CN107601486A - A kind of graphene production method - Google Patents
A kind of graphene production method Download PDFInfo
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- CN107601486A CN107601486A CN201710945530.7A CN201710945530A CN107601486A CN 107601486 A CN107601486 A CN 107601486A CN 201710945530 A CN201710945530 A CN 201710945530A CN 107601486 A CN107601486 A CN 107601486A
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Abstract
The invention discloses the invention discloses a kind of graphene production method, comprise the following steps：（1）Graphite oxide is even added in deionized water, generates the graphite oxide aqueous solution；（2）By the graphite oxide aqueous solution generated ultrasonic wave processing,（3）Obtained graphene oxide solution is stood；（4）Then graphene oxide solution is filtered, and drying with water bath；（5）By dried graphene oxide and deionized water according to 24:10 ratio prepares solution, then adds strong reductant, and is stirred, and makes the pH value of solution between 11 14, so as to obtain graphene solution；（6）Then under vacuum, graphene solution is washed till neutrality with deionized water, filter out upper solution, solution left standstill after filtering is dried, this method avoids having used strong oxidizer in operation,, so as to simplify technique, the service life of equipment is added so as to reduce the residual of other metallic atoms or harmful substance in manufacturing process.
Description
Technical field
The present invention relates to technical field of graphene, specially a kind of graphene production method.
Background technology
Graphene is that the two dimension for the only one layer atomic thickness for being stripped out from graphite material, being made up of carbon atom is brilliant
Body.Graphene has preferable electric conductivity and thermal conductivity, has very strong wilfulness and intensity, has in production and application very big
Prospect, at present the synthetic method of graphene mainly have two kinds：Mechanical means and chemical method, physics stripping method is mainly using low
Honest and clean graphite is raw material, makes graphite layers peeling-off by applying mechanical force to graphite crystal, breaks the model moral of graphite layers
Hua Li, form monolithic graphite alkene.In graphene stripping means, it is necessary to add some auxiliary agents with increase the interlayer spacing of graphite or
It is intercalation, so that graphite is preferably peeled off.Such as using nitric acid, potassium permanganate, chromium trioxide or hydrogen peroxide as oxidant,
The concentrated sulfuric acid is peeled off as intercalator beneficial to follow-up graphite layers.But this chemical substance intercalated technique acid consumption is big, produced
Cheng Zhonghui produces the pollution of pernicious gas or heavy metal ion.There are sulphur residual, and used oxidation in the application in product
Agent can have corrosion to equipment, reduce the service life of equipment, add production cost.
The content of the invention
It is an object of the invention to provide a kind of graphene production method, is asked with solve to propose in above-mentioned background technology
Topic.
To achieve the above object, the present invention provides following technical scheme：A kind of graphene production method, including following step
Suddenly：
（1）Graphite oxide is even added in deionized water, generates the graphite oxide aqueous solution；
（2）The graphite oxide aqueous solution generated is handled into 0.5-1 hours in the presence of ultrasonic wave, and is subject in the process
Stirring obtains graphene oxide solution；
（3）Obtained graphene oxide solution is stood into 6-12 hours at 30-50 DEG C, removes upper solution；
（4）Then graphene oxide solution is filtered, and the drying with water bath 6-8 hours at a temperature of 70-100 DEG C；
（5）By dried graphene oxide and deionized water according to 2-4:10 ratio prepares solution, then adds strong reduction
Agent, and stirred, make the pH value of solution between 11-14, so as to obtain graphene solution；
（6）Then under vacuum, graphene solution is washed till neutrality with deionized water, then in 90-120 DEG C of temperature
Under, stand 8-10 hours, then filter out upper solution, by the solution after filtering at a temperature of 50-60 DEG C standing and drying
8-10 hours, being then dried at room temperature for 2-4 hours can obtain graphene.
Preferably, the weight of the graphite oxide and deionized water ratio is 1-5:800g.
Preferably, the strong reductant is hydrazine hydrate, ethylene glycol, sodium oxide molybdena, potassium hydroxide, lithium hydroxide, sodium carbonate, carbon
The mixture of one or more of solution in sour potassium, lithium carbonate, sodium acid carbonate, saleratus, lithium bicarbonate, ammonium hydroxide.
Compared with prior art, the beneficial effects of the invention are as follows：A kind of graphene production method, it is workable,
Avoid having used strong oxidizer in operating process, so as to reduce in manufacturing process other metallic atoms or harmful substance
Remain so as to simplify technique, at the same it is easy to operate, and reduce erosion of the strong oxidizer to equipment, add making for equipment
Use the life-span.
Embodiment
It is clearly and completely described below in conjunction with the technical scheme in the embodiment of the present invention, it is clear that described reality
It is only part of the embodiment of the present invention to apply example, rather than whole embodiments.It is general based on the embodiment in the present invention, this area
The every other embodiment that logical technical staff is obtained under the premise of creative work is not made, belong to what the present invention protected
Scope.
The present invention provides a kind of technical scheme：A kind of graphene production method, comprises the following steps：
（1）Graphite oxide is even added in deionized water, generates the graphite oxide aqueous solution；
（2）The graphite oxide aqueous solution generated is handled into 0.5-1 hours in the presence of ultrasonic wave, and is subject in the process
Stirring obtains graphene oxide solution；
（3）Obtained graphene oxide solution is stood into 6-12 hours at 30-50 DEG C, removes upper solution；
（4）Then graphene oxide solution is filtered, and the drying with water bath 6-8 hours at a temperature of 70-100 DEG C；
（5）By dried graphene oxide and deionized water according to 2-4:10 ratio prepares solution, then adds strong reduction
Agent, and stirred, make the pH value of solution between 11-14, so as to obtain graphene solution；
（6）Then under vacuum, graphene solution is washed till neutrality with deionized water, then in 90-120 DEG C of temperature
Under, stand 8-10 hours, then filter out upper solution, by the solution after filtering at a temperature of 50-60 DEG C standing and drying
8-10 hours, being then dried at room temperature for 2-4 hours can obtain graphene.
Preferably, the weight of the graphite oxide and deionized water ratio is 1-5:800g.
Preferably, the strong reductant is hydrazine hydrate, ethylene glycol, sodium oxide molybdena, potassium hydroxide, lithium hydroxide, sodium carbonate, carbon
The mixture of one or more of solution in sour potassium, lithium carbonate, sodium acid carbonate, saleratus, lithium bicarbonate, ammonium hydroxide.
Embodiment one
A kind of graphene production method, comprises the following steps：
（1）By the weight of graphite oxide and deionized water according to proportioning be 1-5:800g is even added in deionized water, is added
Time is 15 minutes, and is stirred, and generates the graphite oxide aqueous solution；
（2）The graphite oxide aqueous solution generated is handled 0.7 hour in the presence of ultrasonic wave, and stirred in the process
It is 200-800r/min to mix to obtain graphene oxide solution and speed of agitator；
（3）Obtained graphene oxide solution is stood into 6-12 hours at a temperature of 40 DEG C, and by filtering off except upper strata is molten
Liquid；
（4）Then graphene oxide solution is filtered, and drying with water bath 7 hours at a temperature of 90 DEG C；
（5）By dried graphene oxide and deionized water according to 3:10 ratio prepares solution, then adds strong reductant,
And stirred, make the pH value of solution to 13, so as to obtain graphene solution；
（6）Then under vacuum, graphene solution is washed till neutrality with deionized water, it is quiet then at a temperature of 115 DEG C
Put 9 hours, then filter out upper solution, by the solution after filtering at a temperature of 55 DEG C standing and drying 9 hours, Ran Hou
Dry at room temperature 3 hours and can obtain graphene.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (3)
1. the invention discloses a kind of graphene production method, comprise the following steps：
（1）Graphite oxide is even added in deionized water, generates the graphite oxide aqueous solution；
（2）The graphite oxide aqueous solution generated is handled into 0.5-1 hours in the presence of ultrasonic wave, and is subject in the process
Stirring obtains graphene oxide solution；
（3）Obtained graphene oxide solution is stood into 6-12 hours at 30-50 DEG C, removes upper solution；
（4）Then graphene oxide solution is filtered, and the drying with water bath 6-8 hours at a temperature of 70-100 DEG C；
（5）By dried graphene oxide and deionized water according to 2-4:10 ratio prepares solution, then adds strong reduction
Agent, and stirred, make the pH value of solution between 11-14, so as to obtain graphene solution；
（6）Then under vacuum, graphene solution is washed till neutrality with deionized water, then in 90-120 DEG C of temperature
Under, stand 8-10 hours, then filter out upper solution, by the solution after filtering at a temperature of 50-60 DEG C standing and drying
8-10 hours, being then dried at room temperature for 2-4 hours can obtain graphene.
A kind of 2. graphene production method according to claim 1, it is characterised in that：The graphite oxide and deionized water
Weight ratio be 1-5:800g.
3. profit requires a kind of graphene production method described in 1, it is characterised in that：The strong reductant is hydrazine hydrate, ethylene glycol,
Sodium oxide molybdena, potassium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate, lithium carbonate, sodium acid carbonate, saleratus, lithium bicarbonate, hydrogen-oxygen
Change the mixture of one or more of solution in ammonium.
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| CN201710945530.7A CN107601486A (en) | 2017-10-12 | 2017-10-12 | A kind of graphene production method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761225A (en) * | 2019-03-30 | 2019-05-17 | 山东大学 | A kind of system based on Hydrodynamic cavitation and preparing grapheme through oxidation reduction |
| CN111892043A (en) * | 2020-08-06 | 2020-11-06 | 昆明理工大学 | Method for preparing reduced graphene oxide by one-pot method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387226A (en) * | 2013-07-05 | 2013-11-13 | 清华大学深圳研究生院 | Preparation method for graphene |
| CN104477883A (en) * | 2014-11-13 | 2015-04-01 | 苏州经贸职业技术学院 | Preparation method of graphene |
-
2017
- 2017-10-12 CN CN201710945530.7A patent/CN107601486A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387226A (en) * | 2013-07-05 | 2013-11-13 | 清华大学深圳研究生院 | Preparation method for graphene |
| CN104477883A (en) * | 2014-11-13 | 2015-04-01 | 苏州经贸职业技术学院 | Preparation method of graphene |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761225A (en) * | 2019-03-30 | 2019-05-17 | 山东大学 | A kind of system based on Hydrodynamic cavitation and preparing grapheme through oxidation reduction |
| CN111892043A (en) * | 2020-08-06 | 2020-11-06 | 昆明理工大学 | Method for preparing reduced graphene oxide by one-pot method |
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Application publication date: 20180119 |
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