CN104803376A - Efficient preparation process of graphene oxide nanosheets - Google Patents
Efficient preparation process of graphene oxide nanosheets Download PDFInfo
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- CN104803376A CN104803376A CN201510143599.9A CN201510143599A CN104803376A CN 104803376 A CN104803376 A CN 104803376A CN 201510143599 A CN201510143599 A CN 201510143599A CN 104803376 A CN104803376 A CN 104803376A
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Abstract
The invention discloses an efficient preparation process of efficient graphene oxide nanosheets. The preparation process is characterized in that (1), ordinary graphene powder is taken as a raw material, and the graphene oxide nanosheets with small sheet diameter sizes and small distribution range from 20 nm to 40 nm can be prepared; (2), the preparation cost is low, the cycle is short, and the yield is higher than 60%. The preparation process of the graphene oxide nanosheets comprises main steps as follows: (1), the ordinary graphene powder is taken as the raw material, and the graphene oxide is prepared with an improved Hummers method; (2), a graphene oxide aqueous solution and potassium permanganate are uniformly mixed and placed in a household microwave oven to be heated for a few minutes, and a porous graphene oxide and manganese dioxide mixture is obtained; (3), manganese dioxide in the mixture is removed with diluted hydrochloric acid and washed to be neutral with deionized water; (4), a neutral sample obtained through washing is placed in a water bath for ultrasonic processing for a period of time, and an aqueous solution of the graphene oxide nanosheets with a small size, a small distribution range and stable dispersity is obtained.
Description
Technical field
The invention belongs to the synthesis preparing technical field of carbon nanomaterial, relate to a kind of preparation technology of efficient stannic oxide/graphene nano sheet.
Background technology
Because graphene oxide has high specific surface area, outstanding biocompatibility, is easy to the dispersion stabilization that carries out chemically modified and had in water and in physiological solution, therefore in fields such as bio-nanotechnology and nano biological medical science, there is very vast potential for future development.Particularly sheet footpath size is less than the stannic oxide/graphene nano sheet of 100nm, is more suitable for being applied to biomedical sector.The current method preparing graphene oxide generally adopts the Hummers method of Hummers method or improvement.This method is simple, easy to operate, with low cost, but the sheet footpath of preparation-obtained graphene oxide is from tens nanometers to tens microns, and widely dispersed can not directly apply to above each field well.The approach preparing stannic oxide/graphene nano sheet at present mainly contains two kinds: the first is the graphite raw material adopting size minimum, and as gnf, Nano graphite powder etc., but these cost of material are too expensive; The second carries out reprocessing to the graphene oxide obtained, and as being separated graphene oxide sheet by high speed centrifugation or by being repeatedly oxidized to reduce size, but supercentrifugal process output is too low, and oxidizing process is too loaded down with trivial details repeatedly, and output is not high.Therefore, it is simple, with low cost that we need to explore a kind of technique, the production technique of the stannic oxide/graphene nano sheet that output is higher.Ultrasonic method is the method for the graphene oxide of a kind of conventional preparation different sheet footpaths size, but the distribution of sizes obtaining product is still very wide.And microwave heating method is a kind of method that can be rapidly heated to article in the short period of time, thus accelerate speed of response.Meanwhile, adding of potassium permanganate, can destroy graphene oxide structure at short notice, thus more easily be broken into the less graphene oxide sheet of size.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of efficient stannic oxide/graphene nano sheet.
Technical scheme of the present invention is as follows: first with common graphite powder for raw material, adopt and improve Hummers legal system for graphene oxide, then in graphene oxide water solution, a certain amount of potassium permanganate is added, use microwave heating again, the graphene oxide of porous can be obtained through overpickling, eventually pass water bath sonicator and just can obtain stannic oxide/graphene nano sheet.
Main innovate point of the present invention is as follows: with cheap common graphite powder for graphene oxide prepared by raw material, then by microwave heating method to graphene oxide process, can obtain that size is little, the stannic oxide/graphene nano sheet of narrow distribution range after ultrasonic.The invention provides a kind of novelty, efficient, low cost method to prepare stannic oxide/graphene nano sheet.
The method preparing porous oxidation Graphene in the inventive method is as follows: with 325 order ~ 2000 order Graphite Powder 99s for raw material, adopt the Hummers legal system improved for graphene oxide, preparation graphene oxide water solution, concentration is 0.05 ~ 0.6wt%, adding potassium permanganate to concentration is 1 ~ 20mg/mL, after stirring, put into microwave oven heating 2 ~ 20min (500 ~ 1000W), be cooled to room temperature, by dilute hydrochloric acid and the deionized water wash extremely neutrality of 0.1 ~ 1M, obtain porous oxidation Graphene.
In the inventive method, the preparation process of stannic oxide/graphene nano sheet is as follows: be positioned in water bath sonicator by the porous oxidation graphene aqueous solution obtained, under the power of 100 ~ 500W, ultrasonic 10 ~ 60min can obtain target product.
The present invention finds when preparing stannic oxide/graphene nano sheet, when preparing porous oxidation Graphene, when being less than 10min with the microwave-oven-heating time, graphene oxide sheet can be formed the isolated manganese dioxide nano particle of stochastic distribution, thus form the hole of stochastic distribution, obtain the stannic oxide/graphene nano sheet of size at 40 ~ 100nm after ultrasonic; When extending heat-up time, the manganese dioxide nano grain of formation can cover on graphene oxide sheet completely, and the stannic oxide/graphene nano sheet diameter obtained after finally ultrasonic can be less and distribution range is narrower.
The reagent that the present invention is used and material: Graphite Powder 99, potassium permanganate, SODIUMNITRATE, the vitriol oil, dilute hydrochloric acid and hydrogen peroxide are analytical pure.
Following equipment is have employed to characterize pattern and the structure of prepared stannic oxide/graphene nano sheet: field emission scanning electron microscope (FE-SEM, Nova Nano SEM 430) in the present invention.
Accompanying drawing explanation
Fig. 1 is preparation technology's schematic diagram of stannic oxide/graphene nano sheet.
Fig. 2 is the FE-SEM image of prepared stannic oxide/graphene nano sheet.
Fig. 3 is the sheet footpath statistical Butut of prepared stannic oxide/graphene nano sheet.
Embodiment
Below in conjunction with specific examples, the present invention is elaborated.
With 325 order Graphite Powder 99s for raw material, improvement Hummers method is adopted to prepare graphene oxide.In beaker, prepare the graphene oxide water solution that 100mL concentration is 0.5%, slowly add potassium permanganate while stirring, make its concentration reach 10mg/mL, then Keep agitation 15min.The graphene oxide stirred/potassium permanganate mixing solutions is put into microwave oven, and Modulating Power is 700W, setup times 10min.After reaction terminates, take out, after its temperature is down to room temperature, obtain the mixture of porous oxidation Graphene and Manganse Dioxide.Then thin up, uses hydrochloric acid and the deionized water of 0.1M successively, adopts centrifugal-washing-centrifugal technique, sample is washed till neutrality.Be transferred in water bath sonicator by being washed till neutral sample, arranging ultrasonic power is 100W, and ultrasonic time is 30min, carries out supersound process, finally obtains the aqueous solution of target product.
Claims (9)
1. the preparation technology of an efficient stannic oxide/graphene nano sheet, it is characterized in that preparing that slice footpath size is little, the stannic oxide/graphene nano sheet of narrow distribution range (20-40nm), and preparation cost is low, the cycle is short, output high (> 60%).Preparation process is as follows: adopt the Hummers method improved that common graphite powder is prepared into graphene oxide, then potassium permanganate is added, and with after microwave-oven-heating, obtain porous oxidation Graphene and Manganse Dioxide mixture, then use dilute hydrochloric acid and deionized water, adopt centrifugal-washing-centrifuging process, cleaning obtains porous oxidation Graphene repeatedly, carry out supersound process with water bath sonicator again, finally obtain target product.
2. method according to claim 1, is characterized in that the sheet footpath size obtaining target product concentrates within the scope of 20-40nm.
3. method according to claim 1, it is characterized in that adopted raw material is common graphite powder, it is of a size of 325 order ~ 2000 orders.
4. method according to claim 1, is characterized in that graphene oxide concentration used is 0.05 ~ 0.6%wt%.
5. method according to claim 1, is characterized in that the concentration of potassium permanganate is 1 ~ 20mg/mL.
6. method according to claim 1, is characterized in that condition when adopting microwave heating: heating power 500 ~ 1000W, time 2 ~ 20min.
7. method according to claim 1, is characterized in that dilute hydrochloric acid concentration used is 0.1 ~ 1M.
8. method according to claim 1, it is characterized in that adopted centrifugal-parameter of washing-centrifuging process is: centrifugal rotational speed is 4000 ~ 12000rpm, and centrifugation time is 10 ~ 60min.
9. method according to claim 1, it is characterized in that the power of water bath sonicator is 100 ~ 500W, ultrasonic time is 10 ~ 60min.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293481A (en) * | 2015-12-03 | 2016-02-03 | 中国工程物理研究院化工材料研究所 | Method for ultrasonically cutting graphene oxide |
| CN107128907A (en) * | 2017-05-04 | 2017-09-05 | 上海理工大学 | A kind of size classification method of improved graphene oxide and graphene |
| CN107585764A (en) * | 2017-09-07 | 2018-01-16 | 中国热带农业科学院南亚热带作物研究所 | Porous oxidation graphene and preparation method thereof and porous oxidation graphene coated slow-release chemical fertilizer and preparation method thereof |
| CN108658062A (en) * | 2017-03-28 | 2018-10-16 | 纳米石墨烯股份有限公司 | Method and apparatus for manufacturing non-oxidized graphite alkene plate |
| WO2019089708A1 (en) * | 2017-10-31 | 2019-05-09 | Nitto Denko Corporation | Method for chemically exfoliating graphite |
| CN112226104A (en) * | 2020-09-22 | 2021-01-15 | 广东极客亮技术有限公司 | Ultraviolet-proof graphene coating with hierarchical pore structure, ultraviolet-proof material and preparation method of ultraviolet-proof graphene coating |
| CN115057437A (en) * | 2022-05-30 | 2022-09-16 | 苏州大学 | SnO (stannic oxide) 2 /NiO/graphene ternary composite material and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293481A (en) * | 2015-12-03 | 2016-02-03 | 中国工程物理研究院化工材料研究所 | Method for ultrasonically cutting graphene oxide |
| CN108658062A (en) * | 2017-03-28 | 2018-10-16 | 纳米石墨烯股份有限公司 | Method and apparatus for manufacturing non-oxidized graphite alkene plate |
| CN107128907A (en) * | 2017-05-04 | 2017-09-05 | 上海理工大学 | A kind of size classification method of improved graphene oxide and graphene |
| CN107585764A (en) * | 2017-09-07 | 2018-01-16 | 中国热带农业科学院南亚热带作物研究所 | Porous oxidation graphene and preparation method thereof and porous oxidation graphene coated slow-release chemical fertilizer and preparation method thereof |
| CN107585764B (en) * | 2017-09-07 | 2020-04-14 | 中国热带农业科学院南亚热带作物研究所 | Porous graphene oxide and preparation method thereof, and porous graphene oxide coated slow-release fertilizer and preparation method thereof |
| WO2019089708A1 (en) * | 2017-10-31 | 2019-05-09 | Nitto Denko Corporation | Method for chemically exfoliating graphite |
| CN111315684A (en) * | 2017-10-31 | 2020-06-19 | 日东电工株式会社 | Method for chemically stripping graphite |
| CN112226104A (en) * | 2020-09-22 | 2021-01-15 | 广东极客亮技术有限公司 | Ultraviolet-proof graphene coating with hierarchical pore structure, ultraviolet-proof material and preparation method of ultraviolet-proof graphene coating |
| CN112226104B (en) * | 2020-09-22 | 2021-08-31 | 广东极客亮技术有限公司 | Ultraviolet-proof graphene coating with hierarchical pore structure, ultraviolet-proof material and preparation method of ultraviolet-proof graphene coating |
| CN115057437A (en) * | 2022-05-30 | 2022-09-16 | 苏州大学 | SnO (stannic oxide) 2 /NiO/graphene ternary composite material and preparation method and application thereof |
| CN115057437B (en) * | 2022-05-30 | 2023-11-24 | 苏州大学 | SnO (tin oxide) 2 NiO/graphene ternary composite material and preparation method and application thereof |
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