better catalytic activity, better selectivity and higher repeated usage frequencies in catalytic reactions, etc.

Description

technical field [0001] The invention relates to the field of supported noble metal catalysts, in particular to a preparation method of a highly active nano palladium carbon catalyst. Background technique [0002] As we all know, palladium carbon is a traditional supported noble metal catalyst, which has been widely used in medicine and chemical industry, especially in the hydroprocessing of terephthalic acid, the disproportionation of rosin to produce disproportionated rosin and the synthesis of meropenem. The process stability and repeatability of palladium carbon catalyst prepared by traditional precipitation method and impregnation method are not good, and the production process is cumbersome, consumes a lot, and the operational factors affecting product performance are complex and difficult to control. The prepared palladium carbon catalyst contains active palladium particles. Large particle size, wide distribution range, uneven distribution, low dispersion, poor stabili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44
Inventor 吴伯华于雷白掖卫
Owner SHAANXI KENUOHUA CHEM TECH CO LTD
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