CN104591159A - Preparation process of graphite oxide - Google Patents
Preparation process of graphite oxide Download PDFInfo
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- CN104591159A CN104591159A CN201310525297.9A CN201310525297A CN104591159A CN 104591159 A CN104591159 A CN 104591159A CN 201310525297 A CN201310525297 A CN 201310525297A CN 104591159 A CN104591159 A CN 104591159A
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- graphite oxide
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Abstract
The invention discloses a preparation process of graphite oxide. The process is as below: placing a raw material of flake graphite with concentration greater than 99% in concentrated H2SO4, adding NaNO3, adding KMnO4 in an ice-water bath, and continuously stirring to keep the temperature of the solution at less than 20 DEG C; placing the mixed solution in a water bath of 40 DEG C, stirring and reacting for 20 min; adding deionized water to the mixed solution, and stirring for 20 min; adding deionized water at 60 DEG C for dilution, then adding H2O2 solution with mass fraction of 30% to turn the mixture from brown to bright yellow, and filtering while hot; and cleaning and filtering by using HCl with mass fraction of 5%, and finally drying the filter cake in a vacuum drying box at 60 DEG C for 24 h. The process has the advantages of simple method, convenient operation, short production period and easiness to control, and the produced graphite oxide has good performance.
Description
Technical field
The invention belongs to graphite technology field, be specifically related to a kind of graphite oxide preparation technology.
Background technology
Graphite material has the characteristics such as hot strength is high, conduction good thermal conduction, heat-shock resistance, corrosion-resistant, self-lubricating, become electro-conductive material important on contemporary industry and structured material, graphite oxide is considered to the most excellent persursor material of macroscopic preparation of graphene, can by preparing Graphene through chemical reduction again by after ultrasonic for graphite oxide stripping.Prior art, produce graphite oxide, need repeated oxidation, the production cycle is longer.
Summary of the invention
In order to overcome the above-mentioned technical problem that prior art field exists, the object of the invention is to, provide a kind of graphite oxide preparation technology, technique is simple, and production efficiency is high.
Graphite oxide preparation technology provided by the invention, comprise the following steps: (1) is got concentration and is greater than the crystalline flake graphite of 99% as starting material, be placed in dense H2SO4, and add NaNO3, KMnO4 is added in ice-water bath, continuous stirring, makes the temperature of solution be no more than 20 DEG C, and the proportioning of described graphite, H2SO4, NaNO3, KMnO4 is 1:20:0.5:3; (2) mixing solutions is placed in the water-bath of 40 DEG C, stirring reaction 20 min; (3) add deionized water in mixing solutions, continue stirring 20 min; (4) adding temperature is after the deionized water dilution of 60 DEG C, then adds the H2O2 solution that massfraction is 30%, and mixture is glassy yellow by brown stain, filtered while hot; (5) and then with massfraction be the HCl cleaning and filtering of 5%, finally filter cake be placed in dry 24 h of vacuum drying oven of 60 DEG C.
Graphite oxide preparation technology provided by the invention, its beneficial effect is, method is simple, easy to operate, with short production cycle and be easy to control, and the graphite oxide produced has good performance.
Embodiment
Below in conjunction with an embodiment, graphite oxide preparation technology provided by the invention is described in detail.
Embodiment
The graphite oxide preparation technology of the present embodiment, comprise the following steps: (1) is got concentration and is greater than the crystalline flake graphite of 99% as starting material, be placed in dense H2SO4, and add NaNO3, KMnO4 is added in ice-water bath, continuous stirring, makes the temperature of solution be no more than 20 DEG C, and the proportioning of described graphite, H2SO4, NaNO3, KMnO4 is 1:20:0.5:3; (2) mixing solutions is placed in the water-bath of 40 DEG C, stirring reaction 20 min; (3) add deionized water in mixing solutions, continue stirring 20 min; (4) adding temperature is after the deionized water dilution of 60 DEG C, then adds the H2O2 solution that massfraction is 30%, and mixture is glassy yellow by brown stain, filtered while hot; (5) and then with massfraction be the HCl cleaning and filtering of 5%, finally filter cake be placed in dry 24 h of vacuum drying oven of 60 DEG C.
Claims (1)
1. a graphite oxide preparation technology, it is characterized in that: comprise the following steps: (1) is got concentration and is greater than the crystalline flake graphite of 99% as starting material, be placed in dense H2SO4, and add NaNO3, KMnO4 is added in ice-water bath, continuous stirring, makes the temperature of solution be no more than 20 DEG C, and the proportioning of described graphite, H2SO4, NaNO3, KMnO4 is 1:20:0.5:3; (2) mixing solutions is placed in the water-bath of 40 DEG C, stirring reaction 20 min; (3) add deionized water in mixing solutions, continue stirring 20 min; (4) adding temperature is after the deionized water dilution of 60 DEG C, then adds the H2O2 solution that massfraction is 30%, and mixture is glassy yellow by brown stain, filtered while hot; (5) and then with massfraction be the HCl cleaning and filtering of 5%, finally filter cake be placed in dry 24 h of vacuum drying oven of 60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525297.9A CN104591159A (en) | 2013-10-31 | 2013-10-31 | Preparation process of graphite oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525297.9A CN104591159A (en) | 2013-10-31 | 2013-10-31 | Preparation process of graphite oxide |
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| CN104591159A true CN104591159A (en) | 2015-05-06 |
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| CN201310525297.9A Pending CN104591159A (en) | 2013-10-31 | 2013-10-31 | Preparation process of graphite oxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105097298A (en) * | 2015-05-27 | 2015-11-25 | 北京交通大学 | Method for preparing graphene hydrogel electrode by graphene oxide solution |
| CN106744892A (en) * | 2016-12-17 | 2017-05-31 | 山东金城石墨烯科技有限公司 | A kind of preparation method of nitration Graphene |
| CN113587061A (en) * | 2021-07-12 | 2021-11-02 | 泰兴挚富显示技术有限公司 | High-thermal-conductivity composite graphite radiating fin and preparation method thereof |
-
2013
- 2013-10-31 CN CN201310525297.9A patent/CN104591159A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105097298A (en) * | 2015-05-27 | 2015-11-25 | 北京交通大学 | Method for preparing graphene hydrogel electrode by graphene oxide solution |
| CN106744892A (en) * | 2016-12-17 | 2017-05-31 | 山东金城石墨烯科技有限公司 | A kind of preparation method of nitration Graphene |
| CN113587061A (en) * | 2021-07-12 | 2021-11-02 | 泰兴挚富显示技术有限公司 | High-thermal-conductivity composite graphite radiating fin and preparation method thereof |
| CN113587061B (en) * | 2021-07-12 | 2023-09-08 | 泰兴挚富显示技术有限公司 | High-heat-conductivity composite graphite radiating fin and preparation method thereof |
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Application publication date: 20150506 |