CN105217621A - A kind of graphene oxide preparation method of size uniformity - Google Patents
A kind of graphene oxide preparation method of size uniformity Download PDFInfo
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- CN105217621A CN105217621A CN201510720118.6A CN201510720118A CN105217621A CN 105217621 A CN105217621 A CN 105217621A CN 201510720118 A CN201510720118 A CN 201510720118A CN 105217621 A CN105217621 A CN 105217621A
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Abstract
The invention discloses a kind of preparation method of graphene oxide of size uniformity, first by the effect to graphite and oxygenant, prepare the graphene oxide of preoxidation, after improving the degree of oxidation of Graphite Powder 99, then the preoxidation graphene oxide continued obtaining further is oxidized, the graphene oxide that preparation size is homogeneous.The method is simple to operate, and degree of oxidation is high, environmental protection, the graphene oxide size uniformity prepared.
Description
Technical field
The invention belongs to the preparation field of graphene oxide, particularly relate to a kind of preparation method of graphene oxide of size uniformity.
Background technology
The existence of Graphene, since being found, having received scientists always and has paid close attention to greatly.Graphene is thin, the most tough and tensile material that it is found that at present, has unusual conduction, heat conductivility simultaneously.Due to the performance of Graphene excellence, it is made to play huge effect in multiple field such as electrochemistry, biomedicine.
The preparation of Graphene is significant for the research of Graphene performance.At present, a kind of method the most effectively preparing Graphene of chemical oxidation graphite reduction method, has that requirement of experiment is low, Graphene quality advantages of higher, is widely used in the preparation of Graphene.Wherein the preparation of graphene oxide is vital link in chemical oxidation graphite reduction method, and the preparation of graphene oxide determines the quality of reduced graphene.At present, the graphene oxide that preparation size is homogeneous all has great effect for the research of graphene oxide performance and the preparation of reduced graphene.
The method preparing graphene oxide at present mainly contains Brodie, Staudenmaier and Hummers method.Brodie method need carry out repeatedly oxide treatment to improve degree of oxidation, and the reaction times is relatively long, and because adopting perchlorate to make oxygenant, danger is comparatively large, and can produce more toxic gas in reaction process; Its shortcoming of Staudenmaier method is that the reaction times is longer, and degree of oxidation is lower, need carry out repeatedly oxide treatment; Hummers method adopts the vitriol oil and nitrate system, take permanganate as oxygenant, prepare graphite oxide through low temperature (less than 5 DEG C), middle temperature (about 35 DEG C) and high temperature (about 98 DEG C) three step of reaction, the graphene oxide degree of oxidation of preparation is high but still there is the shortcomings such as graphene oxide is not of uniform size.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of graphene oxide preparation method of size uniformity.
For this reason, the present invention adopts following technical scheme, and a kind of graphene oxide preparation method of size uniformity, is characterized in that taking following steps:
A) react in the mixed system of 2 ~ 4g Graphite Powder 99 and 3 ~ 6g potassium hyposulfate, 3 ~ 6g Vanadium Pentoxide in FLAKES and 12 ~ 24mL vitriol oil in reactor, 80
ostirring 4 ~ 6 hours under C water bath condition, to forming dark blue solution, after cooling, suction filtration, drying, obtaining the graphite of preoxidation;
B) get steps A) obtained by graphite oxide 2 ~ 4g in three-necked flask, with 150 ~ 300mL concentrated sulfuric acid solution under the condition of ice-water bath, add the potassium permanganate of 25 ~ 50g gradually, stir 2 ~ 4 hours;
C) by above-mentioned steps B) three-necked flask proceed to oil bath, be warming up to 35 ~ 40
oc, stirs 0.5 ~ 2 hour, and continuation is stirred and added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:15; Suction filtration is dilute hydrochloric acid and the washed with de-ionized water 1 time of 10% respectively with 4mL massfraction, centrifugal, obtains the graphene oxide of first time oxidation after drying;
D) by step C) in preparation graphene oxide 2 ~ 4g be again mixed in three-necked flask with the concentrated sulfuric acid solution of 50 ~ 100mL under the condition of ice-water bath, add the KMnO of 8 ~ 16g gradually
4, stir 1 ~ 2 hour;
E) by above-mentioned steps D) three-necked flask proceed to oil bath, be warming up to 40
oc, stirs 1 ~ 2 hour, then continues to be warming up to 90
oc, stir after 1 ~ 2 hour, continuation is stirred and is added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:7, continue stirring to cool after 6 ~ 8 hours, suction filtration, be dilute hydrochloric acid and the washed with de-ionized water 2 times of 10% respectively with 4mL massfraction, centrifugal, obtain the graphene oxide of size uniformity after drying.
The method is first by the effect to graphite and oxygenant, prepare the graphene oxide of preoxidation, after improving the degree of oxidation of Graphite Powder 99, the preoxidation graphene oxide then continued obtaining further is oxidized, the graphene oxide that preparation size is homogeneous.The method is simple to operate, and degree of oxidation is high, environmental protection, the graphene oxide size uniformity prepared.
Embodiment
Embodiment 1 takes following steps:
A) react in the mixed system of 2g Graphite Powder 99 and 3g potassium hyposulfate, 3g Vanadium Pentoxide in FLAKES and the 12mL vitriol oil in reactor, 80
ostirring 4 hours under C water bath condition, to forming dark blue solution, after cooling, suction filtration, drying, obtaining the graphite of preoxidation;
B) get steps A) obtained by graphite oxide 2g in three-necked flask, with 150mL concentrated sulfuric acid solution under the condition of ice-water bath, add the potassium permanganate of 25g gradually, stir 2 hours;
C) by above-mentioned steps B) three-necked flask proceed to oil bath, be warming up to 35
oc, stirs 2 hours, and continuation is stirred and added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:15; Suction filtration is dilute hydrochloric acid and the washed with de-ionized water 1 time of 10% respectively with 4mL massfraction, centrifugal, obtains the graphene oxide of first time oxidation after drying;
D) by step C) in preparation graphene oxide 2g be again mixed in three-necked flask with the concentrated sulfuric acid solution of 50mL under the condition of ice-water bath, add the KMnO of 8g gradually
4, stir 1 hour;
E) by above-mentioned steps D) three-necked flask proceed to oil bath, be warming up to 40
oc, stirs 1 hour, then continues to be warming up to 90
oc, stir after 1 hour, continuation is stirred and is added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:7, continue stirring to cool after 6 hours, suction filtration, be dilute hydrochloric acid and the washed with de-ionized water 2 times of 10% respectively with 4mL massfraction, centrifugal, obtain the graphene oxide of size uniformity after drying.
Embodiment 2 takes following steps:
A) react in the mixed system of 3g Graphite Powder 99 and 4.5g potassium hyposulfate, 4.5g Vanadium Pentoxide in FLAKES and the 18mL vitriol oil in reactor, 80
ostirring 5 hours under C water bath condition, to forming dark blue solution, after cooling, suction filtration, drying, obtaining the graphite of preoxidation;
B) get steps A) obtained by graphite oxide 3g in three-necked flask, with 250mL concentrated sulfuric acid solution under the condition of ice-water bath, add the potassium permanganate of 40g gradually, stir 3 hours;
C) by above-mentioned steps B) three-necked flask proceed to oil bath, be warming up to 37
oc, stirs 1 hour, and continuation is stirred and added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:15; Suction filtration is dilute hydrochloric acid and the washed with de-ionized water 1 time of 10% respectively with 4mL massfraction, centrifugal, obtains the graphene oxide of first time oxidation after drying;
D) by step C) in preparation graphene oxide 3g be again mixed in three-necked flask with the concentrated sulfuric acid solution of 75mL under the condition of ice-water bath, add the KMnO of 12g gradually
4, stir 1.5 hours;
E) by above-mentioned steps D) three-necked flask proceed to oil bath, be warming up to 40
oc, stirs 1.5 hours, then continues to be warming up to 90
oc, stir after 1.5 hours, continuation is stirred and is added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:7, continue stirring to cool after 7 hours, suction filtration, be dilute hydrochloric acid and the washed with de-ionized water 2 times of 10% respectively with 4mL massfraction, centrifugal, obtain the graphene oxide of size uniformity after drying.
Embodiment 3 takes following steps:
A) react in the mixed system of 4g Graphite Powder 99 and 6g potassium hyposulfate, 6g Vanadium Pentoxide in FLAKES and the 24mL vitriol oil in reactor, 80
ostirring 6 hours under C water bath condition, to forming dark blue solution, after cooling, suction filtration, drying, obtaining the graphite of preoxidation;
B) get steps A) obtained by graphite oxide 4g in three-necked flask, with 300mL concentrated sulfuric acid solution under the condition of ice-water bath, add the potassium permanganate of 50g gradually, stir 4 hours;
C) by above-mentioned steps B) three-necked flask proceed to oil bath, be warming up to 40
oc, stirs 0.5 hour, and continuation is stirred and added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:15; Suction filtration is dilute hydrochloric acid and the washed with de-ionized water 1 time of 10% respectively with 4mL massfraction, centrifugal, obtains the graphene oxide of first time oxidation after drying;
D) by step C) in preparation graphene oxide 4g be again mixed in three-necked flask with the concentrated sulfuric acid solution of 100mL under the condition of ice-water bath, add the KMnO of 8 ~ 16g gradually
4, stir 2 hours;
E) by above-mentioned steps D) three-necked flask proceed to oil bath, be warming up to 40
oc, stirs 2 hours, then continues to be warming up to 90
oc, stir after 2 hours, continuation is stirred and is added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:7, continue stirring to cool after 8 hours, suction filtration, be dilute hydrochloric acid and the washed with de-ionized water 2 times of 10% respectively with 4mL massfraction, centrifugal, obtain the graphene oxide of size uniformity after drying.
Protection scope of the present invention is not limited to above several embodiment, and therefore, every technical scheme formed by simple numerical value replacement etc., is all formed specific embodiments of the invention, and form protection scope of the present invention.
Claims (1)
1. a graphene oxide preparation method for size uniformity, is characterized in that taking following steps:
A) react in the mixed system of 2 ~ 4g Graphite Powder 99 and 3 ~ 6g potassium hyposulfate, 3 ~ 6g Vanadium Pentoxide in FLAKES and 12 ~ 24mL vitriol oil in reactor, 80
ostirring 4 ~ 6 hours under C water bath condition, to forming dark blue solution, after cooling, suction filtration, drying, obtaining the graphite of preoxidation;
B) get steps A) obtained by graphite oxide 2 ~ 4g in three-necked flask, with 150 ~ 300mL concentrated sulfuric acid solution under the condition of ice-water bath, add the potassium permanganate of 25 ~ 50g gradually, stir 2 ~ 4 hours;
C) by above-mentioned steps B) three-necked flask proceed to oil bath, be warming up to 35 ~ 40
oc, stirs 0.5 ~ 2 hour, and continuation is stirred and added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:15; Suction filtration is dilute hydrochloric acid and the washed with de-ionized water 1 time of 10% respectively with 4mL massfraction, centrifugal, obtains the graphene oxide of first time oxidation after drying;
D) by step C) in preparation graphene oxide 2 ~ 4g be again mixed in three-necked flask with the concentrated sulfuric acid solution of 50 ~ 100mL under the condition of ice-water bath, add the KMnO of 8 ~ 16g gradually
4, stir 1 ~ 2 hour;
E) by above-mentioned steps D) three-necked flask proceed to oil bath, be warming up to 40
oc, stirs 1 ~ 2 hour, then continues to be warming up to 90
oc, stir after 1 ~ 2 hour, continuation is stirred and is added the mixing solutions of 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:7, continue stirring to cool after 6 ~ 8 hours, suction filtration, be dilute hydrochloric acid and the washed with de-ionized water 2 times of 10% respectively with 4mL massfraction, centrifugal, obtain the graphene oxide of size uniformity after drying.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107715856A (en) * | 2017-10-31 | 2018-02-23 | 南京旭羽睿材料科技有限公司 | A kind of graphene composite material |
| CN108374207A (en) * | 2018-04-12 | 2018-08-07 | 中鸿纳米纤维技术丹阳有限公司 | A kind of processing method of graphene nano fiber cotton |
| CN109476487A (en) * | 2016-06-24 | 2019-03-15 | 加利福尼亚大学董事会 | Carbon-based oxides and the large-scale production for restoring carbon-based oxides |
| CN109618433A (en) * | 2018-12-20 | 2019-04-12 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene safe voltage heating film |
| CN109607526A (en) * | 2019-01-23 | 2019-04-12 | 浙江大学 | A kind of graphene oxide preparation method that interlamellar spacing is controllable |
| US11397173B2 (en) | 2011-12-21 | 2022-07-26 | The Regents Of The University Of California | Interconnected corrugated carbon-based network |
| US11569538B2 (en) | 2014-06-16 | 2023-01-31 | The Regents Of The University Of California | Hybrid electrochemical cell |
| US11791453B2 (en) | 2016-08-31 | 2023-10-17 | The Regents Of The University Of California | Devices comprising carbon-based material and fabrication thereof |
| US11810716B2 (en) | 2014-11-18 | 2023-11-07 | The Regents Of The University Of California | Porous interconnected corrugated carbon-based network (ICCN) composite |
| US11842850B2 (en) | 2016-01-22 | 2023-12-12 | The Regents Of The University Of California | High-voltage devices |
| US11891539B2 (en) | 2015-12-22 | 2024-02-06 | The Regents Of The University Of California | Cellular graphene films |
| US11915870B2 (en) | 2012-03-05 | 2024-02-27 | The Regents Of The University Of California | Capacitor with electrodes made of an interconnected corrugated carbon-based network |
| US11961667B2 (en) | 2016-03-23 | 2024-04-16 | The Regents Of The University Of California | Devices and methods for high voltage and solar applications |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11397173B2 (en) | 2011-12-21 | 2022-07-26 | The Regents Of The University Of California | Interconnected corrugated carbon-based network |
| US11915870B2 (en) | 2012-03-05 | 2024-02-27 | The Regents Of The University Of California | Capacitor with electrodes made of an interconnected corrugated carbon-based network |
| US11569538B2 (en) | 2014-06-16 | 2023-01-31 | The Regents Of The University Of California | Hybrid electrochemical cell |
| US11810716B2 (en) | 2014-11-18 | 2023-11-07 | The Regents Of The University Of California | Porous interconnected corrugated carbon-based network (ICCN) composite |
| US11891539B2 (en) | 2015-12-22 | 2024-02-06 | The Regents Of The University Of California | Cellular graphene films |
| US11842850B2 (en) | 2016-01-22 | 2023-12-12 | The Regents Of The University Of California | High-voltage devices |
| US11961667B2 (en) | 2016-03-23 | 2024-04-16 | The Regents Of The University Of California | Devices and methods for high voltage and solar applications |
| CN109476487A (en) * | 2016-06-24 | 2019-03-15 | 加利福尼亚大学董事会 | Carbon-based oxides and the large-scale production for restoring carbon-based oxides |
| US11791453B2 (en) | 2016-08-31 | 2023-10-17 | The Regents Of The University Of California | Devices comprising carbon-based material and fabrication thereof |
| CN107715856A (en) * | 2017-10-31 | 2018-02-23 | 南京旭羽睿材料科技有限公司 | A kind of graphene composite material |
| CN108374207A (en) * | 2018-04-12 | 2018-08-07 | 中鸿纳米纤维技术丹阳有限公司 | A kind of processing method of graphene nano fiber cotton |
| CN109618433A (en) * | 2018-12-20 | 2019-04-12 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene safe voltage heating film |
| CN109618433B (en) * | 2018-12-20 | 2022-04-08 | 四川省中科烯捷石墨烯科技有限公司 | Graphene safe voltage heating film |
| CN109607526B (en) * | 2019-01-23 | 2021-01-01 | 浙江大学 | Preparation method of graphene oxide with controllable interlayer spacing |
| CN109607526A (en) * | 2019-01-23 | 2019-04-12 | 浙江大学 | A kind of graphene oxide preparation method that interlamellar spacing is controllable |
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