CN105036124A - Method for preparing graphene from polysaccharide - Google Patents
Method for preparing graphene from polysaccharide Download PDFInfo
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- CN105036124A CN105036124A CN201510517526.1A CN201510517526A CN105036124A CN 105036124 A CN105036124 A CN 105036124A CN 201510517526 A CN201510517526 A CN 201510517526A CN 105036124 A CN105036124 A CN 105036124A
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Abstract
The invention relates to a method for preparing graphene from polysaccharide, which comprises the following steps: mixing a 0.01-10 wt% polyglucose water solution and a 0.01-1 g/L graphene oxide solution in a volume ratio of 100:1-1:1, carrying out hydrothermal reaction at 180-220 DEG C for 1-24 hours to obtain a graphene solution, and repeatedly washing with ethanol and deionized water, centrifuging and drying to obtain the graphene powder. The graphene is prepared by chemical reduction by using the green environment-friendly polyglucose as the reducer under the condition of not adding any stabilizer or dispersing agent. The method has the advantages of environment friendliness, low cost and simple technique. The prepared graphene has favorable dispersity and stability.
Description
Technical field
The invention belongs to synthesis and the technical field of nano material of Graphene, particularly a kind of saccharan prepares the method for 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 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.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, provide a kind of saccharan to prepare the method for Graphene.
The present invention is achieved by following technical proposals:
According to the volume ratio of 100:1-1:1, the poly-dextrose 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, poly-dextrose is generated by glucose, Sorbic Acid, citric acid thermopolymerization.Poly-dextrose comprises the one in the poly-dextrose of modification or grafting, or their arbitrary combination.
Preferably, modified polyglucose is ketonization poly-dextrose, aldehyde radical poly-dextrose, amination poly-dextrose, and grafting poly-dextrose is Methionin grafting poly-dextrose, L-glutamic acid grafting poly-dextrose, aspartic acid grafting poly-dextrose.
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, with the centrifugal 10-20min of the rotating speed of 10000-12000r/min.
Preferably, drying treatment refers to and loft drier temperature is set in 40-80 DEG C, dry 1-24h under the environment of vacuum.
Poly-dextrose used in the present invention is as one water-soluble dietary fibre of good performance, and because having, heat is low, good stability, tolerance high and cause the concern of people.After FDA's approval poly-dextrose in 1981 uses as foodstuff additive, be developed rapidly in recent years, there are multiple countries and regions also in succession to have approved the use of poly-dextrose successively, in the numerous food that current domestic and international market is sold, all with the addition of poly-dextrose.
Advantage of the present invention:
The present invention adopts the poly-dextrose of environmental protection as reductive agent, method by chemical reduction 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:
The ketonization poly-dextrose of 80ml mass percent 0.5% 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, obtain graphene solution, repeatedly clean with ethanol and deionized water, the centrifugal 10min of rotating speed of 10000r/min, under 40 DEG C of vacuum environments, dry 20h obtains graphene powder.
Embodiment 2:
The amination poly-dextrose aqueous solution of 40ml mass percent 1% is mixed with the 0.05g/L graphene oxide solution of 2ml, hydro-thermal reaction 12h at the temperature of 200 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, the centrifugal 150min of rotating speed of 11000r/min, under 60 DEG C of vacuum environments, dry 10h obtains graphene powder.
Embodiment 3:
The L-glutamic acid grafting poly-dextrose aqueous solution of 10ml mass percent 5% is mixed 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, the centrifugal 20min of rotating speed of 12000r/min, under 80 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 (9)
1. a saccharan prepares the method for Graphene, it is characterized in that: according to certain volume ratio, the poly-dextrose 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.
2. a kind of saccharan according to claim 1 prepares the method for Graphene, it is characterized in that, described volume ratio is 100:1-1:1.
3. a kind of saccharan according to claim 1 prepares the method for Graphene, it is characterized in that: described poly-dextrose is generated by glucose, Sorbic Acid, citric acid thermopolymerization.
4. a kind of saccharan according to claim 1 or 3 prepares the method for Graphene, it is characterized in that: described poly-dextrose comprises the one in the poly-dextrose of modification or grafting, or their arbitrary combination.
5. a kind of saccharan according to claim 4 prepares the method for Graphene, it is characterized in that: described modified polyglucose is ketonization poly-dextrose, aldehyde radical poly-dextrose, amination poly-dextrose.
6. a kind of saccharan according to claim 4 prepares the method for Graphene, it is characterized in that: described grafting poly-dextrose is Methionin grafting poly-dextrose, L-glutamic acid grafting poly-dextrose, aspartic acid grafting poly-dextrose.
7. a kind of saccharan according to claim 1 prepares the method for Graphene, 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.
8. a kind of saccharan according to claim 1 prepares the method for Graphene, it is characterized in that, described centrifugal be with the centrifugal 10-20min of the rotating speed of 10000-12000r/min.
9. a kind of saccharan according to claim 1 prepares the method for Graphene, it is characterized in that, described drying treatment refers to and loft drier temperature is set in 40-80 DEG C, dry 1-24h under the environment of vacuum.
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| CN201510517526.1A CN105036124A (en) | 2015-08-22 | 2015-08-22 | Method for preparing graphene from polysaccharide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107021476A (en) * | 2017-05-24 | 2017-08-08 | 中国药科大学 | A kind of fusion preparation method of nitrogen-doped graphene quantum dot |
| CN107161980A (en) * | 2017-05-24 | 2017-09-15 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | A kind of preparation method of the carbon nanosheet with graphene oxide fold pattern |
| CN105958044B (en) * | 2016-07-26 | 2019-01-22 | 江苏天煌照明集团有限公司 | A kind of cobalt acid lithium electrode material and preparation method thereof of modified graphene doping |
| CN111592640A (en) * | 2020-05-12 | 2020-08-28 | 浙江恒澜科技有限公司 | Preparation method of graphene modified polyester composite material based on liquid phase stripping |
| CN112898953A (en) * | 2021-01-14 | 2021-06-04 | 蒋军良 | Preparation method of graphene heat-conducting film |
-
2015
- 2015-08-22 CN CN201510517526.1A patent/CN105036124A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105958044B (en) * | 2016-07-26 | 2019-01-22 | 江苏天煌照明集团有限公司 | A kind of cobalt acid lithium electrode material and preparation method thereof of modified graphene doping |
| CN107021476A (en) * | 2017-05-24 | 2017-08-08 | 中国药科大学 | A kind of fusion preparation method of nitrogen-doped graphene quantum dot |
| CN107161980A (en) * | 2017-05-24 | 2017-09-15 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | A kind of preparation method of the carbon nanosheet with graphene oxide fold pattern |
| CN111592640A (en) * | 2020-05-12 | 2020-08-28 | 浙江恒澜科技有限公司 | Preparation method of graphene modified polyester composite material based on liquid phase stripping |
| CN112898953A (en) * | 2021-01-14 | 2021-06-04 | 蒋军良 | Preparation method of graphene heat-conducting film |
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