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A method for preparing graphene powder and its dispersion by utilizing fluorine-containing hyperbranched polyethylene copolymer

A technology of hyperbranched polyethylene and graphene dispersion, applied in graphene, chemical instruments and methods, carbon compounds, etc., can solve the problems of poor product quality, low preparation efficiency, poor stability of modified structure, etc.

Active Publication Date: 2020-08-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the covalent method mainly uses reactive groups such as carboxyl, hydroxyl, and epoxy groups contained on the surface of graphene oxide, and through the ideas of "grafting from", "grafting to" or "coupling reaction", the required Functional small molecules or polymers are covalently grafted on the surface of graphene, which can effectively improve the dispersion performance and interfacial interaction of graphene in the polymer matrix; the surface modification structure obtained by this method is relatively stable, but the modification process easily leads to graphene structure. Destroyed, and the modification process is more complicated
The non-covalent idea mainly uses non-covalent interactions such as π-π stacking, hydrogen bonding, static electricity, charge transfer, and lipophilicity between various functional small molecules or polymers and the surface of graphene to make them non-covalently adsorbed on graphite. ene surface, thereby improving the dispersion performance and interfacial interaction of graphene in the polymer matrix; the modification process of this method is conducive to maintaining the integrity of the graphene structure, but the stability of the modified structure is poor
[0007] In a word, although the preparation and surface modification of graphene have made great progress so far, there are still deficiencies such as low preparation efficiency, poor product quality, and complicated process.

Method used

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  • A method for preparing graphene powder and its dispersion by utilizing fluorine-containing hyperbranched polyethylene copolymer
  • A method for preparing graphene powder and its dispersion by utilizing fluorine-containing hyperbranched polyethylene copolymer
  • A method for preparing graphene powder and its dispersion by utilizing fluorine-containing hyperbranched polyethylene copolymer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Embodiment 1, comparative example 1

[0071] 1. Sample preparation

[0072] (1) The preparation of embodiment 1 sample is carried out as follows:

[0073] Step 1: Under the protection of ethylene, 2.12g of bromine-containing monomer BIEA (feeding concentration is 0.4mol / L), 0.2g of acetonitrile-based α-diimine palladium catalyst 1 (feeding concentration is 12.0mmol / L) and 20mL Anhydrous grade dichloromethane was added to a 50 mL dry Schlenk bottle, and the polymerization was continued for 24 h with stirring at a constant temperature of 25 °C and a stable ethylene pressure of 0.1 MPa. After the end of the polymerization, the ethylene gas source was turned off, and the solvent and residual ethylene gas were removed by blowing cold wind at room temperature to obtain the initial polymerization product. Further dissolve it in 10 mL of tetrahydrofuran, add a small amount of hydrochloric acid and hydrogen peroxide (3-5 drops each), stir for 3 h to dissolve the palladium part...

Embodiment 2

[0083] Embodiment 2, comparative example 2

[0084] 1. Sample preparation

[0085] (1) The preparation of embodiment 2 sample is carried out as follows:

[0086] Step 1: Same as Step 1 of Example 1.

[0087] Step 2: Same as Step 2 of Example 1.

[0088] Step 3: Same as Step 3 of Example 1, except that the solvent was changed from chloroform to tetrahydrofuran.

[0089] (2) The preparation of comparative example 2 sample is carried out as follows:

[0090] Step 1: Same as Step 1 of Comparative Example 1.

[0091] Step 2: Same as Step 2 of Comparative Example 1.

[0092] Step 3: Same as step 3 of Comparative Example 1, except that the solvent is changed from toluene to n-heptane.

[0093] 2. Comparison and analysis of test results

[0094] In Example 2 and Comparative Example 2, the fluorine-containing hyperbranched polyethylene copolymer is synthesized by the same steps, and each process parameter is also consistent (see steps 1 and 2 of the two), and both liquid phase e...

Embodiment 3

[0096] Embodiment 3, comparative example 3

[0097] 1. Sample preparation

[0098] (1) The preparation of embodiment 3 sample is carried out as follows:

[0099] Step 1: Same as Step 1 in Example 1.

[0100] Step 2: Same as step 2 in Example 1, except that the polymerization time is changed from 24h to 12h.

[0101] The 3rd step: with embodiment 1 step 3.

[0102] (2) The preparation of comparative example 3 sample is carried out as follows:

[0103] Step 1: Add natural phosphorus flake graphite powder with an average particle size of about 500 mesh and analytically pure chloroform into a test tube with a capacity of 25 mL (wherein the feeding concentration of graphite powder is 2.0 g / L, fluorine-containing hyperbranched polyethylene copolymer The mass ratio to graphite powder is 0), sealed and placed in a 250W ultrasonic cell at room temperature for 48 hours of continuous ultrasonication; the resulting product was centrifuged at 4000rpm at a low speed for 45min to remove ...

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Abstract

The invention discloses a method for preparing graphene powder and dispersion thereof from fluorine-containing hyperbranched polyethylene copolymers. The method includes catalyzing bromine-containingmonomers and ethylene by the aid of alpha-diimine palladium catalysts to carry out copolymerization so as to obtain bromine-containing hyperbranched polyethylene copolymers; initiating fluorine-containing monomers by the aid of the obtained bromine-containing hyperbranched polyethylene copolymers to carry out copolymerization at terminals of hyperbranched polyethylene branch chains so as to obtainthe fluorine-containing hyperbranched polyethylene copolymers; exfoliating graphite powder in organic solvents by means of ultrasonic or high-speed stirring by the aid of the obtained fluorine-containing hyperbranched polyethylene copolymers which are used as stabilizers so as to obtain graphene dispersion; removing free polymers in the graphene dispersion by means of vacuum suction filtration orcentrifugation to obtain the graphene powder with the surfaces modified by fluorine-containing polymers and ultrasonically dispersing the graphene powder in appropriate organic solvents to obtain graphene dispersion with surfaces modified by the fluorine-containing polymers. The method has the advantages that the method is high in preparation efficiency, graphene has few structure defects, and processes are simple and are easy to scale up; the graphene obtained by the aid of the method has a broad application prospect in the field of fluorine-containing polymer composite modification.

Description

technical field [0001] The invention relates to a method for preparing graphene powder and its dispersion liquid by utilizing fluorine-containing hyperbranched polyethylene copolymer. Background technique [0002] As a two-dimensional carbon nanomaterial, graphene consists of a single sp 2 Made of hybridized carbon atoms, it is only one atom thick. This unique structure makes it have a high specific surface area, as well as excellent electrical, thermal, mechanical and optical properties. With its unique structure and the above-mentioned excellent properties, it is expected to significantly improve the mechanical and heat resistance properties of the latter by using it to modify the polymer matrix, and at the same time make it obtain excellent electrical conduction, heat conduction, energy storage, electromagnetic Functions such as shielding and gas barrier are effective ways to achieve high performance and functionalization of polymer materials. Therefore, graphene has i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19C01B32/194C08F255/02C08F220/24C08F210/02C08F220/28
CPCC01B32/19C01B32/194C08F210/02C08F255/02C08F220/24C08F220/282
Inventor 徐立新徐春锋叶会见
Owner ZHEJIANG UNIV OF TECH
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