CN104386679A - Method for preparing graphene oxide and graphene - Google Patents
Method for preparing graphene oxide and graphene Download PDFInfo
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- CN104386679A CN104386679A CN201410638933.3A CN201410638933A CN104386679A CN 104386679 A CN104386679 A CN 104386679A CN 201410638933 A CN201410638933 A CN 201410638933A CN 104386679 A CN104386679 A CN 104386679A
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Abstract
The invention provides a method for preparing graphene oxide and graphene. The method for preparing graphene oxide comprises the following steps: uniformly mixing a graphite raw material, a solvent and an oxidant, putting in a closed reaction container, stirring to react for 0.5-6 hours at 40-120 DEG C, reducing pressure, pumping and filtering, and washing; drying the filtered material in vacuum, and grinding; uniformly dispersing the dried and ground product in deionized water; adding the oxidant under an acidic condition, and stirring to react for 1-4 hours at 0-4 DEG C; increasing the temperature to 20-40 DEG C, and stirring to react for 1-2 hours; separating and purifying the suspension after reacting, dispersing in the deionized water, and carrying out spray drying to obtain the graphene oxide. The method for preparing graphene comprises the following steps: carrying out ultrasonic dispersion on the graphene oxide in deionized water, adding a reducing agent to perform a reduction reaction, washing and drying to obtain graphene.
Description
Technical field
The present invention relates to technical field of graphene, be specifically related to a kind of preparation method of graphene oxide and prepare the method for Graphene with graphene oxide.
Background technology
Graphene is a kind of two-dimentional carbon film only having an atomic thickness, it is uniquely a kind of material by individual layer atomic building that people find so far, hexagonal network is connected into by chemical bond-linking between carbon atom in carbon film, because the chemical bond between carbon atom is made up of sp2 hybridized orbital, therefore Graphene is very indomitable, possesses the good characteristic that other novel materials such as bent, electroconductibility is strong, physical strength good, light transmission is good do not possess.Graphene possesses the conductivity be not of the common run, and resistivity is very little, and electronics can move pole efficiently, and this respect performance is higher than traditional conductor and semi-conductor a lot; Electronics moves the collision that there is not electronics and atom in Graphene, can greatly reduce energy waste; Graphene possesses fabulous light transmission, but airtight, can be used for Development of New Generation protective layer material, and can be used for exploitation transparent electron product and wearable electronic product.The preparation method of graphene product is various; but there are some drawbacks; especially be difficult to control quality product and productive rate in preparation process; processing conditions in production process changes the change as temperature and time a little; bring very large impact will to the quality of product and productive rate, therefore be difficult to realize mass-producing preparation.
Summary of the invention
For above-mentioned existing technologies problem; the invention provides a kind of simple, the easy-operating method preparing graphene oxide and Graphene of technique; preparation condition to quality product and yield impact relatively little, quality product and productive rate be easy to control, be applicable to large-scale production.
The present invention solves the problems of the technologies described above taked technical scheme: the preparation method of a kind of graphene oxide and Graphene, comprises the following steps:
A1. the preparation method of graphene oxide: graphite raw material, solvent and oxygenant are mixed, be placed in closed reaction vessel, stirring reaction 0.5 ~ 6h at 40 ~ 120 DEG C, after decompression, suction filtration, washing, by overanxious thing vacuum-drying, grinding.
A2. secondary oxidation: dried product is dispersed in deionized water, oxygenant is added under acidic conditions, in 0 ~ 4 DEG C of stirring reaction 1 ~ 4h, be warming up to 20 ~ 40 DEG C of stirring reaction 1 ~ 2h, by reacted suspension liquid separating-purifying, be scattered in spraying dry in deionized water and be graphene oxide.
B. the preparation method of Graphene: by graphene oxide ultrasonic disperse in deionized water, add after reductive agent carries out reduction reaction, washing drying treatment obtains Graphene.
As preferably, described graphite raw material is crystalline flake graphite, Graphite Powder 99 or expanded graphite.
As preferably, described solvent is the vitriol oil, and the weight ratio of the vitriol oil and graphite raw material is 10 ~ 50:1.。
As preferably, oxygenant described in a1 is potassium permanganate, and the weight ratio of described potassium permanganate and graphite raw material is 3 ~ 8:1; Oxygenant described in a2 is potassium permanganate and hydrogen peroxide, the weight ratio of described potassium permanganate and graphite raw material is 1 ~ 4:1, the weight ratio of described hydrogen peroxide and graphite raw material is the weight ratio of deionized water and graphite raw material described in 5 ~ 10:1, a2 is 100 ~ 1000:1.
Described in a2, separating-purifying process is: under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring 5 ~ 10min, remove supernatant liquid, repeat to add deionized water and centrifugal process 1 ~ 2 time, get sediment and add dehydrated alcohol, after stirring 5 ~ 10min, carry out centrifugal settling, get after sediment repeats absolute ethanol washing 1 ~ 2 time, by sediment drying treatment.
As preferably, described centrifugal rotational speed is 4500 ~ 6000r/min, and the time is 3 ~ 8min.
As preferably, described reductive agent is NaOH, KOH or hydrazine hydrate.
As preferably, the mass ratio of reductive agent and graphene oxide is 1 ~ 4:1.
Compared with prior art, the advantage that technical scheme of the present invention possesses: invention also provides Graphene and as the preparation method of graphene oxide preparing Graphene raw material, simple and the easy handling of technique, the selection and comparison of supplementary material is common, is applicable to large-scale production; In the preparation process of graphene oxide of the present invention, twice oxidising process makes the oxidized extent of exfoliation of graphite darker; Separation and purification process can obtain the graphite oxide of very high purity, and finally obtains high-quality graphene oxide and Graphene.
Embodiment
A preparation method for graphene oxide and Graphene, comprises the following steps:
A1. graphene oxide is prepared: graphite raw material, solvent and oxygenant are mixed, be placed in closed reaction vessel, stirring reaction 0.5 ~ 6h at 40 ~ 120 DEG C, after decompression, suction filtration, washing, by overanxious thing vacuum-drying, grinding.
A2. secondary oxidation: dried product is dispersed in deionized water, oxygenant is added under acidic conditions, in 0 ~ 4 DEG C of stirring reaction 1 ~ 4h, be warming up to 20 ~ 40 DEG C of stirring reaction 1 ~ 2h, by reacted suspension liquid separating-purifying, be scattered in spraying dry in deionized water and be graphene oxide.
B. the preparation method of Graphene: by graphene oxide ultrasonic disperse in deionized water, add after reductive agent carries out reduction reaction, washing drying treatment obtains Graphene.
The process that the present invention prepares graphene oxide is divided into two steps, comprises twice oxidation, can make graphite deep oxidation and stripping.
Described graphite raw material can be crystalline flake graphite, Graphite Powder 99 or expanded graphite, preferred expanded graphite or 30 ~ 1000 object Graphite Powder 99s, because intumesced graphite structure loosens, graphite powder particle is comparatively thin, and this is all conducive to oxidation and the stripping of graphite.
Described solvent is the vitriol oil, and the weight ratio of the vitriol oil and graphite raw material is 10 ~ 50:1.
Oxygenant described in a1 is potassium permanganate, and the weight ratio of described potassium permanganate and graphite raw material is 3 ~ 8:1, and in the solution of the vitriol oil, the oxygenizement of potassium permanganate is very strong, can graphite oxide comparatively thoroughly; Oxygenant described in a2 is potassium permanganate and hydrogen peroxide, the weight ratio of described potassium permanganate and graphite raw material is 1 ~ 4:1, the weight ratio of described hydrogen peroxide and graphite raw material is the weight ratio of deionized water and graphite raw material described in 5 ~ 10:1, a2 is 100 ~ 1000:1.
The detailed process of secondary oxidation is: by dried product ultrasonic disperse in a small amount of deionized water, the amount of deionized water and the weight ratio of graphite raw material are 10 ~ 30:1, adding hydrochloric acid or sulfuric acid regulates PH to be less than 3, add potassium permanganate in 0 ~ 4 DEG C of stirring reaction 1 ~ 4h, add hydrogen peroxide, be warming up to 20 ~ 40 DEG C of stirring reaction 1 ~ 2h, by reacted suspension liquid separating-purifying, be scattered in spraying dry in deionized water.
Described in a2, separating-purifying process is: under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring 5 ~ 10min, remove supernatant liquid, repeat to add deionized water and centrifugal process 1 ~ 2 time, get sediment and add dehydrated alcohol, after stirring 5 ~ 10min, carry out centrifugal settling, get after sediment repeats absolute ethanol washing 1 ~ 2 time, by sediment drying treatment.
Described sepn process can obtain the very high oxidation graphite solid of purity, and the solid-liquid separation adopting dehydrated alcohol centrifuge washing to overcome to exist in water washing process is difficult and wash halfway problem.
Described centrifugal rotational speed is 4500 ~ 6000r/min, and the time is 3 ~ 8min.
Described reductive agent is NaOH, KOH or hydrazine hydrate, and the mass ratio of reductive agent and graphene oxide is 1 ~ 4:1.
Solution after reduction reaction is filtered, gets filtrate and do microwave heating treatment, after process, cool pickling, washing filtering, filtrate drying be Graphene.
Below in conjunction with specific embodiment, the preparation method to a kind of graphene oxide of the present invention and Graphene is described further:
Embodiment 1:
The preparation method of graphene oxide: get 1 part of Graphite Powder 99 and mix with 10 parts of vitriol oils and 3 parts of potassium permanganate as graphite raw material, be placed in closed reaction vessel, stirring reaction 6h under 40 DEG C of condition of water bath heating, after decompression, suction filtration, washing, by overanxious thing vacuum-drying, grinding.By the product ultrasonic disperse after drying and grinding in 10 parts of deionized waters, adding hydrochloric acid regulates PH to be less than 3, add 1 part of potassium permanganate in 0 DEG C of stirring reaction 4h, add 5 parts of hydrogen peroxide, be warming up to 20 DEG C of stirring in water bath reaction 2h, by reacted suspension liquid separating-purifying, be scattered in spraying dry in deionized water and namely obtain graphene oxide, above-mentioned number is weight part.
The process of above-mentioned separating-purifying is specially: under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring 5min, remove supernatant liquid, repeat to add deionized water and centrifugal process 1 time, get sediment and add dehydrated alcohol, after stirring 5min, carry out centrifugal settling, get after sediment repeats absolute ethanol washing 1 time, by sediment drying treatment.Above-mentioned centrifugal condition is: 4500r/min, centrifugal 3min.
The preparation method of Graphene: get 1 part of graphene oxide ultrasonic disperse in deionized water, add after 1 part of reductive agent NaOH carries out reduction reaction, solution after reduction reaction is filtered, get filtrate and do microwave heating treatment, after process, cool pickling, washing filtering, filtrate drying be Graphene.Described number is weight part.
Embodiment 2:
The preparation method of graphene oxide: get 1 part of crystalline flake graphite and mix with 50 parts of vitriol oils and 8 parts of potassium permanganate as graphite raw material, be placed in closed reaction vessel, stirring reaction 0.5h under 120 DEG C of oil bath heating conditions, after decompression, suction filtration, washing, by overanxious thing vacuum-drying, grinding.By the product ultrasonic disperse after drying and grinding in 30 parts of deionized waters, adding sulfuric acid regulates PH to be less than 3, add 4 parts of potassium permanganate in 4 DEG C of stirring reaction 1h, add 10 parts of hydrogen peroxide, be warming up to 40 DEG C of stirring in water bath reaction 1h, by reacted suspension liquid separating-purifying, be scattered in spraying dry in deionized water and namely obtain graphene oxide, above-mentioned number is weight part.
The process of above-mentioned separating-purifying is specially: under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring 10min, remove supernatant liquid, repeat to add deionized water and centrifugal process 2 times, get sediment and add dehydrated alcohol, after stirring 10min, carry out centrifugal settling, get after sediment repeats absolute ethanol washing 2 times, by sediment drying treatment.Above-mentioned centrifugal condition is: 6000r/min, centrifugal 8min.
The preparation method of Graphene: get 1 part of graphene oxide ultrasonic disperse in deionized water, add after 4 parts of reductive agent KOH carry out reduction reaction, solution after reduction reaction is filtered, gets filtrate and do microwave heating treatment, after process, cool pickling, washing filtering, filtrate drying be Graphene.Described number is weight part.
Embodiment 3:
The preparation method of graphene oxide: get 1 part of expanded graphite and mix with 30 parts of vitriol oils and 5 parts of potassium permanganate as graphite raw material, be placed in closed reaction vessel, stirring reaction 2h under 80 DEG C of condition of water bath heating, after decompression, suction filtration, washing, by overanxious thing vacuum-drying, grinding.By the product ultrasonic disperse after drying and grinding in 20 parts of deionized waters, adding sulfuric acid regulates PH to be less than 3, add 3 parts of potassium permanganate in 2 DEG C of stirring reaction 2.5h, add 7 parts of hydrogen peroxide, be warming up to 30 DEG C of stirring in water bath reaction 2h, by reacted suspension liquid separating-purifying, be scattered in spraying dry in deionized water and namely obtain graphene oxide, above-mentioned number is weight part.
The process of above-mentioned separating-purifying is specially: under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring 7min, remove supernatant liquid, repeat to add deionized water and centrifugal process 1 time, get sediment and add dehydrated alcohol, after stirring 9min, carry out centrifugal settling, get after sediment repeats absolute ethanol washing 2 times, by sediment drying treatment.Above-mentioned centrifugal condition is: 5200r/min, centrifugal 7min.
The preparation method of Graphene: get 1 part of graphene oxide ultrasonic disperse in deionized water, add after 3 parts of reductive agent hydrazine hydrates carry out reduction reaction, solution after reduction reaction is filtered, get filtrate and do microwave heating treatment, after process, cool pickling, washing filtering, filtrate drying be Graphene.Described number is weight part.
It should be noted that embodiment cited by the present invention and raw material are only and be comparatively applicable to method under condition and raw material, simple modification done under the prerequisite not departing from design of the present invention and principle or amendment all will fall within the scope of protection of the present invention.
Claims (8)
1. a preparation method for graphene oxide and Graphene, is characterized in that comprising the following steps:
A1. the preparation method of graphene oxide: graphite raw material, solvent and oxygenant are mixed, is placed in closed reaction vessel, stirring reaction 0.5 ~ 6h at 40 ~ 120 DEG C, after decompression, suction filtration, washing, by overanxious thing vacuum-drying, grinding;
A2. secondary oxidation: dried product is dispersed in deionized water, oxygenant is added under acidic conditions, in 0 ~ 4 DEG C of stirring reaction 1 ~ 4h, be warming up to 20 ~ 40 DEG C of stirring reaction 1 ~ 2h, by reacted suspension liquid separating-purifying, be scattered in spraying dry in deionized water and be graphene oxide;
B. the preparation method of Graphene: by graphene oxide ultrasonic disperse in deionized water, add after reductive agent carries out reduction reaction, washing drying treatment obtains Graphene.
2. the preparation method of a kind of graphene oxide according to claim 1 and Graphene, is characterized in that: described graphite raw material is crystalline flake graphite, Graphite Powder 99 or expanded graphite.
3. the preparation method of a kind of graphene oxide according to claim 1 and Graphene, is characterized in that: described solvent is the vitriol oil, and the weight ratio of the vitriol oil and graphite raw material is 10 ~ 50:1.
4. the preparation method of a kind of graphene oxide according to claim 1 and Graphene, is characterized in that: oxygenant described in a1 is potassium permanganate, and the weight ratio of described potassium permanganate and graphite raw material is 3 ~ 8:1; Oxygenant described in a2 is potassium permanganate and hydrogen peroxide, the weight ratio of described potassium permanganate and graphite raw material is 1 ~ 4:1, the weight ratio of described hydrogen peroxide and graphite raw material is the weight ratio of deionized water and graphite raw material described in 5 ~ 10:1, a2 is 100 ~ 1000:1.
5. the preparation method of a kind of graphene oxide according to claim 1 and Graphene, it is characterized in that: described in a2, separating-purifying process is: under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring 5 ~ 10min, remove supernatant liquid, repeat to add deionized water and centrifugal process 1 ~ 2 time, get sediment and add dehydrated alcohol, after stirring 5 ~ 10min, carry out centrifugal settling, get after sediment repeats absolute ethanol washing 1 ~ 2 time, by sediment drying treatment.
6. the preparation method of a kind of graphene oxide according to claim 5 and Graphene, is characterized in that: described centrifugal rotational speed is 4500 ~ 6000r/min, and the time is 3 ~ 8min.
7. the preparation method of a kind of graphene oxide according to claim 1 and Graphene, is characterized in that: described reductive agent is NaOH, KOH or hydrazine hydrate.
8. a kind of graphene oxide according to claim 1 or 7 and the preparation method of Graphene, is characterized in that: the mass ratio of reductive agent and graphene oxide is 1 ~ 4:1.
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Cited By (21)
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| 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 |
| CN105218872A (en) * | 2015-09-30 | 2016-01-06 | 苏州蔻美新材料有限公司 | A kind of modified chitosan class antibiotic material in medical use and preparation method thereof |
| CN105218871A (en) * | 2015-08-26 | 2016-01-06 | 苏州卓伟企业管理咨询有限公司 | A kind of preparation method of reduced graphene/Chitosan Composites |
| CN105217621A (en) * | 2015-10-30 | 2016-01-06 | 浙江理工大学 | A kind of graphene oxide preparation method of size uniformity |
| CN105271198A (en) * | 2015-11-04 | 2016-01-27 | 宋明智 | Preparation of graphene oxide and preparation of graphene |
| CN106315565A (en) * | 2016-08-10 | 2017-01-11 | 安徽省宁国天成电工有限公司 | Graphene for temperature sensor and preparation method of graphene |
| CN106450331A (en) * | 2016-10-27 | 2017-02-22 | 萝北奥星新材料有限公司 | Method for preparing graphene conducting agent slurry from graphite tailings |
| CN106477573A (en) * | 2016-09-22 | 2017-03-08 | 西北师范大学 | A kind of preparation method with colored fascicular texture graphite oxide |
| WO2017084561A1 (en) * | 2015-11-16 | 2017-05-26 | 复旦大学 | Preparation method for large-size graphene oxide or graphene |
| CN107398265A (en) * | 2017-08-09 | 2017-11-28 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method based on graphene oxide catalysis material |
| CN107585765A (en) * | 2017-10-12 | 2018-01-16 | 南京旭羽睿材料科技有限公司 | A kind of preparation method of graphene or graphene oxide |
| CN107777683A (en) * | 2017-11-20 | 2018-03-09 | 浙江海虹控股集团有限公司 | A kind of new method for producing graphene oxide |
| CN108440286A (en) * | 2018-04-18 | 2018-08-24 | 肖锦 | A kind of method for preparing acetylsalicylic acid |
| CN108440285A (en) * | 2018-04-18 | 2018-08-24 | 肖锦 | A kind of synthetic method of acetylsalicylic acid |
| CN110606481A (en) * | 2019-11-08 | 2019-12-24 | 陕西科技大学 | Few-lamellar graphene oxide dispersion liquid and preparation method thereof |
| CN111892043A (en) * | 2020-08-06 | 2020-11-06 | 昆明理工大学 | Method for preparing reduced graphene oxide by one-pot method |
| CN112048219A (en) * | 2020-09-14 | 2020-12-08 | 多凌新材料科技股份有限公司 | Water-based high-conductivity graphene printing ink and preparation method thereof |
| CN112300857A (en) * | 2020-11-19 | 2021-02-02 | 马鞍山市三川机械制造有限公司 | Preparation method of wear-resistant lubricating oil |
| CN112374493A (en) * | 2020-12-28 | 2021-02-19 | 中国科学技术大学先进技术研究院 | Method for preparing monolayer graphene oxide with controllable sheet diameter size |
| CN115317382A (en) * | 2022-08-11 | 2022-11-11 | 封涛 | Preparation method of dopamine-mediated graphene functional hair dye |
| CN116496086A (en) * | 2023-04-10 | 2023-07-28 | 广西强强碳素股份有限公司 | Preparation method of pollution-free prebaked anode |
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Application publication date: 20150304 |