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Preparation method of nano-palladium catalyst with controllable morphology and size

A nano-palladium and catalyst technology, applied in the field of preparation of nano-palladium catalysts, can solve the problems of short preparation period, mild reaction conditions and the like, and achieve the effects of short preparation period, mild reaction conditions and good catalytic activity

Inactive Publication Date: 2021-09-24
浙江博朗新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there is no preparation method of a nano-palladium catalyst with controllable shape and size, which can achieve the technical effects of mild reaction conditions, short preparation cycle, high stability of the prepared nano-palladium catalyst, and easy mass production.

Method used

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  • Preparation method of nano-palladium catalyst with controllable morphology and size
  • Preparation method of nano-palladium catalyst with controllable morphology and size
  • Preparation method of nano-palladium catalyst with controllable morphology and size

Examples

Experimental program
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Effect test

Embodiment 1

[0033] At room temperature, weigh 3 mg of palladium chloride into a test tube, add 3 mL of dichloromethane, stir until completely dissolved, the solution is bright yellow, and obtain a palladium precursor solution;

[0034] Then add 10 mg of oleic acid as a dispersant to the palladium precursor solution, continue stirring, and then drop 10 μL of phenylsilane into the reaction system, and react for 2 hours to obtain a black colloidal solution;

[0035] Add ethanol to the black colloidal solution to induce aggregation, centrifuge to collect the black product, wash 3 times with ethanol-dichloromethane (volume ratio of ethanol and dichloromethane is 1:1) solution, and then redisperse in dichloromethane to obtain The nano-palladium catalyst, the microscopic appearance is as figure 1 As shown, the nano-palladium particle morphology is spherical, and the particle size is 10nm.

Embodiment 2

[0037] At room temperature, weigh 3 mg of palladium chloride into a test tube, add 3 mL of dichloromethane, stir until completely dissolved, the solution is bright yellow, and obtain a palladium precursor solution;

[0038] Then, 15 mg of oleic acid was added into the palladium precursor solution as a dispersant, and the stirring was continued, and 15 μL of diphenylsilane was added dropwise into the reaction system. After 2 hours of reaction, a black colloidal solution was obtained.

[0039] Add ethanol to the black colloidal solution to induce aggregation, centrifuge to collect the black product, wash 3 times with ethanol-dichloromethane (volume ratio of ethanol and dichloromethane is 1:1) solution, and then redisperse in dichloromethane to obtain The nano-palladium catalyst, the microscopic appearance is as figure 2 As shown, the morphology of nano-palladium particles is ellipsoidal, and the particle size is 15nm.

Embodiment 3

[0041] At room temperature, weigh 3 mg of sodium chloropalladate in a test tube, add 3 mL of dichloromethane, stir until completely dissolved, the solution is bright yellow, and obtain a palladium precursor solution;

[0042] Then, 25 mg of oleic acid was added into the palladium precursor solution as a dispersant, and the stirring was continued, and 30 μL of triphenylsilane was added dropwise into the reaction system. After 2 hours of reaction, a black colloidal solution was obtained.

[0043] Add ethanol to the black colloidal solution to induce aggregation, centrifuge to collect the black product, wash 3 times with ethanol-dichloromethane (volume ratio of ethanol and dichloromethane is 1:1) solution, and then redisperse in dichloromethane to obtain The nano-palladium catalyst, the microscopic appearance is as image 3 As shown, the morphology of nano-palladium particles is hexagonal, and the particle size is 15nm.

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Abstract

The invention discloses a preparation method of a nano-palladium catalyst with controllable morphology and size, and relates to the technical field of nano-palladium catalyst preparation. The preparation method comprises the following steps: S1, adding a palladium source into a solvent, and uniformly stirring to prepare a palladium precursor solution; S2, adding a dispersing agent and a reducing agent into the palladium precursor solution, preparing a mixed solution, performing a reduction reaction, and preparing a colloidal solution; S3, adding ethanol into the colloidal solution for induced aggregation, performing centrifugation and washing, preparing a washed centrifugal product, adding dichloromethane into the washed centrifugal product, and preparing the nano-palladium catalyst with the controllable morphology and size. According to the preparation method provided by the invention, one-step synthesis is adopted, in an organic solvent system, under the protection of oleic acid or oleylamine, an active silicon-hydrogen compound is used as a reducing agent to reduce a palladium precursor, and palladium nanoparticles with various particle sizes and morphologies can be controllably synthesized.

Description

technical field [0001] The invention relates to the technical field of preparing nano-palladium catalysts, in particular to a method for preparing nano-palladium catalysts with controllable shape and size. Background technique [0002] Suzuki coupling reaction refers to a coupling reaction that can effectively generate C-C bonds. The Suzuki coupling reaction uses zero-valent palladium or palladium complexes as catalysts, halogenated aromatic hydrocarbons and boric acid or boric acid esters as reaction substrates, and is a coupling reaction carried out under mild reaction conditions. Compared with the traditional Grignard reaction used to generate C-C bonds, it has the advantages of easy access to boric acid substrates, non-toxicity, insensitivity to water in the system, high yield and easy separation of products. At present, it is widely used in the synthesis system of OLED light-emitting materials and other organic synthesis fields. [0003] For the catalyst selection of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J35/08B01J37/00B01J37/03B01J37/16C07D285/14
CPCB01J23/44B01J37/16B01J37/038B01J37/009B01J37/00C07D285/14B01J35/393B01J35/23B01J35/51
Inventor 陆向红郏侃
Owner 浙江博朗新材料有限公司
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