CN104787760A - Preparation method of graphite oxide - Google Patents
Preparation method of graphite oxide Download PDFInfo
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- CN104787760A CN104787760A CN201510194058.9A CN201510194058A CN104787760A CN 104787760 A CN104787760 A CN 104787760A CN 201510194058 A CN201510194058 A CN 201510194058A CN 104787760 A CN104787760 A CN 104787760A
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Abstract
The invention discloses a preparation method of graphite oxide. The preparation method is to use dipyridine chromium oxide and/or pyriddinium chlorochromate to substitute oxidizing agents KClO4 and KMnO4 used in the existing graphite oxide preparation process, so as to prepare the graphite oxide with a high carbon-oxygen ratio. The preparation method provides an excellent raw material for preparing the high-performance graphene, is beneficial to promote and apply, and is excellent in economic benefits and social benefits.
Description
Technical field
The invention belongs to field of material preparation, be specifically related to a kind of preparation method of graphite oxide.
Background technology
Graphene has the performance of many excellences as new nano-scale carbon material, and its peculiar property derives from sp
2the two-dimension single layer graphite-structure of hydridization, this structure gives Graphene much special physics and chemistry character, such as high electron mobility, high transparent, flexible structure and huge theoretical specific surface area etc.At present, prepare the method that Graphene adopts reduction-oxidation graphite usually, therefore, the quality of graphite oxide directly determines the quality of the Graphene prepared.The oxygenant preparing graphite oxide use is under normal circumstances KClO
4, KMnO
4but, all there is graphite oxidation degree low, the problem that obtained graphite oxide carbon-to-oxygen ratio is lower.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of graphite oxide, with Al2O3 thin films or/and pyriddinium chlorochromate substitutes and existingly prepares the oxygenant KClO used in graphite oxide technique
4, KMnO
4, the graphite oxide of obtained high carbon-oxygen ratio, providing high quality raw material for preparing high performance Graphene, being conducive to applying, possessing significant economic and social benefit.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method of graphite oxide comprises the following steps:
1) 200-500 milligram Graphite Powder 99,200-500 milligram SODIUMNITRATE and the 10-30 milliliter vitriol oil are mixed, 10 DEG C of ultrasonic disperse 15-20 minute;
2) 2-3 gram of oxygenant is slowly added, then ultrasonic disperse 5 minutes;
3) 30-50 DEG C of stirring in water bath 2 hours, slowly drips 15-20 ml deionized water in whipping process;
4) 90 DEG C of stirring in water bath 20-30 minute;
5) add 100 milliliters, the hydrogen peroxide of 3vol.%, with 1M salt acid elution, add deionized water, centrifuge washing is to neutral, and 80 DEG C of vacuum-drying 12 hours, grinding, obtains brown oxidation powdered graphite.
Described oxygenant is one or both in Al2O3 thin films, pyriddinium chlorochromate.
The carbon-to-oxygen ratio (weight ratio) of obtained graphite oxide is 12.
Remarkable advantage of the present invention is: use strong oxidizer Al2O3 thin films or/and pyriddinium chlorochromate, the problem that the graphite oxide carbon-to-oxygen ratio that solution conventional oxidant obtains is low, obtained high carbon-oxygen ratio graphite oxide, high quality raw material are provided for preparing high performance Graphene, be conducive to applying, possess significant economic and social benefit.
Embodiment
embodiment 1
A kind of preparation method of graphite oxide comprises the following steps:
1) by the mixing of 350 milligrams of Graphite Powder 99s, 350 milligrams of SODIUMNITRATE and 20 milliliters of vitriol oils, 10 DEG C of ultrasonic disperse 18 minutes;
2) 2.5 grams of oxygenants are slowly added, then ultrasonic disperse 5 minutes;
3) 40 DEG C of stirring in water bath 2 hours, slowly drip 18 ml deionized water in whipping process;
5) 90 DEG C of stirring in water bath 25 minutes;
5) add 100 milliliters, the hydrogen peroxide of 3vol.%, with 1M salt acid elution, add deionized water, centrifuge washing is to neutral, and 80 DEG C of vacuum-drying 12 hours, grinding, obtains brown oxidation powdered graphite.
Al2O3 thin films and the pyriddinium chlorochromate of described oxygenant to be weight ratio be 1:1.
The carbon-to-oxygen ratio (weight ratio) of obtained graphite oxide is 12.
embodiment 2
A kind of preparation method of graphite oxide comprises the following steps:
1) by the mixing of 200 milligrams of Graphite Powder 99s, 200 milligrams of SODIUMNITRATE and 10 milliliters of vitriol oils, 10 DEG C of ultrasonic disperse 15 minutes;
2) 2 grams of oxygenants are slowly added, then ultrasonic disperse 5 minutes;
3) 30 DEG C of stirring in water bath 2 hours, slowly drip 15 ml deionized water in whipping process;
6) 90 DEG C of stirring in water bath 20 minutes;
5) add 100 milliliters, the hydrogen peroxide of 3vol.%, with 1M salt acid elution, add deionized water, centrifuge washing is to neutral, and 80 DEG C of vacuum-drying 12 hours, grinding, obtains brown oxidation powdered graphite.
Described oxygenant is Al2O3 thin films.
The carbon-to-oxygen ratio (weight ratio) of obtained graphite oxide is 12.
embodiment 3
A kind of preparation method of graphite oxide comprises the following steps:
1) by the mixing of 500 milligrams of Graphite Powder 99s, 500 milligrams of SODIUMNITRATE and 30 milliliters of vitriol oils, 10 DEG C of ultrasonic disperse 20 minutes;
2) 3 grams of oxygenants are slowly added, then ultrasonic disperse 5 minutes;
3) 50 DEG C of stirring in water bath 2 hours, slowly drip 20 ml deionized water in whipping process;
7) 90 DEG C of stirring in water bath 30 minutes;
5) add 100 milliliters, the hydrogen peroxide of 3vol.%, with 1M salt acid elution, add deionized water, centrifuge washing is to neutral, and 80 DEG C of vacuum-drying 12 hours, grinding, obtains brown oxidation powdered graphite.
Described oxygenant is pyriddinium chlorochromate.
The carbon-to-oxygen ratio (weight ratio) of obtained graphite oxide is 12.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (3)
1. a preparation method for graphite oxide, is characterized in that: comprise the following steps:
200-500 milligram Graphite Powder 99,200-500 milligram SODIUMNITRATE and the 10-30 milliliter vitriol oil are mixed, 10 DEG C of ultrasonic disperse 15-20 minute;
Slowly add 2-3 gram of oxygenant, then ultrasonic disperse 5 minutes;
30-50 DEG C of stirring in water bath 2 hours, slowly drips 15-20 ml deionized water in whipping process;
90 DEG C of stirring in water bath 20-30 minute;
Add 100 milliliters, the hydrogen peroxide of 3vol.%, with 1M salt acid elution, add deionized water, centrifuge washing is to neutral, and 80 DEG C of vacuum-drying 12 hours, grinding, obtains brown oxidation powdered graphite.
2. the preparation method of graphite oxide according to claim 1, is characterized in that: described oxygenant is one or both in Al2O3 thin films, pyriddinium chlorochromate.
3. the graphite oxide that the method for claim 1 is obtained, is characterized in that: carbon-to-oxygen ratio is 12.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510194058.9A CN104787760B (en) | 2015-04-23 | 2015-04-23 | Preparation method of graphite oxide |
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| CN201510194058.9A CN104787760B (en) | 2015-04-23 | 2015-04-23 | Preparation method of graphite oxide |
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| CN104787760A true CN104787760A (en) | 2015-07-22 |
| CN104787760B CN104787760B (en) | 2017-01-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108273510A (en) * | 2018-01-18 | 2018-07-13 | 三明学院 | A kind of visible light-responded composite photo-catalyst of Z-type and preparation method thereof |
Citations (4)
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| KR20050064539A (en) * | 2003-12-24 | 2005-06-29 | 재단법인 포항산업과학연구원 | Manufacturing method of exfoliated graphite from surface-treated graphite |
| CN102765714A (en) * | 2012-06-18 | 2012-11-07 | 河北工业大学 | Preparation method of graphite oxide with high degree of oxidation and high dispersibility |
| 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 |
-
2015
- 2015-04-23 CN CN201510194058.9A patent/CN104787760B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050064539A (en) * | 2003-12-24 | 2005-06-29 | 재단법인 포항산업과학연구원 | Manufacturing method of exfoliated graphite from surface-treated graphite |
| CN102765714A (en) * | 2012-06-18 | 2012-11-07 | 河北工业大学 | Preparation method of graphite oxide with high degree of oxidation and high dispersibility |
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| 万臣等: "不同氧化程度氧化石墨烯的制备及湿敏性能研究", 《无机化学学报》 * |
| 刘海彬等: "氧化程度对氧化石墨改性环氧树脂涂层摩擦学性能的影响", 《理化检验-物理分册》 * |
| 王培草等: "氧化程度对氧化石墨烯a-b轴结构及电学性能的影响", 《无机化学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108273510A (en) * | 2018-01-18 | 2018-07-13 | 三明学院 | A kind of visible light-responded composite photo-catalyst of Z-type and preparation method thereof |
| CN108273510B (en) * | 2018-01-18 | 2020-06-30 | 三明学院 | Z-shaped visible light response composite photocatalyst and preparation method thereof |
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|---|---|
| CN104787760B (en) | 2017-01-25 |
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Effective date of registration: 20210507 Address after: 158100 Central South Committee of Jieli office, Lishu District, Jixi City, Heilongjiang Province Patentee after: Jixi Dingyuan graphite Co.,Ltd. Address before: 365004, No. 25 Jing Dong Road, three yuan, Fujian, Sanming City Patentee before: SANMING University |
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