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Preparation method of fragment-free super-large graphene oxide sheet

A technology of ultra-large flakes and fossils, applied in the field of nanomaterials, to achieve the effect of simple preparation process, low pollution, safe and controllable preparation process

Active Publication Date: 2016-06-22
ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the deficiencies in the prior art, to provide a kind of easy preparation method of non-fragmented ultra-large graphene oxide, the area of ​​the graphene oxide sheet prepared by the method is large and free of fragments; the process is simple to operate, fast, And alleviate the pollution problem to a certain extent

Method used

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  • Preparation method of fragment-free super-large graphene oxide sheet
  • Preparation method of fragment-free super-large graphene oxide sheet
  • Preparation method of fragment-free super-large graphene oxide sheet

Examples

Experimental program
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Effect test

Embodiment 1

[0023] at -10 o Slowly add potassium permanganate into the rapidly stirring concentrated sulfuric acid at C, add graphite after fully dissolving, stir slowly at 60 rpm for 2 hours, then stop stirring, o C, 50 o Respectively react 6h under C, obtain the graphite oxide crystal of broad distribution respectively; figure 1 As shown, there are more fragments in the graphite oxide wafers obtained at two temperatures, which makes the corresponding graphene oxide also have a lot of fragments ( figure 2 ).

[0024] Dilute the reaction solution obtained in step 1 with concentrated sulfuric acid (the dilution factor can be any number of times, and the dilution rate is about 10 times in this example), and filter the graphite oxide crystals through a titanium alloy mesh screen with a pore size of 150um (140 mesh) (reaction solution Recovery), and slowly poured into rapidly stirred ice water 10 times the volume of the filtered product, let it stand for 2h, and slowly added H 2 o 2 , t...

Embodiment 2

[0027] at -10 o Slowly add potassium permanganate into the rapidly stirring concentrated sulfuric acid at 0°C. After fully dissolving, add graphite, stir slowly at 60 rpm for 2 hours, then stop stirring. o C, ) to react for 48 hours to obtain a reaction solution; dilute the reaction solution with concentrated sulfuric acid with a mass fraction of more than 98% and dilute sulfuric acid with a mass fraction of 10%, and then filter the graphite oxide crystals with a titanium alloy mesh screen with a pore size of 150um out (reaction liquid recovery), and slowly poured into rapidly stirred ice water 10 times the volume of the filtered product, let it stand for 2 hours, and slowly added H 2 o 2 , to remove excess potassium permanganate in the reaction, add an appropriate amount of hydrochloric acid until the flocculent graphite oxide disappears, and then filter out the graphite oxide wafers with a titanium alloy mesh sieve; slowly shake and wash the shaker to obtain the reaction pr...

Embodiment 3

[0030] at -10 o Slowly add potassium permanganate into the rapidly stirring concentrated sulfuric acid at C, add graphite after fully dissolving, stir slowly at 60 rev / min for 2 hours, then stop the stirring, at low temperature (20 o C) React for 28 hours to obtain broad-distributed graphite oxide crystals; dilute the reaction solution with concentrated sulfuric acid and filter the graphite oxide crystals with a 150um pore size titanium alloy mesh screen (recovery of the reaction solution), and slowly pour them into rapidly stirred relative Put the filtered product in 5 times volume, 8 times volume, and 10 times volume of ice water, let it stand for 2 hours, and slowly add H 2 o 2 , to remove the excess potassium permanganate in the reaction, add an appropriate amount of hydrochloric acid until the flocculent graphite oxide disappears, and then filter out the graphite oxide wafers with a titanium alloy mesh screen; slowly shake and wash the shaker to obtain the reaction produ...

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Abstract

The invention discloses a preparation method of a super-large fragment-free graphene oxide sheet. According to the method, before a graphite oxide crystal is washed by water, a fragment is separated out by adopting a mesh screen separation method. The graphite oxide crystal is diluted by adopting ice water of above 10 times of volume, so that a wafer of the graphite oxide crystal cannot be destroyed due to the solution heat of sulfuric acid. The wafer is further shocked and washed by adopting a shaking table, so that a graphene oxide sheet layer is prevented from being broken by mechanical force when being stripped. The preparation method of the super-large fragment-free graphene oxide sheet is simple, safe and controllable in preparation process and little in time consumption and energy consumption; the fragment-free super-large graphene oxide sheet is obtained by one step through simple separation operation before a product.

Description

technical field [0001] The invention relates to the field of nanomaterials, in particular to a method for preparing a fragment-free super large sheet of graphene oxide. Background technique [0002] In 2004, the research group of Professor A.K. Geim of the University of Manchester successfully prepared graphene by mechanical exfoliation, overturning the conclusion that the perfect two-dimensional crystal structure cannot exist stably at non-absolute zero. Then graphene's excellent mechanical properties, electrical properties, thermal properties, and optical properties were discovered one after another. Graphene has a large theoretical specific surface area, coupled with the excellent performance of the monolithic structure, carbon-based materials with graphene as the source material have been greatly developed and applied. The preparation of graphene by oxidation-reduction method is considered to be the most important method to realize the industrial production of graphene....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01B2204/32C01P2004/62
Inventor 高超彭蠡孙海燕杨清
Owner ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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