Method for reducing manganese content in graphene oxide

A technology of manganese content and graphene is applied in the field of reducing manganese content in graphene oxide, which can solve problems such as unfavorable graphene oxide purification, high equipment requirements, large water consumption, etc., and achieves low equipment requirements, uniform particle size distribution, Low water consumption

Active Publication Date: 2013-11-20
山东金利特新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For using potassium permanganate as an oxidant, the graphene oxide prepared by the graphite oxide method is easy to contain manganese ions, which is not conducive to the purification of graphene oxide. The prior art uses distilled water or concentrated acid repeated washing to achieve the purification of graphite oxide. However, there are disadvantages such as large water consumption, high requirements for equipment, and complicated operation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] ① Dissolve graphite in a mixed solution of concentrated sulfuric acid and concentrated phosphoric acid; add potassium permanganate to the above solution; react at 40°C for 10 hours, then add ice water of 2 times the volume of the mixed acid; stir the above solution to evenly cool to room temperature , Adding hydrogen peroxide solution 3 times the mass of graphite to reduce; washing the above solution with distilled water to PH=4~6, and filtering to obtain graphite oxide wet material.

[0016] ②Prepare 5% ammonium chloride aqueous solution;

[0017] ③Prepare 0.05 M ethylenediaminetetraacetic acid low concentration solution and 0.1 M ethylenediaminetetraacetic acid high concentration solution with 5% ammonium chloride aqueous solution;

[0018] ④ Dissolve 5g of the above wet graphite oxide filter cake in 1L 0.05 M ethylenediaminetetraacetic acid solution, stir for 30min, ultrasonically disperse for 90min, and filter;

[0019] ⑤The filter cake treated by ④ is dissolved in 1L 0.1M ...

Embodiment 2

[0021] ① Dissolve graphite in a mixed solution of concentrated sulfuric acid and concentrated phosphoric acid; add potassium permanganate to the above solution; react at 40°C for 10 hours, then add ice water of 2 times the volume of the mixed acid; stir the above solution to evenly cool to room temperature , Adding hydrogen peroxide solution 3 times the mass of graphite to reduce; washing the above solution with distilled water to PH=4~6, and filtering to obtain graphite oxide wet material.

[0022] ②Prepare 5% ammonium chloride aqueous solution;

[0023] ③Prepare 0.02 M ethylenediaminetetraacetic acid low concentration solution and 0.2 M ethylenediaminetetraacetic acid high concentration solution with 5% ammonium chloride aqueous solution;

[0024] ④ Dissolve 5g of the above wet graphite oxide filter cake in 1L 0.05 M ethylenediaminetetraacetic acid solution, stir for 30min, ultrasonically disperse for 90min, and filter;

[0025] ⑤The filter cake treated by ④ is dissolved in 1L 0.1M ...

Embodiment 3

[0027] ① Dissolve graphite in a mixed solution of concentrated sulfuric acid and concentrated phosphoric acid; add potassium permanganate to the above solution; react at 40°C for 10 hours, then add ice water of 2 times the volume of the mixed acid; stir the above solution to evenly cool to room temperature , Adding hydrogen peroxide solution 3 times the mass of graphite to reduce; washing the above solution with distilled water to PH=4~6, and filtering to obtain graphite oxide wet material.

[0028] ②Prepare 5% ammonium chloride aqueous solution;

[0029] ③Prepare 0.05 M ethylenediaminetetraacetic acid low concentration solution and 0.1 M ethylenediaminetetraacetic acid high concentration solution with 5% ammonium chloride aqueous solution;

[0030] ④ Dissolve 5g of the above wet graphite oxide filter cake in 1L 0.05 M ethylenediaminetetraacetic acid solution, stir for 30min, ultrasonically disperse for 60min, and filter;

[0031] ⑤The filter cake treated by ④ is dissolved in 1L 0.1M ...

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PUM

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Abstract

The invention relates to a method for reducing manganese content in graphene oxide. The method is characterized by comprising: dissolving graphite in a concentrated sulfuric acid and concentrated phosphoric acid mixed solution, adding potassium permanganate to the obtained solution, carrying out a reaction for 9-15 h at a temperature of 40-60 DEG C, adding ice water having a volume of 1-4 times the volume of the mixed acid, uniformly stirring the solution, cooling to achieve a room temperature, adding a hydrogen peroxide solution having a mass of 3-5 times the mass of the graphite to reduce, washing the obtained solution by using distilled water until the pH value is 4-6, and filtering to obtain the graphite oxide wet material. The method has the following beneficial effects that: the method has advantages of simple operation, low water consumption, uniform particle size distribution, no high equipment requirements, and the like, and the graphene oxide with characteristics of uniform particle size distribution and manganese content of less than 20 mug / g can be obtained.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a method for reducing the manganese content in graphene oxide. Background technique [0002] After graphene won the 2010 Nobel Prize in Physics, the research progress of graphene was accelerated. Graphene is not only the thinnest known material, but also very strong and hard. As a single substance, it can transfer electrons faster than known conductors at room temperature. Graphite oxide is a compound obtained by hydrolysis of graphite after oxidation by a strong oxidant , due to the functional groups such as hydroxyl, carboxyl, epoxy, etc., it is easy to disperse in water or organic solvents by ultrasonic treatment to form a graphene oxide dispersion, and it is easy to react with other chemical substances and be modified. It is used in supercapacitors, lithium-ion batteries, and adsorption Heavy metals and other aspects have a wide range of application prospects. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/198C01B32/23
Inventor 苏燕刘同浩渠凤丽侯士峰
Owner 山东金利特新材料有限责任公司
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