CN104340978B - A kind of preparation method of graphene-based matrix material - Google Patents
A kind of preparation method of graphene-based matrix material Download PDFInfo
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- 239000011159 matrix material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims abstract description 26
- 229920001661 Chitosan Polymers 0.000 claims abstract description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 18
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
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- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000009413 insulation Methods 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 4
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- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 230000002829 reductive effect Effects 0.000 abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 229910021529 ammonia Inorganic materials 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 14
- 239000002131 composite material Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
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- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- -1 bio-imaging Substances 0.000 description 2
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- 230000004048 modification Effects 0.000 description 2
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- 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
- 229920002101 Chitin Polymers 0.000 description 1
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- 241000238424 Crustacea Species 0.000 description 1
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- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to a kind of preparation method of graphene-based matrix material, chitosan is dissolved in the acetic acid solution of 3%, bath raio 1:50, ultrasonic 1-12h, adds the sodium periodate of 2-10g/L subsequently, lucifuge reaction 10-60min at 40-80 DEG C, repeatedly clean with deionized water, centrifugal, dry for standby; According to the volume ratio of 10:1:1-1:1:1, by chitosan solution modified for 0.1-100g/L sodium periodate, mix with the silver ammino solution of 0.1-100g/L, the graphene oxide solution of 0.01-0.5g/L, ultrasonic 1-12h under the temperature condition of 40 DEG C-100 DEG C, then move to 160-220 DEG C of insulation 1-48h in teflon-lined hydrothermal reaction kettle, after naturally cooling, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene-based matrix material after drying treatment.The present invention utilizes graphene oxide, silver-colored ammonia is raw material, the chitosan solution adopting sodium periodate modified is as reductive agent, under the condition of not adding any stablizer/dispersion agent, single stage method obtains graphene-based matrix material, possess that technique is simple, raw material sources extensively, reaction temperature and, the advantage such as environmental protection.
Description
Technical field
The invention belongs to technical field of nano material, particularly a kind of preparation method of graphene-based matrix material.
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.
Nanometer silver has excellent thermal conduction, electroconductibility, surfactivity and catalytic performance, has huge using value in optics, catalysis, microelectronics, bio-sensing, the field such as antibacterial.
Graphene is the two-dimentional graphitic carbon material of monoatomic thickness, there is a series of excellent properties such as high-specific surface area, outstanding heat conductivility and mechanical property, outstanding electron transmission performance, it is the ideal carrier of nanometer silver, and the nano silver particles be present between graphene layer can play the contiguous graphene sheet layer of separation, prevent Graphene from the effect of reuniting occurring.Have many documents in recent years or patent reports the Synthesis and applications of nanometer silver-graphene composite material, but their poisonous hydrazine and sodium borohydrides of adopting as reductive agent more.Such as JianfengShen etc. utilize the mixing reductive agent of sodium borohydride and ethylene glycol to prepare Graphene silver nano particle composite material (NanoRes., 2010,3 (5): 339-349).
In recent years, green, environmental protection, efficient and cheap method is adopted to prepare the focus that nanometer silver, Graphene and nanometer silver-graphene composite material become research gradually.He Guangyu etc. are that reductive agent passes through hydro-thermal reaction with polyoxyethylene glycol, redox graphene is simultaneously at graphenic surface growth in situ Nano silver grain, prepare nanometer silver graphene composite material, have studied the bacteriostasis property of matrix material simultaneously, result shows that nanometer silver graphene composite material is a kind of Novel antibacterial material (fine chemistry industry of Be very effective, 2012,09:840-843).Chinese invention patent CN201210054952.2 adopts N, dinethylformamide (DMF) as reductive agent, the graphene powder of high purity 99% as carrier, under the reaction conditions of gentleness, silver on graphene layer forming core, grow up, obtain Graphene/silver nano particle composite material.
Chitin is a kind of natural organic high-molecular polysaccharide, is distributed widely in the cell walls of the crust of nature Crustaceans (shrimp, crab, insect), fungi and plant.Account for second in standing stock natural organic high-molecular material on earth, be only second to Mierocrystalline cellulose.Chitosan is the product after chitin deacetylase base, is a kind of linear macromolecule.
Selective oxidation refers to the oxidation suppressing other position hydroxyl while certain specific position hydroxyl of SURGICEL, and can cellulosic degraded in inhibited oxidation reaction process effectively.After sodium periodate selective oxidation Mierocrystalline cellulose, can by C
2, C
3hydroxyl oxygen on position changes into aldehyde radical, for cellulosic functional modification provides reactive behavior point, active aldehyde radical can be utilized to carry out functional modification to Mierocrystalline cellulose, can generate numerous functional fiber element derivative, greatly expand cellulosic range of application.Yet there are no with sodium periodate selective oxidation chitosan as reductive agent single stage method prepares the report of graphene-based matrix material.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, a kind of preparation method of graphene-based matrix material is provided.
Present invention employs following technical scheme:
Chitosan is dissolved in the acetic acid solution of 3%, bath raio 1:50, ultrasonic 1-12h, adds 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 10:1:1-1:1:1, by chitosan solution modified for 0.1-100g/L sodium periodate, mix with the silver ammino solution of 0.1-100g/L, the graphene oxide solution of 0.01-0.5g/L, ultrasonic 1-12h under the temperature condition of 40 DEG C-100 DEG C, then move to 160-220 DEG C of insulation 1-48h in teflon-lined hydrothermal reaction kettle, after naturally cooling, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene-based matrix material after drying treatment.
Preferably, silver ammino solution is the complex compound that nitrate or Sulfuric acid disilver salt and ammoniacal liquor are formed.
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.
The present invention has following beneficial effect:
The present invention utilizes graphene oxide, silver-colored ammonia is raw material, the chitosan adopting sodium periodate modified is as reductive agent, under the condition of not adding any stablizer/dispersion agent, single stage method obtains graphene-based matrix material, possess that technique is simple, raw material sources extensively, reaction temperature and, the advantage such as environmental protection.
Embodiment
Below in conjunction with embodiment, set forth the present invention further.
Embodiment 1:
2g chitosan is dissolved in 3% acetic acid solution of 100ml, ultrasonic 1h, adds the sodium periodate of 2g/L subsequently, at 80 DEG C, lucifuge reaction 60min, cleans repeatedly with deionized water, centrifugal, dry for standby;
1g modified chitosan is dissolved in 100ml deionized water, obtain the aqueous solution of the modified chitosan of concentration 10g/L, mix with the silver ammino solution of the 10g/L of 10ml, the graphene oxide solution of the 0.1g/L of 10ml mixes, ultrasonic 8h under the temperature condition of 40 DEG C, then move to 160 DEG C of insulation 24h in teflon-lined hydrothermal reaction kettle, after naturally cooling, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene-based matrix material after drying treatment.
Embodiment 2:
2g chitosan is dissolved in 3% acetic acid solution of 100ml, ultrasonic 5h, adds the sodium periodate of 5g/L subsequently, at 60 DEG C, lucifuge reaction 30min, cleans repeatedly with deionized water, centrifugal, dry for standby;
1g modified chitosan is dissolved in 50ml deionized water, obtain the aqueous solution of the modified chitosan of concentration 20g/L, mix with the silver ammino solution of the 20g/L of 10ml, the graphene oxide solution of the 0.5g/L of 10ml mixes, ultrasonic 5h under the temperature condition of 60 DEG C, then move to 200 DEG C of insulation 15h in teflon-lined hydrothermal reaction kettle, after naturally cooling, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene-based matrix material after drying treatment.
Embodiment 3:
2g chitosan is dissolved in 3% acetic acid solution of 100ml, ultrasonic 10h, adds the sodium periodate of 10g/L subsequently, at 40 DEG C, lucifuge reaction 10min, cleans repeatedly with deionized water, centrifugal, dry for standby;
1g modified chitosan is dissolved in 20ml deionized water, obtain the aqueous solution of the modified chitosan of concentration 50g/L, mix with the graphene oxide solution of the silver ammino solution of the 50g/L of 10ml, the 0.05g/L of 10ml, ultrasonic 2h under the temperature condition of 100 DEG C, then move to 220 DEG C of insulation 2h in teflon-lined hydrothermal reaction kettle, after naturally cooling, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene-based matrix material 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 (3)
1. a preparation method for graphene-based matrix material, is characterized in that:
(1) chitosan is dissolved in the acetic acid solution of 3%, bath raio 1:50, ultrasonic 1-12h, add the sodium periodate of 2-10g/L subsequently, and at 40-80 DEG C, lucifuge reaction 10-60min, cleans repeatedly with deionized water, centrifugal, dry for standby;
(2) according to the volume ratio of 10:1:1-1:1:1, by chitosan solution modified for 0.1-100g/L sodium periodate, mix with the silver ammino solution of 0.1-100g/L, the graphene oxide solution of 0.01-0.5g/L, ultrasonic 1-12h under the temperature condition of 40 DEG C-100 DEG C, then move to 160-220 DEG C of insulation 1-48h in teflon-lined hydrothermal reaction kettle, after naturally cooling, repeatedly clean with ethanol and deionized water, centrifugal, obtain graphene-based matrix material after drying treatment.
2. the preparation method of a kind of graphene-based matrix material according to claim 1, is characterized in that, described silver ammino solution is the complex compound that Silver Nitrate or Sulfuric acid disilver salt and ammoniacal liquor are formed.
3. the preparation method of a kind of graphene-based matrix material 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.
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| CN107140623B (en) * | 2017-05-24 | 2019-11-15 | 郑州大学 | A method of preparing graphene |
| CN108529603A (en) * | 2018-06-26 | 2018-09-14 | 西南交通大学 | Alcohol heat-treats the method and graphene of graphene oxide |
| CN108751179B (en) * | 2018-08-17 | 2020-04-14 | 山西太行鑫升碳素有限公司 | Preparation method of transparent graphene conductive film |
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| CN102160998A (en) * | 2011-04-25 | 2011-08-24 | 北京航空航天大学 | Preparation method of graphene-silver nano particle composite material |
| KR101359771B1 (en) * | 2012-02-17 | 2014-02-13 | 영남대학교 산학협력단 | Composites of graphene decorated with silver nanoparticles and preparation method thereof |
| CN102698747B (en) * | 2012-06-14 | 2013-10-16 | 聊城大学 | Silver/graphene compound material and application |
| CN103318877B (en) * | 2013-06-24 | 2015-04-22 | 华南理工大学 | Method for preparing graphene through water-soluble chitosan derivative |
| CN103467620A (en) * | 2013-09-12 | 2013-12-25 | 深圳先进技术研究院 | Activity modification method for chitosan materials |
| CN103787322B (en) * | 2014-01-25 | 2016-01-20 | 华南理工大学 | One supports graphene layer Layered Silicate Nanocomposites And Their Preparation Methods |
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