CN111892043A - Method for preparing reduced graphene oxide by one-pot method - Google Patents
Method for preparing reduced graphene oxide by one-pot method Download PDFInfo
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- CN111892043A CN111892043A CN202010781227.XA CN202010781227A CN111892043A CN 111892043 A CN111892043 A CN 111892043A CN 202010781227 A CN202010781227 A CN 202010781227A CN 111892043 A CN111892043 A CN 111892043A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000005580 one pot reaction Methods 0.000 title claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 35
- 239000010439 graphite Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 15
- 230000001590 oxidative effect Effects 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 230000004913 activation Effects 0.000 claims abstract description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 239000007800 oxidant agent Substances 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 6
- 238000010791 quenching Methods 0.000 claims abstract description 5
- 230000003213 activating effect Effects 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 230000000171 quenching effect Effects 0.000 claims abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000006722 reduction reaction Methods 0.000 claims description 12
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000001694 spray drying Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 claims description 2
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 2
- 230000003647 oxidation Effects 0.000 abstract description 9
- 239000002585 base Substances 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 14
- 239000000843 powder Substances 0.000 description 12
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 12
- 238000004108 freeze drying Methods 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 235000010344 sodium nitrate Nutrition 0.000 description 6
- 239000004317 sodium nitrate Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Abstract
The invention discloses a method for preparing reduced graphene oxide by a one-pot method, which specifically comprises the following steps: adding a strong oxidant into a strong acid solution containing graphite at room temperature, oxidizing to obtain graphite oxide, adding water, quenching, reacting, and then carrying out acid washing, ultrasonic treatment and centrifugation to obtain graphene oxide slurry; adding a strong base compound into the graphene oxide slurry, and reacting at 40-180 ℃ for 0.5-24 h to obtain an alkaline reduced graphene oxide suspension; and drying the reduced graphene oxide suspension, activating by microwave, washing by water until the suspension is neutral and free of impurities, and drying to obtain reduced graphene oxide powder. The method comprises the steps of directly synthesizing a graphite oxide solution at room temperature in an oxidation stage, directly adding alkali for rapid reduction after acid washing, ultrasonic treatment and centrifugation, and washing to obtain reduced graphene oxide with high porosity and high specific surface area after microwave activation; the method simplifies the oxidation process, realizes the rapid synthesis of the reduced graphene oxide, reduces the energy consumption and shortens the synthesis time.
Description
Technical Field
The invention belongs to the technical field of graphene materials, and particularly relates to a method for preparing reduced graphene oxide by a one-pot method.
Background
Graphene is the first two-dimensional monatomic material discovered, and has been kept at a high research heat by researchers since 2004 due to its excellent physical and chemical properties. Among the known methods for synthesizing graphene composites, modification and functionalization of Graphene Oxide (GO) containing oxygen-rich groups and active sites is the most common and most extensive method. Graphene oxide, the most widespread derivative of graphene, plays an important role in supercapacitors and electrodes, and is widely used in the fields of sensors, chemical and biological markers, catalyst carriers, polymer fillers and the like.
Graphene oxide is a thin-layer product in which layered graphite is intercalated and peeled by high-valence metal salts with strong oxidizing properties such as potassium permanganate and potassium dichromate in a strong acid atmosphere. Among the numerous oxidation methods, the classical Hummers method is widely introduced for its safety, mainly by edge oxidation at 0 ℃, deep oxidation at 35 ℃ and hydrolysis at 98 ℃ for the purpose of oxidative exfoliation. However, neither the classical nor the modified Hummers method provides a low-temperature or high-temperature atmosphere from the outside, which greatly increases the manufacturing cost of graphene oxide and also puts higher demands on equipment. Meanwhile, the classical or improved Hummers method for preparing graphene oxide needs to transfer the reaction liquid to a higher temperature, so that the process is complicated and certain risks are not generated in the shape. For example, a chinese patent discloses a method for preparing graphene oxide (patent No. CN 106115669 a, application date 20160620), in which potassium permanganate is added to an oxidation system at a temperature of less than 10 ℃, the reaction is continued for 2 to 5 hours at a temperature of 80 ℃ after 2 to 4 days at room temperature, and hydrogen peroxide and water are added to quench the reaction. The method has long reaction time, needs external continuous energy supply, greatly increases the synthesis cost, and simultaneously, the subsequent filtration and purification process is time-consuming and labor-consuming and is easy to generate more acid-containing wastewater.
Aiming at the problems of long reaction time, high energy consumption and the like in the prior art, it is necessary to research a preparation method of the reduced graphene oxide with high efficiency and low energy consumption.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for preparing reduced graphene oxide by a one-pot method.
The invention aims to realize the purpose that the method for preparing the reduced graphene oxide by the one-pot method comprises an oxidation reaction, a reduction reaction and drying activation, and specifically comprises the following steps:
(1) and (3) oxidation reaction: adding a strong oxidant into a strong acid solution containing graphite at room temperature, oxidizing to obtain graphite oxide, adding water, quenching, reacting, and then carrying out acid washing, ultrasonic treatment and centrifugation to obtain graphene oxide slurry;
(2) reduction reaction: adding a strong base compound into the graphene oxide slurry to perform a reduction reaction, and obtaining an alkaline reduced graphene oxide suspension after the reaction is completed;
(3) microwave activation: and drying the reduced graphene oxide suspension, activating by microwave, washing by water until the suspension is neutral and free of impurities, and drying to obtain reduced graphene oxide powder.
The invention has the beneficial effects that:
the method comprises the steps of directly synthesizing a graphite oxide solution at room temperature in an oxidation stage, directly adding alkali for rapid reduction after acid washing, ultrasonic treatment and centrifugation, directly drying, then performing microwave activation, and washing to obtain the reduced graphene oxide with high porosity and high specific surface area; the method avoids the need of external continuous refrigeration or heating in the traditional oxidation stage, simplifies the oxidation process, realizes the rapid synthesis of the reduced graphene oxide, and simultaneously reduces the energy consumption and shortens the time. The method has the advantages of short period of the whole oxidation-reduction process, simple working procedure, simple requirement on equipment and easy realization of continuous and large-scale operation mode; in addition, after the reduced graphene oxide containing alkali is activated by microwave, the specific surface area and the porosity of the reduced graphene oxide can be obviously improved, and the product can be widely applied to the fields of adsorption, supercapacitors, graphene-based composite materials and the like.
Drawings
Fig. 1 is an XRD pattern of reduced graphene oxide prepared in example 1 of the present invention;
fig. 2 is a Raman chart of reduced graphene oxide prepared in example 1 of the present invention;
fig. 3 is an XPS chart of reduced graphene oxide prepared in example 1 of the present invention.
Detailed Description
The present invention is further described with reference to the following specific embodiments, which should be noted that the following examples are only illustrative of the present invention, but not limiting the present invention, and all persons skilled in the art who have the spirit of the present invention will make equivalent substitutions of the present invention.
The invention relates to a method for preparing reduced graphene oxide by a one-pot method, which comprises an oxidation reaction, a reduction reaction and microwave activation, and specifically comprises the following steps:
(1) and (3) oxidation reaction: adding a strong oxidant into a strong acid solution containing graphite at room temperature, oxidizing to obtain graphite oxide, adding water, quenching, reacting, and then carrying out acid washing, ultrasonic treatment and centrifugation to obtain graphene oxide slurry;
(2) reduction reaction: adding a strong base compound into the graphene oxide slurry to perform a reduction reaction, and obtaining an alkaline reduced graphene oxide suspension after the reaction is completed;
(3) microwave activation: and drying the reduced graphene oxide suspension, activating by microwave, washing by water until the suspension is neutral and free of impurities, and drying to obtain reduced graphene oxide powder.
In the step 1, the room temperature is 10-40 ℃, and the time of the oxidation reaction is 0.5-48 h.
In the step 1, the strong oxidant is one or a combination of more of potassium permanganate, potassium dichromate and potassium ferrate, the ratio of the combination is 1-X: X (X = 0-1), and the weight ratio of the strong oxidant to graphite is 1-6: 1.
In the step 1, the ultrasonic power is 10-500W, and the ultrasonic time is 30-300 min.
In the step 1, the acid adopted in the acid washing is hydrochloric acid with the concentration of 5-20% until the solution does not contain metal ions.
In the step 2, the reduction reaction temperature is 40-180 ℃, and the reaction time is 0.5-24 h.
In the step 2, the strong base compound is one or a combination of potassium hydroxide, sodium hydroxide or ammonia water, the addition amount of the strong base is larger than the neutralization amount of acid in the graphene oxide slurry, and after the acid is completely neutralized, the strong base is continuously added to enable the pH value of the alkaline reduced graphene oxide suspension to be larger than or equal to 9.
In the step 3, the drying mode is any one or combination of a plurality of modes of vacuum drying, freeze drying or spray drying.
In the step 3, the microwave activation power is 100-10000 w, and the microwave treatment time is 0.5-300 min.
In the steps 1-3, the water is deionized water or ultrapure water.
The steps 1-2 are all completed in the same container, and the container can be stirred and heated.
The present invention is further illustrated by the following examples.
Example 1
Under the condition that the temperature is 25 ℃, 1g of crystalline flake graphite and 0.5g of sodium nitrate are added into 23mL of concentrated sulfuric acid and stirred for 30min, then 3g of potassium permanganate is slowly added and reacted for 2h, then deionized water is slowly added to stop the reaction, and then hydrogen peroxide is dropwise added until no bubbles are generated to obtain a graphite oxide solution. Washing the obtained graphite oxide with 1000ml of 10% hydrochloric acid, treating in ultrasonic with the power of 200W for 1h, centrifuging, adding 112g of potassium hydroxide, stirring in a water bath kettle at 80 ℃ for reaction for 2h, directly spray-drying the obtained precipitate into powder, reacting in a 1000W microwave oven for 30min, washing with water to neutrality, and freeze-drying to obtain reduced graphene oxide powder, wherein an XRD (X-ray diffraction) diagram, a Raman diagram and an XPS (X-ray diffraction) diagram are respectively shown in figures 1-3.
Example 2
Under the condition that the temperature is 30 ℃, 1g of flake graphite and 0.5g of sodium nitrate are added into 23mL of concentrated sulfuric acid and stirred for 40min, then 6g of potassium dichromate is slowly added and reacted for 12h, then deionized water is slowly added to stop the reaction, and then hydrogen peroxide is dropwise added until no bubbles are generated to obtain a graphite oxide solution. Washing the obtained graphite oxide solution with 2000ml of 5% hydrochloric acid, treating in 400W ultrasonic for 3h, centrifuging, adding 224g of sodium hydroxide, stirring in a 60 ℃ water bath kettle for reacting for 8h, directly vacuum-drying the obtained precipitate into powder, reacting in a 100W microwave oven for 60min, washing with water to neutrality, and vacuum-drying to obtain reduced graphene oxide powder.
Example 3
Under the condition that the temperature is 40 ℃, 1g of crystalline flake graphite and 0.5g of sodium nitrate are added into 23mL of concentrated sulfuric acid and stirred for 45min, then 5g of potassium permanganate is slowly added and reacted for 24h, then deionized water is slowly added to stop the reaction, and then hydrogen peroxide is dropwise added until no bubbles are generated to obtain a graphite oxide solution. Washing the obtained graphite oxide solution with 1000ml of 15% hydrochloric acid, treating the obtained graphene oxide in ultrasonic with the power of 300W for 2h, centrifuging, adding 169g of sodium hydroxide and 100g of potassium hydroxide, stirring and reacting in a water bath kettle at 100 ℃ for 1h, directly freeze-drying the obtained precipitate into powder, reacting in a 10000W microwave oven for 0.5min, washing with water to neutrality, and freeze-drying to obtain reduced graphene oxide powder.
Example 4
Under the condition that the temperature is 10 ℃, 1g of crystalline flake graphite and 0.5g of sodium nitrate are added into 23mL of concentrated sulfuric acid and stirred for 50min, then 1g of potassium permanganate is slowly added and reacted for 10h, then deionized water is slowly added to stop the reaction, and then hydrogen peroxide is dropwise added until no bubbles are generated to obtain a graphite oxide solution. Washing the obtained graphite oxide with 1000ml of 18% hydrochloric acid, treating the graphite oxide in ultrasonic waves with the power of 500W for 1h, centrifuging the graphite oxide, adding 112g of potassium hydroxide, stirring the mixture in a water bath kettle at the temperature of 70 ℃ for reaction for 4h, directly spraying and drying the obtained precipitate into powder, reacting the powder in a 500W microwave oven for 100min, washing the powder to be neutral, and freeze-drying the powder to obtain the reduced graphene oxide powder.
Example 5
Under the condition that the temperature is 15 ℃, 1g of flake graphite and 0.5g of sodium nitrate are added into 23mL of concentrated sulfuric acid and stirred for 25min, then 2g of potassium dichromate is slowly added and reacted for 8h, then deionized water is slowly added to stop the reaction, and then hydrogen peroxide is dropwise added until no bubbles are generated to obtain a graphite oxide solution. Washing the obtained graphite oxide solution with 2000ml of 8% hydrochloric acid, treating the graphite oxide solution in ultrasonic with the power of 500W for 3h, centrifuging the graphite oxide solution, adding 78g of sodium hydroxide, 53g of potassium hydroxide and 116g of ammonia water, stirring the mixture in a water bath kettle at the temperature of 65 ℃ for reaction for 7h, directly drying the obtained precipitate in vacuum to form powder, reacting the powder in a 3000W microwave oven for 7min, washing the powder to be neutral, and drying the powder in vacuum to obtain reduced graphene oxide powder.
Example 6
Under the condition that the temperature is 20 ℃, 1g of crystalline flake graphite and 0.5g of sodium nitrate are added into 23mL of concentrated sulfuric acid and stirred for 30min, then 4g of potassium permanganate is slowly added and reacted for 16h, then deionized water is slowly added to stop the reaction, and then hydrogen peroxide is dropwise added until no bubbles are generated to obtain a graphite oxide solution. Washing the obtained graphite oxide solution with 1000ml of 12% hydrochloric acid, treating the obtained graphene oxide in ultrasonic with the power of 400W for 4h, centrifuging, adding 97g of potassium hydroxide and 164g of ammonia water, stirring in a water bath kettle at 90 ℃ for reaction for 1h, directly freeze-drying the obtained precipitate into powder, reacting in a microwave oven with the power of 5000W for 5min, washing with water to neutrality, and freeze-drying to obtain reduced graphene oxide powder.
Claims (10)
1. A method for preparing reduced graphene oxide by a one-pot method comprises an oxidation reaction, a reduction reaction and microwave activation, and is characterized by comprising the following steps:
(1) and (3) oxidation reaction: adding a strong oxidant into a strong acid solution containing graphite at room temperature, oxidizing to obtain graphite oxide, adding water, quenching, reacting, and then carrying out acid washing, ultrasonic treatment and centrifugation to obtain graphene oxide slurry;
(2) reduction reaction: adding a strong base compound into the graphene oxide slurry to perform a reduction reaction, and obtaining an alkaline reduced graphene oxide suspension after the reaction is completed;
(3) microwave activation: and drying the reduced graphene oxide suspension, activating by microwave, washing by water until the suspension is neutral and free of impurities, and drying to obtain reduced graphene oxide powder.
2. The method for preparing reduced graphene oxide by the one-pot method according to claim 1, wherein in the step 1, the room temperature is 10-40 ℃, and the time of the oxidation reaction is 0.5-48 h.
3. The method for preparing reduced graphene oxide by the one-pot method according to claim 1, wherein in the step 1, the strong oxidant is one or more of potassium permanganate, potassium dichromate or potassium ferrate, and the weight ratio of the strong oxidant to graphite is 1-6: 1.
4. The method for preparing reduced graphene oxide by the one-pot method according to claim 1, wherein in the step 1, the power of ultrasound is 10-500W, and the ultrasound time is 30-300 min.
5. The method for preparing reduced graphene oxide according to claim 1, wherein in the step 1, the acid used for acid washing is hydrochloric acid with a concentration of 5-20%.
6. The method for preparing reduced graphene oxide according to claim 1, wherein in the step 2, the reduction reaction temperature is 40-180 ℃ and the reaction time is 0.5-24 h.
7. The method for preparing reduced graphene oxide by the one-pot method according to claim 1, wherein in the step 2, the strong base compound is one or a combination of potassium hydroxide, sodium hydroxide or ammonia water, the addition amount of the strong base is greater than the neutralization amount of acid in the graphene oxide slurry, and after the acid is completely neutralized, the strong base is continuously added to enable the pH of the alkaline reduced graphene oxide suspension to be greater than or equal to 9.
8. The method for preparing reduced graphene oxide according to claim 1, wherein in the step 3, the drying manner is any one or more of vacuum drying, freeze drying or spray drying.
9. The method for preparing reduced graphene oxide according to claim 1, wherein in the step 3, the microwave activation power is 100-10000 w, and the microwave treatment time is 0.5-300 min.
10. The method for preparing reduced graphene oxide according to claim 1, wherein in the steps 1 to 3, the water is deionized water or ultrapure water.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070140A (en) * | 2011-02-28 | 2011-05-25 | 无锡第六元素高科技发展有限公司 | Method for preparing high-specific surface area graphene material by utilizing strong base chemical treatment |
| CN103224230A (en) * | 2013-04-16 | 2013-07-31 | 谭彬 | Preparation method of graphene |
| CN103641104A (en) * | 2013-11-22 | 2014-03-19 | 简玉君 | Preparation method of graphene |
| CN104386679A (en) * | 2014-11-13 | 2015-03-04 | 苏州经贸职业技术学院 | Method for preparing graphene oxide and graphene |
| CN104477883A (en) * | 2014-11-13 | 2015-04-01 | 苏州经贸职业技术学院 | Preparation method of graphene |
| WO2017084561A1 (en) * | 2015-11-16 | 2017-05-26 | 复旦大学 | Preparation method for large-size graphene oxide or graphene |
| CN107032337A (en) * | 2017-06-15 | 2017-08-11 | 山东海迈新材料有限公司 | The method that commercial graphites alkene is produced with oxidation-reduction method |
| CN107601486A (en) * | 2017-10-12 | 2018-01-19 | 南京旭羽睿材料科技有限公司 | A kind of graphene production method |
| US20180286599A1 (en) * | 2017-03-31 | 2018-10-04 | Nanotek Instruments, Inc. | Direct Microwave Production of Graphene |
| CN109019578A (en) * | 2018-10-16 | 2018-12-18 | 上海应用技术大学 | A kind of method of microwave reduction graphene oxide |
| CN110342501A (en) * | 2019-08-28 | 2019-10-18 | 徐州宇帆机电科技有限公司 | A kind of method that pulsed high energy microwave quickly restores preparation high quality reduced graphene |
-
2020
- 2020-08-06 CN CN202010781227.XA patent/CN111892043A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070140A (en) * | 2011-02-28 | 2011-05-25 | 无锡第六元素高科技发展有限公司 | Method for preparing high-specific surface area graphene material by utilizing strong base chemical treatment |
| CN103224230A (en) * | 2013-04-16 | 2013-07-31 | 谭彬 | Preparation method of graphene |
| CN103641104A (en) * | 2013-11-22 | 2014-03-19 | 简玉君 | Preparation method of graphene |
| CN104386679A (en) * | 2014-11-13 | 2015-03-04 | 苏州经贸职业技术学院 | Method for preparing graphene oxide and graphene |
| CN104477883A (en) * | 2014-11-13 | 2015-04-01 | 苏州经贸职业技术学院 | Preparation method of graphene |
| WO2017084561A1 (en) * | 2015-11-16 | 2017-05-26 | 复旦大学 | Preparation method for large-size graphene oxide or graphene |
| US20180286599A1 (en) * | 2017-03-31 | 2018-10-04 | Nanotek Instruments, Inc. | Direct Microwave Production of Graphene |
| CN107032337A (en) * | 2017-06-15 | 2017-08-11 | 山东海迈新材料有限公司 | The method that commercial graphites alkene is produced with oxidation-reduction method |
| CN107601486A (en) * | 2017-10-12 | 2018-01-19 | 南京旭羽睿材料科技有限公司 | A kind of graphene production method |
| CN109019578A (en) * | 2018-10-16 | 2018-12-18 | 上海应用技术大学 | A kind of method of microwave reduction graphene oxide |
| CN110342501A (en) * | 2019-08-28 | 2019-10-18 | 徐州宇帆机电科技有限公司 | A kind of method that pulsed high energy microwave quickly restores preparation high quality reduced graphene |
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