CN105016334A - Method for reducing graphene oxide through alkylated cyclodextrin - Google Patents
Method for reducing graphene oxide through alkylated cyclodextrin Download PDFInfo
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- CN105016334A CN105016334A CN201510517542.0A CN201510517542A CN105016334A CN 105016334 A CN105016334 A CN 105016334A CN 201510517542 A CN201510517542 A CN 201510517542A CN 105016334 A CN105016334 A CN 105016334A
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- graphene
- alkylated cyclodextrin
- graphene oxide
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- cyclodextrin
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 25
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical class O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 5
- 229920000858 Cyclodextrin Polymers 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- -1 cyclic oligosaccharide Chemical class 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 3
- 125000003535 D-glucopyranosyl group Chemical group [H]OC([H])([H])[C@@]1([H])OC([H])(*)[C@]([H])(O[H])[C@@]([H])(O[H])[C@]1([H])O[H] 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 230000032798 delamination Effects 0.000 claims description 2
- 229920001542 oligosaccharide Polymers 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- DIIIISSCIXVANO-UHFFFAOYSA-N 1,2-Dimethylhydrazine Chemical compound CNNC DIIIISSCIXVANO-UHFFFAOYSA-N 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000001116 FEMA 4028 Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 229960004853 betadex Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 229940080345 gamma-cyclodextrin Drugs 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a method for reducing graphene oxide through alkylated cyclodextrin. The method comprises steps as follows: an alkylated cyclodextrin aqueous solution with the mass percent of 0.1%-10% and 0.01-1 g/L of a graphene oxide solution are mixed in a volume ratio being (100:1)-(1:1), the mixture has a hydrothermal reaction for 1-24 h at the temperature of 180-220 DEG C, and a graphene solution is obtained; the graphene solution is repeatedly washed with ethanol and deionized water, is configured and dried, and graphene powder is obtained. According to the method for reducing graphene oxide through alkylated cyclodextrin, alkylated cyclodextrin is adopted as a reducing agent, the graphene is prepared through the hydrothermal reaction under the condition of no addition of any stabilizing agent and dispersing agent, environmental protection is realized, the cost is low, the process is simple, and the prepared graphene has good dispersibility and stability.
Description
Technical field
The invention belongs to synthesis and the technical field of nano material of Graphene, particularly a kind of method of alkylated cyclodextrin redox graphene.
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.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, a kind of method of alkylated cyclodextrin redox graphene is provided.
The present invention is achieved by following technical proposals:
According to the volume ratio of 100:1-1:1, the alkylated cyclodextrin aqueous solution of mass percent 0.01%-10% is mixed with the graphene oxide solution of 0.01-1g/L, hydro-thermal reaction 1-24h at the temperature of 180-220 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
Preferably, described cyclodextrin contains the cyclic oligosaccharide of 6-12 D-glucopyranose units.
Preferably, the molecule outside surface of described alkylated cyclodextrin connects at least one chain alkyl C
3-C
20.
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.
Advantage of the present invention:
The present invention adopts the alkylated cyclodextrin of environmental protection as reductive agent, method by hydro-thermal reaction under the condition of not adding any stablizer, dispersion agent prepares Graphene, environmental protection, with low cost, technique are simple, and the Graphene prepared has good dispersiveness and stability.
Embodiment
Below in conjunction with embodiment, set forth the present invention further.
Embodiment 1:
Own for the 2-0-of 80ml mass percent 0.5% group-beta-cyclodextrin is mixed with the graphene oxide solution of the 0.1g/L of 2ml, hydro-thermal reaction 10h at the temperature of 180 DEG C, obtains graphene solution, repeatedly cleans with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
Embodiment 2:
The 2-0-of 40ml mass percent 1% pentadecyl-alpha-cylodextrin aqueous solution is mixed with the 0.05g/L graphene oxide solution of 2ml, hydro-thermal reaction 12h at the temperature of 200 DEG C, obtains graphene solution, repeatedly cleans with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
Embodiment 3:
By 2 of 10ml mass percent 5%, 6-bis--0-amyl group-γ-cyclodextrin aqueous solution mixes with the graphene oxide solution of the 0.5g/L of 5ml, hydro-thermal reaction 24h at the temperature of 220 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
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 (5)
1. the method for an alkylated cyclodextrin redox graphene, it is characterized in that: according to certain volume ratio, the alkylated cyclodextrin aqueous solution of mass percent 0.1%-10% is mixed with the graphene oxide solution of 0.01-1g/L, hydro-thermal reaction 1-24h at the temperature of 180-220 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
2. the method for a kind of alkylated cyclodextrin redox graphene according to claim 1, is characterized in that, described volume ratio is 100:1-1:1.
3. the method for a kind of alkylated cyclodextrin redox graphene according to claim 1, is characterized in that: described cyclodextrin contains the cyclic oligosaccharide of 6-12 D-glucopyranose units.
4. the method for a kind of alkylated cyclodextrin redox graphene according to claim 1, is characterized in that: the molecule outside surface of described alkylated cyclodextrin connects at least one chain alkyl C
3-C
20.
5. the method for a kind of alkylated cyclodextrin redox graphene according to claim 1, it 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510517542.0A CN105016334A (en) | 2015-08-22 | 2015-08-22 | Method for reducing graphene oxide through alkylated cyclodextrin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510517542.0A CN105016334A (en) | 2015-08-22 | 2015-08-22 | Method for reducing graphene oxide through alkylated cyclodextrin |
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| Publication Number | Publication Date |
|---|---|
| CN105016334A true CN105016334A (en) | 2015-11-04 |
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|---|---|---|---|
| CN201510517542.0A Pending CN105016334A (en) | 2015-08-22 | 2015-08-22 | Method for reducing graphene oxide through alkylated cyclodextrin |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102183557A (en) * | 2011-01-22 | 2011-09-14 | 青岛大学 | Preparation method of cyclodextrin functionalized graphene |
| WO2014183243A1 (en) * | 2013-05-14 | 2014-11-20 | 中国科学院福建物质结构研究所 | Method for preparing graphene material and use thereof in chemical energy storage and/or conversion |
| US20150045311A1 (en) * | 2012-02-28 | 2015-02-12 | Cydex Pharmaceuticals Inc. | Alkylated cyclodextrin compositions and processes for preparing and using the same |
-
2015
- 2015-08-22 CN CN201510517542.0A patent/CN105016334A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102183557A (en) * | 2011-01-22 | 2011-09-14 | 青岛大学 | Preparation method of cyclodextrin functionalized graphene |
| US20150045311A1 (en) * | 2012-02-28 | 2015-02-12 | Cydex Pharmaceuticals Inc. | Alkylated cyclodextrin compositions and processes for preparing and using the same |
| WO2014183243A1 (en) * | 2013-05-14 | 2014-11-20 | 中国科学院福建物质结构研究所 | Method for preparing graphene material and use thereof in chemical energy storage and/or conversion |
Non-Patent Citations (1)
| Title |
|---|
| 于金海: "石墨烯的非共价功能化修饰及载药系统研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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Application publication date: 20151104 |