CN104276567A - Preparation method of reduced graphene oxide (RGO) - Google Patents
Preparation method of reduced graphene oxide (RGO) Download PDFInfo
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- CN104276567A CN104276567A CN201410565385.6A CN201410565385A CN104276567A CN 104276567 A CN104276567 A CN 104276567A CN 201410565385 A CN201410565385 A CN 201410565385A CN 104276567 A CN104276567 A CN 104276567A
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Abstract
The invention relates to a preparation method of reduced graphene oxide (RGO). The preparation method comprises the following steps: dissolving hydroxypropyl methyl cellulose into deionized water in a bath ratio of 1:50, performing ultrasonic treatment for 1-12 hours, then, adding 2-10g/L sodium periodate, reacting for 10-60 minutes at 40-80 DEG C in a dark place, repeatedly cleaning by use of deionized water, centrifuging and drying for later use; mixing 0.01-100g/L modified hydroxypropyl methyl cellulose aqueous solution with 0.01-0.5g/L graphene oxide solution in a volume ratio of (10:1) to (1:1), performing hydrothermal reaction for 1-10 hours at a temperature of 120-160 DEG C to obtain graphene solution; repeatedly cleaning the graphene solution by use of alcohol and deionized water, centrifuging and drying to obtain graphene powder. According to the preparation method disclosed by the invention, hydroxypropyl methyl cellulose modified by sodium periodate is used as a reducing agent, and graphene is prepared by virtue of a hydrothermal reaction method, and therefore, the preparation method is environmentally friendly, low in cost and simple in process; and the prepared graphene has good dispersity and stability.
Description
Technical field
The invention belongs to synthesis and the technical field of nano material of Graphene, particularly the preparation method of a kind of redox graphene RGO.
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.
Vltra tears, has another name called hypromellose, HPMC, is to select the gossypin of high purity as raw material, obtains in the basic conditions through special etherificate.Vltra tears water soluble and segment polarity solvent, can be used for the industry such as building, chemistry, makeup, food, medicine.
Selective oxidation refers to the oxidation suppressing other position hydroxyl while certain specific position hydroxyl of oxidation of polysaccharides, and can the degraded of polysaccharide in inhibited oxidation reaction process effectively.After sodium periodate selective oxidation polysaccharide, can by C
2, C
3hydroxyl oxygen on position changes into aldehyde radical, and the functional modification for polysaccharide provides reactive behavior point, and active aldehyde radical can be utilized to carry out functional modification to polysaccharide, can generate numerous functional polysaccharide derivative, has greatly expanded the range of application of polysaccharide.Have no at present with sodium periodate selective oxidation Vltra tears as the report of Graphene prepared by reductive agent.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, the preparation method of a kind of redox graphene RGO is provided.
The present invention is achieved by following technical proposals:
Be dissolved in by Vltra tears in deionized water, bath raio 1:50, ultrasonic 1-12h, add the sodium periodate of 2-10g/L subsequently, at 40-80 DEG C, lucifuge reaction 10-60min, cleans repeatedly with deionized water, centrifugal, dry for standby; According to the volume ratio of 10:1-1:1, by the modification Vltra tears aqueous solution of 0.01-100g/L, mix with the graphene oxide solution of 0.01-0.5g/L, hydro-thermal reaction 1-10h 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, 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: adopt sodium periodate by Vltra tears C
2and C
3position selective oxidation is aldehyde radical, and as reductive agent, prepares Graphene by the method for hydro-thermal reaction, and environmental protection, with low cost, technique simple, and the Graphene prepared has good dispersiveness and stability.
Embodiment
Below in conjunction with embodiment, set forth the present invention further.
Embodiment 1:
Be dissolved in by 2g Vltra tears in 100ml deionized water, ultrasonic 1h, add the sodium periodate of 2g/L subsequently, at 80 DEG C, lucifuge reaction 60min, cleans repeatedly with deionized water, centrifugal, dry for standby;
Vltra tears modified for 1g is dissolved in 100ml deionized water, obtain the aqueous solution of the modification Vltra tears of concentration 10g/L, mix with the graphene oxide solution of 10ml concentration 0.01g/L, hydro-thermal reaction 2h at the temperature of 120 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
Embodiment 2:
Be dissolved in by 2g Vltra tears in 100ml deionized water, ultrasonic 5h, add the sodium periodate of 5g/L subsequently, at 60 DEG C, lucifuge reaction 30min, cleans repeatedly with deionized water, centrifugal, dry for standby;
Vltra tears modified for 1g is dissolved in 50ml deionized water, obtain the aqueous solution of the modification Vltra tears of concentration 20g/L, mix with the graphene oxide solution of 10ml concentration 0.1g/L, hydro-thermal reaction 5h at the temperature of 140 DEG C, obtain graphene solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene powder after drying treatment.
Embodiment 3:
Be dissolved in by 2g Vltra tears in 100ml deionized water, ultrasonic 10h, add the sodium periodate of 10g/L subsequently, at 40 DEG C, lucifuge reaction 10min, cleans repeatedly with deionized water, centrifugal, dry for standby;
Vltra tears modified for 1g is dissolved in 20ml deionized water, obtain the aqueous solution of the modification Vltra tears of concentration 50g/L, mix with the graphene oxide solution of 10ml concentration 0.5g/L, hydro-thermal reaction 10h at the temperature of 160 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. a preparation method of redox graphene RGO, is characterized in that:
(1) be dissolved in deionized water by Vltra tears, bath raio 1:50, ultrasonic 1-12h, add the sodium periodate of 2-10g/L subsequently, at 40-80 DEG C, lucifuge reaction 10-60min, cleans repeatedly with deionized water, centrifugal, dry for standby;
(2) according to certain volume ratio, by the certain density modification Vltra tears aqueous solution, mix with certain density graphene oxide solution, hydro-thermal reaction 1-10h 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. the preparation method of a kind of redox graphene RGO according to claim 1, is characterized in that, the volume ratio described in step 2 is 10:1-1:1.
3. the preparation method of a kind of redox graphene RGO according to claim 1, is characterized in that, described in step 2, the concentration of modification Vltra tears is 0.01-100g/L.
4. the preparation method of a kind of redox graphene RGO according to claim 1, is characterized in that, the concentration of graphene oxide described in step 2 is 0.01-0.5g/L.
5. the preparation method of a kind of redox graphene RGO according to claim 1, it is characterized in that, the graphene oxide described in step 2 is obtained through ultrasonic delamination by graphite oxide, is single-layer graphene oxide, multilayer graphene oxide or the mixture of the two.
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| CN109354011A (en) * | 2018-11-17 | 2019-02-19 | 璧典附 | A kind of environment-friendly preparation method thereof of graphene |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130175182A1 (en) * | 2010-09-14 | 2013-07-11 | Council Of Scientific & Industrial Research | Electrochemical process for synthesis of graphene |
| CN103771406A (en) * | 2014-01-22 | 2014-05-07 | 中国工程物理研究院化工材料研究所 | Graphene/manganese tetraoxide nanocomposite and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130175182A1 (en) * | 2010-09-14 | 2013-07-11 | Council Of Scientific & Industrial Research | Electrochemical process for synthesis of graphene |
| CN103237756A (en) * | 2010-09-14 | 2013-08-07 | 科学与工业研究委员会 | Electrochemical process for synthesis of graphene |
| CN103771406A (en) * | 2014-01-22 | 2014-05-07 | 中国工程物理研究院化工材料研究所 | Graphene/manganese tetraoxide nanocomposite and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109354011A (en) * | 2018-11-17 | 2019-02-19 | 璧典附 | A kind of environment-friendly preparation method thereof of graphene |
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Effective date of registration: 20170615 Address after: 510670 Guangdong city of Guangzhou province high tech Industrial Development Zone No. 31 by a Ke Feng Lu Southern China new material innovation park building G1 No. 220 Patentee after: GUANGDONG NANOLUTION SCIENCE AND TECHNOLOGY Co.,Ltd. Address before: 215000 No. 2, Taishan Road, Suzhou hi tech Zone, Jiangsu, Suzhou Patentee before: SUZHOU ZHENGYECHANG INTELLIGENT TECHNOLOGY Co.,Ltd. |
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