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Preparation method of graphene gradient-coated polyacrylic acid composite conductive particles

A polyacrylic acid, conductive particle technology, applied in the direction of dyeing polymer organic compounds, fibrous fillers, etc., can solve the problems of easy shedding conductivity, non-abrasion, poor adhesion of the surface coating layer, etc., and achieve dimensional stability. Good, reduce the density, avoid the effect of poor adhesion

Active Publication Date: 2021-03-26
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a preparation method of high conductivity and low cost graphene gradient coated polyacrylic acid composite conductive particles, to solve the problem of poor adhesion, non-abrasion resistance and easy falling off of the surface coating layer in the prior art Or cover the conductivity of the sacrificial conductive layer through covalent bonds, etc.

Method used

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  • Preparation method of graphene gradient-coated polyacrylic acid composite conductive particles
  • Preparation method of graphene gradient-coated polyacrylic acid composite conductive particles
  • Preparation method of graphene gradient-coated polyacrylic acid composite conductive particles

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preparation example Construction

[0035] See figure 1 , The preparation method of the graphene gradient coated polyacrylic acid composite conductive particles, including the following steps:

[0036] S110 dispersed the graphene powder prepared by the expanded insertion layer to the deionized water, then concentrated sulfuric acid and concentrated nitric acid were added, and after 6 to 10 hours of 50 ° C, the product was centrifuged and washed, resulting in carboxylated Graphene. Its main reaction equation is as follows:

[0037]

[0038]

[0039] Among them, the graphene powder prepared by the expanded cladding method is less than 1%, and the diameter of the sheet is between 100 nm to 10 μm. The concentration of the graphene powder prepared from the expanded hindered method was 1.2 to 5 mg / ml. The high quality concentration of concentrated sulfuric acid was 70%, and the mass concentration of concentrated nitric acid was 70%, the volume ratio of concentrated sulfuric acid and concentrated nitric acid was 3: ...

Embodiment 1

[0053] In the present embodiment, the preparation method of the polyacrylic acid composite conductive particles coated in graphene gradient is as follows:

[0054] 1. Weighing the expansion inserted graphene raw material 150mg, the percentage of the oxygen in the graphene powder is 0.5%, the diameter of the sheet is 3 to 5 μm, soluble in concentrated sulfuric acid and concentrated nitric acid, ultrasonic 1 hour, concentrate The volume ratio of sulfuric acid and concentrated nitric acid is 3: 1, and the volume of concentrated sulfuric acid and concentrated nitric acid is 40 ml.

[0055] 2. Place the ultrasonic dispersion in a three-neck flask, reflux reaction at a thermostatic magnetic stirrer, and the reaction temperature is 90 ° C, and the reaction time is 7 hours.

[0056] 3. Pour the reaction liquid into a large amount of deionized water to terminate the reaction, and then press the upper liquid, and the remaining mixed liquid is separated by vacuum filtration, and the filter f...

Embodiment 2

[0066] In the present embodiment, the preparation method of the polyacrylic acid composite conductive particles coated in graphene gradient is as follows:

[0067] 1. Weighing the expansion inserted graphene raw material 150mg, the percentage of the oxygen in the graphene powder is 0.5%, the diameter of the sheet is 3 to 5 μm, soluble in concentrated sulfuric acid and concentrated nitric acid, ultrasonic 1 hour, concentrate The volume ratio of sulfuric acid and concentrated nitric acid is 3: 1, and the volume of concentrated sulfuric acid and concentrated nitric acid is 40 ml.

[0068] 2. Place the ultrasonic dispersion in a three-neck flask, reflux reaction at a thermostatic magnetic stirrer, and the reaction temperature is 90 ° C, and the reaction time is 7 hours.

[0069] 3. Pour the reaction liquid into a large amount of deionized water to terminate the reaction, and then press the upper liquid, and the remaining mixed liquid is separated by vacuum filtration, and the filter f...

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Abstract

The invention relates to the technical field of the composite conductivity and in particular to a preparation method of graphene gradient-coated polyacrylic acid composite conducting particles. The preparation method comprises the following steps: enabling graphene powder prepared by an expansion intercalation method to be dispersed in mixed liquid of concentrated sulfuric acid and concentrated nitric acid, and performing an oil bath reaction, to obtain carboxylated graphene; enabling the carboxylated graphene to be dispersed in N,N-dimethylformamide, adding 1-ethyl-(3-dimethyl aminopropyl) carbodiimide hydrochloride, after ultrasonic dispersion, adding ethidene diamine into dispersing liquid, performing the oil bath reaction, to obtain amination graphene; enabling dry polyacrylic acid particles to be placed in water dispersing liquid of the amination graphene, under the action of an osmotic pressure and an electrostatic attraction force, coating the surface of the polyacrylic acid particles with graphene, and along a gap between molecular chains, diffusing to a particle core part; and then adjusting a pH value of the water dispersing liquid of the polyacrylic acid particles and the graphene to be 1-2, after drying in vacuum, to obtain the graphene gradient-coated polyacrylic acid composite conducting particles.

Description

Technical field [0001] The present invention relates to the field of composite conductive techniques, and more particularly to a method of preparing a graphene gradient coated polyacrylic acid composite conductive particles. Background technique [0002] The conductive filler mainly has metal fillers, carbon fillers, metal oxide fillers, composite filler, etc., composite conductive fillers, including metal plating powder and fibers. [0003] Common metal conductive filler has silver, copper, nickel, iron, etc., wherein the silver has the advantages of good conductivity and strong antioxidant capacity, but the price is expensive, and it is easy to generate electromigration in a wet heat environment, resulting in silver conductive glue. Electrical resistance is unstable; copper, nickel, iron and other antioxidant resistance, poor corrosion resistance, affecting its long-term use. The metal oxide-based filler is poor and the corrosion resistance is poor, and it is not suitable for l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/21C08L33/02C08K9/04C08K9/02C09C3/10C09C1/44C08K3/04
CPCC08J3/215C08J2333/02C08K9/02C08K9/04C08K9/08C08K2201/001C09C1/44C09C3/10C08K3/042
Inventor 曾尤郝亚斌张藤心方明赫英哲王函成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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