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Simple preparation method of palladium-based catalyst and palladium-based catalyst prepared by using same

A catalyst and a palladium-based technology, applied in the field of palladium-based catalysts, can solve the problems of complicated preparation process, the uniformity of palladium particle size needs to be further improved, etc., and achieve the effects of simple preparation process, high stability and high activity

Inactive Publication Date: 2013-05-22
BEIJING GREENCHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Palladium-based catalysts prepared by traditional methods, although the size of palladium nanoparticles is small and highly dispersed, the size uniformity of palladium particles needs to be further improved; and the preparation process is complicated, requiring high temperature reduction, and high temperature often has a negative impact on catalyst activity , thus limiting its application to a certain extent

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  • Simple preparation method of palladium-based catalyst and palladium-based catalyst prepared by using same
  • Simple preparation method of palladium-based catalyst and palladium-based catalyst prepared by using same
  • Simple preparation method of palladium-based catalyst and palladium-based catalyst prepared by using same

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preparation example Construction

[0035] Palladium-based catalyst preparation method of the present invention, comprises the steps:

[0036] (1) Preparation of monodisperse, small-sized palladium nanoparticles

[0037] Under the protection of the surfactant, the metal palladium salt is reduced with a reducing agent to obtain monodisperse, small-sized palladium nanoparticles. Wherein, surfactant can be cetyl sodium sulfonate, polypyrrolidone and / or citric acid etc.; Metal palladium salt can be palladium chloride, palladium acetate and / or sodium chloropalladate etc.; Sodium, hydrazine hydrate and / or sodium formate, etc., preferably use sodium borohydride as the reducing agent. Surfactants are adsorbed on the surface of palladium nanoparticles to prevent particle aggregation and growth. The specific preparation method is as follows:

[0038] Adding a hydrochloric acid solution with a concentration of 0.2 to 2M or a sodium chloride solution with a mass percentage concentration of 10 to 30% into a certain amount...

Embodiment 1

[0049] Dissolve 1g of palladium chloride in 100mL of deionized water, then add 1mL of 2M hydrochloric acid solution, stir until the palladium chloride is completely dissolved, add 2g of citric acid, and obtain a brown solution A after ultrasonic dispersion. In addition, 2 g of sodium borohydride was weighed and added to 100 mL of deionized water, and a clear and transparent solution B was obtained after ultrasonic dissolution. Under vigorous stirring conditions, solution B was quickly poured into solution A, continued to stir for 2 hours, centrifuged, washed with deionized water and ethanol 5 times, and dried in vacuum at 80 ° C for 12 hours to obtain palladium nanoparticle solids. Figure 1A Transmission electron microscopy (TEM) of the prepared palladium nanoparticles. Depend on Figure 1A It can be seen that the size of palladium nanoparticles is relatively uniform, and the particle diameter is about 2-5 nm. The nanoparticles were dispersed and no agglomeration was observed...

Embodiment 2

[0052] Dissolve 1g of palladium chloride in 100mL of deionized water, then add 1mL of 2M hydrochloric acid solution, stir until the palladium chloride is completely dissolved, add 2g of citric acid, and obtain a brown solution A after ultrasonic dispersion. In addition, 2 g of sodium borohydride was weighed and added to 100 mL of deionized water, and a clear and transparent solution B was obtained after ultrasonic dissolution. Under vigorous stirring conditions, solution B was quickly poured into solution A, continued to stir for 2 hours, centrifuged, washed with deionized water and ethanol 5 times, and dried in vacuum at 80 ° C for 12 hours to obtain palladium nanoparticle solids.

[0053] 100g of activated carbon was added in 200mL of concentrated nitric acid solution, heated and boiled and refluxed for 4 hours, washed 5 times with deionized water, and dried at 80°C to obtain an acidified activated carbon carrier. The surface of the acidified carrier contains a large number ...

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Abstract

The invention relates to a simple preparation method of a high-activity and high-stability palladium-based catalyst, which comprises the following steps: preparing small monodisperse palladium nano particles, and adsorbing the palladium nano particles on the surface of a carrier. The simple preparation method specifically comprises the following steps: under the protection action of surfactant, reducing metal palladium salt with reducer to obtain the small monodisperse palladium nano particles; and ultrasonically dispersing the palladium nano particle and the carrier in deionized water, adsorbing while stirring for 10-24 hours, performing centrifugal separation, washing, and drying to obtain the palladium-based catalyst. The palladium nano particles of the palladium-based catalyst prepared by the method are uniform in size, and the particle size is 2-5 nm. The palladium-based catalyst preparation method provided by the invention is simple and low in cost; high-temperature treatment is not required; and the prepared catalyst has excellent catalytic activity and stability, can be used circularly and repeatedly and has wide application prospects.

Description

technical field [0001] The invention relates to a simple preparation method for obtaining a palladium-based catalyst with high activity and high stability by adsorbing palladium nanoparticles on a carrier, and also relates to a palladium-based catalyst prepared by the method, which belongs to the technical field of organic synthesis. Background technique [0002] Due to its high activity, high selectivity and good cycle performance, palladium catalysts are widely used in the hydrogenation of unsaturated organic compounds, C-C coupling reaction, terephthalic acid purification, etc., such as widely used in industry palladium carbon catalyst. [0003] High activity, high selectivity and long life are the main technical performance indicators of palladium-based catalysts. The main factors affecting the performance of palladium-based catalysts are the content of active metal palladium, the size and dispersion of palladium particles, and the strength of the interaction between pa...

Claims

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Application Information

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IPC IPC(8): B01J23/44
Inventor 宋卫国宫宁瑞曹昌燕刘华
Owner BEIJING GREENCHEM TECH
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