Preparation method of graphene oxide with small layer number and freeze-drying method of graphene oxide

A drying method and graphene technology, applied in the fields of graphene, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as unfavorable dispersion, easy agglomeration of graphite oxide into hard blocks, poor thermal stability of graphite oxide, etc., and achieve excellent dispersion performance, Small number of layers, good preservation of functional groups

Active Publication Date: 2019-03-08
SICHUAN JUCHUANG SHIMOXI TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Usually, due to the poor thermal stability of graphite oxide, pyrolysis often occurs during the drying process, and the graphite oxide after heating and drying is easy to agglomerate into hard blocks, which is not conducive to subsequent dispersion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] The graphene oxide with a layer number of 25 ± 2 is dispersed in secondary deionized water, and the dispersion effect is further strengthened by ultrasonic dispersion during the dispersion process to obtain a graphene oxide hydrogel. After testing, before dispersion, the specific surface area of ​​graphene oxide is 170m 2 / g; The solid content of graphene oxide hydrogel is 10wt%.

[0024] 1000 g of graphene oxide hydrone gel was loaded into a ceramic crucible. Use crawlers to transfer the ceramic crucible to the pre-freezing system, and then transfer it to the freeze-drying constant temperature area. After processing at -58±3°C and 1000±50Pa for 10 hours, use the crawler to transfer it to the discharge port.

[0025] After testing, the water content in the graphene oxide product is less than 0.01wt%, the dispersion is good, the number of layers is 5-7, and the specific surface area is 350m 2 / g.

example 2

[0027] Graphene oxide with a layer number of 30±2 was dispersed in distilled water by ultrasonic to obtain a graphene oxide hydrogel. After testing, before dispersion, the specific surface area of ​​graphene oxide is 150m 2 / g; The solid content of graphene oxide hydrogel is 10wt%.

[0028] 2000 g of graphene oxide hydrone gel was loaded into a ceramic crucible. Use crawlers to transport the ceramic crucible to the freeze-drying constant temperature area, and after 20 hours of treatment at -54±2°C and 300±10Pa, use the crawlers to transfer to the discharge port.

[0029] After testing, the water content in the graphene oxide product is less than 0.01wt%, the dispersion is good, the number of layers is 5-7, and the specific surface area is 375m 2 / g.

example 3

[0031] Graphene oxide with a layer number of 20 is dispersed in pure water by stirring and ultrasonic dispersion to obtain a graphene oxide hydrogel. After testing, before dispersion, the specific surface area of ​​graphene oxide is 200m 2 / g; The solid content of graphene oxide hydrogel is 5wt%.

[0032] Load the graphene oxide hydrogel into a ceramic crucible. Use crawlers to transport the ceramic crucible to the freeze-drying constant temperature area, and after 20 hours of treatment at -60±4°C and 80±10Pa, use crawlers to transfer to the discharge port.

[0033] After testing, the water content in the graphene oxide product is less than 0.01wt%, the dispersion is good, the number of layers is 5-7, and the specific surface area is 395m 2 / g.

[0034]In summary, the present invention can further "stretch" the graphene oxide sheet during the drying process, and at the same time, the graphene oxide material maintains a low entropy value at low temperature, which is benefici...

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Abstract

The invention provides a preparation method of graphene oxide with a small layer number and a freeze-drying method of the graphene oxide. The preparation method comprises the following steps: dispersing graphene oxide having a first layer number in water and forming graphene oxide hydrogel; placing the graphene oxide hydrogel at a first temperature and a first pressure intensity to coagulate watermolecules in the graphene oxide hydrogel into ice molecules, and sublimating the ice molecules, so as to obtain graphene oxide having a second layer number, wherein the first layer number ranges fromten to tens of layers, and the second layer number is less than the first layer number. The preparation method has the beneficial effects that the freeze-drying process does not destroy the structureof a graphite oxide sheet layer, and functional groups are better preserved; the freeze-dried graphite oxide is less prone to agglomeration; the interlamellar spacing of the freeze-dried graphite oxide sheet layer is greater than that of a graphene oxide product dried by a conventional drying method; the graphene oxide is more excellent in dispersion property and has a smaller layer number and alarger specific surface area.

Description

technical field [0001] The invention relates to the technical field of graphene oxide production, in particular to a preparation method of low-layer graphene oxide and a freeze-drying method of graphene oxide. Background technique [0002] Usually, due to the poor thermal stability of graphite oxide, pyrolysis often occurs during the drying process, and the graphite oxide after heating and drying tends to agglomerate into hard blocks, which is not conducive to subsequent dispersion. Contents of the invention [0003] The purpose of the present invention is to solve at least one of the above-mentioned deficiencies in the prior art. For example, one of the objects of the present invention is to provide a new method for drying graphene oxide. [0004] In order to achieve the above object, one aspect of the present invention provides a method for preparing graphene oxide with a low number of layers, the preparation method comprising the following steps: dispersing graphene ox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198
CPCC01B2204/04C01B2204/30C01B2204/32C01B32/198
Inventor 李星蔡雨婷刘长虹漆长席蒋虎南
Owner SICHUAN JUCHUANG SHIMOXI TECH CO LTD
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