CN102718209A - Method for preparing graphene based on reduction of divalent iron ion - Google Patents
Method for preparing graphene based on reduction of divalent iron ion Download PDFInfo
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Abstract
The invention relates to a method for preparing graphene based on reduction of divalent iron ion, and belongs to the technical field of materials. According to the method, a divalent iron ion salt is used as a reducing agent of graphene oxide, and the graphene oxide can be efficiently reduced in an alkaline environment and an inert protective atmosphere at room temperature to prepare the graphene. Compared with the traditional method for preparing the grapheme, the used reducing agent is green, safe, efficient and cheap, and has a significant industrial value.
Description
Technical field
The invention belongs to the material technology field, relate to the carbon nanomaterial technology of preparing, particularly graphene preparation method.
Background technology
Graphene (Graphene) is the two-dimentional carbon atom crystal of monatomic thickness, is considered to constitute the basic structural unit of soccerballene, carbon nanotube and graphite.Grapheme material has some advantageous properties of materials such as graphite and carbon nanotube concurrently, like outstanding heat conductivility, mechanical property and outstanding electron transport performance etc.The excellent properties that Graphene and graphene-based nano composite material showed makes it have important application prospects in fields such as lithium ion cell electrode, electrode of super capacitor, gas sensor, field emmision materials.
Efficiently, green, cheap graphene preparation method is the prerequisite of Graphene and further investigation of graphene-based nano composite material performance and widespread use.The main preparation methods of Graphene has micromechanical forces to peel off (Novoselov KS, Geim AK, Morozov SV, et al.Science.2004 at present; 306 (5696): 666-9), chemical vapour deposition (Kim KS, Zhao Y, Jang H; Et al.Nature.2009,457 (7230): 706-10), oriented growth (Forbeaux I, Themlin JM; Debever JM.Physical Review B.1998,58 (24): 16396-406), graphene oxide chemical reduction (Stankovich S, Dikin DA; Piner RD, et al.Carbon.2007,45 (7): method such as 1558-65).Micromechanical forces is peeled off, chemical vapour deposition and oriented growth preparation method owing to complicated operation, condition is harsh, yielding poorly is not suitable for large-scale commercial applications production, so the graphene oxide chemical reduction method is considered to most possibly realize the extensive cheap effective ways of producing of Graphene.The graphene oxide chemical reduction at first is raw material with the crystalline flake graphite, and (Graphene oxide GO), is reduced to Graphene through certain reduction reaction with graphene oxide again through obtaining graphene oxide after strong oxidizer oxidation, the supersound process.The advantage of this method is that energy consumption is low; The preparation process is simple; The Graphene productive rate is high, and the Graphene that obtains is prone to be scattered in water, the pure equal solvent, therefore is easy to be applied to prepare lithium ion cell electrode, electrode of super capacitor and other graphene-based matrix materials.The reductive agent that is used for redox graphene at present mainly contains Hydrazine Hydrate 80, dimethylhydrazine, Peng Qinghuana, quinhydrones etc., but this type reductive agent is owing to characteristics such as easy blast in high poison and the use are not suitable in extensive graphene oxide reduction process, using.Other novel reductive agent such as nanometer iron powder, aluminium powder, (Chinese patent though ZL200910054919.8) wait and to have eco-friendly characteristics, costs an arm and a leg xitix, makes that production cost is too high and is unfavorable for that large-scale industrialization uses.
Technology contents
The present invention proposes a kind of safe, efficient, cheap graphene preparation method; This method adopts the reductive agent of ferrous ion salt as graphene oxide; Under alkaline environment, inert protective atmosphere and room temperature, can realize efficient reduction, prepare Graphene graphene oxide.Present method is compared with existing graphene preparation method, and the reductive agent system of employing is green, safe, efficient, cheap, has significant industrial application value.
Technical scheme of the present invention is following:
A kind of based on ferrous ion reductive graphene preparation method, may further comprise the steps:
Step 1: the colloidal suspensions of preparation graphene oxide.
In natural flake graphite or high oriented graphite powder of pyrolysis and strong oxidizer adding strongly acidic solution; After mixing system temperature is risen to 35 ~ 45 ℃; Continue to stir after 1 ~ 3 hour and add deionized water; Make system temperature rise to 80 ~ 100 ℃ and kept 1 hour, reaction finishes the back and drips a certain amount of H
2O
2, stop to stir standing demix, take off layer graphite oxide suspension-s and carry out pickling, washing successively until removing various gritty particles, after ultrasonic agitation is handled the individual layer of realizing graphene oxide and peeled off, obtain the graphene oxide colloidal suspensions.
Step 2: the preparation of Graphene.
Detailed process is: in reaction solvent; The graphene oxide colloidal suspensions that adds the step 1 preparation adds basic soln under stirring and regulates pH to 10 ~ 13, adds the compound of ferrous ion under the inert protective atmosphere; Stirring reaction under-10 ~ 50 ℃ temperature of reaction; Reaction finishes the back solid-liquid separation, and separating obtained solid is used Hydrogen chloride, deionized water wash repeatedly successively, promptly obtains Graphene after the drying.
Or: in reaction solvent; The graphene oxide colloidal suspensions that adds the step 1 preparation, the compound of adding ferrous ion under the inert protective atmosphere adds basic soln under stirring and regulates pH to 10 ~ 13; Stirring reaction under-10 ~ 50 ℃ temperature of reaction; Reaction finishes the back solid-liquid separation, and separating obtained solid is used Hydrogen chloride, deionized water wash repeatedly successively, promptly obtains Graphene after the drying.
In the technique scheme: 1, the compound of said ferrous ion comprises inorganic salt (as: one or more in iron protochloride, ferrous sulfate, Iron nitrate, iron protocarbonate or the ferrous phosphate) or the organic salt (as: one or more in Ferrox, Iron diacetate or the yellow prussiate of potash) that contains ferrous ion; 2, said inert protective atmosphere is by one or more realizations in nitrogen, argon gas or the helium; 3, basic soln described in the step 2 is one or more in ammoniacal liquor, sodium hydroxide, Pottasium Hydroxide or the sodium ethylate aqueous solution; 4, temperature of reaction described in the step 2 is preferably 0 ~ 25 ℃, 10 seconds ~ 24 hours reaction times (being preferably 60 seconds ~ 2 hours); 5, reaction solvent described in the step 2 is one or more (preferably water, methyl alcohol or the ethanol) in water, alcohol, acetone and the N; 6, strongly acidic solution described in the step 1 is one or more in the vitriol oil, oleum, concentrated nitric acid or the nitrosonitric acid; 7, strong oxidizer described in the step 1 is one or more in potassium permanganate, Potcrate or the SRM 935a.
Essence of the present invention is to utilize the ferrous ion redox graphene; Add alkaline matter (solution) and ferrous ion salt (solution) or ferrous ion salt (solution) and alkaline matter (solution) successively to the graphene oxide colloidal suspensions; Under the condition that hydroxide radical exists, ferrous ion obtains Graphene as reductive agent and graphite oxide alkene reaction.
The used compound that contains ferrous ion is common cheap common reagent in above-mentioned preparation process, though the reductibility of ferrous ion in acidity or neutral environment very a little less than, its reducing power is not enough to realize the height reduction of Graphene; But the reductibility of ferrous ion in alkaline environment can strengthen greatly; This is because the ferrous hydroxide that ferrous ion and hydroxide radical generate is a strong reductant; Because ferrous hydroxide very easily is oxidized to ironic hydroxide by dissolved oxygen molecule in the solution or airborne oxygen, so the inert reaction environment that adopts shielding gas to provide is realized the height reduction of ferrous hydroxide to Graphene.
Have following remarkable advantage according to present method synthetic graphene nano material: (1) the present invention uses the method for ferrous ion redox graphene to prepare Graphene first; This method has been accelerated reduction rate; Reduced reduction temperature; Simple to operate, help the batch process of high quality Graphene; (2) as reductive agent, with respect to having toxic hydrazine reducing agent, ferrous ion is green fully reductive agent with the ferrous ion compound in the present invention; With respect to reductive agent nanometer iron powder, aluminium powder or the benzoquinones of costliness, the ferrous ion compound is an industrial chemicals cheap and easy to get; (3) Graphene in prepared the be scattered in solution of the present invention can be widely used in lithium ion battery electrode material, in the industrialization products such as electrode material for super capacitor.
Figure of description
Fig. 1 is a schematic flow sheet of the present invention.
Fig. 2 is the infrared spectrum of prepared graphene of the present invention and graphene oxide.
Fig. 3 is the X ray diffracting spectrum of prepared graphene of the present invention and graphene oxide.
Fig. 4 is the thermogravimetric analysis collection of illustrative plates of prepared graphene of the present invention and graphene oxide.
Embodiment
Embodiment 1: Presfersul prepares Graphene as the reductive agent redox graphene.
(1) preparation of graphene oxide: in three mouthfuls of round-bottomed flasks, add the 55ml vitriol oil; Add 1g natural flake graphite and 7g potassium permanganate then successively; Mix, system temperature is risen to 35 ~ 45 ℃, continue to stir adding 100ml deionized water after 1 ~ 3 hour; Make system temperature rise to 80 ~ 100 ℃ and kept 1 hour, reaction finishes back Dropwise 5 mlH in reaction system
2O
2Stop to stir standing demix; Take off layer graphite oxide suspension-s and carry out pickling, washing successively until removing various gritty particles; Utilize operating frequency to be 40kHz then, ultrasonic power is that the individual layer that the ultrasonic device of 350W carries out ultrasonic agitation processing realization graphene oxide to the graphite oxide colloidal suspensions peels off, thereby obtains the graphene oxide colloidal suspensions.
(2) preparation of Graphene: under the room temperature, configuration 50mL, 0.5mg/mL graphite oxide aqueous solution; Place the 150mL Erlenmeyer flask; Making in the Erlenmeyer flask with the interior oxygen of Erlenmeyer flask in the feeding nitrogen eliminating solution is oxygen-free atmosphere, and elder generation adds 20mL ammoniacal liquor, adds the 2.5g Presfersul then.Fully stir 10min, reaction finishes after-filtration and uses 200ml Hydrogen chloride and 500ml deionized water wash successively repeatedly, promptly obtains Graphene behind the solid drying.
Resultant Graphene can stable dispersion in solution such as water, ethanol, N, show the dispersed fine of Graphene.The infrared spectrum of resultant Graphene (referring to Fig. 2) shows that graphene oxide oxy radical after reduction is all sloughed basically, has formed Graphene lamella structure.Adopt X ray polycrystalline diffractometer that the product of gained is carried out material phase analysis, X ray diffracting spectrum (referring to Fig. 3) shows the reduction through ferrous ion, and graphene oxide has been reduced into Graphene, is characterized as (002) diffraction peak that about 26 degree, occurs.Thermogravimetric analysis collection of illustrative plates (referring to Fig. 4) by graphene oxide and Graphene can find out that after graphene oxide was reduced into Graphene, most of oxy radical was removed, makes Graphene have extraordinary thermostability.
2: two oxalic acid hydrates of embodiment are ferrous to prepare Graphene as the reductive agent redox graphene.
(1) preparation of graphene oxide: referring to embodiment 1 step (1).
(2) preparation of Graphene: under the room temperature, configuration 50mL, 1mg/mL graphite oxide aqueous solution; Place the 150mL Erlenmeyer flask; Feed nitrogen get rid of in the solution with Erlenmeyer flask in oxygen make and be oxygen-free atmosphere in the Erlenmeyer flask, add 20mL ammoniacal liquor earlier, it is ferrous to add 2.0g two oxalic acid hydrates then.Fully stir 60min, reaction finishes after-filtration and uses 200ml Hydrogen chloride and 500ml deionized water wash successively repeatedly, promptly obtains Graphene behind the solid drying.
Embodiment 3: Iron dichloride tetrahydrate prepares Graphene as the reductive agent redox graphene.
(1) preparation of graphene oxide: referring to embodiment 1 step (1).
(2) preparation of Graphene: under the room temperature; Configuration 50mL; 1mg/mL graphene oxide ethanolic soln places the 150mL Erlenmeyer flask, and making in the Erlenmeyer flask with the interior oxygen of Erlenmeyer flask in the feeding argon gas eliminating solution is oxygen-free atmosphere; Add 2g sodium hydrate solid powder earlier, add the 4.0g Iron dichloride tetrahydrate then.Fully stir 30min, reaction finishes after-filtration and uses 200ml Hydrogen chloride and 500ml deionized water wash successively repeatedly, promptly obtains Graphene behind the solid drying.
Above embodiments of the invention have been done detailed description, embodiment is being to have provided detailed embodiment and concrete operating process under the prerequisite with technical scheme of the present invention, but protection scope of the present invention is not limited to the above embodiments.
Claims (10)
1. one kind based on ferrous ion reductive graphene preparation method, may further comprise the steps:
Step 1: the colloidal suspensions of preparation graphene oxide;
In natural flake graphite or high oriented graphite powder of pyrolysis and strong oxidizer adding strongly acidic solution; After mixing system temperature is risen to 35 ~ 45 ℃; Continue to stir after 1 ~ 3 hour and add deionized water; Make system temperature rise to 80 ~ 100 ℃ and kept 1 hour, reaction finishes the back and drips a certain amount of H
2O
2, stop to stir standing demix, take off layer graphite oxide suspension-s and carry out pickling, washing successively until removing various gritty particles, after ultrasonic agitation is handled the individual layer of realizing graphene oxide and peeled off, obtain the graphene oxide colloidal suspensions.
Step 2: the preparation of Graphene;
Detailed process is: the graphene oxide colloidal suspensions of getting the step 1 preparation; Stir and add basic soln adjusting pH to 10 ~ 13 down; The compound that adds ferrous ion under the inert protective atmosphere, stirring reaction under-10 ~ 50 ℃ temperature of reaction, reaction finishes the back solid-liquid separation; Separating obtained solid is used Hydrogen chloride, deionized water wash repeatedly successively, promptly obtain Graphene after the drying.
Or: the graphene oxide colloidal suspensions of getting the step 1 preparation; The compound that adds ferrous ion under the inert protective atmosphere; Stir adding basic soln adjusting pH to 10 ~ 13 down, stirring reaction under-10 ~ 50 ℃ temperature of reaction, reaction finishes the back solid-liquid separation; Separating obtained solid is used Hydrogen chloride, deionized water wash repeatedly successively, promptly obtain Graphene after the drying.
2. according to claim 1ly it is characterized in that based on ferrous ion reductive graphene preparation method the compound of said ferrous ion comprises inorganic salt or the organic salt that contains ferrous ion.
3. according to claim 2ly it is characterized in that based on ferrous ion reductive graphene preparation method the said inorganic salt that contain ferrous ion are one or more in iron protochloride, ferrous sulfate, Iron nitrate, iron protocarbonate or the ferrous phosphate; The said organic salt that contains ferrous ion is one or more in Ferrox, Iron diacetate or the yellow prussiate of potash.
4. according to claim 1ly it is characterized in that based on ferrous ion reductive graphene preparation method said inert protective atmosphere is by one or more realizations in nitrogen, argon gas or the helium.
5. according to claim 1ly it is characterized in that based on ferrous ion reductive graphene preparation method basic soln described in the step 2 is one or more in ammoniacal liquor, sodium hydroxide, Pottasium Hydroxide or the sodium ethylate aqueous solution.
6. according to claim 1ly it is characterized in that based on ferrous ion reductive graphene preparation method temperature of reaction described in the step 2 is 0 ~ 25 ℃, the reaction times is 10 seconds ~ 24 hours.
7. according to claim 6ly it is characterized in that based on ferrous ion reductive graphene preparation method, the reaction times described in the step 2 is preferably 60 seconds ~ and 2 hours.
8. according to claim 1ly it is characterized in that based on ferrous ion reductive graphene preparation method reaction solvent described in the step 2 is one or more in water, alcohol, acetone and the N.
9. according to claim 1ly it is characterized in that based on ferrous ion reductive graphene preparation method strongly acidic solution described in the step 1 is one or more in the vitriol oil, oleum, concentrated nitric acid or the nitrosonitric acid.
10. according to claim 1ly it is characterized in that based on ferrous ion reductive graphene preparation method strong oxidizer described in the step 1 is one or more in potassium permanganate, Potcrate or the SRM 935a.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JP2015048302A (en) * | 2013-08-29 | 2015-03-16 | インダストリー−アカデミック コーペレイション ファウンデイション， ヨンセイ ユニバーシティ | Method for synthesizing graphene-based nano composite material, and graphene-based nano composite material synthesized using the method |
| CN105271214A (en) * | 2015-11-25 | 2016-01-27 | 合肥国轩高科动力能源有限公司 | Oxidation-reduction preparation method for graphene |
| EP2982974A1 (en) * | 2014-08-06 | 2016-02-10 | Martechnic GmbH | Method of determining the iron content in a lubricating oil |
| CN105838115A (en) * | 2016-04-27 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for preparing graphene-based conductive pearlescent pigment |
| CN113233448A (en) * | 2021-06-10 | 2021-08-10 | 北京航空航天大学 | Surface modification method for reduced graphene oxide |
| CN113402946A (en) * | 2021-05-26 | 2021-09-17 | 广州盛门新材料科技有限公司 | High-molecular light-reflecting coating and preparation method thereof |
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| CN101941842A (en) * | 2010-10-11 | 2011-01-12 | 东华大学 | Method for preparing graphene loaded ferroferric oxide magnetic nanometer particle composite material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JP2015048302A (en) * | 2013-08-29 | 2015-03-16 | インダストリー−アカデミック コーペレイション ファウンデイション， ヨンセイ ユニバーシティ | Method for synthesizing graphene-based nano composite material, and graphene-based nano composite material synthesized using the method |
| EP2982974A1 (en) * | 2014-08-06 | 2016-02-10 | Martechnic GmbH | Method of determining the iron content in a lubricating oil |
| CN105271214A (en) * | 2015-11-25 | 2016-01-27 | 合肥国轩高科动力能源有限公司 | Oxidation-reduction preparation method for graphene |
| CN105838115A (en) * | 2016-04-27 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for preparing graphene-based conductive pearlescent pigment |
| CN105838115B (en) * | 2016-04-27 | 2018-03-06 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of graphene-based Electro-conductive pearlescent pigment |
| CN113402946A (en) * | 2021-05-26 | 2021-09-17 | 广州盛门新材料科技有限公司 | High-molecular light-reflecting coating and preparation method thereof |
| CN113233448A (en) * | 2021-06-10 | 2021-08-10 | 北京航空航天大学 | Surface modification method for reduced graphene oxide |
| CN113233448B (en) * | 2021-06-10 | 2022-04-08 | 北京航空航天大学 | Surface modification method for reduced graphene oxide |
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