High-solubility multi-fold dry-state graphene oxide microsphere and preparation method thereof

A high-solubility, graphene microsphere technology, applied in the field of graphene materials, can solve problems that hinder industrialization and commercialization, affect the performance of graphene oxide, processability, and the existence of single-layer forms, and achieve good solubility.

Active Publication Date: 2016-05-04
ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the solubility of the dry graphene oxide obtained by the existing drying method is very poor, which is reflected in two aspects: one is that the dispersibility itself is not good, and it will precipitate in a short time; Layers exist
These two points seriously affect the performance and processability of graphene oxide itself, hindering its industrialization and commercialization
Patent 201010593157.1 "A Method for Preparing Graphene Powder" uses the method of spray drying first and then heat treatment to obtain graphene powder, which mentions that the graphene oxide powder obtained by spray drying can be uniformly dispersed in water, but it is not oxidized Whether graphene exists in the

Method used

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  • High-solubility multi-fold dry-state graphene oxide microsphere and preparation method thereof
  • High-solubility multi-fold dry-state graphene oxide microsphere and preparation method thereof
  • High-solubility multi-fold dry-state graphene oxide microsphere and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0030] (1) dilute the graphene oxide dispersion prepared by Hummers method with dimethylformamide; the mass ratio of dimethylformamide and graphene oxide dispersion is 50:1;

[0031] (2) The dispersion liquid after step (1) is diluted, obtains graphene oxide microsphere by the method for atomization drying, and drying temperature is 130 ℃;

[0032] Through the above steps, the obtained multi-fold dry graphene oxide microspheres have a diameter of 500 nm to 30 μm, such as figure 1 , 2 shown. Its density is 0.1g / cm 3 , the specific surface area is 1400m 2 / g, the carbon-oxygen ratio is 2.3. Its solubility in water and common organic solvents is 30mg / g, and graphene oxide exists in the form of a single layer in the obtained dispersion, and can be dispersed stably for a long time (such as image 3 , 4 shown). The obtained dry graphene oxide powder is compressed into a block using a press, such as Figure 5 As shown, its density is 1.26g / cm 3 , can still be well dispersed....

Embodiment 2

[0034] (1) dilute the graphene oxide dispersion prepared by the Hummers method with ethanol; the mass ratio of ethanol to the graphene oxide dispersion is 1:1;

[0035] (2) The dispersion liquid after step (1) is diluted, obtains graphene oxide microsphere by the method for atomization drying, and drying temperature is 150 ℃;

[0036] After the above steps, the obtained multi-fold dry graphene oxide microspheres have a diameter of 500nm-30μm and a density of 0.13g / cm 3 , the specific surface area is 800m 2 / g, the carbon-oxygen ratio is 2.6. Its solubility in water and common organic solvents is 20mg / g, and the graphene oxide in the obtained dispersion exists in the form of a single layer, and can be dispersed stably for a long time.

Embodiment 3

[0038] (1) dilute the graphene oxide dispersion prepared by the Hummers method with methanol; the mass ratio of methanol to the graphene oxide dispersion is 5:1;

[0039](2) The dispersion liquid after step (1) is diluted, obtains graphene oxide microsphere by the method for atomization drying, and drying temperature is 125 ℃;

[0040] After the above steps, the obtained multi-fold dry graphene oxide microspheres have a diameter of 500nm-30μm and a density of 0.09g / cm 3 , the specific surface area is 710m 2 / g, the carbon-oxygen ratio is 2.1. Its solubility in water and common organic solvents is 20mg / g, and the graphene oxide in the obtained dispersion exists in the form of a single layer, and can be dispersed stably for a long time.

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Abstract

The invention discloses a high-solubility multi-fold dry-state graphene oxide microsphere and a preparation method thereof. According to the dry-state graphene oxide microsphere, firstly graphene oxide dispersion liquid is prepared through an organic solvent dilution Hummers method, and then atomized drying is performed so that the dry-state graphene oxide microsphere can be obtained. The dry-state graphene oxide microsphere obtained through the preparation method is good in solubility, the solubility in water and common organic solvents is 20-30 mg/g, and the dry-state graphene oxide microsphere can be stably dispersed for a long time in the mode of a single-layer graphene oxide sheet; good solubility can still be kept after the dry-state graphene oxide microsphere is compressed into high-density blocks; the preparation method is simple, convenient and fast, low in energy consumption and suitable for large-scale industrial production. The problem that the solubility of graphene oxide obtained through an existing drying method is poor is solved, transportation, storage and use of the dry-state graphene oxide microsphere are facilitated because of high density, the dry-state graphene oxide microsphere can be used in the fields of graphene macroscopic assembly materials, functional graphene materials, graphene composite materials and the like.

Description

technical field [0001] The invention belongs to the field of graphene materials, and relates to a highly soluble multi-fold dry graphene oxide microsphere and a preparation method thereof. Background technique [0002] As a new type of two-dimensional carbon material, graphene has attracted more and more attention from the world. Due to its outstanding mechanical properties, electrical properties, thermal properties and unique electromagnetic properties, graphene has shown broad application prospects in many fields and has gradually moved towards practical applications. The preparation of graphene oxide by chemical oxidation is the most common route for large-scale preparation of graphene materials. Because of the rich carboxyl, hydroxyl, epoxy and other polar functional groups on the surface, graphene oxide can be dispersed in a single layer in many solvents, and can form a liquid crystal texture, which can be assembled into fibers, films, and aerogels. And other macrosco...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01P2004/03C01P2004/32C01P2004/61C01P2006/10
Inventor 高超陈琛孙海燕
Owner ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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