CN105218841A - A kind of by the simple method for preparing of graphite to composite graphite alkene paper - Google Patents
A kind of by the simple method for preparing of graphite to composite graphite alkene paper Download PDFInfo
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- CN105218841A CN105218841A CN201410312133.2A CN201410312133A CN105218841A CN 105218841 A CN105218841 A CN 105218841A CN 201410312133 A CN201410312133 A CN 201410312133A CN 105218841 A CN105218841 A CN 105218841A
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Abstract
The object of the present invention is to provide a kind of by the simple method for preparing of graphite to composite graphite alkene paper, it is characterized in that: graphite is added in nano-cellulose aqueous liquid dispersion, after carrying out mechanical stirring and supersound process, obtain uniform and stable graphene/nanometer Mierocrystalline cellulose dispersion liquid, go out upper strata mixed solution by centrifugation, then moisture evaporation is fallen rear obtained composite graphite alkene paper.The method is simple, cost is low, without the need to complex apparatus, environmental friendliness, can solve that the Graphene film-forming properties existed in prior art is poor, intensity is low, the problem such as complex process and environmental pollution.Adopt the composite membrane physical strength prepared of the method and snappiness good, size is controlled.
Description
Technical field
The invention belongs to Graphene and nano-cellulose Application Areas, provide especially a kind of with nano-cellulose and natural graphite for raw material is aided with the method that ultrasonic dispersion prepares graphene/nanometer cellulose composite material.
Background technology
Nano-cellulose is with the starting material of rich cellulose (as agricultural crop straw, wood type, crudefiber crop and shell etc.), the diameter obtained by technology such as chemical hydrolysis, mechanical separation or biological enzymolysis is in several whisker to tens nanometers or fibrous natural polymer nano material, there is the characteristics such as renewable, degradable, nontoxicity and mechanical property are excellent, in food, medicine, beauty treatment, electronic material and field of compound material, there is wide application prospect.Be rich in hydroxyl in cellulose molecular chain, intermolecular very easily hydrogen bond, thus nano-cellulose can form flexible transparent film.With common high molecular materials matrix phase ratio, except the feature that it has as natural polymer, nano-cellulose film has lower thermal expansivity, if give conducting particles by this composite membrane, can flexible transparent conducting composite film be obtained, be expected to alternative conventional transparent electro-conductive material and obtain widespread use.
Graphene a kind ofly forms with sp2 hybridized orbital the two-dimensional material that hexangle type is honeycomb lattice by carbon atom.Because it has excellent electricity, calorifics and mechanical property, be expected to obtain application in fields such as nano electron device, transparent conductive film, matrix material, antistatic material, energy storage material and inductor blocks, thus become the new carbon got most of the attention after CNT (carbon nano-tube).The special performance that Graphene has makes it have application prospect in novel flexible field of electrical components, prepared by nano-cellulose and Graphene compound for develop flexible electrode and energy storage material significant.
Graphene or the graphene oxide of reduction and the aqueous liquid dispersion of nano-cellulose are mainly mixed to get composite membrane by the research report at present about nano-cellulose/graphene composite material.No matter select Graphene or the graphene oxide reduced, all relate to and complicated treatment process is carried out to graphite.It is raw material by intercalation or the graphene powder (aggregates of less than ten layers graphene films) that obtains after peeling off that existing Graphene is generally with graphite, simultaneously prepare in Graphene process also relate to stripping/intercalated graphite after annealing expansion process after obtain the less graphene powder of the number of plies.If select the graphene oxide of reduction, need first graphite strong oxidizer to be oxidized to increase graphite layers distance, utilize ultrasonic assistant to disperse to obtain graphene oxide liquid mixture, then carry out reduction with reductive agent and obtain Graphene.Such Graphene could be mixed with nano-cellulose after utilizing ultrasonic dispersion can obtain the cellulosic dispersion liquid of graphene/nanometer to prepare composite graphite alkene paper.Therefore existing technological process is loaded down with trivial details, and the production cycle is long, equipment is complicated, and production cost is expensive, uses a large amount of chemical reagent, have pollution to environment in oxidation and reduction process.
The present invention is that dispersion liquid is aided with mechanical stirring, ultrasonic wave is disperseed and centrifugation can obtain the cellulosic dispersion liquid of graphene/nanometer with nano-cellulose, can obtain Graphene Composite Paper by moisture evaporation.Compared with traditional method, the method technique is simple, and production cost is low, device simple, environmental protection.
Summary of the invention
The object of the present invention is to provide a kind of by the simple method for preparing of graphite to composite graphite alkene paper, adopt the composite membrane physical strength prepared of the method and snappiness good, size is controlled.
The present invention specifically provides a kind of preparation method of composite graphite alkene paper, it is characterized in that: graphite is added in nano-cellulose aqueous liquid dispersion, after carrying out mechanical stirring and supersound process, obtain uniform and stable graphene/nanometer Mierocrystalline cellulose dispersion liquid, go out upper strata mixed solution by centrifugation, then moisture evaporation is fallen rear obtained Graphene and nano cellulose composite film (i.e. composite graphite alkene paper).
Nano-cellulose selected by the present invention is natural polymer, and content is many on earth, distribution is wide for its starting material, and its raw material can be the stalk the like waste of wooden class, crudefiber crop, shell and farm crop.The own good mechanical property of nano-cellulose (Young's modulus 150GPa, tensile strength 6GPa), surface is active large because being rich in hydroxy functional group, and has renewable, degradable, the advantage such as nontoxic, is eco-friendly Preen nono material.The suspension of nano-cellulose in water plays effective stripping, dispersion, film forming and enhancement to graphite, forms complete membrane.Adopt the composite membrane physical strength prepared of the method and snappiness good, size is controlled.
The preparation method of composite graphite alkene paper of the present invention, is characterized in that: sonication treatment time is 0.5-12h, and plant capacity is 100-1000W.
The preparation method of composite graphite alkene paper of the present invention, it is characterized in that: in described nano-cellulose aqueous liquid dispersion, the concentration of nano-cellulose is 0.1-0.5wt.%, its preparation method is: add in Erlenmeyer flask by nano-cellulose and water, supersound process 0.5-12h is aided with after at room temperature stirring 0.5-12h, plant capacity is 100-1000W, and nano-cellulose is fully disperseed in water.
The preparation method of composite graphite alkene paper of the present invention, is characterized in that: carry out centrifugation 5-30min to graphene/nanometer Mierocrystalline cellulose dispersion liquid, and rotating speed is 5000-16000rpm.
The preparation method of composite graphite alkene paper of the present invention, is characterized in that: the addition of graphite accounts for the 0.1-95% of graphite and nano-cellulose total mass.
The preparation method of composite graphite alkene paper of the present invention, it is characterized in that, concrete preparation process is:
1), nano-cellulose be placed in Erlenmeyer flask and add water, the concentration of nano-cellulose is made to be 0.1-0.5wt.%, supersound process 0.5-12h is aided with after at room temperature stirring 0.5-12h, plant capacity is 100-1000W, nano-cellulose is fully disperseed in water, now obtains the dispersion liquid of nano-cellulose in water;
2), in nano-cellulose dispersion liquid add graphite, the addition of graphite accounts for the 0.1-95% of graphite and nano-cellulose total mass, through stirring and obtain after supersound process the mixed solution of homodisperse nano-cellulose and Graphene; Wherein supersound process equipment used power is 100-1000W, process 0.5-12h;
3), by step 2) the dispersion liquid whizzer that obtains carries out centrifuging treatment, process 5-30min, and rotating speed is 5000-16000rpm, and the suspension taking out upper strata is stand-by; (can by be deposited on bottom solid granulates drying after weigh, by calculating ultimate yield);
4), by the mixture of nano-cellulose and Graphene culture dish is injected, at room temperature or heating condition after moisture evaporation, by film from Graphene and the complete composite membrane of nano-cellulose that can obtain compliant conductive after culture dish is taken off.
The preparation method of composite graphite alkene paper of the present invention, is characterized in that: in step 4) in Heating temperature not higher than 100 degrees Celsius.
The invention provides a kind of Green synthesis technology of graphene/nanometer cellulose composite membrane, its method is simple, cost is low, without the need to complex apparatus, environmental friendliness, can solve that the Graphene film-forming properties existed in prior art is poor, intensity is low, the problem such as complex process and environmental pollution.Compared with prior art, the graphene composite film intensity adopting the method to obtain is good, size is controlled.Nano-cellulose is as natural polymer nano material, having mechanical property excellence, renewable, degradable, avirulent advantage, is the nano material in fields such as food product pack, electronic product, biological medicine, cosmetics, matrix materials with broad prospect of application.Due to nano-cellulose physical strength and film transparence high, snappiness is good, and thermal expansivity is low, has application prospect, thus develop its functional materials significant in the electron device product in future.
Accompanying drawing explanation
The photo of Fig. 1 graphite in nano-cellulose dispersion liquid before and after mechanical stirring ultrasonic disperse, wherein before (a), ultrasonic disperse, the Graphene obtained after (b), ultrasonic disperse and nano-cellulose mixed solution.
Fig. 2 peels off transmission electron microscope photo and the selected area electron diffraction style of rear Graphene.
The cellulosic composite membrane of Fig. 3 graphene/nanometer.
The cellulosic composite film surface stereoscan photograph of Fig. 4 graphene/nanometer.
The X ray diffracting spectrum of Fig. 5 graphene/nanometer cellulose composite membrane.
The differential thermal analysis curve of Fig. 6 graphene/nanometer cellulose composite membrane.
The Raman spectrum of Fig. 7 graphene/nanometer cellulose composite membrane.
Embodiment
Embodiment 1
Nano-cellulose is obtained by chemical hydrolysis flax fiber, 0.1g nano-cellulose powder is added in the Erlenmeyer flask containing 20g water, to stir after 0.5h supersound process 0.5h under the power of 800W again, obtain the dispersion liquid of nano-cellulose, then 0.9g graphite is added, stir this mixed solution and by mixed solution under 100W power through supersound process 12h to be uniformly dispersed (Fig. 1 asked for an interview by photo before and after supersound process), then by mixed solution centrifugal 15min under 10000rpm condition, upper strata dispersion liquid is slowly poured in culture dish, and to be placed in temperature be that the loft drier inner drying of 80 DEG C all volatilizees to moisture, then film is taken off from culture dish and can obtain the cellulosic composite membrane of graphene/nanometer (see Fig. 3, 4), Fig. 2 is transmission electron microscope photo and the selected area electron diffraction style of Graphene after peeling off, Fig. 5 is the X ray diffracting spectrum of graphene/nanometer cellulose composite membrane, Fig. 6 is the differential thermal analysis curve of graphene/nanometer cellulose composite membrane, Fig. 7 is the Raman spectrum of graphene/nanometer cellulose composite membrane.
Embodiment 2
Nano-cellulose is obtained by chemical hydrolysis wood pulp cellulose, 0.25g nano-cellulose powder is added in the Erlenmeyer flask containing 50g water, to stir after 0.5h supersound process 0.5h under the power of 800W again, obtain the dispersion liquid of nano-cellulose, then 0.75g graphite is added, stir this mixed solution and through supersound process 10h under 100W power, then by mixed solution centrifugal 30min under 5000rpm condition, upper strata dispersion liquid is slowly poured in culture dish, and to be placed in temperature be that the loft drier inner drying of 60 DEG C all volatilizees to moisture, then film is taken off from culture dish and can obtain graphene nano cellulose composite membrane.
Embodiment 3
Nano-cellulose is obtained by chemical hydrolysis shinyleaf yellowhorn fruit shell fiber, 0.5g nano-cellulose powder is added in the Erlenmeyer flask containing 100g water, to stir after 12h supersound process 12h under the power of 100W again, obtain the dispersion liquid of nano-cellulose, then 0.5g graphite is added, stir this mixed solution and through supersound process 2h under 800W power, then mixed solution is carried out centrifugation and (be separated 5min, rotating speed 16000rpm), upper strata dispersion liquid is slowly poured in culture dish, and to be placed in temperature be that the loft drier inner drying of 40 DEG C all volatilizees to moisture, then film is taken off from culture dish and can obtain graphene/nanometer cellulose composite membrane.
Embodiment 4
Nano-cellulose is obtained by chemical hydrolysis rice straw fiber.0.75g nano-cellulose powder is added in the Erlenmeyer flask containing 450g water, to stir after 6h supersound process 6h under the power of 200W again, obtain the dispersion liquid of nano-cellulose, then 0.25g powdered graphite is added, stir this mixed solution and through supersound process 0.5h under 1000W power, then by mixed solution at the centrifugal 10min of 14000rpm, upper strata dispersion liquid is poured in culture dish slowly, and to be placed in temperature be that the loft drier inner drying of 100 DEG C all volatilizees to moisture, then film is taken off can obtain the cellulosic composite membrane of graphene/nanometer from culture dish.
Embodiment 5
Nano-cellulose is obtained by chemical hydrolysis rice straw fiber, 0.9g nano-cellulose powder is added in the Erlenmeyer flask containing 450g water, to stir after 6h supersound process 6h under the power of 100W again, obtain the dispersion liquid of nano-cellulose, then 0.1g powdered graphite is added, stir this mixed solution and through supersound process 0.5h under 1000W power, then by mixed solution at the centrifugal 15min of 13000rpm, upper strata dispersion liquid is slowly poured in culture dish, and to be placed in temperature be that the loft drier inner drying of 100 DEG C all volatilizees to moisture, then film is taken off from culture dish and can obtain the cellulosic composite membrane of graphene/nanometer.
Above-described embodiment, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (7)
1. the preparation method of a composite graphite alkene paper, it is characterized in that: graphite is added in nano-cellulose aqueous liquid dispersion, after carrying out mechanical stirring and supersound process, obtain uniform and stable graphene/nanometer Mierocrystalline cellulose dispersion liquid, upper strata mixed solution is gone out by centrifugation, then moisture evaporation is fallen rear obtained Graphene and nano cellulose composite film, i.e. composite graphite alkene paper.
2. according to the preparation method of composite graphite alkene paper described in claim 1, it is characterized in that: sonication treatment time is 0.5-12h, plant capacity is 100-1000W.
3. according to the preparation method of composite graphite alkene paper described in claim 1 or 2, it is characterized in that: in described nano-cellulose aqueous liquid dispersion, the concentration of nano-cellulose is 0.1-0.5wt.%, its preparation method is: add in Erlenmeyer flask by nano-cellulose and water, supersound process 0.5-12h is aided with after at room temperature stirring 0.5-12h, plant capacity is 100-1000W, and nano-cellulose is fully disperseed in water.
4. according to the preparation method of composite graphite alkene paper described in claim 1 or 2, it is characterized in that: carry out centrifugation 5-30min to graphene/nanometer Mierocrystalline cellulose dispersion liquid, rotating speed is 5000-16000rpm.
5. according to the preparation method of composite graphite alkene paper described in claim 1 or 2, it is characterized in that: the addition of graphite accounts for the 0.1-95% of graphite and nano-cellulose total mass.
6., according to the preparation method of composite graphite alkene paper described in claim 1, it is characterized in that, concrete preparation process is:
1), nano-cellulose be placed in Erlenmeyer flask and add water, the concentration of nano-cellulose is made to be 0.1-0.5wt.%, supersound process 0.5-12h is aided with after at room temperature stirring 0.5-12h, plant capacity is 100-1000W, nano-cellulose is fully disperseed in water, now obtains the dispersion liquid of nano-cellulose in water;
2), in nano-cellulose dispersion liquid add graphite, the addition of graphite accounts for the 0.1-95% of graphite and nano-cellulose total mass, through stirring and obtain after supersound process the mixed solution of homodisperse nano-cellulose and Graphene; Wherein supersound process equipment used power is 100-1000W, process 0.5-12h;
3), by step 2) the dispersion liquid whizzer that obtains carries out centrifuging treatment, process 5-30min, and rotating speed is 5000-16000rpm, and the suspension taking out upper strata is stand-by;
4), by the mixture of nano-cellulose and Graphene culture dish is injected, at room temperature or heating condition after moisture evaporation, by film from Graphene and the complete composite membrane of nano-cellulose that can obtain compliant conductive after culture dish is taken off.
7., according to the preparation method of composite graphite alkene paper described in claim 5, it is characterized in that: in step 4) in Heating temperature not higher than 100 degrees Celsius.
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Cited By (8)
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| CN105754146A (en) * | 2016-03-31 | 2016-07-13 | 华南理工大学 | Nanocellulose/two-dimensional material composite flame-resistant material and preparation method thereof |
| CN105860143A (en) * | 2016-05-14 | 2016-08-17 | 上海大学 | Flexible nanocellulose-graphene composite membrane and preparation method thereof |
| CN106832425A (en) * | 2016-09-20 | 2017-06-13 | 济南圣泉集团股份有限公司 | High performance Graphene composite nano fiber element and preparation method thereof, application |
| CN108130772A (en) * | 2017-12-23 | 2018-06-08 | 林荣铨 | A kind of method that anti-bacteria paper is prepared using graphene/shell |
| CN109896522A (en) * | 2017-12-11 | 2019-06-18 | 山东省圣泉生物质石墨烯研究院 | A kind of graphene composite nano fiber element, preparation method and purposes |
| CN109942720A (en) * | 2019-03-29 | 2019-06-28 | 济南圣泉集团股份有限公司 | A kind of nano cellulose material and its preparation method and application |
| 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 |
| CN110408080A (en) * | 2019-08-13 | 2019-11-05 | 沈阳航空航天大学 | Graphene oxide and its composite nano fiber element conductive flexible film and its preparation method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105754146A (en) * | 2016-03-31 | 2016-07-13 | 华南理工大学 | Nanocellulose/two-dimensional material composite flame-resistant material and preparation method thereof |
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| CN105860143A (en) * | 2016-05-14 | 2016-08-17 | 上海大学 | Flexible nanocellulose-graphene composite membrane and preparation method thereof |
| CN106832425A (en) * | 2016-09-20 | 2017-06-13 | 济南圣泉集团股份有限公司 | High performance Graphene composite nano fiber element and preparation method thereof, application |
| CN109896522A (en) * | 2017-12-11 | 2019-06-18 | 山东省圣泉生物质石墨烯研究院 | A kind of graphene composite nano fiber element, preparation method and purposes |
| CN108130772A (en) * | 2017-12-23 | 2018-06-08 | 林荣铨 | A kind of method that anti-bacteria paper is prepared using graphene/shell |
| 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 |
| CN109942720A (en) * | 2019-03-29 | 2019-06-28 | 济南圣泉集团股份有限公司 | A kind of nano cellulose material and its preparation method and application |
| CN110408080A (en) * | 2019-08-13 | 2019-11-05 | 沈阳航空航天大学 | Graphene oxide and its composite nano fiber element conductive flexible film and its preparation method |
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