CN104072808A - Graphene nanosheet material dispersed in natural polysaccharides and preparing method thereof - Google Patents
Graphene nanosheet material dispersed in natural polysaccharides and preparing method thereof Download PDFInfo
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Abstract
The invention relates to a graphene nanosheet material dispersed in natural polysaccharides and a preparing method thereof. The graphene nanosheet material is dispersed in the natural polysaccharides. The graphene nanosheet material, which has a thickness of 0.35-7 nm, is single-layered or multi-layered and dispersed in the natural polysaccharides, is prepared by mixing the natural polysaccharides and solid graphite, and adding a solvent in a certain ratio or directly subjecting the mixture to mechanical lapping without adding anything. According to the prepared graphene nanosheet material, the natural polysaccharides are adopted as a dispersing agent to be dispersed around graphene nanosheets, interfacial lyophobic parts of the graphene nanosheets and the natural polysaccharides reach fusion at a nanometer level, strong interaction (Van der Waals' force) is generated, and mutual affinity is enhanced, thus inhibiting re-aggregation of graphene nanosheets, inhibiting common transformation of some crystal forms of the natural polysaccharides and obtaining the graphene nanosheet material with stable properties.
Description
Technical field
The invention belongs to technical field of nano material, particularly a kind of graphene nano sheet material in Mierocrystalline cellulose and preparation method thereof that is dispersed in.
Background technology
Graphene is a kind of carbonaceous novel material by the tightly packed one-tenth bi-dimensional cellular of monolayer carbon atom shape crystalline network.The graphite material with laminate structure can obtain single or multiple lift graphene nanometer sheet after peeling off.Connection in Graphene between each carbon atom is very pliable and tough, and in the time applying external mechanical force, carbon atom face occurs bending and deformation, thereby makes carbon atom needn't rearrange to adapt to external force, has kept Stability Analysis of Structures.This stable crystalline network of Graphene makes it have abnormal excellent electroconductibility, perfectly quantum tunneling effect, half integral quantum hall effect, and good mechanics, optics and thermal property.Have wide practical use at electronics, information, the energy, material and biomedicine field.But the hydrophobicity that Graphene has and the feature of easily reuniting, limited its widespread use.
At present, the main preparation methods of Graphene has: chemical reduction method and the mechanical split the law of the epitaxial growth method in chemical Vapor deposition process (CVD), silicon carbide substrate, the direct synthesis technique based on graphite and derivative thereof, electrochemical method, cutting carbon nanotubes method, template, organic synthesis method, graphene oxide (GO).But the preparation level of Graphene is just in laboratory scale up to now, suitability for industrialized production also faces low cost how, prepare on a large scale the problem such as Graphene of desired structure.The chemical reduction method of graphite oxide GO is the more method of preparing graphene nanometer sheet of applying at present, but still there is the problem of complexity, small scale in its preparation process, the graphene nano sector-meeting that reduced graphene obtains in addition because method of reducing not exclusively cause in structure, there is certain defect.
Graphene, because of its excellent performance, great specific surface area, is very suitable for the exploitation of high performance composite.Current existing graphene composite material can be divided into two classes: Graphene/composite material of inorganic matter and Graphene/polymer composites.And the existing method of preparing graphene composite material also mainly contains two kinds: first allow graphite oxide and other materials compound, then graphite oxide reduction is wherein obtained to graphene nanocomposite material; Or compound with Graphene and the other materials of modification.The matrix material report of polysaccharide and Graphene is not also a lot.The preparation of the existing a smaller number of matrix material about the polymkeric substance such as Mierocrystalline cellulose, chitosan and graphene nanometer sheet at present also takes off not open this two kinds of conventional preparation methods, and such composite effect will certainly be subject to the impact of blend degree each other.In order effectively to embody the function of graphene nanometer sheet, graphene nanometer sheet should be scattered in matrix material equably.
We have invented a kind of preparation method, can prepare simply, on a large scale graphene nanometer sheet, and obtain the graphene nano sheet material by cellulose nano material stable dispersion.
Summary of the invention
First technical problem that the present invention will solve provides a kind of graphene nano sheet material being dispersed in natural polysaccharide.
Second technical problem that the present invention will solve is to provide a kind of preparation method who is dispersed in the graphene nano sheet material in natural polysaccharide.
In order to solve above-mentioned first technical problem, the invention provides a kind of graphene nano sheet material being dispersed in natural polysaccharide, graphene nanometer sheet dispersion of materials is in natural polysaccharide.
Described natural polysaccharide is selected from one or more in Mierocrystalline cellulose, chitin, starch, chitosan.
Preferably, described Mierocrystalline cellulose is one or more of natural herb plant or natural xylophyta.
Preferably, described Mierocrystalline cellulose comprises one or more of the regenerated cellulose that obtained by natural herb plant or natural xylophyta.
Preferably, described Mierocrystalline cellulose comprises one or more of the derivatived cellulose that obtained by natural herb plant or natural xylophyta.
In order to solve second technical problem, the invention provides the preparation method who is dispersed in the graphene nano sheet material in natural polysaccharide described in a kind of preparation, the method comprises the following steps: natural polysaccharide mixes with solid graphite, mixture is carried out to mechanical mill, and the thickness that obtains being dispersed in natural polysaccharide nano material is the graphene nanometer sheet matrix material of 0.35nm～7nm, single or multiple lift.
Preferably, carry out again mechanical mill add solvent in natural polysaccharide and solid graphite mixture after.
Preferably, solid graphite accounts for the 0.1wt%-80wt% of natural polysaccharide weight.More preferably, solid graphite accounts for the 0.5%-30% of natural polysaccharide weight.
Preferably, grinding condition is 100-500r.p.m, and milling time is 1-100 hour.More preferably, grinding condition is 200-400r.p.m, and milling time is 2-50 hour.
Preferably, described solvent is selected from one or more in DMF, toluene, benzene, acetone, water; Preferably, solvent quality is natural polysaccharide 0.01 times-500 times.More preferably, solvent quality is natural polysaccharide 0.05 times-100 times.
The invention has the beneficial effects as follows:
The graphene nano sheet material of 1, being disperseed by natural polysaccharide makes graphene nanometer sheet and natural polysaccharide nanofiber reach the fusion on nanoscale, thereby suppress reassociating of graphene nanometer sheet, also suppressed some common crystal phase transitions of natural polysaccharide, obtained the more stable graphene nano sheet material of performance simultaneously.
2, adopt the present invention preparation to be dispersed in the graphene nanometer sheet in natural polysaccharide, by mechanical mill obtained in enormous quantities, by the graphene nano sheet material of natural polysaccharide stable dispersion, simple, with low cost, be easy to realize scale operation.
Brief description of the drawings
The accompanying drawing that the present invention comprises is for providing a further understanding of the present invention.
Fig. 1: gained of the present invention is dispersed in the transmission electron microscope photo of the graphene nano sheet material in Mierocrystalline cellulose
Fig. 2: the stereoscan photograph of the graphene nanometer sheet that gained of the present invention is disperseed by derivatived cellulose carboxyl methyl cellulose.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment, the present invention is described further, but content of the present invention is not only confined to the following examples.
Embodiment 1:
A preparation method who is dispersed in the graphene nano sheet material in natural polysaccharide described in preparing, the method comprises the following steps:
The Microcrystalline Cellulose in natural herb Mierocrystalline cellulose source mixes by 99:1 weight with solid graphite, mixture is joined in shredder, do not add any abrasive and carry out mechanical mill, grind revolution 300r.p.m, time 16h, the thickness that has obtained being dispersed in natural herb Mierocrystalline cellulose is 0.35～7nm single-layer graphene nanometer sheet material.
Embodiment 2:
With embodiment 1, difference is natural herb Mierocrystalline cellulose to replace to natural woody Mierocrystalline cellulose; Described natural woody Mierocrystalline cellulose mixes by 20:1 weight with solid graphite; Grind revolution 500r.p.m, time 2h; The thickness that has obtained being dispersed in natural woody Mierocrystalline cellulose is 0.35～7nm single-layer graphene nanometer sheet material.
Embodiment 3:
Described in a kind of preparation, be dispersed in the preparation method of the graphene nano sheet material in natural polysaccharide, the method comprises the following steps: natural herb Mierocrystalline cellulose mixes by 1:1 weight with solid graphite, mixture is joined in shredder, add again the solvent DMF of 50 times of natural polysaccharide quality to carry out mechanical mill, grind revolution 300r.p.m, time 24h; Obtain being dispersed in thickness in the natural herb Mierocrystalline cellulose single or multiple lift graphene nano sheet material (as Fig. 1) within the scope of 0.35nm～7nm.
Embodiment 4:
With embodiment 3, difference is natural herb Mierocrystalline cellulose to replace to natural woody Mierocrystalline cellulose, natural woody Mierocrystalline cellulose mixes by 5:1 weight with solid graphite, mixture is joined in shredder, add again the toluene solvant of 500 times of natural woody cellulosic materials amounts to carry out mechanical mill, grind revolution 300r.p.m, time 100h.Obtain being dispersed in thickness in the natural woody Mierocrystalline cellulose single or multiple lift graphene nano sheet material within the scope of 0.35nm～7nm.
Embodiment 5:
With embodiment 3, difference is natural herb Mierocrystalline cellulose to replace to starch, starch mixes by 10:1 weight with solid graphite, mixture is joined in shredder, add again the acetone solvent of 100 times of starch qualities to carry out mechanical mill, grind revolution 300r.p.m, time 50h, the thickness that has obtained being dispersed in starch is the single or multiple lift graphene nano sheet material within the scope of 0.35nm～7nm.
Embodiment 6:
With embodiment 3, difference is natural herb Mierocrystalline cellulose to replace to chitin, and chitin mixes by 20:1 weight with solid graphite, mixture is joined in shredder, then add the DMF solvent of 0.05 times of chitin quality to carry out mechanical mill, grind revolution 200r.p.m, time 40h.Obtain being dispersed in thickness in the chitin single or multiple lift graphene nano sheet material within the scope of 0.35nm～7nm.
Embodiment 7:
With embodiment 3, difference is natural herb Mierocrystalline cellulose to replace to chitosan.Obtain being dispersed in thickness in the chitosan single or multiple lift graphene nano sheet material within the scope of 0.35nm～7nm.
Embodiment 8:
With embodiment 3, difference is solvent DMF to replace to water.Obtain being dispersed in thickness in the natural herb Mierocrystalline cellulose single or multiple lift graphene nano sheet material within the scope of 0.35nm～7nm.
Embodiment 9:
With embodiment 3, difference is solvent DMF to replace to toluene.Obtain being dispersed in thickness in the natural herb Mierocrystalline cellulose single or multiple lift graphene nano sheet material within the scope of 0.35nm～7nm.
Embodiment 10:
With embodiment 3, difference is solvent DMF to replace to benzene.Obtain being dispersed in thickness in the natural herb Mierocrystalline cellulose single or multiple lift graphene nano sheet material within the scope of 0.35nm～7nm.
Embodiment 11:
Described in a kind of preparation, be dispersed in the preparation method of the graphene nano sheet material in natural polysaccharide, the method comprises the following steps: derivatived cellulose carboxymethyl cellulose (CMC) mixes by 1:1 weight with solid graphite, mixture is joined and in shredder, adds the water of 100mL to carry out mechanical mill again, grind revolution 200r.p.m, milling time 24h, has obtained being dispersed in thickness in the natural cellulose nano material single or multiple lift graphene nano sheet material within the scope of 0.35nm～7nm.(as Fig. 2)
Embodiment 12:
With embodiment 11, difference is derivatived cellulose Walocel MT 20.000PV to replace to regenerated cellulose.Obtain being dispersed in thickness in the regenerated cellulose single or multiple lift graphene nano sheet material within the scope of 0.35nm～7nm.
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.Everyly belong to apparent variation or the still row in protection scope of the present invention of variation that technical scheme of the present invention extends out.
Claims (10)
1. be dispersed in the graphene nano sheet material in natural polysaccharide, it is characterized in that: graphene nanometer sheet dispersion of materials is in natural polysaccharide.
2. the graphene nano sheet material being dispersed in natural polysaccharide as claimed in claim 1, is characterized in that, described natural polysaccharide is selected from one or more in Mierocrystalline cellulose, chitin, starch, chitosan.
3. the graphene nano sheet material being dispersed in natural polysaccharide as claimed in claim 2, is characterized in that, preferably, described Mierocrystalline cellulose is one or more of natural herb plant or natural xylophyta.
4. the graphene nano sheet material being dispersed in natural polysaccharide as claimed in claim 2, is characterized in that, preferably, described Mierocrystalline cellulose comprises one or more of the regenerated cellulose that obtained by natural herb plant or natural xylophyta.
5. the graphene nano sheet material being dispersed in natural polysaccharide as claimed in claim 2, is characterized in that, preferably, described Mierocrystalline cellulose comprises one or more of the derivatived cellulose that obtained by natural herb plant or natural xylophyta.
6. prepare the preparation method who is dispersed in the graphene nano sheet material in natural polysaccharide as claimed in claim 1 for one kind, it is characterized in that, the method comprises the following steps: natural polysaccharide mixes with solid graphite, mixture is carried out to mechanical mill, and the thickness that obtains being dispersed in natural polysaccharide nano material is the graphene nanometer sheet matrix material of 0.35nm～7nm, single or multiple lift.
7. the preparation method who is dispersed in the graphene nano sheet material in natural polysaccharide as claimed in claim 6, is characterized in that, preferred, carries out mechanical mill after adding solvent in natural polysaccharide and solid graphite mixture again.
8. the preparation method who is dispersed in the graphene nano sheet material in natural polysaccharide as described in claim 6 or 7, is characterized in that, preferred, solid graphite accounts for the 0.1wt%-80wt% of natural polysaccharide weight; More preferably, solid graphite accounts for the 0.5wt%-30wt% of natural polysaccharide weight.
9. the preparation method who is dispersed in the graphene nano sheet material in natural polysaccharide as described in claim 6 or 7, is characterized in that, preferred, grinding condition is 100-500r.p.m, and milling time is 0.5-100 hour; More preferably, grinding condition is 200-400r.p.m, and milling time is 2-50 hour.
10. a kind of preparation method who is dispersed in the graphene nano sheet material in natural polysaccharide as claimed in claim 7, is characterized in that, preferably, described solvent is selected from one or more in DMF, toluene, benzene, acetone, water; Preferably, solvent quality is natural polysaccharide 0.01 times-500 times; More preferably, solvent quality is natural polysaccharide 0.05 times-100 times.
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| CN105622989A (en) * | 2016-02-29 | 2016-06-01 | 成都新柯力化工科技有限公司 | Compound graphene gel used for rubber filler and preparation method thereof |
| CN105800594A (en) * | 2016-02-19 | 2016-07-27 | 四川大学 | Graphene material based on solid state mechanochemical reactor and preparation method of graphene material |
| CN106365156A (en) * | 2016-08-28 | 2017-02-01 | 桂林新艺制冷设备有限责任公司 | Method for preparing graphene |
| CN106744862A (en) * | 2017-03-20 | 2017-05-31 | 青岛科技大学 | A kind of large stretch of layer graphene aqueous dispersions and preparation method thereof |
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| CN108793138A (en) * | 2017-04-26 | 2018-11-13 | 中国科学院理化技术研究所 | A kind of preparation method of functionalization graphene slurry |
| CN110183733A (en) * | 2019-05-30 | 2019-08-30 | 秦月 | A kind of preparation method of conducting foam |
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| CN104108700A (en) * | 2014-06-20 | 2014-10-22 | 宁波墨西科技有限公司 | Graphene material powder and preparation method |
| CN105800594A (en) * | 2016-02-19 | 2016-07-27 | 四川大学 | Graphene material based on solid state mechanochemical reactor and preparation method of graphene material |
| CN105800594B (en) * | 2016-02-19 | 2019-07-23 | 四川大学 | A kind of grapheme material and preparation method thereof based on solid state mechanochemistry reactor |
| CN105622989A (en) * | 2016-02-29 | 2016-06-01 | 成都新柯力化工科技有限公司 | Compound graphene gel used for rubber filler and preparation method thereof |
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| CN107311160A (en) * | 2016-04-22 | 2017-11-03 | 秦皇岛中科瀚祺科技有限公司 | A kind of graphene nanometer sheet and preparation method thereof |
| CN106365156B (en) * | 2016-08-28 | 2018-07-06 | 桂林新艺制冷设备有限责任公司 | A kind of method for preparing graphene |
| CN106365156A (en) * | 2016-08-28 | 2017-02-01 | 桂林新艺制冷设备有限责任公司 | Method for preparing graphene |
| CN106832426A (en) * | 2016-12-12 | 2017-06-13 | 山东圣泉新材料股份有限公司 | A kind of method for preparing nano-cellulose and gained nano-cellulose |
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| CN106744862B (en) * | 2017-03-20 | 2019-01-08 | 青岛科技大学 | A kind of big lamella graphene aqueous dispersions and preparation method thereof |
| CN108793138A (en) * | 2017-04-26 | 2018-11-13 | 中国科学院理化技术研究所 | A kind of preparation method of functionalization graphene slurry |
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