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Microwave method for synthesizing attapulgite and palladium nanocomposite catalyst

A composite material and catalyst technology, applied in physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of long preparation process, achieve high catalytic activity, specific The effect of large surface area

Inactive Publication Date: 2013-01-02
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation process of the patent application is relatively long

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  • Microwave method for synthesizing attapulgite and palladium nanocomposite catalyst
  • Microwave method for synthesizing attapulgite and palladium nanocomposite catalyst

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Embodiment 1

[0026] The method for synthesizing attapulgite / palladium nanocomposite catalyst by microwave method comprises the following steps:

[0027] 1) Add 0.25 g of polyvinylpyrrolidone to 40 mL of distilled water, stir to dissolve, then add 0.1 g of purified attapulgite, and ultrasonically disperse;

[0028] 2) Add 2.6 mL of PdCl to the above mixture 2 (10 mg / mL) solution was stirred for 1 hour;

[0029] 3) Finally, add 5 mL of ascorbic acid (80 g / L) and mix well, transfer the solution to a microwave chemical reactor, connect with condensed water, set the power to 200 W, and react with microwave for 3 minutes, take it out, and naturally Cool to room temperature, take out the sample, wash it ultrasonically, wash it with water and ethanol three times each, and dry it at 60°C to obtain the attapulgite / palladium nanocomposite catalyst.

[0030] Observation by transmission electron microscope shows that in the obtained attapulgite / palladium nanocomposite catalyst, the surface of the att...

Embodiment 2

[0032] The method for synthesizing attapulgite / palladium nanocomposite catalyst by microwave method comprises the following steps:

[0033] 1) Add 0.20 g of polyvinylpyrrolidone to 40 mL of distilled water, stir to dissolve, then add 0.1 g of purified attapulgite, and ultrasonically disperse;

[0034] 2) Add 4 mL of Na to the above mixture 2 PdCl 4 (10 mg / mL) solution was stirred for 1 hour;

[0035] 3) Finally, add 5 mL of ascorbic acid (80 g / L) and mix well, transfer the solution to a microwave chemical reactor, connect with condensed water, set the power to 200 W, and react with microwave for 3 minutes, take it out, and naturally Cool to room temperature, take out the sample, wash it ultrasonically, wash it with water and ethanol three times each, and dry it at 60°C to obtain the attapulgite / palladium nanocomposite catalyst. Observation by transmission electron microscope shows that compared with the product obtained in Example 1, the structure is basically similar.

Embodiment 3

[0037] The method for synthesizing attapulgite / palladium nanocomposite catalyst by microwave method comprises the following steps:

[0038] 1) Add 0.25 g of polyvinylpyrrolidone to 50 mL of distilled water, stir to dissolve, then add 0.1 g of purified attapulgite, and ultrasonically disperse;

[0039] 2) Add 4.5 mL of K to the above mixture 2 PdCl 4 (10 mg / mL) solution was stirred for 1 hour;

[0040] 3) Finally, add 5 mL of ascorbic acid (80 g / L) and mix well, transfer the solution to a microwave chemical reactor, connect it with condensed water, set the power at 200 W, and heat it in microwave for 3 minutes, take it out, and naturally Cool to room temperature, take out the sample, wash it ultrasonically, wash it with water and ethanol three times each, and dry it at 60°C to obtain the attapulgite / palladium nanocomposite catalyst. Observation by transmission electron microscope shows that compared with the product obtained in Example 1, the structure is basically similar. ...

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Abstract

The invention discloses a microwave method for synthesizing an attapulgite and palladium nanocomposite catalyst. The microwave method comprises the following steps of: ultrasonically dispersing purified attapulgite into a polyvinylpyrrolidone solution; adding a Pd II salt solution into the polyvinylpyrrolidone solution, and fully and uniformly mixing the two solutions; adding a reducing agent into the mixed solution, uniformly mixing the mixed solution and the reducing agent, and then carrying out reaction on the mixture under microwave radiation; reducing palladium ions onto the surface of attapulgite; and cooling, scouring and drying reaction products, thus obtaining the attapulgite and palladium nanocomposite catalyst, wherein nanometre particles of palladium in the obtained attapulgite and palladium nanocomposite catalyst are uniformly loaded on a rod-shaped attapulgite structure. The microwave method disclosed by the invention has the characteristics of energy conservation, environmental friendliness, rapidity and simple process; and the prepared catalyst can be used for rapidly catalyzing sodium borohydride to reduce p-nitrophenol.

Description

technical field [0001] The invention relates to the preparation of an attapulgite clay nanocomposite material, in particular to a method for preparing an attapulgite / palladium nanocomposite catalyst, that is, a method for preparing an attapulgite-supported palladium nanocomposite catalyst. Background technique [0002] In the production process of chemical products, more than 85% of the reactions are carried out under the action of catalysts. Noble metal Pd catalysts occupy an extremely important position in chemical production due to their excellent catalytic activity and selectivity. For example, palladium catalyst is used to reduce nitrobenzene to phenyl hydroxylamine, which is then converted to p-aminophenol; palladium-gold-copper catalyst is used to synthesize vinyl acetate; palladium-containing solid catalyst is used to synthesize aldehydes or ketones, etc. [0003] On the other hand, by adopting a suitable catalyst support, it is also beneficial to improve the utiliz...

Claims

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Application Information

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IPC IPC(8): B01J23/44C07C215/76C07C213/02
Inventor 张卉林慧清蔡称心吴萍
Owner NANJING NORMAL UNIVERSITY
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