CN104108702A - Preparation method of nano oxidized graphite - Google Patents
Preparation method of nano oxidized graphite Download PDFInfo
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- CN104108702A CN104108702A CN201410286282.6A CN201410286282A CN104108702A CN 104108702 A CN104108702 A CN 104108702A CN 201410286282 A CN201410286282 A CN 201410286282A CN 104108702 A CN104108702 A CN 104108702A
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Abstract
The invention discloses a preparation method of nano oxidized graphite, which comprises the following steps: 1)placing a beaker under ice bath environment at temperature of 5 DEG C, adding concentrated sulfuric acid in the beaker, uniformly stirring; 2)uniformly and slowly adding graphite in the beaker, then adding calcium nitrate and potassium perchlorate, slowly stirring for fully reacting; 3)keeping the temperature of the beaker below than 14 DEG C; 4)heating the temperature of the beaker to 45 DEG C, adding postassium hypochlorite, adding deionized water, performing a medium temperature reaction; 5)heating the liquid temperature in the beaker to 75 DEG C, stirring and reacting; 6)centrifuging the liquid in the beaker, washing to obtain the oxidized graphite; and 7)performing ultrasonic treatment on the oxidized graphite to obtain the nano oxidized graphite. The prepared nano oxidized graphite has the advantages of large specific surface area, small particle size and high carbon-oxygen ratio.
Description
Technical field
The invention belongs to field of nanometer material technology, relate to a kind of preparation method of graphite oxide, particularly relate to a kind of preparation method of nano oxidized graphite.
Background technology
Natural graphite is the material of laminate structure, bonding force between each layer a little less than, the spacing of natural graphite interlayer is less, by natural graphite is processed, obtain graphite oxide or expanded graphite, the functional group between once will increase, and its spacing also can increase simultaneously, improve to a certain extent its chemically reactive, there is application comparatively widely.
The application of Graphene is more and more, and in order to prepare Graphene, by preparing graphite oxide, then reaction obtains graphene oxide, finally restore for Graphene be a kind of common method.Graphite oxide is as an indispensable composition in whole preparation process, and its preparation is determining the character of last Graphene.
Summary of the invention
The technical problem solving: the graphite oxide specific surface area that the preparation method of conventional graphite oxide prepares is little, particle diameter is large, carbon-to-oxygen ratio is very low, has reduced the problem of the range of application of graphite oxide.
Technical scheme: for the problems referred to above, the invention discloses a kind of preparation method of nano oxidized graphite, the preparation method of described nano oxidized graphite comprises the following steps:
(1) beaker being placed under the ice bath environment of 5 ℃, is 65g～95g to slowly adding the vitriol oil in beaker, stirs;
(2) to evenly slowly adding Graphite Powder 99 in the beaker in step (1), be 3～5g, then to add nitrocalcite be that 4～5g, potassium perchlorate are 3～7g, add after nitrocalcite and potassium perchlorate, be slowly stirred to abundant reaction;
(3) keep the temperature of beaker below 14 ℃, the time of oxidizing reaction is 25min～55min;
(4) beaker temperature is increased to 45 ℃, adding potassium hypochlorite is 5～9g, and adding deionized water is 80g～90g, again carries out middle temperature reaction, and the stirring reaction time is 35min～45min;
(5) again fluid temperature in beaker is increased to 75 ℃, then the stirring reaction time is 15min～20min;
(6) liquid in beaker in step (5) is carried out centrifugal, centrifugal rotational speed is 5000rpm, and the time is 5min, washs after centrifugal again, and washing obtains graphite oxide;
(7) graphite oxide is carried out to supersound process, obtain nano oxidized graphite.
The preparation method of described a kind of nano oxidized graphite, the vitriol oil described in preparation process is preferably 95g.
The preparation method of described a kind of nano oxidized graphite, the potassium hypochlorite described in preparation process is preferably 7g.
The preparation method of described a kind of nano oxidized graphite, supersound process power is preferably 50w, and the treatment time is preferably 30min.
Beneficial effect: preparation method of the present invention is by the selection to the kind of the oxygenant in graphite oxide preparation process and quality, and optimized temperature of reaction, the specific surface area of the nano oxidized graphite obtaining is higher than conventional graphite oxide specific surface area, its carbon-to-oxygen ratio is also higher than common graphite oxide simultaneously, reached 2.94 to 3.02, particle diameter is at 25nm to 43nm.
Embodiment
Embodiment 1
(1) beaker being placed under the ice bath environment of 5 ℃, is 65g to slowly adding the vitriol oil in beaker, stirs;
(2) to evenly slowly adding Graphite Powder 99 in the beaker in step (1), be 3g, then to add nitrocalcite be that 4g, potassium perchlorate are 7g, add after nitrocalcite and potassium perchlorate, be slowly stirred to abundant reaction;
(3) keep the temperature of beaker below 14 ℃, the time of oxidizing reaction is 25min;
(4) beaker temperature is increased to 45 ℃, adding potassium hypochlorite is 9g, and adding deionized water is 80g, again carries out middle temperature reaction, and the stirring reaction time is 35min;
(5) again fluid temperature in beaker is increased to 75 ℃, then the stirring reaction time is 20min;
(6) liquid in beaker in step (5) is carried out centrifugal, centrifugal rotational speed is 5000rpm, and the time is 5min, washs after centrifugal again, and washing obtains graphite oxide;
(7) graphite oxide is carried out to supersound process, obtain nano oxidized graphite.
The nano oxidized graphite carbon-to-oxygen ratio of embodiment 1 is 2.99, and particle diameter is 25nm.
Embodiment 2
(1) beaker being placed under the ice bath environment of 5 ℃, is 80g to slowly adding the vitriol oil in beaker, stirs;
(2) to evenly slowly adding Graphite Powder 99 in the beaker in step (1), be 4g, then to add nitrocalcite be that 5g, potassium perchlorate are 3g, add after nitrocalcite and potassium perchlorate, be slowly stirred to abundant reaction;
(3) keep the temperature of beaker below 14 ℃, the time of oxidizing reaction is 55min;
(4) beaker temperature is increased to 45 ℃, adding potassium hypochlorite is 7g, and adding deionized water is 90g, again carries out middle temperature reaction, and the stirring reaction time is 45min;
(5) again fluid temperature in beaker is increased to 75 ℃, then the stirring reaction time is 15min;
(6) liquid in beaker in step (5) is carried out centrifugal, centrifugal rotational speed is 5000rpm, and the time is 5min, washs after centrifugal again, and washing obtains graphite oxide;
(7) graphite oxide is carried out to supersound process, obtain nano oxidized graphite.
The nano oxidized graphite carbon-to-oxygen ratio of embodiment 2 is 2.94, and particle diameter is 33nm.
Embodiment 3
(1) beaker being placed under the ice bath environment of 5 ℃, is 95g to slowly adding the vitriol oil in beaker, stirs;
(2) to evenly slowly adding Graphite Powder 99 in the beaker in step (1), be 5g, then to add nitrocalcite be that 4g, potassium perchlorate are 5g, add after nitrocalcite and potassium perchlorate, be slowly stirred to abundant reaction;
(3) keep the temperature of beaker below 14 ℃, the time of oxidizing reaction is 40min;
(4) beaker temperature is increased to 45 ℃, adding potassium hypochlorite is 5g, and adding deionized water is 85g, again carries out middle temperature reaction, and the stirring reaction time is 40min;
(5) again fluid temperature in beaker is increased to 75 ℃, then the stirring reaction time is 20min;
(6) liquid in beaker in step (5) is carried out centrifugal, centrifugal rotational speed is 5000rpm, and the time is 5min, washs after centrifugal again, and washing obtains graphite oxide;
(7) graphite oxide is carried out to supersound process, obtain nano oxidized graphite.
The nano oxidized graphite carbon-to-oxygen ratio of embodiment 3 is 3.02, and particle diameter is 43nm.
Claims (4)
1. a preparation method for nano oxidized graphite, is characterized in that the preparation method of described nano oxidized graphite comprises the following steps:
Beaker being placed under the ice bath environment of 5 ℃, is 65g～95g to slowly adding the vitriol oil in beaker, stirs;
To evenly slowly adding Graphite Powder 99 in the beaker in step (1), be 3～5g, then to add nitrocalcite be that 4～5g, potassium perchlorate are 3～7g, add after nitrocalcite and potassium perchlorate, be slowly stirred to abundant reaction;
Keep the temperature of beaker below 14 ℃, the time of oxidizing reaction is 25min～55min;
Beaker temperature is increased to 45 ℃, and adding potassium hypochlorite is 5～9g, and adding deionized water is 80g～90g, again carries out middle temperature reaction, and the stirring reaction time is 35min～45min;
Again fluid temperature in beaker is increased to 75 ℃, then the stirring reaction time is 15min～20min;
Liquid in beaker in step (5) is carried out centrifugal, centrifugal rotational speed is 5000rpm, and the time is 5min, washs after centrifugal again, and washing obtains graphite oxide;
Graphite oxide is carried out to supersound process, obtain nano oxidized graphite.
2. the preparation method of a kind of nano oxidized graphite according to claim 1, is characterized in that the vitriol oil described in preparation process is 95g.
3. the preparation method of a kind of nano oxidized graphite according to claim 1, is characterized in that the potassium hypochlorite described in preparation process is 7g.
4. the preparation method of a kind of nano oxidized graphite according to claim 1, is characterized in that supersound process power is 50w, and the treatment time is 30min.
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| CN201410286282.6A CN104108702A (en) | 2014-06-25 | 2014-06-25 | Preparation method of nano oxidized graphite |
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| CN201410286282.6A CN104108702A (en) | 2014-06-25 | 2014-06-25 | Preparation method of nano oxidized graphite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104787760A (en) * | 2015-04-23 | 2015-07-22 | 三明学院 | Preparation method of graphite oxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010159209A (en) * | 2004-07-27 | 2010-07-22 | National Institute Of Advanced Industrial Science & Technology | Aligned single-walled carbon nanotube bulk structure and its production method |
| CN102292285A (en) * | 2009-01-26 | 2011-12-21 | 陶氏环球技术有限责任公司 | Nitrate salt-based process for manufacture of graphite oxide |
| CN102795873A (en) * | 2012-07-30 | 2012-11-28 | 哈尔滨工业大学 | Method for interface modification of carbon/carbon composite material by graphene/polymer coating |
| CN103407995A (en) * | 2013-07-17 | 2013-11-27 | 苏州艾特斯环保材料有限公司 | Graphite oxide preparation method |
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2014
- 2014-06-25 CN CN201410286282.6A patent/CN104108702A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010159209A (en) * | 2004-07-27 | 2010-07-22 | National Institute Of Advanced Industrial Science & Technology | Aligned single-walled carbon nanotube bulk structure and its production method |
| CN102292285A (en) * | 2009-01-26 | 2011-12-21 | 陶氏环球技术有限责任公司 | Nitrate salt-based process for manufacture of graphite oxide |
| CN102795873A (en) * | 2012-07-30 | 2012-11-28 | 哈尔滨工业大学 | Method for interface modification of carbon/carbon composite material by graphene/polymer coating |
| CN103407995A (en) * | 2013-07-17 | 2013-11-27 | 苏州艾特斯环保材料有限公司 | Graphite oxide preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104787760A (en) * | 2015-04-23 | 2015-07-22 | 三明学院 | Preparation method of graphite oxide |
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Application publication date: 20141022 |