CN104445168A - Preparation method of graphene oxide - Google Patents
Preparation method of graphene oxide Download PDFInfo
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- CN104445168A CN104445168A CN201410697232.7A CN201410697232A CN104445168A CN 104445168 A CN104445168 A CN 104445168A CN 201410697232 A CN201410697232 A CN 201410697232A CN 104445168 A CN104445168 A CN 104445168A
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Abstract
The invention discloses a preparation method of graphene oxide in the field of chemical industry. The preparation method comprises three steps of pre-oxidation of graphite, preparation of graphite oxide, and preparation of graphene oxide solution. The graphene oxide prepared by the method has the benefits that the prepared graphene oxide can reach nanoscale in scale; good basis is provided for the preparation of subsequent nano-composites; a stable aqueous solution can be formed by the graphene oxide prepared by the preparation method.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of preparation method of graphene oxide.
Background technology
Graphene has excellent process based prediction model, shows many stem-winding performances and potential application prospect in the field such as electronics, material.Graphene oxide is also called the Graphene of functionalization, is the oxygenatedchemicals of Graphene, and as one of raw material preparing Graphene, graphene oxide also shows much excellent physical and chemical performance, is subject to concern and the research interest of scientific circles in recent years always.Compared with expensive carbon nanotube, graphene oxide cheap, preparation process is simple, introduce a large amount of containing oxygen polar group in preparation process, as hydroxyl, carboxyl, these functional group ~ aspects expand the interlamellar spacing of graphite oxide, make it in " intercalation chemistry ", illustrate good applicability, impart the chemical property of graphene oxide excellence simultaneously, compound can be carried out with many macromolecular compounds, obtain the mixture that performance is more excellent.
The preparation of graphene oxide can be divided into two steps: first utilize chemical method that graphite oxidation is become graphite oxide, then peels off graphite oxide by external force (as thermal expansion, ultrasonic) and obtains graphene oxide sheet.The chemical preparation of graphite oxide mainly contains three kinds of methods: Brodie method, Staudenmaier method and Hummers method.The ultimate principle of these three kinds of methods is all destroy carbon-coating structure under strong oxidizer effect, is incorporated into by Sauerstoffatom on carbon atom, and the intervention of oxy radical can cause graphite linings to ask the expansion of distance.
Summary of the invention
In order to overcome the above problems, the invention provides a kind of preparation method of graphene oxide.
A preparation method for graphene oxide, said method comprising the steps of:
(1) in there-necked flask, add the vitriol oil, Potassium Persulfate, Vanadium Pentoxide in FLAKES, be heated to 90-100 DEG C;
(2), after stirring 15-30min, 80 DEG C are cooled to;
(3) slowly add 2-5 part Graphite Powder 99, maintain the temperature at 80 DEG C, stir 5 h;
(4) mixture is cooled to room temperature after terminating by reaction, with deionized water dilution, leaves standstill a night;
(5) with distilled water, the graphite after process is washed till neutrality, at room temperature dry 24h, obtains the graphite of pre-oxidation treatment;
(6) 20-25 part vitriol oil is joined in there-necked flask, be cooled with an ice bath to 0 DEG C;
(7) add the graphite of pre-oxidation treatment under stirring, rapid stirring is entirely molten to Graphite Powder 99;
(8) slowly add 10-20 part potassium permanganate, control temperature is no more than 10 DEG C, and finish rear continuation and stir 2h, this stage is the low-temp reaction stage;
(9) mixture is warming up to 40-50 DEG C of reaction 2h, along with the carrying out of reaction, mixture can become thickness, presents brown, and this stage is middle temperature step of reaction;
(10), after temperature reaction terminates in, in there-necked flask, slowly add 100-150 part deionized water, now have larger temperature rise, therefore need control temperature to be no more than 60 DEG C, after deionized water finishes, temperature is risen to 100-105 DEG C, keep 30min, this stage is high temperature dehydration step of reaction;
(11) add deionized water and hydrogen peroxide to reaction system, reacted mixture is left standstill a night;
(12) use the HCl solution washing of prepare in advance 3% until without S0
4 2-, then being washed with distilled water to neutrality, poured into by washed colloid in clean watch-glass, 55-65 DEG C of dry 48h, grinding, sealing is preserved, and obtains graphite oxide;
(13) graphite oxide and deionized water are made into the suspension that massfraction is 0.15%, till being dispersed to thering is no throw out with 100W ultrasonic echography, obtain graphene oxide solution.
Further, the parts by weight adding each reactant in step (1) are: massfraction be 98% vitriol oil 5-10 part, Potassium Persulfate 2-5 part, Vanadium Pentoxide in FLAKES 1-5 part.
The beneficial effect that the present invention reaches is: the graphene oxide of preparation can reach nano level on yardstick, and the preparation for follow-up nano-complex provides good basis; The graphene oxide that the present invention obtains can form the stable aqueous solution, on the one hand owing to its intrinsic wetting ability, be due to the hydroxy-acid group of graphene oxide structural edge and the protonated of surperficial oh group on the other hand, make graphene oxide lamella produce electrostatic repulsion effect with very strong electronegativity and make molten liquid stable; The solvability of graphene oxide in polar solvent is relatively better, and this is relevant with the polarity size of organic solution, because containing hydroxyl, carboxyl isopolarity group in graphene oxide structure, therefore have good avidity to polar solvent.
Embodiment
Embodiment 1
A preparation method for graphene oxide, said method comprising the steps of:
(1) in there-necked flask, add the vitriol oil, Potassium Persulfate, Vanadium Pentoxide in FLAKES, be heated to 90-100 DEG C, the parts by weight wherein adding each reactant are: massfraction is the vitriol oil 5 parts, Potassium Persulfate 2 parts, the Vanadium Pentoxide in FLAKES 1 part of 98%;
(2), after stirring 15min, 80 DEG C are cooled to;
(3) slowly add 2 parts of Graphite Powder 99s, maintain the temperature at 80 DEG C, stir 5 h;
(4) mixture is cooled to room temperature after terminating by reaction, with deionized water dilution, leaves standstill 12h;
(5) with distilled water, the graphite after process is washed till neutrality, at room temperature dry 24h, obtains the graphite of pre-oxidation treatment;
(6) 20 parts of vitriol oils are joined in there-necked flask, be cooled with an ice bath to 0 DEG C;
(7) add the graphite of pre-oxidation treatment under stirring, rapid stirring is entirely molten to Graphite Powder 99;
(8) the low-temp reaction stage, slowly add 10 parts of potassium permanganate, control temperature is no more than 10 DEG C, finishes rear continuation and stirs 2h;
(9) warm step of reaction in, is warming up to 40 DEG C of reaction 2h by mixture;
(10) high temperature dehydration step of reaction, in there-necked flask, slowly add 100 parts of deionized waters, control temperature is no more than 60 DEG C, after deionized water finishes, and temperature is risen to 100-105 DEG C, keeps 30min;
(11) add deionized water and hydrogen peroxide to reaction system, reacted mixture is left standstill 12h;
(12) use the HCl solution washing of prepare in advance 3% until without S0
4 2-, then being washed with distilled water to neutrality, poured into by washed colloid in clean watch-glass, 55-65 DEG C of dry 48h, grinding, sealing is preserved, and obtains graphite oxide;
(13) graphite oxide and deionized water are made into the suspension that massfraction is 0.15%, till being dispersed to thering is no throw out with 100W ultrasonic echography, obtain graphene oxide solution.
Embodiment 2
A preparation method for graphene oxide, said method comprising the steps of:
(1) in there-necked flask, add the vitriol oil, Potassium Persulfate, Vanadium Pentoxide in FLAKES, be heated to 90-100 DEG C, the parts by weight wherein adding each reactant are: massfraction is the vitriol oil 10 parts, Potassium Persulfate 5 parts, the Vanadium Pentoxide in FLAKES 5 parts of 98%;
(2), after stirring 15-30min, 80 DEG C are cooled to;
(3) slowly add 5 parts of Graphite Powder 99s, maintain the temperature at 80 DEG C, stir 5 h;
(4) mixture is cooled to room temperature after terminating by reaction, with deionized water dilution, leaves standstill 12h;
(5) with distilled water, the graphite after process is washed till neutrality, at room temperature dry 24h, obtains the graphite of pre-oxidation treatment;
(6) 25 parts of vitriol oils are joined in there-necked flask, be cooled with an ice bath to 0 DEG C;
(7) add the graphite of pre-oxidation treatment under stirring, rapid stirring is entirely molten to Graphite Powder 99;
(8) the low-temp reaction stage, slowly add 20 parts of potassium permanganate, control temperature is no more than 10 DEG C, finishes rear continuation and stirs 2h;
(9) warm step of reaction in, is warming up to 40-50 DEG C of reaction 2h by mixture;
(10) high temperature dehydration step of reaction, in there-necked flask, slowly add 150 parts of deionized waters, control temperature is no more than 60 DEG C, after deionized water finishes, and temperature is risen to 100-105 DEG C, keeps 30min;
(11) add deionized water and hydrogen peroxide to reaction system, reacted mixture is left standstill 24h;
(12) use the HCl solution washing of prepare in advance 3% until without S0
4 2-, then being washed with distilled water to neutrality, poured into by washed colloid in clean watch-glass, 55-65 DEG C of dry 48h, grinding, sealing is preserved, and obtains graphite oxide;
(13) graphite oxide and deionized water are made into the suspension that massfraction is 0.15%, till being dispersed to thering is no throw out with 100W ultrasonic echography, obtain graphene oxide solution.
Embodiment 3
A preparation method for graphene oxide, said method comprising the steps of:
(1) in there-necked flask, add the vitriol oil, Potassium Persulfate, Vanadium Pentoxide in FLAKES, be heated to 90-100 DEG C, the parts by weight wherein adding each reactant are: massfraction is the vitriol oil 8 parts, Potassium Persulfate 4 parts, the Vanadium Pentoxide in FLAKES 4 parts of 98%;
(2), after stirring 30min, 80 DEG C are cooled to;
(3) slowly add 4 parts of Graphite Powder 99s, maintain the temperature at 80 DEG C, stir 5 h;
(4) mixture is cooled to room temperature after terminating by reaction, with deionized water dilution, leaves standstill 24h;
(5) with distilled water, the graphite after process is washed till neutrality, at room temperature dry 24h, obtains the graphite of pre-oxidation treatment;
(6) 22 parts of vitriol oils are joined in there-necked flask, be cooled with an ice bath to 0 DEG C;
(7) add the graphite of pre-oxidation treatment under stirring, rapid stirring is entirely molten to Graphite Powder 99;
(8) the low-temp reaction stage, slowly add 15 parts of potassium permanganate, control temperature is no more than 10 DEG C, finishes rear continuation and stirs 2h;
(9) warm step of reaction in, is warming up to 40-50 DEG C of reaction 2h by mixture;
(10) high temperature dehydration step of reaction, in there-necked flask, slowly add 120 parts of deionized waters, control temperature is no more than 60 DEG C, after deionized water finishes, and temperature is risen to 100-105 DEG C, keeps 30min;
(11) add deionized water and hydrogen peroxide to reaction system, reacted mixture is left standstill 24h;
(12) use the HCl solution washing of prepare in advance 3% until without S0
4 2-, then being washed with distilled water to neutrality, poured into by washed colloid in clean watch-glass, 55-65 DEG C of dry 48h, grinding, sealing is preserved, and obtains graphite oxide;
(13) graphite oxide and deionized water are made into the suspension that massfraction is 0.15%, till being dispersed to thering is no throw out with 100W ultrasonic echography, obtain graphene oxide solution.
Claims (2)
1. a preparation method for graphene oxide, is characterized in that, said method comprising the steps of:
(1) in there-necked flask, add the vitriol oil, Potassium Persulfate, Vanadium Pentoxide in FLAKES, be heated to 90-100 DEG C;
(2), after stirring 15-30min, 80 DEG C are cooled to;
(3) slowly add 2-5 part Graphite Powder 99, maintain the temperature at 80 DEG C, stir 5 h;
(4) mixture is cooled to room temperature after terminating by reaction, with deionized water dilution, leaves standstill 12-24h;
(5) with distilled water, the graphite after process is washed till neutrality, at room temperature dry 24h, obtains the graphite of pre-oxidation treatment;
(6) 20-25 part vitriol oil is joined in there-necked flask, be cooled with an ice bath to 0 DEG C;
(7) add the graphite of pre-oxidation treatment under stirring, rapid stirring is entirely molten to Graphite Powder 99;
(8) the low-temp reaction stage, slowly add 10-20 part potassium permanganate, control temperature is no more than 10 DEG C, finishes rear continuation and stirs 2h;
(9) warm step of reaction in, is warming up to 40-50 DEG C of reaction 2h by mixture;
(10) high temperature dehydration step of reaction, in there-necked flask, slowly add 100-150 part deionized water, control temperature is no more than 60 DEG C, after deionized water finishes, and temperature is risen to 100-105 DEG C, keeps 30min;
(11) add deionized water and hydrogen peroxide to reaction system, reacted mixture is left standstill 12-24h;
(12) use the HCl solution washing of prepare in advance 3% until without S0
4 2-, then being washed with distilled water to neutrality, poured into by washed colloid in clean watch-glass, 55-65 DEG C of dry 48h, grinding, sealing is preserved, and obtains graphite oxide;
(13) graphite oxide and deionized water are made into the suspension that massfraction is 0.15%, till being dispersed to thering is no throw out with 100W ultrasonic echography, obtain graphene oxide solution.
2. the preparation method of a kind of graphene oxide according to claim 1, is characterized in that, the parts by weight adding each reactant in step (1) are: massfraction be 98% vitriol oil 5-10 part, Potassium Persulfate 2-5 part, Vanadium Pentoxide in FLAKES 1-5 part.
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| CN104787755A (en) * | 2015-04-01 | 2015-07-22 | 广东烛光新能源科技有限公司 | Preparation method of graphene |
| CN105056899A (en) * | 2015-07-28 | 2015-11-18 | 华南理工大学 | Adsorbent for treating dye-containing wastewater, and preparation and application thereof |
| CN105217621A (en) * | 2015-10-30 | 2016-01-06 | 浙江理工大学 | A kind of graphene oxide preparation method of size uniformity |
| CN105347335A (en) * | 2015-11-27 | 2016-02-24 | 湖北大学 | Method for preparing graphene oxide by taking K2FeO4 as oxidizing agent |
| CN105418492A (en) * | 2015-11-27 | 2016-03-23 | 浙江大学 | Preparation method of 2,3-dichloropyridine |
| CN106276868A (en) * | 2016-07-21 | 2017-01-04 | 东华大学 | A kind of preparation method based on graphene oxide antioxidant |
| CN106634264A (en) * | 2016-12-04 | 2017-05-10 | 亚士漆(上海)有限公司 | Graphene-reinforced superhydrophobic finish-coat paint and preparation method thereof |
| CN107195879A (en) * | 2017-05-09 | 2017-09-22 | 东南大学 | A kind of preparation method of the graphite oxide negative material of high performance lithium ion battery |
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| WO2018187921A1 (en) * | 2017-04-11 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Improved preparation method for graphene oxide |
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| CN104787755A (en) * | 2015-04-01 | 2015-07-22 | 广东烛光新能源科技有限公司 | Preparation method of graphene |
| CN105056899B (en) * | 2015-07-28 | 2017-10-20 | 华南理工大学 | A kind of adsorbent that can be used for processing waste water containing dye and its preparation and application |
| CN105056899A (en) * | 2015-07-28 | 2015-11-18 | 华南理工大学 | Adsorbent for treating dye-containing wastewater, and preparation and application thereof |
| CN105217621A (en) * | 2015-10-30 | 2016-01-06 | 浙江理工大学 | A kind of graphene oxide preparation method of size uniformity |
| CN105347335A (en) * | 2015-11-27 | 2016-02-24 | 湖北大学 | Method for preparing graphene oxide by taking K2FeO4 as oxidizing agent |
| CN105418492A (en) * | 2015-11-27 | 2016-03-23 | 浙江大学 | Preparation method of 2,3-dichloropyridine |
| CN106276868A (en) * | 2016-07-21 | 2017-01-04 | 东华大学 | A kind of preparation method based on graphene oxide antioxidant |
| CN106634264A (en) * | 2016-12-04 | 2017-05-10 | 亚士漆(上海)有限公司 | Graphene-reinforced superhydrophobic finish-coat paint and preparation method thereof |
| WO2018187921A1 (en) * | 2017-04-11 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Improved preparation method for graphene oxide |
| CN107195879A (en) * | 2017-05-09 | 2017-09-22 | 东南大学 | A kind of preparation method of the graphite oxide negative material of high performance lithium ion battery |
| CN107880291A (en) * | 2017-11-30 | 2018-04-06 | 中国科学院合肥物质科学研究院 | A kind of preparation method of self assembly high heat conduction antistatic polyester perforated membrane |
| CN107880291B (en) * | 2017-11-30 | 2021-02-26 | 中国科学院合肥物质科学研究院 | Preparation method of self-assembled high-thermal-conductivity antistatic polyester porous membrane |
| CN108933261A (en) * | 2018-07-17 | 2018-12-04 | 河南电池研究院有限公司 | A kind of nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping |
| CN109262924A (en) * | 2018-07-20 | 2019-01-25 | 黄河科技学院 | The board making and stress determination method of basalt fibre enhancing unsaturated-resin |
| CN112638823A (en) * | 2018-08-24 | 2021-04-09 | 上海特瑞思材料科技有限公司 | Water filtration membrane device and method of making |
| CN112638823B (en) * | 2018-08-24 | 2023-11-28 | 上海特瑞思材料科技有限公司 | Water filtration membrane device and preparation method |
| CN109368634A (en) * | 2018-11-14 | 2019-02-22 | 贵州大学 | A kind of preparation method and applications of graphene-based material precursor |
| CN111607168A (en) * | 2020-06-30 | 2020-09-01 | 贵州宏润管业有限公司 | Graphene oxide modified polypropylene-based square corrugated pipe and manufacturing method thereof |
| CN112174124A (en) * | 2020-10-20 | 2021-01-05 | 大同通扬碳素有限公司 | Porous graphene electrode and preparation method thereof |
| CN113908803A (en) * | 2021-10-11 | 2022-01-11 | 福建省海凝环保科技有限公司 | Graphene oxide compound prepared based on intumescent flame retardant, preparation method thereof and application of graphene oxide compound in copper ion and mercury ion adsorption |
| CN114988401A (en) * | 2022-05-16 | 2022-09-02 | 南通赛可特电子有限公司 | Method for directly blackening PCB modified graphene oxide |
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