CN105399084A - Preparation method of powder type graphene oxide - Google Patents
Preparation method of powder type graphene oxide Download PDFInfo
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- CN105399084A CN105399084A CN201510860186.2A CN201510860186A CN105399084A CN 105399084 A CN105399084 A CN 105399084A CN 201510860186 A CN201510860186 A CN 201510860186A CN 105399084 A CN105399084 A CN 105399084A
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Abstract
The invention provides a preparation method of powder type graphene oxide. The preparation method includes the specific steps that graphite powder and sodium nitrate are added to concentrated sulfuric acid for low-temperature oxidation, potassium permanganate is added for further oxidation and intercalation under the intermediate temperature condition, finally the mixture reacts at high temperature, centrifugal washing is conducted, and the mixture is ground into the powder type graphene oxide after freeze drying. The prepared graphene oxide has the advantages that operation is easy, and a product is easy to weigh and convenient to store.
Description
Technical field
The present invention relates to graphene oxide technical field, espespecially a kind of preparation method of powder-type graphene oxide.
Technical background
Graphene-based material is as the emerging material of one, open the research field that scientific circles are new, graphene oxide is as the presoma of Graphene, it is a kind of carbon nanomaterial of novel two dimension, its monolithic has a lot of oxygen-containing functional group as epoxy group(ing) and hydroxyl, and containing carboxyl on the edge of monolithic, it all has excellent properties in mechanics, electricity, optics and chemical field etc., chemical in recent years, the study hotspot in Materials science and physics field.
The graphene oxide of current preparation mostly is liquid, and is much all ultrasonic obtaining.Ultrasonic to graphene oxide lamella being smashed for a long time, but consuming time longer, substantially reduce the work-ing life of ultrasound machine, and there will be precipitation after storing certain hour, take up room comparatively large, be unfavorable for environmental protection.The bad grasp of concentration of simultaneously liquid graphene oxide, often needs the graphene oxide evaporating or dry certain volume, weighs its quality, then calculate concentration.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, a kind of Powder Oxidation Graphene being easy to weigh, store is provided.
A preparation method for powder-type graphene oxide, concrete grammar step is:
(1) add Graphite Powder 99, SODIUMNITRATE in the vitriol oil, wherein the mass ratio of Graphite Powder 99, SODIUMNITRATE and the vitriol oil is 2: 1: 84.64, and under ice bath, churning time is 5min
(2) ice bath terminates slowly to add potassium permanganate afterwards, adds potassium permanganate and Graphite Powder 99 mass ratio is 3: 1, and temperature is no more than in 20 DEG C, reacts 2h at flask being placed in 35 ± 3 DEG C.
(3) after in, temperature reaction terminates, slowly add deionized water, the volume wherein added is 46mL/1g Graphite Powder 99, temperature is increased to 98 DEG C, add warm water after keeping 15min, now add the warm water that volume is 140mL/1g Graphite Powder 99, wherein warm water is heated to temperature with electric furnace is in advance 70 ~ 80 DEG C, add the H202 that massfraction is 30% after stirring 5min, adding volume is 15mL/1g Graphite Powder 99.
(4) pyroreaction terminates rear naturally cooling, and adding volume is 40mL/1g Graphite Powder 99 1+9HCl.After leaving standstill 12h, remove supernatant liquid, washing centrifuge washing lower floor solution is to about pH=6, and centrifugal reservation lower floor material, is syrupy shape graphene oxide.
(5) at about-60 DEG C lyophilize 24h ~ 32h, powder is made in grinding, namely obtains graphene oxide.
Advantage of the present invention:
On the basis of Hummers improved method, liquid oxidatively Graphene is converted to powder solid, convenient storage and quantitative analysis.Find in a lot of research, the amount of the graphene oxide added in the preparation of graphene oxide based composites is all determined with quality, the present invention accurately can determine the quality adding graphene oxide easily, decrease liquid oxidatively Graphene evaporation drying calculating concentration, converse the tedious steps adding volume number again, shorten experimental period.
Accompanying drawing explanation
Fig. 1: graphene oxide optical picture
Fig. 2: graphene oxide SEM schemes
Fig. 3: graphene oxide TEM schemes
Embodiment
Be below specific embodiments of the invention, described embodiment is for describing the present invention, instead of restriction the present invention.
Embodiment 1:
(1) 2g Graphite Powder 99 and 1gNaNO is taken
3in round-bottomed flask, add the 46mL vitriol oil, ice bath stirs 5min;
(2) slowly 6gKMnO is added after
4, temperature is no more than 20 DEG C.Remove ice bath, at flask being placed in 35 ± 3 DEG C, react 2h.Now, solution is blackish green;
(3) slowly add 92mL deionized water, temperature is increased to 98 DEG C, adds 280mL warm water after keeping 15min, adds 30mLH after stirring 5min
2o
2;
(4) 1+9HCl80mL is added after cooling.After leaving standstill 12h, remove supernatant liquid, wash centrifuge washing lower floor solution to about pH=6,
(5) at about-60 DEG C lyophilize 24h, powder is made in grinding, namely obtains graphene oxide (GO).
Claims (6)
1. the preparation method of a powder-type graphene oxide, it is characterized in that: by Graphite Powder 99 and SODIUMNITRATE, the first ice bath stirring reaction of the vitriol oil, slowly add potassium permanganate mixing heating and oxidation for some time, add warm water afterwards and hydrogen peroxide is oxidized further, add 1+9HCl and remove unreacted oxide compound, centrifuge washing is neutral to pH, obtains golden yellow syrupy shape material, last lyophilize obtains sponge stratiform solid oxidation Graphene, after grinding, obtain Powder Oxidation Graphene.
2. the preparation method of Powder Oxidation Graphene according to claim 1, is characterized in that: the mass ratio of Graphite Powder 99, SODIUMNITRATE and the vitriol oil is 2: 1: 84.64, and under ice bath, churning time is 5min.
3. the preparation method of Powder Oxidation Graphene according to claim 1, is characterized in that: slowly add potassium permanganate, adds potassium permanganate and Graphite Powder 99 mass ratio is 3: 1, and temperature is no more than in 20 DEG C, reacts 2h at flask being placed in 35 ± 3 DEG C.
4. the preparation method of Powder Oxidation Graphene according to claim 1, it is characterized in that: after middle temperature reaction terminates, slowly add deionized water, the volume wherein added is 46mL/1g Graphite Powder 99, temperature is increased to 98 DEG C, add warm water after keeping 15min, now add the warm water that volume is 140mL/1g Graphite Powder 99, after stirring 5min, add the H that massfraction is 30%
2o
2, adding volume is 15mL/1g Graphite Powder 99.
5. the preparation method of Powder Oxidation Graphene according to claim 1, is characterized in that: pyroreaction terminates rear naturally cooling, and adding volume is 40mL/1g Graphite Powder 99 1+9HCl.After leaving standstill 12h, remove supernatant liquid, washing centrifuge washing lower floor solution, to about pH=6, obtains syrupy shape graphene oxide.
6. the preparation method of Powder Oxidation Graphene according to claim 1, is characterized in that: at about-60 DEG C lyophilize 24h ~ 32h, and powder is made in grinding, namely obtains graphene oxide.
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| CN201510860186.2A CN105399084A (en) | 2015-12-01 | 2015-12-01 | Preparation method of powder type graphene oxide |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107779038A (en) * | 2017-10-30 | 2018-03-09 | 汪涛 | Based on graphene water-base resin electrically-conducting paint and preparation method thereof |
| CN108478854A (en) * | 2018-04-28 | 2018-09-04 | 蒋春霞 | A kind of bearing hydrocolloid dressing and preparation method thereof |
| CN109179403A (en) * | 2018-11-20 | 2019-01-11 | 运城学院 | A kind of preparation method of graphite oxide |
| CN109529879A (en) * | 2018-12-26 | 2019-03-29 | 盐城锦明药业有限公司 | A kind of PdNi/RGO nanocatalyst and preparation method thereof |
| CN112028554A (en) * | 2020-08-28 | 2020-12-04 | 山东领军科技集团有限公司 | Graphene oxide modified diatomite fireproof insulation board |
| 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 |
| WO2021097660A1 (en) * | 2019-11-19 | 2021-05-27 | 南京先进生物材料与过程装备研究院有限公司 | Method for preparing graphene composite coating |
| CN115532296A (en) * | 2022-09-29 | 2022-12-30 | 兰州大学 | Composite catalyst, preparation method thereof and application thereof in degrading organic matters |
| US12017189B2 (en) | 2019-08-21 | 2024-06-25 | Shanghai Tetrels Material Technology Co., Ltd. | Devices and methods for water filtration membrane |
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| CN102795873A (en) * | 2012-07-30 | 2012-11-28 | 哈尔滨工业大学 | Method for interface modification of carbon/carbon composite material by graphene/polymer coating |
| CN103833020A (en) * | 2012-11-26 | 2014-06-04 | 东丽先端材料研究开发（中国）有限公司 | Method for preparing oxidized graphite |
| CN104163420A (en) * | 2014-07-25 | 2014-11-26 | 中国科学院深圳先进技术研究院 | Silver-doped graphene composite paper and preparation method |
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Patent Citations (3)
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| CN102795873A (en) * | 2012-07-30 | 2012-11-28 | 哈尔滨工业大学 | Method for interface modification of carbon/carbon composite material by graphene/polymer coating |
| CN103833020A (en) * | 2012-11-26 | 2014-06-04 | 东丽先端材料研究开发（中国）有限公司 | Method for preparing oxidized graphite |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107779038A (en) * | 2017-10-30 | 2018-03-09 | 汪涛 | Based on graphene water-base resin electrically-conducting paint and preparation method thereof |
| CN108478854A (en) * | 2018-04-28 | 2018-09-04 | 蒋春霞 | A kind of bearing hydrocolloid dressing and preparation method thereof |
| 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 |
| CN109179403A (en) * | 2018-11-20 | 2019-01-11 | 运城学院 | A kind of preparation method of graphite oxide |
| CN109529879A (en) * | 2018-12-26 | 2019-03-29 | 盐城锦明药业有限公司 | A kind of PdNi/RGO nanocatalyst and preparation method thereof |
| CN109529879B (en) * | 2018-12-26 | 2022-04-05 | 盐城师范学院 | PdNi/RGO nano-catalyst and preparation method thereof |
| US12017189B2 (en) | 2019-08-21 | 2024-06-25 | Shanghai Tetrels Material Technology Co., Ltd. | Devices and methods for water filtration membrane |
| WO2021097660A1 (en) * | 2019-11-19 | 2021-05-27 | 南京先进生物材料与过程装备研究院有限公司 | Method for preparing graphene composite coating |
| CN112028554A (en) * | 2020-08-28 | 2020-12-04 | 山东领军科技集团有限公司 | Graphene oxide modified diatomite fireproof insulation board |
| CN115532296A (en) * | 2022-09-29 | 2022-12-30 | 兰州大学 | Composite catalyst, preparation method thereof and application thereof in degrading organic matters |
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