CN104261400A - Reduction method of graphene oxide - Google Patents

Reduction method of graphene oxide Download PDF

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Publication number
CN104261400A
CN104261400A CN201410540915.1A CN201410540915A CN104261400A CN 104261400 A CN104261400 A CN 104261400A CN 201410540915 A CN201410540915 A CN 201410540915A CN 104261400 A CN104261400 A CN 104261400A
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graphene oxide
graphene
reducing
solution
aqueous solution
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CN104261400B (en
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钱景
赵兵
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Zhuhai Carbon Carbon Composite Material Co Ltd
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Abstract

The invention relates to a reduction method of graphene oxide. The method comprises steps as follows: preparing aloe gel salable in the market into an aqueous solution of 0.1-100 g/L in a volume ratio of 10:1-1:1, mixing the aqueous solution with a graphene oxide solution with the mass fraction of 0.01-0.5 g/L, stirring the mixture at the temperature of 20-80 DEG C for 1-48 h to obtain a graphene solution, repeatedly washing the graphene solution with ethanol and deionized water, and performing centrifugation and drying treatment to obtain graphene powder. According to the method, the aloe gel salable in the market is directly used as a reducing agent, and the method has the advantages of simple technology, wide raw material source, mild reaction, environment-friendliness and the like.

Description

A kind of method of reducing of graphene oxide
Technical field
The invention belongs to synthesis and the technical field of nano material of Graphene, particularly a kind of method of reducing of graphene oxide.
Background technology
2004, Univ Manchester UK physicist An Deliehaimu and Constantine Nuo Woxiaoluofu, utilize the method for tearing scotch tape, from graphite, successfully isolate the Graphene of individual layer atomic arrangement, therefore two people also obtain the Nobel Prize in physics (Science of 2010,2004,306 (5696): 666-669).Graphene by carbon atom with sp 2hybridized orbital composition hexangle type honeycomb lattice, its structural unit is carbon six-ring, and it is a kind of two-dimensional material only having monolayer carbon atomic thickness.Graphene is the basic system unit forming carbon-based material.It can be wrapped to form zero dimension Fullerenes, is rolled into one dimension carbon nanotube, is piled into three-dimensional graphite layer by layer.From that day that Graphene finds, Graphene has just become focus and the focus of research, is widely used in fields such as ultracapacitor, transparency electrode, sea water desaltination, photodiode, sensor, Chu Qing, solar cell, support of the catalyst, matrix material, biologic bracket material, bio-imaging, drug conveying, weaving, printing and dyeing.
Graphene has excellent machinery, electricity, thermal property, anti-microbial property.Graphene is material the thinnest in the world, and it only has the thickness of individual layer atom, is about 0.335nm.Graphene is almost completely transparent, and only absorb the light of 2.3%, transmittance is up to 97.7%.Resistivity 10 -6Ω/cm, than copper or silver lower, be the material that at present resistivity is minimum in the world.Graphene has great specific surface area, and its theoretical value is up to 2630m 2/ g.Thermal conductivity is up to 5300W/mK, and under normal temperature, electronic mobility is more than 15000cm 2/ Vs, than carbon nanotube and silicon single crystal high.Young's modulus is 1.1TPa, and breaking tenacity is up to 130GPa.
The preparation method of Graphene mainly contains: micromechanics stripping method, seal cut transfer printing, liquid phase stripping method, chemical Vapor deposition process, aerosol high-temperature decomposition, epitaxial growth method, decolorizing carbon compound film conversion method, graphene oxide (GO) reduction method and organic synthesis method etc.Wherein GO reduction method has the features such as cost is low, productive rate is high and can be mass, and is used widely.Reductive agent conventional at present comprises hydrazine hydrate, dimethylhydrazine, phenols, sodium borohydride, sulfocompound, alcohols etc. (charcoal element technology, 2013,32 (5): 30-36).But because GO reduction method often uses the poisonous or expensive reagent such as hydrazine or sodium borohydride as reductive agent, therefore developing green, environmental protection, efficient and cheap chemical reduction technology are very necessary.
Aloe (formal name used at school Aloe), originates in Mediterranean Sea, Africa, is Eremurus chinensis section per nnial herb, according to wild aloe kind kind more than 300 of textual criticism, is mainly distributed in the ground such as Africa.Aloe is easy to plantation because of it, and quite liking by masses, is the ornamental plant that floral leaf has both.Edible kind only has six kinds.Containing more than 200 kinds of compounds in the blade of aloe, comprising having 20 kinds of mineral substance, 18 seed amino acids, 12 kinds of VITAMIN and multiple mucopolysaccharide, lipid acid, Anthraquinones and flavonoid compound, sugar, organized enzyme etc.
Aloe can as astringent matter, lubricant, can antifungal, bacterium and virus, be applied to the aspect such as healing and irritation cell regeneration of burn, wound.For oral administration can help to reduce cholesterol, reduce the inflammatory response caused because of radiotherapy, the hyperplasia of the people's peripheral vessel increasing poor circulation and relax gastrointestinal stimulation state, help healing and as laxative.
Aloe vera gel extracts to form from natural herbs aloe, purity is very high, have no side effect, incised wound, scratch, wound are festered, scalded, skin pruritus, comedo, blackspot, mosquito bite, toothache, labial angle fester, operative scar etc. has obvious booster action, safe and reliable, be called as multi-purpose adhesive.Aloe vera gel brand on sale in the market mainly contains: perfect aloe vera gel, Korea S's nature paradise moisturizing aloe vera gel, the clean aloe vera gel of Artline, Han Shu aloe vera gel, the organic beauty treatment aloe vera gel of Webster, all alizarin aloe vera gels etc.
At present, existing xitix, pyrogallol, Resorcinol, tea-polyphenol, Trisodium Citrate, glucose, fructose, sucrose etc. are as the report of the reductive agent of graphene oxide.But yet there are no and Aloe extract or the aloe vera gel that can sell on the market are directly used in redox graphene.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, a kind of method of reducing of graphene oxide is provided.
The present invention is achieved by following technical proposals:
According to the volume ratio of 10:1-1:1, the aloe vera gel can sold on the market is configured to the aqueous solution of 0.1-100g/L, mix with the graphene oxide solution of massfraction 0.01-0.5g/L, 1-48h is stirred under the temperature condition of 20 DEG C-80 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
Preferably, graphene oxide is obtained through ultrasonic delamination by graphite oxide, is single-layer graphene oxide, multilayer graphene oxide or the mixture of the two.
Preferably, centrifugal is with the centrifugal 5-20min of the rotating speed of 8000-12000r/min.
Preferably, drying treatment refers to and loft drier temperature is set in 40 DEG C, dry 1-24h under the environment of vacuum.
The present invention has following beneficial effect:
The aloe vera gel can sold on the market, can directly as the reductive agent of graphene oxide mostly containing the composition such as polysaccharide, amino acid, VITAMIN, anthraquinone, possess that technique is simple, raw material sources extensive, reaction temperature and, the advantage such as environmental protection.
Embodiment
Below in conjunction with embodiment, set forth the present invention further.
Embodiment 1:
Perfect aloe vera gel (Perfect's production) is configured to the aqueous solution of the 10g/L of 10ml, mix with the graphene oxide solution of 10ml massfraction 0.1g/L, 24h is stirred under the temperature condition of 20 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, the centrifugal 10min of rotating speed of 9000r/min, under 40 DEG C of vacuum environments, dry 20h obtains graphene powder.
Embodiment 2:
Han Shu aloe vera gel (production of Shanghai Han Shu makeup company limited) is configured to the aqueous solution of the 20g/L of 10ml, mix with the graphene oxide solution of 2ml massfraction 0.4g/L, 4h is stirred under the temperature condition of 40 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, the centrifugal 10min of rotating speed of 8000r/min, under 40 DEG C of vacuum environments, dry 24h obtains graphene powder.
Embodiment 3:
Korea S's nature paradise moisturizing aloe vera gel (nature paradise makeup Co., Ltd. of Korea S produces) is configured to the aqueous solution of the 50g/L of 10ml, mix with the graphene oxide solution of 5ml massfraction 0.05g/L, 12h is stirred under the temperature condition of 60 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, the centrifugal 15min of rotating speed of 10000r/min, under 40 DEG C of vacuum environments, dry 4h is to graphene powder.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.

Claims (8)

1. the method for reducing of a graphene oxide, it is characterized in that: according to certain volume ratio, the aloe vera gel can sold on the market is configured to the aqueous solution of certain mass mark, mix with the graphene oxide water solution of certain mass mark, under certain temperature condition, stir 1-48h, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
2. the method for reducing of a kind of graphene oxide according to claim 1, is characterized in that, described volume ratio is 10:1-1:1.
3. the environment-friendly preparation method thereof of a kind of nanometer silver according to claim 1, is characterized in that, the massfraction of the aloe vera gel aqueous solution is 0.1-100g/L.
4. the method for reducing of a kind of graphene oxide according to claim 1, is characterized in that, the massfraction of graphene oxide is 0.01-0.5g/L.
5. the method for reducing of a kind of graphene oxide according to claim 1, is characterized in that, described graphene oxide is obtained through ultrasonic delamination by graphite oxide, is single-layer graphene oxide, multilayer graphene oxide or the mixture of the two.
6. the method for reducing of a kind of graphene oxide according to claim 1, is characterized in that, described temperature condition is 20 DEG C-80 DEG C.
7. the method for reducing of a kind of graphene oxide according to claim 1, is characterized in that, described centrifugal be with the centrifugal 5-20min of the rotating speed of 8000-12000r/min.
8. the method for reducing of a kind of graphene oxide according to claim 1, is characterized in that, described drying treatment refers to and loft drier temperature is set in 40 DEG C, dry 1-24h under the environment of vacuum.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104826629A (en) * 2015-04-17 2015-08-12 华南师范大学 Synthetic method and applications of porous graphene composite catalyst
CN104986754A (en) * 2015-06-11 2015-10-21 中国科学院山西煤炭化学研究所 Graphene-based thermal conductive film preparing method
CN112998037A (en) * 2021-03-09 2021-06-22 赵平胜 Novel leather sterilization, mildew removal, decontamination and renovation compound repairing liquid and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101602504A (en) * 2009-07-16 2009-12-16 上海交通大学 Graphene preparation method based on xitix
CN102530927A (en) * 2010-12-24 2012-07-04 中国科学院兰州化学物理研究所 Graphene preparation method
CN102786047A (en) * 2012-06-21 2012-11-21 金陵科技学院 Method for preparing environment-friendly water-soluble graphene
WO2013081248A1 (en) * 2011-11-30 2013-06-06 한국전기연구원 Graphene oxide reduced material dispersed at high concentration by cation-π interaction and method for manufacturing same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101602504A (en) * 2009-07-16 2009-12-16 上海交通大学 Graphene preparation method based on xitix
CN102530927A (en) * 2010-12-24 2012-07-04 中国科学院兰州化学物理研究所 Graphene preparation method
WO2013081248A1 (en) * 2011-11-30 2013-06-06 한국전기연구원 Graphene oxide reduced material dispersed at high concentration by cation-π interaction and method for manufacturing same
CN102786047A (en) * 2012-06-21 2012-11-21 金陵科技学院 Method for preparing environment-friendly water-soluble graphene

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104826629A (en) * 2015-04-17 2015-08-12 华南师范大学 Synthetic method and applications of porous graphene composite catalyst
CN104826629B (en) * 2015-04-17 2018-08-07 华南师范大学 A kind of synthetic method of porous graphene composite catalyst and application
CN104986754A (en) * 2015-06-11 2015-10-21 中国科学院山西煤炭化学研究所 Graphene-based thermal conductive film preparing method
CN112998037A (en) * 2021-03-09 2021-06-22 赵平胜 Novel leather sterilization, mildew removal, decontamination and renovation compound repairing liquid and preparation method thereof

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Inventor after: Chen Xiaogang

Inventor after: Ma Ning

Inventor before: Qian Jing

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Address after: 519000 Guangdong city of Zhuhai province Hengqin Baohua Road No. 6, room 105 -14433

Patentee after: Zhuhai carbon carbon composite material Co Ltd

Address before: Jiangsu city of Suzhou province Xiangcheng District 215000 yuan street and imperial kiln road and the junction of Cambridge Xi An Yuan Lu shore garden 5 building 2101

Patentee before: Qian Jing