CN104276567B - A kind of preparation method of redox graphene RGO - Google Patents
A kind of preparation method of redox graphene RGO Download PDFInfo
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- CN104276567B CN104276567B CN201410565385.6A CN201410565385A CN104276567B CN 104276567 B CN104276567 B CN 104276567B CN 201410565385 A CN201410565385 A CN 201410565385A CN 104276567 B CN104276567 B CN 104276567B
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Abstract
The preparation method that the present invention relates to a kind of redox graphene RGO, hydroxypropyl methyl cellulose is dissolved in deionized water, the mass ratio 1:50 of described hydroxypropyl methyl cellulose and deionized water, ultrasonic 1-12h, being subsequently added the sodium metaperiodate of 2-10g/L, at 40-80 DEG C, lucifuge reaction 10-60min, cleans repeatedly with deionized water, centrifugal, dry for standby；Volume ratio according to 10:1-1:1, by the modified hydroxypropyl methyl cellulose 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 dried.The present invention adopts the modified hydroxypropyl methyl cellulose of sodium metaperiodate as reducing agent, prepares Graphene by the method for hydro-thermal reaction, and environmental protection, with low cost, technique simple, and the Graphene prepared has good dispersibility and stability.
Description
Technical field
The invention belongs to the synthesis of Graphene and technical field of nano material, particularly to the preparation method of a kind of redox graphene RGO.
Background technology
2004, Univ Manchester UK physicist An Deliehaimu and Constantine's Nuo Woxiao love, utilize the method tearing adhesive tape, from graphite, successfully isolate the Graphene of monolayer 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 sp2Hybrid orbital composition hexangle type honeycomb lattice, its construction unit is carbon hexatomic ring, and it is the two-dimensional material of a kind of only monolayer carbon atomic thickness.Graphene is the basic system unit constituting carbon-based material.It can be wrapped to form zero dimension Fullerenes, is rolled into one-dimensional carbonnanotube, is piled into three-dimensional graphite layer by layer.From that day that Graphene finds, Graphene just has become as focus and the focus of research, is widely used in fields such as ultracapacitor, transparency electrode, desalinization, light emitting diode, sensor, hydrogen storage, solaode, catalyst carrier, composite, biologic bracket material, bio-imaging, medicine conveying, weaving, printing and dyeing.
Graphene has the machinery of excellence, electricity, thermal property, anti-microbial property.Graphene is material the thinnest in the world, and it only has the thickness of monolayer atom, is about 0.335nm.Graphene is almost fully transparent, only absorbs the light of 2.3%, and light transmittance is up to 97.7%.Resistivity 10-6Ω/cm, lower than copper or silver, for the material that resistivity is minimum in the world at present.Graphene has great specific surface area, and its theoretical value is up to 2630m2/ g.Heat conductivity is up to 5300W/m K, and under room temperature, electron mobility is more than 15000cm2/ V s is higher than CNT and monocrystal silicon.Young's modulus is 1.1TPa, and fracture strength is up to 130GPa.
The preparation method of Graphene mainly has: micromechanics stripping method, seal cut transfer printing, liquid phase stripping method, chemical vapour deposition technique, aerosol high-temperature decomposition, epitaxial growth method, amorphous carbon compound thin film conversion method, graphene oxide (GO) reducing process and organic synthesis method etc..Wherein GO reducing process has the features such as cost is low, productivity is high and can be mass, and is used widely.Reducing agent conventional at present includes (charcoal element technology, 2013,32 (5): 30-36) such as hydrazine hydrate, dimethylhydrazine, phenols, sodium borohydride, sulfur-containing compound, alcohols.But, often use hydrazine or sodium borohydride etc. poisonous due to GO reducing process or expensive reagent is as reducing agent, therefore developing green, environmental protection, efficient and cheap electronation technology are very necessary.
Hydroxypropyl methyl cellulose, has another name called hypromellose, HPMC, be select high purity gossypin as raw material, prepare through special etherificate in the basic conditions.Hydroxypropyl methyl cellulose water soluble and segment polarity solvent, can be used for building, the industry such as chemistry, cosmetics, food, medicine.
Selective oxidation refers to the oxidation suppressing other position hydroxyl while certain ad-hoc location hydroxyl of oxidation of polysaccharides, and can the degraded of polysaccharide in inhibited oxidation course of reaction effectively.After sodium metaperiodate selective oxidation polysaccharide, can by C2、C3Hydroxyl oxygen chemical conversion aldehyde radical on position, the functional modification for polysaccharide provides reactivity point, and polysaccharide is carried out functional modification by available activity aldehyde radical, can generate numerous functional polysaccharide derivant, significantly expand the range of application of polysaccharide.Have no the report preparing Graphene with sodium metaperiodate selective oxidation hydroxypropyl methyl cellulose for reducing agent at present.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, it is provided that the preparation method of a kind of redox graphene RGO.
The technical scheme is that:
Hydroxypropyl methyl cellulose is dissolved in deionized water, the mass ratio 1:50, ultrasonic 1-12h of described hydroxypropyl methyl cellulose and deionized water, being subsequently added the sodium metaperiodate of 2-10g/L, at 40-80 DEG C, lucifuge reaction 10-60min, cleans repeatedly with deionized water, centrifugal, dry for standby；Volume ratio according to 10:1-1:1, by the modified hydroxypropyl methyl cellulose 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 dried.
Preferably, graphene oxide is prepared through ultrasonic delamination by graphite oxide, for single-layer graphene oxide, multilayer oxygen functionalized graphene or the mixture of the two.
Advantages of the present invention: adopt sodium metaperiodate by hydroxypropyl methyl cellulose C2And C3Position selective oxidation is aldehyde radical, and as reducing agent, prepares Graphene by the method for hydro-thermal reaction, and environmental protection, with low cost, technique simple, and the Graphene prepared has good dispersibility and stability.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is expanded on further.
Embodiment 1:
2g hydroxypropyl methyl cellulose is dissolved in 100ml deionized water, ultrasonic 1h, it is subsequently added the sodium metaperiodate of 2g/L, at 80 DEG C, lucifuge reaction 60min, cleans repeatedly with deionized water, centrifugal, dry for standby；
Hydroxypropyl methyl cellulose modified for 1g is dissolved in 100ml deionized water, obtain the aqueous solution of the modified hydroxypropyl methyl cellulose 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 dried.
Embodiment 2:
2g hydroxypropyl methyl cellulose is dissolved in 100ml deionized water, ultrasonic 5h, it is subsequently added the sodium metaperiodate of 5g/L, at 60 DEG C, lucifuge reaction 30min, cleans repeatedly with deionized water, centrifugal, dry for standby；
Hydroxypropyl methyl cellulose modified for 1g is dissolved in 50ml deionized water, obtain the aqueous solution of the modified hydroxypropyl methyl cellulose 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 dried.
Embodiment 3:
2g hydroxypropyl methyl cellulose is dissolved in 100ml deionized water, ultrasonic 10h, it is subsequently added the sodium metaperiodate of 10g/L, at 40 DEG C, lucifuge reaction 10min, cleans repeatedly with deionized water, centrifugal, dry for standby；
Hydroxypropyl methyl cellulose modified for 1g is dissolved in 20ml deionized water, obtain the aqueous solution of the modified hydroxypropyl methyl cellulose 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 dried.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, 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 all of embodiment be given exhaustive.Every belong to apparent change that technical scheme amplified out or the variation row still in protection scope of the present invention.
Claims (2)
1. the preparation method of a redox graphene RGO, it is characterised in that:
(1) hydroxypropyl methyl cellulose is dissolved in deionized water, the mass ratio 1:50 of described hydroxypropyl methyl cellulose and deionized water, ultrasonic 1-12h, it is subsequently added the sodium metaperiodate of 2-10g/L, at 40-80 DEG C, lucifuge reaction 10-60min, cleans repeatedly with deionized water, centrifugal, dry for standby, it is thus achieved that modified hydroxypropyl methyl cellulose；
(2) according to the volume ratio of 10:1-1:1, by the above-mentioned modified hydroxypropyl methyl cellulose 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 dried.
2. the preparation method of a kind of redox graphene RGO according to claim 1, it is characterised in that the graphene oxide described in step 2 is prepared through ultrasonic delamination by graphite oxide, for single-layer graphene oxide, multilayer oxygen functionalized graphene or the mixture of the two.
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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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