CN105217607A - A kind of graphene preparation method based on xylogen - Google Patents
A kind of graphene preparation method based on xylogen Download PDFInfo
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- CN105217607A CN105217607A CN201510517524.2A CN201510517524A CN105217607A CN 105217607 A CN105217607 A CN 105217607A CN 201510517524 A CN201510517524 A CN 201510517524A CN 105217607 A CN105217607 A CN 105217607A
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Abstract
The present invention relates to a kind of graphene preparation method based on xylogen, first by lignin dissolution in deionized water, be configured to the xylogen aqueous solution of mass percent 5%-10%, add NaOH adjust ph=10-12, then according to the volume ratio of 10:1-1:1, the xylogen aqueous solution of NaOH process is mixed with the graphene oxide solution of 0.01-1g/L, hydro-thermal reaction 1-24h at the temperature of 120-160 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.The present invention adopts the xylogen after alkaline purification as reductive agent, prepares Graphene by hydro-thermal reaction method, and environmental protection, with low cost, technique are simple, and the Graphene prepared has good dispersiveness and stability.
Description
Technical field
The invention belongs to synthesis and the technical field of nano material of Graphene, particularly a kind of graphene preparation method based on xylogen.
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 carbonnanotube, 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.
Xylogen is a kind of complexity, noncrystalline, three-dimensional netted phenols high molecular polymer, containing a large amount of phenolic hydroxyl group, carboxyl and carbonyl isoreactivity group in molecular structure.Xylogen is extensively present in higher plant cell, is one of basic chemical constitution of coniferals, deciduous tree class and straw or like vegetable, is that occurring in nature is only second to cellulosic second largest renewable resources.Form supramolecular system at xylogen in plant materials together with Mierocrystalline cellulose, hemicellulose etc., xylogen as cellulosic tackiness agent, to strengthen the physical strength of plant materials.It take xylogen as the method that Graphene prepared by raw material that Chinese invention patent CN201310472057.7 discloses a kind of, prepares Graphene by the method for xylogen being carried out to simple thermal treatment.But yet there are no with xylogen is the report that redox graphene RGO prepared by reductive agent.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, a kind of graphene preparation method based on xylogen is provided.
The present invention is achieved by following technical proposals:
By lignin dissolution in deionized water, be configured to the xylogen aqueous solution of mass percent 5%-10%, add NaOH adjust ph=10-12, then according to the volume ratio of 10:1-1:1, the xylogen aqueous solution of NaOH process is mixed with the graphene oxide solution of 0.01-1g/L, hydro-thermal reaction 1-24h at the temperature of 120-160 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
Preferably, xylogen is the one in alkali lignin, sulfonated lignin.
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 60-80 DEG C, dry 1-12h under the environment of vacuum.
Advantage of the present invention:
The present invention adopts the xylogen of environmental protection as reductive agent, the groups such as the phenolic hydroxyl group of xylogen surface containing reductibility, Graphene is prepared by the method for chemical reduction, this preparation method's 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:
0.5g alkali lignin is dissolved in 9.5ml deionized water, be configured to the alkali lignin aqueous solution of mass percent 5%, add NaOH adjust ph=10, the xylogen aqueous solution of NaOH process is mixed with the graphene oxide solution of the 0.1g/L of 1ml, hydro-thermal reaction 12h at the temperature of 120 DEG C, obtains graphene solution, repeatedly cleans with ethanol and deionized water, with the centrifugal 20min of the rotating speed of 8000r/min, under the environment of 60 DEG C of vacuum, dry 12h obtains graphene powder.
Embodiment 2:
1g sulfonated lignin is dissolved in 9ml deionized water, be configured to the xylogen aqueous solution of mass percent 10%, add NaOH adjust ph=11, the xylogen aqueous solution of NaOH process is mixed with the graphene oxide solution of the 0.5g/L of 2ml, hydro-thermal reaction 18h at the temperature of 140 DEG C, obtains graphene solution, repeatedly cleans with ethanol and deionized water, with the centrifugal 10min of the rotating speed of 10000r/min, under the environment of 70 DEG C of vacuum, dry 6h obtains graphene powder.
Embodiment 3:
0.8g alkali lignin is dissolved in 9.2ml deionized water, be configured to the xylogen aqueous solution of mass percent 8%, add NaOH adjust ph=12, the xylogen aqueous solution of NaOH process is mixed with the graphene oxide solution of the 0.05g/L of 5ml, hydro-thermal reaction 2h at the temperature of 160 DEG C, obtains graphene solution, repeatedly cleans with ethanol and deionized water, with the centrifugal 5min of the rotating speed of 12000r/min, under the environment of 80 DEG C of vacuum, dry 2h obtains 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 (6)
1., based on a graphene preparation method for xylogen, it is characterized in that:
(1) by lignin dissolution in deionized water, be configured to the xylogen aqueous solution of mass percent 5%-10%, add NaOH adjust ph=10-12, then according to certain volume ratio, the xylogen aqueous solution of NaOH process is mixed with the graphene oxide solution of 0.01-1g/L, hydro-thermal reaction 1-24h at the temperature of 120-160 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
2. a kind of graphene preparation method based on xylogen according to claim 1, is characterized in that, described xylogen is the one in alkali lignin, sulfonated lignin.
3. a kind of graphene preparation method based on xylogen according to claim 1, is characterized in that, described volume ratio is 10:1-1:1.
4. a kind of graphene preparation method based on xylogen 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.
5. a kind of graphene preparation method based on xylogen according to claim 1, is characterized in that, described centrifugal be with the centrifugal 5-20min of the rotating speed of 8000-12000r/min.
6. a kind of graphene preparation method based on xylogen according to claim 1, is characterized in that, described drying treatment refers to and loft drier temperature is set in 60-80 DEG C, dry 1-12h under the environment of vacuum.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106024423A (en) * | 2016-05-25 | 2016-10-12 | 华南理工大学 | Lignin-based graphene/zinc oxide hybrid composite material and preparation method and application |
| CN107814378A (en) * | 2017-11-03 | 2018-03-20 | 福州大学 | Lignin functional modification graphene and preparation method thereof |
| CN108977198A (en) * | 2018-07-12 | 2018-12-11 | 北京林业大学 | A kind of method that lignin prepares single crystal graphene quantum dot |
| CN109023520A (en) * | 2018-07-12 | 2018-12-18 | 北京林业大学 | A kind of method that black liquid prepares high quality single crystal graphene |
| CN109205603A (en) * | 2017-06-30 | 2019-01-15 | 中国科学院宁波材料技术与工程研究所 | The dispersing method of graphene |
| CN109336107A (en) * | 2018-11-05 | 2019-02-15 | 浙江科技学院 | A kind of preparation method of alkali lignin porous carbon electrode material |
| CN109437168A (en) * | 2019-01-03 | 2019-03-08 | 兖矿集团有限公司 | A kind of graphene hydrogel and preparation method thereof |
| CN110092947A (en) * | 2018-01-30 | 2019-08-06 | 山东省圣泉生物质石墨烯研究院 | A kind of micro-nano cellulose compound, and its preparation method and application |
| CN111415825A (en) * | 2020-03-18 | 2020-07-14 | 齐鲁工业大学 | Lignin-based flexible fibrous electrode and preparation method and application thereof |
| CN111454497A (en) * | 2019-01-22 | 2020-07-28 | 南京工业大学 | Graphene modified lignin enhanced polyolefin wood-plastic composite material and preparation method thereof |
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| CN102219211A (en) * | 2011-04-16 | 2011-10-19 | 华南理工大学 | Method for reducing and decorating graphene oxide by plant polyphenol and derivant thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106024423B (en) * | 2016-05-25 | 2018-09-14 | 华南理工大学 | Lignin-base graphene/zinc oxide hybridization composite material and preparation method and application |
| CN106024423A (en) * | 2016-05-25 | 2016-10-12 | 华南理工大学 | Lignin-based graphene/zinc oxide hybrid composite material and preparation method and application |
| CN109205603A (en) * | 2017-06-30 | 2019-01-15 | 中国科学院宁波材料技术与工程研究所 | The dispersing method of graphene |
| CN107814378A (en) * | 2017-11-03 | 2018-03-20 | 福州大学 | Lignin functional modification graphene and preparation method thereof |
| CN110092947A (en) * | 2018-01-30 | 2019-08-06 | 山东省圣泉生物质石墨烯研究院 | A kind of micro-nano cellulose compound, and its preparation method and application |
| CN108977198A (en) * | 2018-07-12 | 2018-12-11 | 北京林业大学 | A kind of method that lignin prepares single crystal graphene quantum dot |
| CN109023520A (en) * | 2018-07-12 | 2018-12-18 | 北京林业大学 | A kind of method that black liquid prepares high quality single crystal graphene |
| CN109336107A (en) * | 2018-11-05 | 2019-02-15 | 浙江科技学院 | A kind of preparation method of alkali lignin porous carbon electrode material |
| CN109437168A (en) * | 2019-01-03 | 2019-03-08 | 兖矿集团有限公司 | A kind of graphene hydrogel and preparation method thereof |
| CN109437168B (en) * | 2019-01-03 | 2021-11-05 | 兖矿集团有限公司 | Graphene hydrogel and preparation method thereof |
| CN111454497A (en) * | 2019-01-22 | 2020-07-28 | 南京工业大学 | Graphene modified lignin enhanced polyolefin wood-plastic composite material and preparation method thereof |
| CN111415825A (en) * | 2020-03-18 | 2020-07-14 | 齐鲁工业大学 | Lignin-based flexible fibrous electrode and preparation method and application thereof |
| CN111415825B (en) * | 2020-03-18 | 2022-04-15 | 齐鲁工业大学 | Lignin-based flexible fibrous electrode and preparation method and application thereof |
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