CN102730669A - Method for preparing graphene oxide by using graphitized carbon fibers - Google Patents
Method for preparing graphene oxide by using graphitized carbon fibers Download PDFInfo
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- CN102730669A CN102730669A CN2012101654526A CN201210165452A CN102730669A CN 102730669 A CN102730669 A CN 102730669A CN 2012101654526 A CN2012101654526 A CN 2012101654526A CN 201210165452 A CN201210165452 A CN 201210165452A CN 102730669 A CN102730669 A CN 102730669A
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Abstract
The invention relates to a method for preparing a graphene oxide by using graphitized carbon fibers. The method specifically comprises three steps: A) taking 0-5 g of graphitized carbon fibers, 1-5 g of sodium nitrate, 5-30 g of potassium permanganate, and 50-300 ml of concentrated sulfuric acid, carrying out a reaction for 1-24 hours in a water bath with a temperature of 30-40 DEG C and observing the color change, adding 100-500 mL of deionized water and observing the color change, transferring the resulting solution to an environment with a temperature of 90-100 DEG C, carrying out a reaction for 0-5 hours, adding 50-300 mL of deionized water and 0-50 ml of hydrogen peroxide, and filtering while hot to obtain a black velvet-like substance; B) drying the obtained primary carbon oxide fibers for 2 hours at a temperature of 100 DEG C, weighing 0-5 g of the primary carbon oxide fibers, repeated performing the step A) and observing the color change until the suspension with the color from brown-yellow to yellow is generated, and filtering while hot to obtain the secondary carbon oxide fibers, wherein the secondary carbon oxide fibers are the graphite oxide carbon fibers; C) drying the obtained graphite oxide carbon fibers, dissolving in water, and carrying out an ultrasonic treatment for 0-5 hours to obtain the graphene oxide. The obtained graphene solution of the present invention is uniform and stable, and can be stored for a long time, the preparation method is simple, and the cost is low.
Description
Technical field
The present invention relates to a kind of method of utilizing graphitized carbon fibre to prepare graphene oxide.
Background technology
Graphene is with sp by the monolayer carbon atom
2The cellular two-dimentional atomic crystal of six sides that hydridization constitutes is present optimal two-dimensional nano material, has the physicochemical property of a lot of uniquenesses, and the specific conductivity of Graphene and thermal conductivity are high, and specific surface area is big, and (theoretical specific surface area is 2630m
2/ g), physical strength is high.Given this, Graphene is expected to be used widely in fields such as nano electron device, matrix material, energy storage and gas sensors.
Nowadays the method for preparing Graphene is a lot, and the most frequently used preparation method then is to be raw material with graphite, and the utilization chemical oxidization method carries out oxidation to be peeled off, and at first prepares graphene oxide, and reduction obtains Graphene then.In all methods of preparation graphene oxide, graphite has been undisputable fact as starting material, obtains graphene oxide through oxidation, intercalation and last supersound process.In theory, other has the material of graphite-like structure, through close method, can prepare graphene oxide equally, still, up to the present, does not almost have bibliographical information to utilize other raw material of wood-charcoal material to prepare graphene oxide.Graphitized carbon fibre is through carbonization and graphitization processing and the micro crystal graphite material that obtains by organic fibre.The similar synthetic graphite of the microtexture of thomel is a random graphits structure.Therefore, in theory, graphitized carbon fibre can be used as the raw material of preparation Graphene.A large amount of chopped carbon fibers can occur in the preparation process of thomel in the prior art, if can it be utilized, will be save energy, improving utilization ratio of raw materials provides method, and is that the starting material scope that enlarges the preparation Graphene is offered reference.
Summary of the invention
The invention discloses a kind of method of utilizing graphitized carbon fibre to prepare graphene oxide; Its purpose is to overcome the single drawback of starting material that available technology adopting graphite exists for the feedstock production Graphene; The inventive method is simple to operate, and is with low cost, workable.
A kind of method of utilizing graphitized carbon fibre to prepare graphene oxide is the feedstock production Graphene with the graphitized carbon fibre, it is characterized in that: specifically comprise following three steps:
A) get the 0.5-5g graphitized carbon fibre, 1-5g SODIUMNITRATE, 5-30g potassium permanganate, the 50-300ml vitriol oil reacts 1-24h in 30-40 ℃ of water-bath, observe change in color; Add the 100-500mL deionized water, and observe colour-change, move to 90-100 ℃ of reaction 0-5h down then, add 50-300mL deionized water and 0-50mL ydrogen peroxide 50, filtered while hot obtains the velvet-like material of black, obtains the once oxidation thomel;
B) with 100 ℃ of dry 2h of the above-mentioned once oxidation thomel that obtains.Take by weighing exsiccant once oxidation thomel 0.5-5g, repeating step A), observe change in color, up to pale brown look occurring to yellow suspension, filtered while hot obtains the secondary oxidation thomel, is the graphite oxide thomel;
C) with step B) the graphite oxide thomel that obtains is dry, and ultrasonic 0.5-5h soluble in water then obtains graphene oxide.
Prepare in the graphene oxide at graphitized carbon fibre, the graphitized fibre of selecting for use is polyacrylonitrile-radical or asphaltic base graphitized carbon fibre.
The present invention utilizes graphitized carbon fibre to prepare the method for graphene oxide, has advantages such as simple to operate, with low cost, workable.
Embodiment
Below in conjunction with embodiment the present invention is carried out detailed assorted explanation.
Instance 1:
Oxidation for the first time takes by weighing the 3g PAN-based carbon fiber, and 2.5g SODIUMNITRATE, and measure the 115mL vitriol oil and pour in the 500mL beaker is adjusted into 30 ℃ with the Heating temperature of induction stirring water bath, keeps temperature-resistant, reacts about 3h.And move to subsequently in 98 ℃ of water-baths, reaction 1h is measured 230mL deionized water and 10mL ydrogen peroxide 50 and is added in the beaker.Filtration drying obtains the sample of oxidation for the first time.
Oxidation for the second time takes by weighing the sample 5g of first oxidation, SODIUMNITRATE 5g; And measure vitriol oil 200mL, and add in the 500mL beaker, under 35 ℃ of water-baths, fully react 5h; Move to subsequently in 98 ℃ of water-baths, reaction 3h is measured 160mL deionized water and 10mL ydrogen peroxide 50 and is added in the beaker.Can obtain being close to bright orange-yellow solution, filter, be scattered in ultrasonic 2h in the water after the drying, obtain graphene oxide.
Instance 2:
Oxidation for the first time takes by weighing the 0.5g asphalt base carbon fiber, and 1g SODIUMNITRATE, and measure the 50mL vitriol oil and pour in the 500mL beaker is adjusted into 35 ℃ with the Heating temperature of induction stirring water bath, keeps temperature-resistant, reacts about 15h.And move to subsequently in 98 ℃ of water-baths, reaction 3h is measured 150mL deionized water and 5mL ydrogen peroxide 50 and is added in the beaker.Filtration drying obtains the sample of oxidation for the first time.
Oxidation for the second time takes by weighing the sample 1g of first oxidation, SODIUMNITRATE 2g; And measure vitriol oil 50mL, and add in the 500mL beaker, under 35 ℃ of water-baths, fully react 6h; Move to subsequently in 98 ℃ of water-baths, reaction 5h is measured 50mL deionized water and 10mL ydrogen peroxide 50 and is added in the beaker.Can obtain being close to bright orange-yellow solution, filter, be scattered in ultrasonic 2h in the water after the drying, obtain graphene oxide.
Instance 3:
Oxidation for the first time takes by weighing the 5g PAN-based carbon fiber, and 5g SODIUMNITRATE, and measure the 300mL vitriol oil and pour in the 500mL beaker is adjusted into 38 ℃ with the Heating temperature of induction stirring water bath, keeps temperature-resistant, reacts 24h.And move to subsequently in 98 ℃ of water-baths, reaction 3h is measured 300mL deionized water and 50mL ydrogen peroxide 50 and is added in the beaker.Filtration drying obtains the sample of oxidation for the first time.
Oxidation for the second time takes by weighing the sample 3g of first oxidation, SODIUMNITRATE 2g; And measure vitriol oil 50mL, and add in the 500mL beaker, under 35 ℃ of water-baths, fully react 6h; Move to subsequently in 98 ℃ of water-baths, reaction 5h is measured 150mL deionized water and 20mL ydrogen peroxide 50 and is added in the beaker.Can obtain being close to bright orange-yellow solution, filter, be scattered in ultrasonic 2h in the water after the drying, obtain graphene oxide.
Claims (2)
1. a method of utilizing graphitized carbon fibre to prepare graphene oxide is the feedstock production Graphene with the graphitized carbon fibre, it is characterized in that: specifically comprise following three steps:
A) get the 0.5-5g graphitized carbon fibre, 1-5g SODIUMNITRATE, 5-30g potassium permanganate, the 50-300ml vitriol oil reacts 1-24h in 30-40 ℃ of water-bath, observe change in color; Add the 100-500mL deionized water, and observe colour-change, move to 90-100 ℃ of reaction 0-5h down then, add 50-300mL deionized water and 0-50mL ydrogen peroxide 50, filtered while hot obtains the velvet-like material of black, obtains the once oxidation thomel;
B) with 100 ℃ of dry 2h of the above-mentioned once oxidation thomel that obtains.Take by weighing exsiccant once oxidation thomel 0-5g, repeating step A), observe change in color, up to pale brown look occurring to yellow suspension, filtered while hot obtains the secondary oxidation thomel, is the graphite oxide thomel;
C) with step B) the graphite oxide thomel that obtains is dry, and ultrasonic 0-5h soluble in water then obtains graphene oxide.
2. a kind of method of utilizing graphitized carbon fibre to prepare graphene oxide according to claim 1 is characterized in that: prepare in the graphene oxide at graphitized carbon fibre, the graphitized fibre of selecting for use is polyacrylonitrile-radical or asphaltic base graphitized carbon fibre.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103422196A (en) * | 2013-07-29 | 2013-12-04 | 中国科学院生态环境研究中心 | Preparation method for graphene and graphite core sheath structured fiber |
| CN104386676A (en) * | 2014-11-05 | 2015-03-04 | 北京化工大学 | Preparation method of graphene |
| CN105217621A (en) * | 2015-10-30 | 2016-01-06 | 浙江理工大学 | A kind of graphene oxide preparation method of size uniformity |
| CN105585012A (en) * | 2015-12-16 | 2016-05-18 | 杭州师范大学 | Method for preparing graphene nanoribbon with width being 100-1000 nm |
| CN106467767A (en) * | 2015-08-17 | 2017-03-01 | 清华大学 | A kind of preparation method of micro crystal graphite alkene lube oil additive |
| CN107416812A (en) * | 2017-08-07 | 2017-12-01 | 蚌埠学院 | A kind of method that graphene oxide is prepared using walnut shell as carbon source |
| CN108557816A (en) * | 2018-06-26 | 2018-09-21 | 武汉大学 | A kind of preparation method of high specific surface area porous graphitized charcoal |
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| US20100055025A1 (en) * | 2008-09-03 | 2010-03-04 | Jang Bor Z | Process for producing dispersible Nano Graphene Platelets from oxidized graphite |
| CN102153075A (en) * | 2011-03-22 | 2011-08-17 | 桂林理工大学 | Method for synthesizing graphene oxide by ultrasonic assistance Hummers method |
| CN102249220A (en) * | 2011-03-18 | 2011-11-23 | 太原理工大学 | Quick preparation method for graphene oxide film |
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2012
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20100055025A1 (en) * | 2008-09-03 | 2010-03-04 | Jang Bor Z | Process for producing dispersible Nano Graphene Platelets from oxidized graphite |
| CN102249220A (en) * | 2011-03-18 | 2011-11-23 | 太原理工大学 | Quick preparation method for graphene oxide film |
| CN102153075A (en) * | 2011-03-22 | 2011-08-17 | 桂林理工大学 | Method for synthesizing graphene oxide by ultrasonic assistance Hummers method |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103422196A (en) * | 2013-07-29 | 2013-12-04 | 中国科学院生态环境研究中心 | Preparation method for graphene and graphite core sheath structured fiber |
| CN103422196B (en) * | 2013-07-29 | 2015-07-15 | 中国科学院生态环境研究中心 | Preparation method for graphene and graphite core sheath structured fiber |
| CN104386676A (en) * | 2014-11-05 | 2015-03-04 | 北京化工大学 | Preparation method of graphene |
| CN104386676B (en) * | 2014-11-05 | 2017-09-26 | 北京化工大学 | A kind of preparation method of graphene |
| CN106467767A (en) * | 2015-08-17 | 2017-03-01 | 清华大学 | A kind of preparation method of micro crystal graphite alkene lube oil additive |
| CN105217621A (en) * | 2015-10-30 | 2016-01-06 | 浙江理工大学 | A kind of graphene oxide preparation method of size uniformity |
| CN105585012A (en) * | 2015-12-16 | 2016-05-18 | 杭州师范大学 | Method for preparing graphene nanoribbon with width being 100-1000 nm |
| CN105585012B (en) * | 2015-12-16 | 2017-11-24 | 杭州师范大学 | A kind of preparation method of the 1000nm of width 100 graphene nanobelt |
| CN107416812A (en) * | 2017-08-07 | 2017-12-01 | 蚌埠学院 | A kind of method that graphene oxide is prepared using walnut shell as carbon source |
| CN108557816A (en) * | 2018-06-26 | 2018-09-21 | 武汉大学 | A kind of preparation method of high specific surface area porous graphitized charcoal |
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Application publication date: 20121017 |