CN103407995A - Graphite oxide preparation method - Google Patents
Graphite oxide preparation method Download PDFInfo
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- CN103407995A CN103407995A CN2013102994106A CN201310299410A CN103407995A CN 103407995 A CN103407995 A CN 103407995A CN 2013102994106 A CN2013102994106 A CN 2013102994106A CN 201310299410 A CN201310299410 A CN 201310299410A CN 103407995 A CN103407995 A CN 103407995A
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Abstract
The invention relates to a graphite oxide preparation method, which comprises the following steps: setting a reaction container at a temperature of 3 DEG C, adding 150-250 g of concentrated sulfuric acid to the reaction container, and uniformly stirring; adding 5-8 g of graphite flakes to the reaction container, adding 6-8 g of magnesium nitrate, adding 5-10 g of potassium dichromate, and uniformly stirring; setting the reaction container at a temperature of 20 DEG C, wherein a reaction time is 40-70 min; setting a temperature to 60 DEG C, adding 250-350 g of purified water, and adding 8-18 g of sodium hypochlorite, wherein a reaction time is 50-70 min; after completing the reaction, centrifugating the reactant, wherein a centrifugation rotation speed is 8000 rpm, and a time is 15-25 min; and washing the precipitate three times with purified water to obtain the graphite oxide. The prepared graphite oxide has a high carbon-oxygen ratio.
Description
Technical field
The present invention relates to a kind of method for preparing graphite oxide, particularly relate to a kind of method for preparing the graphite oxide with high carbon-oxygen ratio.
Background technology
Graphene, in preparation process, has a variety of methods at present.Wherein for example chemical reduction method can be used graphite oxide, and the quality of graphite oxide quality is directly connected to the Graphene quality prepared.As incomplete as some graphite oxide oxidising processs, cause carbon-to-oxygen ratio too low, can affect preparation process and the preparation result of Graphene.Traditional method for preparing graphite oxide has a variety of, but the carbon-to-oxygen ratio of the graphite oxide prepared is too low, has limited the preparation method's of relevant Graphene development.
Summary of the invention
The technical problem solved: the lower problem of graphite oxide carbon-to-oxygen ratio that the preparation method of conventional graphite oxide obtains.
Technical scheme: a kind of preparation method of graphite oxide is characterized in that comprising the following steps: (1) is set as 3 ℃ by reaction vessel, adds vitriol oil 150g～250g in container, stirs; (2) in reaction vessel, add graphite scale 5～8g, then add magnesium nitrate 6～8g, then add potassium bichromate 5～10g, uniform stirring; (3) by the reaction vessel Temperature Setting, be 20 ℃, the reaction times is 40min～70min; (4) by Temperature Setting, be 60 ℃, adding pure water is 250g～350g, then to add clorox 8～18g, reaction times be 50min～70min.(5) after reflection finished, reactant is centrifugal, and centrifugal rotational speed was 8000rpm, and the time is 15～25min; (6) will precipitate with pure water washing three times, can obtain graphite oxide.
Wherein the weight of the vitriol oil is preferably 180g, and the weight of magnesium nitrate is preferably 7g, and the weight of potassium bichromate is preferably 8g.
Beneficial effect: the graphite oxide prepared has higher carbon-to-oxygen ratio.
Embodiment
Embodiment 1
Reaction vessel is set as to 3 ℃, adds vitriol oil 150g in container, stir; In reaction vessel, add graphite scale 5g, then add magnesium nitrate 8g, then add potassium bichromate 10g, uniform stirring; By the reaction vessel Temperature Setting, be 20 ℃, the reaction times is 40min; By Temperature Setting, be 60 ℃, adding pure water is 350g, then to add clorox 18g, reaction times be 70min.After reflection finished, reactant is centrifugal, and centrifugal rotational speed was 8000rpm, and the time is 15min; To precipitate with pure water washing three times, can obtain graphite oxide.By the xps analytical procedure, measure the carbon-to-oxygen ratio of graphite oxide, measurement result is 2.83.
Embodiment 2
Reaction vessel is set as to 3 ℃, adds vitriol oil 250g in container, stir; In reaction vessel, add graphite scale 6g, then add magnesium nitrate 6g, then add potassium bichromate 8g, uniform stirring; By the reaction vessel Temperature Setting, be 20 ℃, the reaction times is 60min; By Temperature Setting, be 60 ℃, adding pure water is 250g, then to add clorox 8g, reaction times be 50min.After reflection finished, reactant is centrifugal, and centrifugal rotational speed was 8000rpm, and the time is 20min; To precipitate with pure water washing three times, can obtain graphite oxide.By the xps analytical procedure, measure the carbon-to-oxygen ratio of graphite oxide, measurement result is 2.76.
Embodiment 3
Reaction vessel is set as to 3 ℃, adds vitriol oil 180g in container, stir; In reaction vessel, add graphite scale 8g, then add magnesium nitrate 7g, then add potassium bichromate 5g, uniform stirring; By the reaction vessel Temperature Setting, be 20 ℃, the reaction times is 70min; By Temperature Setting, be 60 ℃, adding pure water is 300g, then to add clorox 14g, reaction times be 60min.After reflection finished, reactant is centrifugal, and centrifugal rotational speed was 8000rpm, and the time is 25min; To precipitate with pure water washing three times, can obtain graphite oxide.By the xps analytical procedure, measure the carbon-to-oxygen ratio of graphite oxide, measurement result is 2.78.
From above three embodiment, finding out, the graphite oxide prepared has possessed higher carbon-to-oxygen ratio, and degree of oxidation is very high, can expand the raw material sources of Graphene.
Claims (4)
1. the preparation method of a graphite oxide, it is characterized in that comprising the following steps: (1) is set as 3 ℃ by reaction vessel, adds vitriol oil 150g～250g in container, stirs; (2) in reaction vessel, add graphite scale 5～8g, then add magnesium nitrate 6～8g, then add potassium bichromate 5～10g, uniform stirring; (3) by the reaction vessel Temperature Setting, be 20 ℃, the reaction times is 40min～70min; (4) by Temperature Setting, be 60 ℃, adding pure water is 250g～350g, then to add clorox 8～18g, reaction times be 50min～70min; (5) after reflection finished, reactant is centrifugal, and centrifugal rotational speed was 8000rpm, and the time is 15～25min; (6) will precipitate with pure water washing three times, can obtain graphite oxide.
2. the preparation method of a kind of graphite oxide according to claim 1, is characterized in that vitriol oil addition is 180g.
3. the preparation method of a kind of graphite oxide according to claim 1, is characterized in that magnesium nitrate is 7g.
4. the preparation method of a kind of graphite oxide according to claim 1, is characterized in that potassium bichromate is 8g.
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| CN2013102994106A CN103407995A (en) | 2013-07-17 | 2013-07-17 | Graphite oxide preparation method |
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| CN2013102994106A CN103407995A (en) | 2013-07-17 | 2013-07-17 | Graphite oxide preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104108702A (en) * | 2014-06-25 | 2014-10-22 | 苏州世优佳电子科技有限公司 | Preparation method of nano oxidized graphite |
| CN104118867A (en) * | 2014-07-07 | 2014-10-29 | 苏州世优佳电子科技有限公司 | Preparation method of graphite oxide |
| CN104692372A (en) * | 2015-03-05 | 2015-06-10 | 苏州经贸职业技术学院 | Graphene oxide and preparation method and application thereof |
| CN109485981A (en) * | 2017-09-12 | 2019-03-19 | 丹阳市丹达防腐设备有限公司 | A kind of steel lining plastic fluoroplastics material and preparation method thereof |
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| US20110280787A1 (en) * | 2009-01-26 | 2011-11-17 | Shu Tao Chen | Nitrate salt-based process for manufacture of graphite oxide |
| CN102583343A (en) * | 2012-02-08 | 2012-07-18 | 中国科学院福建物质结构研究所 | Method for preparing graphene on large scale |
| CN102701195A (en) * | 2012-06-27 | 2012-10-03 | 华南理工大学 | Method for preparing expandable graphite by using ozone |
| CN102718209A (en) * | 2012-06-11 | 2012-10-10 | 电子科技大学 | Method for preparing graphene based on reduction of divalent iron ion |
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| US20110280787A1 (en) * | 2009-01-26 | 2011-11-17 | Shu Tao Chen | Nitrate salt-based process for manufacture of graphite oxide |
| CN101613098A (en) * | 2009-06-12 | 2009-12-30 | 中国科学院宁波材料技术与工程研究所 | A kind of solution phase preparation method of Graphene |
| CN101966988A (en) * | 2010-11-17 | 2011-02-09 | 哈尔滨工业大学 | Method for preparing graphene powder |
| CN102583343A (en) * | 2012-02-08 | 2012-07-18 | 中国科学院福建物质结构研究所 | Method for preparing graphene on large scale |
| CN102718209A (en) * | 2012-06-11 | 2012-10-10 | 电子科技大学 | Method for preparing graphene based on reduction of divalent iron ion |
| CN102701195A (en) * | 2012-06-27 | 2012-10-03 | 华南理工大学 | Method for preparing expandable graphite by using ozone |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108702A (en) * | 2014-06-25 | 2014-10-22 | 苏州世优佳电子科技有限公司 | Preparation method of nano oxidized graphite |
| CN104118867A (en) * | 2014-07-07 | 2014-10-29 | 苏州世优佳电子科技有限公司 | Preparation method of graphite oxide |
| CN104692372A (en) * | 2015-03-05 | 2015-06-10 | 苏州经贸职业技术学院 | Graphene oxide and preparation method and application thereof |
| CN109485981A (en) * | 2017-09-12 | 2019-03-19 | 丹阳市丹达防腐设备有限公司 | A kind of steel lining plastic fluoroplastics material and preparation method thereof |
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Application publication date: 20131127 |