CN107720742A - It is a kind of to use the graphene oxide preparation method containing hydrogen peroxide catalyzed system - Google Patents
It is a kind of to use the graphene oxide preparation method containing hydrogen peroxide catalyzed system Download PDFInfo
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Abstract
The invention belongs to graphene sciemtifec and technical sphere, and in particular to a kind of preparation method of graphene oxide.A kind of preparation method of graphene oxide of the present invention, is comprised the following steps that：（1）Pretreatment of raw material：After graphite and deionization are well mixed, regulation system pH value, temperature reaction, acidic mixed material is obtained；（2）Oxidation：After acidic mixed material is cooled, addition Fenton reagent, deionized water are reacted, and it is graphite solution to obtain oxidation；（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；（4）Ultrasound：By step（3）Resulting solution is diluted, and ultrasound, freeze-drying obtains graphene oxide product.The preparation method of graphene oxide of the present invention a kind of is simple to operate, mild condition and pollution-free, and the graphene oxide individual layer rate of preparation is high.
Description
Technical field
The present invention relates to technical field of graphene, and in particular to a kind of graphene oxide preparation method.
Technical background
Graphene is with sp by carbon atom2The cellular flat film that hydridization form is formed, only an atomic layer level thickness
Quasi- two-dimensional material, also known as monoatomic layer graphite.The design feature of graphene, make it have good intensity, it is flexible, lead
The performances such as electricity, heat conduction, optics, are widely used in every field.Graphene oxide is the oxide of graphene, has higher ratio
The functional group that surface area and surface are enriched.At present, the preparation method of graphene oxide is mainly improved hummer methods etc.,
The methods of hummer, all employ the strong oxidizers such as the strong acid such as the concentrated sulfuric acid, perchloric acid, concentrated nitric acid and potassium permanganate in preparing.So that
Preparation process danger is high, seriously polluted, cost is high, and preparation process is cumbersome, less efficient.
The content of the invention
In order to solve the above-mentioned technical problem, the present invention provides a kind of using the graphene oxide containing hydrogen peroxide catalyzed system
Preparation method.The preparation method of graphene oxide of the present invention, is comprised the following steps that：
（1）Pretreatment of raw material：After graphite and the aqueous solution are well mixed, regulation system pH value, heating, acidic mixture is obtained
Material；
（2）Oxidation：After acidic mixed material is cooled, add and reacted containing hydrogen peroxide catalyzed system, deionized water, obtained
Graphite oxide solution；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）Resulting solution is diluted, and ultrasound, freeze-drying obtains graphene oxide product.
Wherein：
Step（1）In, it is Fenton reagent or Fenton-type reagent containing hydrogen peroxide catalyzed system.
Step（1）In, described graphite is crystalline flake graphite either expanded graphite or pre-oxidation graphite.Because expanded graphite
Loose with preliminary oxidation graphite-structure, piece interlamellar spacing is larger, is advantageous to the progress of oxidation reaction, and lamella is easily peeled off.
Step（1）In, the scope of described pH value is 2 ~ 5.Preferably, pH value 3.
Step（1）In, described reaction temperature is 50 ~ 90 DEG C, and the reaction time is 1 ~ 8 h.
Step（2）In, described to be cooled to 30 ~ 70 DEG C, the reaction time is 2 ~ 24h.Reaction temperature is too high so that Fenton reagent
Bury in oblivion, influence the degree of oxidation of graphite；Reaction temperature is too low so that Fenton reagent or Fenton-type reagent utilization rate are low.
Step（2）In, described Fenton reagent is hydrogen peroxide（Hereinafter referred to as：H2O2）/ ferrous sulfate（Hereinafter referred to as：
FeSO4）System, H2O2With FeSO4Quality Wei 7:1~11:1；Described Fenton-type reagent is hydrogen peroxide and Fe3O4/β-
CD or Fe/Cu/HMS, Si/Al/@Fe/MWCNT or Fe3O4/ Al-Fe-P-B or CuFe2O4NPs or EGCG/Fe3O4Or β-
FeOOH/rGO or α-（Fe、Cu）OOH catalyst.Preferably, H2O2With FeSO4Quality Wei 8:1.
Step（2）In, the reaction system is under water bath condition or under the conditions of water-bath and ultra violet lamp or water-bath and super
Under the conditions of sound or under the conditions of electrochemical redox.Preferably, system reaction is under the conditions of water-bath and ultra violet lamp or water-bath
With under ultrasound condition or under the conditions of electrochemical redox.
Step（4）In, described graphite oxide diluted concentration is 0.5 ~ 2 g/L, and the ultrasonic time is 0.5 ~ 5 h.It is excellent
Choosing, the graphite oxide diluted concentration is 1 g/L.
The present invention compared with prior art, has the advantages that：
The green Fenton reagent that the present invention uses is oxidant, and reaction speed is fast, and reaction condition is gentle, and equipment is simple, and energy consumption is small,
Other impurities, the complete H of unreacted are not introduced in oxidizing process2O2It can voluntarily decompose, secondary pollution will not be caused.Fenton reagent produces
Hydroxyl radical free radical and carbon-carbon double bond addition reaction occurs, the network structure of graphene oxide is destroyed smaller, is advantageous to prepare
The high graphene of conductance；Hydroxyl radical free radical small volume, is easily inserted graphite flake layer, adds spacing between layers,
It is easy to prepare the high graphene oxide of individual layer rate.
Embodiment
Embodiment 1
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g crystalline flake graphites and deionization are well mixed, regulation system pH=4 are worth, and are warming up to 85 DEG C instead
1h is answered, obtains acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 60 DEG C, Fenton reagent, deionized water is added, 2 h is reacted under water-bath, are obtained
To graphite oxide solution, the Fenton reagent：H2O2With FeSO4Quality Wei 8:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 1 g/L, 1.5 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains aoxidizing stone
Black alkene product.
Embodiment 2
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g expanded graphites and deionization are well mixed, regulation system pH=3 are worth, and are warming up to 80 DEG C instead
1.5 h are answered, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 70 DEG C, Fenton reagent, deionized water is added, 1.5 h is reacted under water-bath,
Obtain graphite oxide solution, the Fenton reagent：H2O2With FeSO4Quality Wei 8:1.5；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 1.5 g/L, 3 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains aoxidizing stone
Black alkene product.
Embodiment 3
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g pre-oxidation graphite and deionization are well mixed, regulation system pH=5 are worth, and are warming up to 90 DEG C
2h is reacted, obtains acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 50 DEG C, Fenton reagent, deionized water is added, reacts 24h under water-bath, obtain
To graphite oxide solution, the Fenton reagent：H2O2With FeSO4Quality Wei 10:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 0.5 g/L, 2 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains aoxidizing stone
Black alkene product.
Embodiment 4
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g expanded graphites and deionization are well mixed, regulation system pH=3 are worth, and are warming up to 90 DEG C instead
2 h are answered, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 50 DEG C, Fenton reagent, deionized water are added, in water-bath and 185 ~ 250nm
3 h are reacted under ultra violet lamp, obtain graphite oxide solution, the Fenton reagent：H2O2With FeSO4Quality Wei 8:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 0.5 g/L, 1.5 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying is aoxidized
Graphene product.
Embodiment 5
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g expanded graphites and deionization are well mixed, regulation system pH=3 are worth,
90 DEG C of 2 h of reaction are warming up to, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 50 DEG C, Fenton reagent, deionized water are added, in water-bath and 40KHz, 500W
10 h of the lower reaction of ultrasound, the Fenton reagent in ultrasonic cleaning machine：H2O2With FeSO4Quality Wei 8:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 0.5 g/L, 1 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains aoxidizing stone
Black alkene product.
Embodiment 6
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g expanded graphites and deionization are well mixed, regulation system pH=3 are worth, and are warming up to 90 DEG C instead
2 h are answered, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 50 DEG C, adds Fenton reagent, deionized water, adds electrochemical reactor
In, by anode, porous carbon electrodes of flat board iron it is negative electrode in reactor, electrode both end voltage is 30V, in electrochemical redox
Lower 12h, obtain graphite oxide solution, the Fenton reagent：H2O2With FeSO4Quality Wei 8:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 0.5 g/L, 1 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains aoxidizing stone
Black alkene product.
Embodiment 7
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g expanded graphites and the aqueous solution are well mixed, regulation system pH=4 are worth, and are warming up to 80 DEG C instead
1 h is answered, obtains acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 60 DEG C, Fenton-type reagent, deionization is added, 2 h is reacted under water-bath, are obtained
To graphite oxide solution, the Fenton-type reagent：H2O2With Fe3O4/ β-CD quality Wei 5:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 1 g/L, 1.5 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains aoxidizing stone
Black alkene product.
Embodiment 8
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1.5 g expanded graphites and the aqueous solution are well mixed, regulation system pH=3 are worth, and are warming up to 80 DEG C
2 h are reacted, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 60 DEG C, Fenton-type reagent, deionization is added, 2 h is reacted under water-bath, are obtained
To graphite oxide solution, the Fenton-type reagent：H2O2With Fe/Cu/HMS quality Wei 6:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 1 g/L, 2 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains graphite oxide
Alkene product.
Embodiment 9
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 0.5 g preliminary oxidations graphite and the aqueous solution are well mixed, regulation system pH=4 are worth, and are warming up to
80 DEG C of 2 h of reaction, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 60 DEG C, Fenton-type reagent, deionization is added, 2 h is reacted under water-bath, are obtained
To graphite oxide solution, the Fenton-type reagent：H2O2With Si/Al/@Fe/MWCNT quality Wei 7:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 1 g/L, 2.5 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains aoxidizing stone
Black alkene product.
Embodiment 10
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g expanded graphites and the aqueous solution are well mixed, regulation system pH=4 are worth, and are warming up to 80 DEG C instead
2 h are answered, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 60 DEG C, Fenton-type reagent, deionization is added, 2 h is reacted under water-bath, are obtained
To graphite oxide solution, the Fenton-type reagent：H2O2With Fe3O4/ Al-Fe-P-B quality Wei 5:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 0.5 g/L, 2.5 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying is aoxidized
Graphene product.
Embodiment 11
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g expanded graphites and the aqueous solution are well mixed, regulation system pH=4 are worth, and are warming up to 80 DEG C instead
2 h are answered, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 60 DEG C, Fenton-type reagent, deionization is added, 2 h is reacted under water-bath, are obtained
To graphite oxide solution, the Fenton-type reagent：H2O2With CuFe2O4NPs quality Wei 8:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 0.5 g/L, 1.5 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying is aoxidized
Graphene product.
Embodiment 12
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 2 g expanded graphites and the aqueous solution are well mixed, regulation system pH=3 are worth, and are warming up to 80 DEG C instead
2 h are answered, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 60 DEG C, Fenton-type reagent, deionization is added, 2 h is reacted under water-bath, are obtained
To graphite oxide solution, the Fenton-type reagent：H2O2With EGCG/Fe3O4Quality Wei 5:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 1 g/L, 1.5 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains aoxidizing stone
Black alkene product.
Embodiment 13
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g expanded graphites and the aqueous solution are well mixed, regulation system pH=3 are worth, and are warming up to 80 DEG C instead
2 h are answered, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 60 DEG C, Fenton-type reagent, deionization is added, 2 h is reacted under water-bath, are obtained
To graphite oxide solution, the Fenton-type reagent：H2O2With β-FeOOH/rGO quality Wei 7:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 1.5 g/L, 1.5 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying is aoxidized
Graphene product.
Embodiment 14
It is described a kind of as follows using the graphene oxide preparation method containing hydrogen peroxide catalyzed system, step：
（1）Pretreatment of raw material：After 1 g expanded graphites and the aqueous solution are well mixed, regulation system pH=3 are worth, and are warming up to 80 DEG C instead
2 h are answered, obtain acidic mixed material；
（2）Oxidation：Acidic mixed material is cooled to 60 DEG C, Fenton-type reagent, deionization is added, 2 h is reacted under water-bath, are obtained
To graphite oxide solution, the Fenton-type reagent：H2O2With α-（Fe、Cu）OOH quality Wei 6:1；
（3）Washing：Centrifugation, washing graphite oxide solution to neutrality；
（4）Ultrasound：By step（3）It is 1 g/L, 1.5 h of ultrasound that resulting solution, which is diluted concentration, and freeze-drying obtains aoxidizing stone
Black alkene product.
Claims (8)
- A kind of 1. graphene oxide preparation method using Fenton reagent, it is characterised in that：Comprise the following steps：(1) pretreatment of raw material：After graphite and deionized water are well mixed, acid reagent regulation system pH value is added, heating is anti- Should, obtain acidic mixed material；(2) aoxidize：After acidic mixed material is cooled, addition Fenton reagent, deionized water are reacted, and it is molten to obtain graphite oxide Liquid；(3) wash：Centrifugation, washing graphite oxide solution to neutrality；(4) it is ultrasonic：By step（3）Resulting solution is diluted, and ultrasound, freeze-drying obtains graphene oxide product.
- A kind of 2. graphene oxide preparation method using Fenton reagent according to claim 1, it is characterised in that：It is described Graphite for crystalline flake graphite either expanded graphite or pre-oxidation graphite.
- A kind of 3. graphene oxide preparation method using Fenton reagent according to claim 1, it is characterised in that：It is described PH value scope be 2 ~ 5.
- A kind of 4. graphene oxide preparation method using Fenton reagent according to claim 1, it is characterised in that：Step (1) the temperature reaction temperature in is 50 ~ 90 DEG C, and the reaction time is 1 ~ 8 h.
- A kind of 5. graphene oxide preparation method using Fenton reagent according to claim 1, it is characterised in that：Step (2) acidic mixed material is cooled to 30 ~ 70 DEG C in, and the reaction time is 2 ~ 6 h.
- A kind of 6. graphene oxide preparation method using Fenton reagent according to claim 1, it is characterised in that：It is described Fenton reagent be H2O2/ FeSO4System, H2O2With FeSO4Mass ratio be 7:1~11:1.
- A kind of 7. graphene oxide preparation method using Fenton reagent according to claim 1, it is characterised in that：It is described Reaction system is under water bath condition or under the conditions of water-bath and ultra violet lamp or under water-bath and ultrasound condition or electrochemical oxidation bar Under part.
- A kind of 8. graphene oxide preparation method using Fenton reagent according to claim 1, it is characterised in that：Step （4）Middle graphite oxide diluted concentration is 0.5 ~ 2 g/L, and the ultrasonic time is 0.5 ~ 5 h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108394893A (en) * | 2018-03-14 | 2018-08-14 | 南京信息工程大学 | One type graphene oxide composite material and its application |
| CN108910872A (en) * | 2018-09-28 | 2018-11-30 | 嘉兴烯成新材料有限公司 | A kind of preparation method of graphene oxide |
| CN109019585A (en) * | 2018-09-28 | 2018-12-18 | 嘉兴烯成新材料有限公司 | Fenton reagent prepares graphene oxide |
| CN110760159A (en) * | 2019-11-01 | 2020-02-07 | 嘉兴烯成新材料有限公司 | Preparation method of xanthium-shaped carbon material reinforced epoxy resin mechanical property |
| CN110773142A (en) * | 2019-11-14 | 2020-02-11 | 嘉兴烯成新材料有限公司 | Preparation and application of reduced hydroxylated graphene composite semiconductor catalyst |
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| CN106672957A (en) * | 2016-07-18 | 2017-05-17 | 中国科学院兰州化学物理研究所 | Method for preparing graphene oxide according to Fenton oxidation method |
| CN106744911A (en) * | 2017-01-23 | 2017-05-31 | 宣城亨旺新材料有限公司 | The production method of graphene oxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108394893A (en) * | 2018-03-14 | 2018-08-14 | 南京信息工程大学 | One type graphene oxide composite material and its application |
| CN108910872A (en) * | 2018-09-28 | 2018-11-30 | 嘉兴烯成新材料有限公司 | A kind of preparation method of graphene oxide |
| CN109019585A (en) * | 2018-09-28 | 2018-12-18 | 嘉兴烯成新材料有限公司 | Fenton reagent prepares graphene oxide |
| CN110760159A (en) * | 2019-11-01 | 2020-02-07 | 嘉兴烯成新材料有限公司 | Preparation method of xanthium-shaped carbon material reinforced epoxy resin mechanical property |
| CN110773142A (en) * | 2019-11-14 | 2020-02-11 | 嘉兴烯成新材料有限公司 | Preparation and application of reduced hydroxylated graphene composite semiconductor catalyst |
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