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Separating and impurity-removing method for graphene oxide

A graphene and graphite technology, applied in the field of graphene oxide preparation, can solve the problems of low efficiency, high energy consumption and high cost of graphene oxide, and achieve the effects of reducing time, improving economic benefits and reducing usage

Inactive Publication Date: 2016-10-12
SANDA FILM SCI & TECH XIAMEN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, large-scale preparation of graphene oxide by centrifugation faces problems such as low efficiency, low output, high cost, and high energy consumption.

Method used

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  • Separating and impurity-removing method for graphene oxide
  • Separating and impurity-removing method for graphene oxide
  • Separating and impurity-removing method for graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Preparation of graphene oxide: dry 6g graphite powder at 60°C for 12h; cool 720ml concentrated sulfuric acid and 80ml phosphoric acid to below 5°C, then stir and mix magnetically while dissipating heat; add 6g of dried graphite powder to sulfuric acid / Phosphoric acid mixed acid, stir; slowly add 36g potassium permanganate powder (when adding potassium permanganate must be slow to avoid explosion); after adding potassium permanganate, raise the temperature of the reaction vessel to 60℃, Open the mouth and react for 12 hours. After the reaction is over, cool to room temperature naturally; pour the cooled reaction solution into a container of 800ml solution (containing 10ml, 30% hydrogen peroxide) frozen in advance, and rinse the reaction vessel with the same proportion of dilute hydrogen peroxide solution On the surface, add dilute hydrogen peroxide solution to the container and stir continuously until the solution turns bright yellow, which is the graphite oxide reacti...

Embodiment 2

[0030] 1) Preparation of graphene oxide: Add 15g of sodium nitrate to a container containing 675ml of concentrated sulfuric acid, dissolve the solid under magnetic stirring, then weigh 20g of graphite powder into the above mixed solution, stir evenly, in an ice bath Then slowly add 90 g of potassium permanganate to control the reaction temperature not to exceed 10°C. The reactant was stirred under ice bath conditions for 2 hours and at room temperature for 5 days. After the reaction was completed, 2000 ml of 5 wt% sulfuric acid solution was added for dilution and stirred at room temperature for 2 hours. Then add 60ml of dilute hydrogen peroxide to obtain a yellow reaction solution, and stir for 2 hours at room temperature to obtain a graphite oxide reaction solution;

[0031] 2) With reference to the method of Example 1, the graphite oxide reaction solution is vacuum filtered with a 0.3μm pore size silica ceramic flat membrane to obtain a solid mud cake-like filter cake and filtr...

Embodiment 3

[0035] 1) Preparation of graphene oxide: fully cool the vessel, graphite, potassium permanganate, and concentrated sulfuric acid of the hydrothermal synthesis reactor to 2°C, place the reactor vessel in a stainless steel shell, and add 2.5g graphite and 12.5g After potassium permanganate pour 125ml of concentrated sulfuric acid, quickly cover the reaction kettle and screw it tightly, let the reaction kettle stand at 2℃ for 1.5 hours, take out the reaction kettle and tighten the reaction kettle again and place it in a 100℃ oven for 1.5 hours, take it out After the reaction kettle is naturally cooled, open it, pour the product into 300ml pure water and dilute it, add hydrogen peroxide until the solution turns yellow, which is the graphite oxide reaction liquid;

[0036] 2) With reference to the method of Example 1, the graphite oxide reaction solution was vacuum filtered with an alumina ceramic flat membrane with a pore size of 0.05 μm to obtain a solid mud cake-like filter cake and...

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Abstract

The invention discloses a separating and impurity-removing method for graphene oxide. Vacuum filtration, cross flow filtration and a ceramic membrane are combined, rapid recycling of waste high acid of graphite oxide reaction liquid and efficient and low-cost removing of metal ion impurities in a graphite oxide solution are achieved, discharging of waste acid wastewater is reduced, the efficiency of preparing high-purity graphene oxide products is improved, and the separating and impurity-removing method is suitable for preparing small-scale high-purity graphene oxide products of scientific-research units and university laboratories, and is also suitable for preparing graphene oxide and grapheme products in an industrialization and large-scale mode.

Description

Technical field [0001] The invention belongs to the field of graphene oxide preparation, and specifically relates to a method for separating and removing impurities from graphene oxide. Background technique [0002] In 2004, scientists Geim and Novoselov of the University of Manchester in the United Kingdom used the method of repeated sticking of tape and discovered the two-dimensional carbon atom crystal-graphene. Since then, the scientific community has developed a research on graphene and graphene oxide for more than ten years. An enthusiastic research boom. The discovery of graphene has not only enriched the family of nano-carbon materials, but also formed a complete system from zero-dimensional fullerenes, to one-dimensional carbon nanotubes, to two-dimensional graphene and then to three-dimensional diamonds. Its unique nanostructure and Excellent mechanical, thermal, electrical and optical properties make the development and research of graphene materials another internati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01P2002/72C01P2002/85C01P2004/03C01P2004/04
Inventor 高克洪昱斌陈云强蓝伟光
Owner SANDA FILM SCI & TECH XIAMEN
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