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Method for preparing graphene organic dispersion solution from hyperbranched polyethylene

A hyperbranched polyethylene and graphene dispersion technology, applied in the direction of graphene, nano-carbon, etc., can solve the problems of weak dispersion and stability, decreased performance of graphene, low concentration of graphene, etc., and achieve less destructive surface structure , low concentration of surface defects, and mild polymerization conditions

Active Publication Date: 2015-04-22
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, using this method to prepare graphene has the following disadvantages: firstly, the concentration of graphene obtained is low; secondly, the surfactant is difficult to completely remove, resulting in a decrease in the performance of graphene obtained; in addition, this method is only suitable for graphene in aqueous media. Dispersion in , but unable to obtain graphene organic dispersion
In most organic solvents, the above-mentioned polymers have very weak ability to disperse and stabilize graphene. For example, in tetrahydrofuran (THF), the concentration of graphene dispersion obtained from the above-mentioned polymers is generally only 6-22 mg / L. Obviously, Difficult to meet the needs of practical applications

Method used

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  • Method for preparing graphene organic dispersion solution from hyperbranched polyethylene
  • Method for preparing graphene organic dispersion solution from hyperbranched polyethylene
  • Method for preparing graphene organic dispersion solution from hyperbranched polyethylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1, comparative example 1~2

[0049] 1. Sample preparation

[0050] (1) The preparation of the sample of Example 1 is carried out according to the following steps:

[0051] Step 1: Under the protection of ethylene, inject 100 mL of anhydrous dichloromethane into a 250 mL Schlenk reaction flask, stir for 30 min to keep the temperature at 35 ° C; then add acetonitrile-based Pd-diimine catalyst A (0.2 g, dissolved in 10 mL of anhydrous dichloromethane in advance, with a concentration of 1.82 g / L based on the total reaction volume) under the protection of ethylene. At a constant polymerization temperature (35 ° C) Stir the above solution under ethylene pressure (1 atm) to continue the polymerization for 24 h, immediately add 0.5 mL triethylsilane (0.005 times the total volume of the polymerization reaction) to the product and stir for 1 h to terminate the polymerization. The obtained polymeric product was purified as follows: firstly, the solvent was removed by...

Embodiment 2、 comparative example 2~3

[0068] 1. Sample preparation

[0069] (1) The preparation of the sample of Example 2 is carried out according to the following steps:

[0070] The 1st step: the synthesis technique of HBPE is the same as the 1st step in the embodiment 1.

[0071] Step 2: Add 500 mesh natural phosphorus flake graphite powder, chloroform and HBPE synthesized by the above step 1 into a 140 mL cylindrical glass bottle in sequence, and control the initial feeding ratio of each raw material as follows: The total volume of solvent is 100 mL, the initial concentration of graphite powder was 2 mg / mL, and the initial mass ratio of polymer / graphite powder was 2; ° C was continuously ultrasonicated for 48 h at constant temperature to obtain the initial dispersion of graphene. It was further centrifuged at a low speed (room temperature, 4000 rpm, 45 min), and after standing for 8 h, the centrifuged supernatant was collected, and finally a graphene dispersion containing excess HBPE was obtained.

[0072]...

Embodiment 3、 comparative example 2

[0086] 1. Sample preparation

[0087] (1) The preparation of the sample of Example 3 is carried out according to the following steps:

[0088] The 1st step: the synthesis of HBPE is with the 1st step in embodiment 1;

[0089] Step 2: Add 500-mesh natural phosphorus flake graphite powder, THF and HBPE synthesized by the above-mentioned step 1 into a glass container of 250 mL in order, and control the initial feeding ratio of each raw material as follows: the total volume of solvent is 150 mL, graphite The initial concentration of powder was 3 mg / mL, and the initial mass ratio of polymer / graphite powder was 2; ° C was continuously ultrasonicated for 112 h at a constant temperature to obtain the initial dispersion of graphene. It was further centrifuged at a low speed (room temperature, 4000 rpm, 45 min), and after standing for 8 h, the centrifuged supernatant was collected, and finally a graphene dispersion containing excess HBPE was obtained.

[0090] Step 3: Ultra-high-spee...

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Abstract

The invention discloses a method for preparing a graphene organic dispersion solution from hyperbranched polyethylene, which comprises the following steps: (1) proportionally mixing graphite powder, organic solvent B and hyperbranched polyethylene, and then performing ultrasonic dispersion on the obtained mixture to obtain a graphene initial dispersion solution C; and further performing low-speed centrifugation and standing treatment to obtain a graphene dispersion solution D containing excessive hyperbranched polyethylene, wherein the organic solvent B is selected from one of the following chemically pure or analytically pure agents: tetrahydrofuran, trichloromethane, n-heptane, chlorobenzene and dichloromethane; and (2) performing ultra-high-speed centrifugation or vacuum filtration on the graphene dispersion solution D obtained in the steps (1) to remove the contained excessive hyperbranched polyethylene, and further performing ultrasonic dispersion in the organic solvent B to obtain the graphene organic dispersion solution. The preparation process causes less damage to the surface structure of graphene; and the obtained graphene is low in surface defect concentration and can better take the performance advantages.

Description

technical field [0001] The invention relates to a graphene preparation technology, in particular to a method for preparing graphene organic dispersion liquid by utilizing hyperbranched polyethylene. Background technique [0002] Graphene consists of a single sp 2 Composed of hybridized carbon atoms, its thickness is only a single atom thick, and it is a regular two-dimensional grid-like carbon nanomaterial (see attached figure 1 ). This unique structure of graphene makes it have extremely excellent mechanical strength, electrical conductivity and thermal conductivity, so it has broad and important application prospects in many fields such as electronics, biology, energy and high-performance polymer nanocomposites. Since it was first reported in 2004, the preparation and application research of graphene has attracted widespread attention in various fields. [0003] Obtaining a high-concentration and stable graphene dispersion in a specific solvent is the first prerequisite...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/09C08L23/06C08K3/04C08F110/02C08F2/38C08F4/70C01B31/04C01B32/19
Inventor 徐立新钟明强
Owner ZHEJIANG UNIV OF TECH
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