CN108117068A - A kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid - Google Patents
A kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid Download PDFInfo
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- CN108117068A CN108117068A CN201810001109.5A CN201810001109A CN108117068A CN 108117068 A CN108117068 A CN 108117068A CN 201810001109 A CN201810001109 A CN 201810001109A CN 108117068 A CN108117068 A CN 108117068A
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Abstract
The invention discloses a kind of preparation methods of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid.The present invention first, nano micro crystal cellulose is dispersed in water, the dispersion A of certain solid content is made；Meanwhile by graphene dispersion in water, the dispersion B of certain solid content is made.Then, dispersion A is dispersed in dispersion B, regulates and controls the additional proportion of nano micro crystal cellulose and graphene, regulation system pH to certain value obtains A/B water phase composite dispersion liquids.Finally, the A/B water phase composite dispersion liquids of acquisition are placed in ultrasonic cell disruptor and are ultrasonically treated certain time under certain power, highly stable graphene/nanometer microcrystalline cellulose aqueous dispersion liquid is prepared.The present invention is based on electrostatic interaction, space steric effect and the associative mechanisms of ultrasonication to prepare high-stability graphene/nano micro crystal cellulose aqueous dispersion liquid；The present invention realizes synergistic effect, avoids simple technique superposition.
Description
Technical field
The invention belongs to graphene composite material fields, and in particular to a kind of highly stable scattered graphene Aqueous dispersions
The preparation method of liquid.
Background technology
Graphene possesses unique two-dimentional honeycomb lattice structure, is presently found most thin two dimensional crystal material,
Thickness is only 0.335 nm.Graphene has excellent electricity, mechanics and optically and mechanically property, graphene are unique and excellent
Performance so that it can be widely applied to solar cell, ultracapacitor, biological detection, display, fuel cell etc..
The effective of strain in composite material, conduction and heat transfer can be greatly promoted by improving the dispersiveness of graphene particle
The formation of network, so that graphene has outstanding potentiality in functional material production.However, due between graphene particle
In the presence of very strong Van der Waals force, graphene film layer structure is easy to be condensed into graphene, this hinder significantly graphene into one
Step application.In this sense, how to realize that graphene uniform is stablized scattered with important in matrices of composite material
Realistic meaning.Generally believe that scattered in aqueous medium of hydrophobicity graphene is a very big challenge at present, because it is essential
Above film, coating or composite material are further processed into for graphene provide more possible applications.
To make full use of the surface of graphene and interfacial characteristics, it is necessary to adopt a series of measures, be at good, abundant
Dispersity.In film, coating or field of compound material, the scattered and dispersion stabilization of graphene directly affects it should
Use performance.Therefore graphene to be made to be utilized effectively in film, coating or composite material, solves the scattering problem of graphene
It is most important.
At present, based on electrostatic interaction, space steric effect and the associative mechanism of ultrasonication prepare the graphene of high stable/
The research of nano micro crystal cellulose aqueous dispersion liquid, there is not been reported both at home and abroad.Physico-chemical property of the present invention from graphene in itself
Start with, it is theoretical based on stably dispersing on the basis of redox graphene reunion reason is understood（Dlvo theory）, disperseed
Property good graphene/nanometer microcrystalline cellulose aqueous dispersion liquid, be graphene it is special in film, coating or field of compound material
Change, functionalized application provide theoretical foundation and technical support, have important theory significance and practical significance.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of graphene/nanometer microcrystalline cellulose aqueous dispersion liquids
Preparation method.
The purpose of the present invention is what is be achieved through the following technical solutions：
First, nano micro crystal cellulose is dispersed in water, the dispersion A of certain solid content is made；Meanwhile graphene is divided
It dissipates in water, the dispersion B of certain solid content is made.Then, dispersion A is dispersed in dispersion B, regulates and controls nanometer
The additional proportion of microcrystalline cellulose and graphene, regulation system pH to certain value obtain A/B water phase composite dispersion liquids.Then, will
The A/B water phase composite dispersion liquids of acquisition are placed in ultrasonic cell disruptor is ultrasonically treated certain time under certain power,
Highly stable graphene/nanometer microcrystalline cellulose aqueous dispersion liquid is prepared.
Furtherly, the solid content of the nano micro crystal cellulose Aqueous dispersions system A is 0.2~1.0%.
Furtherly, the pH of the nano micro crystal cellulose Aqueous dispersions system A is 6~7.
Furtherly, the nano micro crystal cellulose for 300~600 nanometers of length, 30~80 nanometers of width it is rodlike
Cellulose nanocrystal.
Furtherly, the solid content of the dispersion B is 0.5~2%.
Furtherly, the pH of the dispersion B is adjusted to 7~8.
Furtherly, the graphene of the dispersion B is redox graphene.
Furtherly, the pH of the A/B water phase composite dispersion liquids is adjusted to 6~7.
Furtherly, the additional proportion of the nano micro crystal cellulose is the 0~4% of graphene quality.
Furtherly, the ultrasonic power is 720W, sonication treatment time 5min.
Beneficial effects of the present invention：
（1）, overall technology using water as decentralized medium, meet the theory of Green design, also comply with environmentally friendly nano-graphite material
The developing goal of material；
（2）Electrostatic interaction, the synergistic effect of space steric effect and ultrasonication are played, graphene water is easily solved and is mutually difficult to point
Scattered key issue；
（3）Simple production process, it is easy to operate, it achieves noticeable achievement；
（4）Production process is safe and non-toxic, pollution-free.
Description of the drawings
Fig. 1 graphene suspensions (a1, a2), nano micro crystal cellulose suspension (b1, b2) and graphene/nano
The TEM figures of rice microcrystalline cellulose aqueous dispersion liquid (c1, c2)；
The ultraviolet-visible absorption spectroscopy spectrogram of Fig. 2 graphene/nanometer microcrystalline cellulose aqueous dispersion liquids；
The sedimentation experiment electronic photo of Fig. 3 graphene/nanometer microcrystalline cellulose aqueous dispersion liquids.
Specific embodiment
With reference to embodiment, the present invention is described further, but the scope of protection of present invention is not limited to
The scope of embodiment expression.Unless otherwise indicated.
The principle of the present invention is analyzed：For dispersion stabilizations of the NCC in graphene aqueous phase system, can be managed according to DLVO
Resultant action potential energy U between particle inTTo be evaluated：UT=UA+UR+UHR+USTIn formula：UAFor model ylid bloom action potential energy, URFor
Effect of Electric Double Layer potential energy, UHRRepel potential energy, U for aquationSTFor steric hindrance potential energy.When NCC is dispersed in graphene aqueous phase system
In, the dispersion stabilization of suspended substance will depend on intergranular model ylid bloom action potential energy UA, Effect of Electric Double Layer potential energy UR, space bit
Hinder potential energy USTAnd aquation repels potential energy UHRThe sum of.UAIt is always attraction energy； URSize rely on particle surface potential value, and
The size of particle surface current potential depends on system pH； USTIt is related to the high molecular polymer in dispersion； UHRThen with
The hydrophilicrty on grain surface is closely related.
The present invention is by strengthening electrostatic interaction（Based on dlvo theory, NCC can be adsorbed by hydrogen bond action etc. in graphene
On）, space steric effect（NCC is chain macromolecule compound, there is certain molecule internal tension）And ultrasonication（Ultrasonic wave with
A kind of form of energy acts on reactant, helps to improve reaction efficiency, have power is big, penetration power is strong, good directionality and
The advantages that cavitation, improves the repulsion potential energy between graphene particles）, improve its dispersiveness in water phase, stability, be graphite
Functionalized application of the alkene in film, coating or composite material lays the foundation.
Embodiment 1：
First, nano micro crystal cellulose is dissolved in the water, regulation system pH to 6.5, solid content 0.2%, and persistently disperse
20min obtains dispersion A.Secondly, by certain graphene dispersion in water, the dispersion that solid content is 0.5% is made,
Regulation system pH persistently disperses 20min to 7.5, obtains dispersion B.Then, dispersion A is dispersed in dispersion B
In, regulate and control 0%, regulation system pH to 7.0 of the addition of nano micro crystal cellulose for the addition of graphene, obtain A/B water phases
Composite dispersion liquid.Finally, the A/B water phase composite dispersion liquids of acquisition are placed in ultrasonic cell disruptor and surpassed under power 720W
5~8min of sonication, sample ultrasonic environment are tepidarium.Experience more than joint step, obtains graphene aqueous dispersion liquid.And lead to
TEM, ultraviolet-visible absorption spectroscopy, sedimentation experiment etc. is crossed to be analyzed and compareed.As shown in figure, NCC more can equably divide
It is dispersed in graphene aqueous phase solution.Figure two with the increase of UV, visible light optical wavelength, the compound aqueous dispersion liquids of graphene/NCC
Absorbance is consequently increased, and further proves that NCC can improve dispersiveness and stability of the graphene in water phase.From the heavy of figure three
Drop Experimental electron photo can be clear and intuitive find out increasing with NCC additional proportions, compound aqueous phase solution disperses more equal
It is even.
Embodiment 2：
First, nano micro crystal cellulose is dissolved in the water, regulation system pH to 6.5, solid content 0.2%, and persistently disperse
20min obtains dispersion A.Secondly, by certain graphene dispersion in water, the dispersion that solid content is 0.5% is made,
Regulation system pH persistently disperses 20min to 7.5, obtains dispersion B.Then, dispersion A is dispersed in dispersion B
In, regulate and control 1%, regulation system pH to 7.0 of the addition of nano micro crystal cellulose for the addition of graphene, obtain A/B water phases
Composite dispersion liquid.Finally, the A/B water phase composite dispersion liquids of acquisition are placed in ultrasonic cell disruptor and surpassed under power 720W
5~8min of sonication, sample ultrasonic environment are tepidarium.Experience more than joint step, obtains graphene/nanometer microcrystalline cellulose
Aqueous dispersion liquid.And pass through TEM, ultraviolet-visible absorption spectroscopy, sedimentation experiment etc. and analyzed and compareed.As shown in Figure 1, NCC
It can more be evenly dispersed in graphene aqueous phase solution.For Fig. 2 with the increase of UV, visible light optical wavelength, graphene/NCC is compound
The absorbance of aqueous dispersion liquid is consequently increased, and it is dispersed and stable in water phase further to prove that NCC can improve graphene
Property.From the sedimentation experiment electronic photo of figure three can be clear and intuitive find out increasing with NCC additional proportions, compound aqueous phase solution
Scattered is more uniformly distributed.
Embodiment 3：
First, nano micro crystal cellulose is dissolved in the water, regulation system pH to 6.5, solid content 0.2%, and persistently disperse
20min obtains dispersion A.Secondly, by certain graphene dispersion in water, the dispersion that solid content is 0.5% is made,
Regulation system pH persistently disperses 20min to 7.5, obtains dispersion B.Then, dispersion A is dispersed in dispersion B
In, regulate and control 2%, regulation system pH to 7.0 of the addition of nano micro crystal cellulose for the addition of graphene, obtain A/B water phases
Composite dispersion liquid.Finally, the A/B water phase composite dispersion liquids of acquisition are placed in ultrasonic cell disruptor and surpassed under power 720W
5~8min of sonication, sample ultrasonic environment are tepidarium.Experience more than joint step, obtains graphene/nanometer microcrystalline cellulose
Aqueous dispersion liquid.And pass through TEM, ultraviolet-visible absorption spectroscopy, sedimentation experiment etc. and analyzed and compareed.As shown in figure, NCC
It can more be evenly dispersed in graphene aqueous phase solution.For figure two with the increase of UV, visible light optical wavelength, graphene/NCC is multiple
The absorbance of Heshui phase dispersant liquid is consequently increased, and it is dispersed and steady in water phase further to prove that NCC can improve graphene
It is qualitative.From the sedimentation experiment electronic photo of Fig. 3 can be clear and intuitive find out increasing with NCC additional proportions, Compound Water mixes
What liquid disperseed is more uniformly distributed.
Embodiment 4：
First, nano micro crystal cellulose is dissolved in the water, regulation system pH to 6.5, solid content 0.2%, and persistently disperse
20min obtains dispersion A.Secondly, by certain graphene dispersion in water, the dispersion that solid content is 0.5% is made,
Regulation system pH persistently disperses 20min to 7.5, obtains dispersion B.Then, dispersion A is dispersed in dispersion B
In, regulate and control 3%, regulation system pH to 7.0 of the addition of nano micro crystal cellulose for the addition of graphene, obtain A/B water phases
Composite dispersion liquid.Finally, the A/B water phase composite dispersion liquids of acquisition are placed in ultrasonic cell disruptor and surpassed under power 720W
5~8min of sonication, sample ultrasonic environment are tepidarium.Experience more than joint step, obtains graphene/nanometer microcrystalline cellulose
Aqueous dispersion liquid.And pass through TEM, ultraviolet-visible absorption spectroscopy, sedimentation experiment etc. and analyzed and compareed.As shown in Figure 1, NCC
It can more be evenly dispersed in graphene aqueous phase solution.For Fig. 2 with the increase of UV, visible light optical wavelength, graphene/NCC is compound
The absorbance of aqueous dispersion liquid is consequently increased, and it is dispersed and stable in water phase further to prove that NCC can improve graphene
Property.From the sedimentation experiment electronic photo of Fig. 3 can be clear and intuitive find out increasing with NCC additional proportions, compound aqueous phase solution
Scattered is more uniformly distributed.
Embodiment 5：
First, nano micro crystal cellulose is dissolved in the water, regulation system pH to 6.5, solid content 0.2%, and persistently disperse
20min obtains dispersion A.Secondly, by certain graphene dispersion in water, the dispersion that solid content is 0.5% is made,
Regulation system pH persistently disperses 20min to 7.5, obtains dispersion B.Then, dispersion A is dispersed in dispersion B
In, regulate and control 4%, regulation system pH to 7.0 of the addition of nano micro crystal cellulose for the addition of graphene, obtain A/B water phases
Composite dispersion liquid.Finally, the A/B water phase composite dispersion liquids of acquisition are placed in ultrasonic cell disruptor and surpassed under power 720W
5~8min of sonication, sample ultrasonic environment are tepidarium.Experience more than joint step, obtains graphene/nanometer microcrystalline cellulose
Aqueous dispersion liquid.And pass through TEM, ultraviolet-visible absorption spectroscopy, sedimentation experiment etc. and analyzed and compareed.As shown in Figure 1, NCC
It can more be evenly dispersed in graphene aqueous phase solution.For Fig. 2 with the increase of UV, visible light optical wavelength, graphene/NCC is compound
The absorbance of aqueous dispersion liquid is consequently increased, and it is dispersed and stable in water phase further to prove that NCC can improve graphene
Property.From the sedimentation experiment electronic photo of Fig. 3 can be clear and intuitive find out increasing with NCC additional proportions, compound aqueous phase solution
Scattered is more uniformly distributed.
It can be seen that original graphite alkene easily reunites in aqueous phase system, is difficult to disperse, received so as to lose to a certain extent
Meter Xiao Ying.And the method for the present invention is used, highly stable graphene/nanometer microcrystalline cellulose aqueous dispersion liquid can be made, this
Be conducive to preparation and the functionalized application of film, coating or composite material.
Although the embodiments of the present invention have been disclosed as above, but its be not restricted in specification and embodiment it is listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, it is of the invention and unlimited
In specific details and shown here as the example with description.
Claims (10)
1. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid, rich by nano micro crystal cellulose surface
Rich hydrophilic radical assigns graphene water phase moisture dispersibility；Electrostatic force, steric hindrance based on nano micro crystal cellulose
Effect improves graphene Aqueous dispersions stability, is specifically：
First, nano micro crystal cellulose is dispersed in water, the dispersion A of certain solid content is made；Meanwhile graphene is divided
It dissipates in water, the dispersion B of certain solid content is made；Secondly, dispersion A is dispersed in dispersion B, regulates and controls nanometer
The additional proportion of microcrystalline cellulose and graphene, regulation system pH to certain value obtain A/B water phase composite dispersion liquids；Finally, will
The A/B water phase composite dispersion liquids of acquisition are placed in ultrasonic cell disruptor is ultrasonically treated certain time under certain power,
Highly stable graphene/nanometer microcrystalline cellulose aqueous dispersion liquid is prepared.
2. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid according to claim 1, feature
It is：The solid content of the nano micro crystal cellulose Aqueous dispersions system A is 0.2~1.0%.
3. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid according to claim 1, feature
It is：The pH of the nano micro crystal cellulose Aqueous dispersions system A is 6~7.
4. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid according to claim 1, feature
It is：The nano micro crystal cellulose is 300~600 nanometers of length, the rod-like fibre element of 30~80 nanometers of width is nanocrystalline.
5. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid according to claim 1, feature
It is：The solid content of the dispersion B is 0.5~2%.
6. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid according to claim 1, feature
It is：The pH of the dispersion B is adjusted to 7~8.
7. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid according to claim 1, feature
It is：The graphene of the dispersion B is redox graphene.
8. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid according to claim 1, feature
It is：The pH of the A/B water phase composite dispersion liquids is adjusted to 6~7.
9. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid according to claim 1, feature
It is：The additional proportion of the nano micro crystal cellulose is the 0~4% of graphene quality.
10. a kind of preparation method of graphene/nanometer microcrystalline cellulose aqueous dispersion liquid according to claim 1, special
Sign is：The ultrasonic power is 720W, sonication treatment time 5min.
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Cited By (5)
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| CN109665519A (en) * | 2019-01-25 | 2019-04-23 | 复旦大学 | A method of cellulose up-stripping graphene in alkali systems altogether |
| CN109970874A (en) * | 2019-03-20 | 2019-07-05 | 武汉理工大学 | Improve Cellulose nanocrystal redispersibility, the end modified method of stability of suspension |
| CN110204791A (en) * | 2019-07-03 | 2019-09-06 | 桂林理工大学 | A kind of acid imide functionalization graphene/sisal cellulose nano microcrystalline composite heat-conducting film and preparation method thereof |
| WO2020195974A1 (en) * | 2019-03-22 | 2020-10-01 | 北越コーポレーション株式会社 | Nanocarbon dispersion liquid, method for producing same, nanocarbon dispersing agent, and electromagnetic wave-shielding material |
| CN114381343A (en) * | 2022-01-27 | 2022-04-22 | 鲁西工业装备有限公司 | Ultrasonic descaling additive and descaling method thereof |
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| CN106633791A (en) * | 2016-10-20 | 2017-05-10 | 国家纳米科学中心 | Preparation method of nano-cellulose-based flexible conductive film |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665519A (en) * | 2019-01-25 | 2019-04-23 | 复旦大学 | A method of cellulose up-stripping graphene in alkali systems altogether |
| CN109970874A (en) * | 2019-03-20 | 2019-07-05 | 武汉理工大学 | Improve Cellulose nanocrystal redispersibility, the end modified method of stability of suspension |
| WO2020195974A1 (en) * | 2019-03-22 | 2020-10-01 | 北越コーポレーション株式会社 | Nanocarbon dispersion liquid, method for producing same, nanocarbon dispersing agent, and electromagnetic wave-shielding material |
| JPWO2020195974A1 (en) * | 2019-03-22 | 2020-10-01 | ||
| WO2020194380A1 (en) * | 2019-03-22 | 2020-10-01 | 北越コーポレーション株式会社 | Nanocarbon dispersion liquid, method for producing same, and nanocarbon dispersing agent |
| JP7177912B2 (en) | 2019-03-22 | 2022-11-24 | 北越コーポレーション株式会社 | Method for producing nanocarbon dispersion, nanocarbon dispersant and electromagnetic wave shielding material |
| CN110204791A (en) * | 2019-07-03 | 2019-09-06 | 桂林理工大学 | A kind of acid imide functionalization graphene/sisal cellulose nano microcrystalline composite heat-conducting film and preparation method thereof |
| CN114381343A (en) * | 2022-01-27 | 2022-04-22 | 鲁西工业装备有限公司 | Ultrasonic descaling additive and descaling method thereof |
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