CN110272039A - A kind of high-concentration biological base two-dimensional material dispersion liquid, preparation method and application - Google Patents
A kind of high-concentration biological base two-dimensional material dispersion liquid, preparation method and application Download PDFInfo
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- CN110272039A CN110272039A CN201810214925.4A CN201810214925A CN110272039A CN 110272039 A CN110272039 A CN 110272039A CN 201810214925 A CN201810214925 A CN 201810214925A CN 110272039 A CN110272039 A CN 110272039A
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Abstract
The invention discloses a kind of high-concentration biological base two-dimensional material dispersion liquid, preparation method and applications.The preparation method of the high-concentration biological base two-dimensional material dispersion liquid includes: offer modifying agent comprising Congo red；Two-dimensional material, modifying agent and solvent are uniformly mixed, and it is ultrasonically treated, two-dimensional material is removed by the intermolecular conjugation of π-π between two-dimensional material lamella and Congo red molecules phenyl ring, later centrifugal treating, obtains high-concentration biological base two-dimensional material dispersion liquid.Preparation method of the invention is simple, high production efficiency, obtained two-dimensional material dispersion liquid is higher with concentration, method is simple and has the characteristics such as excellent storage stability, there is excellent application prospect in fields such as energy-storage battery, supercapacitor, conductive and heat-conductive film, polymer composites, and, Congo red modifying agent used in the present invention is bio-based materials, its is from a wealth of sources, no pollution to the environment, prepared by the extensive high yield that this method is suitable for two-dimensional material.
Description
Technical field
Green that is high the present invention relates to a kind of two-dimensional material dispersion liquid more particularly to a kind of concentration and being stabilized is raw
Substance two-dimensional material dispersion liquid, preparation method and application belong to two-dimensional material removing and dispersion technology field.
Background technique
Graphene, a kind of thickness only have the sheet two dimension carbon nanomaterial of an atomic diameter size (about 0.35nm).Stone
Black alkene has surprising electric conductivity, and carrier mobility at room temperature is about 15000cm2/(V·s)；Graphene has non-
Often good heat-conductive characteristic, it is thermally conductive so far that the thermal coefficient of pure flawless single-layer graphene, which is up to 5300W/mK,
The highest carbon material of coefficient；Graphene has very good optical characteristics, is about in wider wave-length coverage internal absorption factor
2.3%, it appears that almost transparent.The plurality of advantages of graphene makes it be expected to become follow-on revolutionary material.Graphite
The common preparation method of alkene is mechanical stripping method and oxidation-reduction method.Since chemical method passes through the stone that graphene oxide restores
Black alkene is second-rate, and directly obtaining graphene by the removing of graphite is a kind of method being simple and efficient.However, due to graphite linings
Between Van der Waals force it is larger, interlamellar spacing is smaller, therefore efficient removing has certain difficulty.In order to improve graphene in water and other solvents
Dispersion, it usually needs some dispersing agents, such as the small molecule containing aromatic structure or macromolecular or surfactant is added
Deng.The dispersing agent include neopelex, 1- pyrene formic acid, 1- pyrene sulfonic acid, how hydrochlorate, lipid surfactant, or
Person's polyvinylpyrrolidone (PVP) etc..But that there is toxicity is big for these dispersing agents, dispersion effect is poor, dispersion stability is poor and
The problems such as higher cost, it is often more important that gained graphene concentration is too small, generally less than 1mg/mL.
Summary of the invention
The main purpose of the present invention is to provide a kind of high-concentration biological base two-dimensional material dispersion liquid and preparation method thereof, with
Overcome deficiency in the prior art.
Another object of the present invention is to provide the purposes of aforementioned high-concentration biological base two-dimensional material dispersion liquid.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the invention provides a kind of preparation methods of high-concentration biological base two-dimensional material dispersion liquid comprising:
Modifying agent is provided, the modifying agent includes Congo red；
Two-dimensional material, modifying agent and solvent are uniformly mixed, and are ultrasonically treated, two-dimensional material lamella and the Congo are passed through
The intermolecular conjugation of π-π between red molecule phenyl ring removes two-dimensional material, later centrifugal treating, obtains high-concentration biological base two
Tie up material dispersion liquid.
In some embodiments, the modifying agent and the mass ratio of two-dimensional material are 1:0.01~1:1.
In some embodiments, the two-dimensional material includes appointing in graphite, boron nitride, molybdenum disulfide and tungsten disulfide
Meaning a combination of one or more.
In some embodiments, the solvent includes polar solvent.
Further, the polar solvent includes any one in water, ethyl alcohol, methanol, acetone and methylene chloride or two
Kind or more combination.
Further, the time of the ultrasonic treatment is 1~72h, and temperature is 20~40 DEG C.
Further, the ultrasonic power used that is ultrasonically treated is 20~650W.
Further, the centrifuge speeds that the centrifugal treating uses for 500~2000rpm, the time be 30~
90min。
One of preferably, the preparation method further include: with filter membrane to the high-concentration biological base two dimension material
Material dispersion liquid is filtered, and obtains biology base two-dimensional material.
Further, the aperture of the filter membrane is 0.01~0.45 μm.
The embodiment of the invention also provides the high-concentration biological base two-dimensional material dispersion liquids prepared by preceding method comprising
Modified two-dimensional material, modifying agent and solvent, the modifying agent include Congo red.
Further, the concentration of the high-concentration biological base two-dimensional material dispersion liquid is 0.01~50mg/mL.
The embodiment of the invention also provides high-concentration biological base two-dimensional material dispersion liquids above-mentioned to prepare energy-storage battery, surpass
Purposes in grade capacitor, conductive and heat-conductive film or polymer composites.
Compared with prior art, the invention has the advantages that
Preparation method provided by the invention is simple, high production efficiency, and raw materials used from a wealth of sources, is applicable in extensive raw
It produces, is two-dimensional materials removing preparation and the dispersion technologies such as a kind of green, environmental protection, efficient graphene, prepared biology base two
Dimension material dispersion liquid is higher with concentration, method is simple and has the characteristics such as excellent storage stability, in energy-storage battery, surpasses
The fields such as grade capacitor, conductive and heat-conductive film, polymer composites have excellent application prospect, also, change used in the present invention
Property agent it is Congo red be bio-based materials, from a wealth of sources, no pollution to the environment, this method is extensible suitable for graphene, nitridation
It is prepared by the extensive high yield of the two-dimensional materials such as boron, molybdenum disulfide, tungsten disulfide.
Detailed description of the invention
Fig. 1 is schematic arrangement Congo red in a typical embodiments of the invention.
Fig. 2 is the removing of graphene and dispersion process schematic diagram in a typical embodiments of the invention.
Fig. 3 is obtained the schematic diagram of the various concentration redisperse liquid of graphene by the embodiment of the present invention 3.
Fig. 4 a for the obtained graphene of a typical embodiments of the invention transmission scanning electron microscope figure.
Fig. 4 b for the obtained graphene of a typical embodiments of the invention atomic force scanning electron microscope (SEM) photograph.
Fig. 5 for the obtained graphene redisperse liquid of a typical embodiments of the invention optical microscope.
The XPS that Fig. 6 obtains removing graphene by graphite powder and a typical embodiments of the invention schemes.
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose of the invention
Technical solution, it mainly includes walking as follows that being mainly to provide one kind, which can be realized two-dimensional material removing and high concentration dispersing method,
It is rapid: using Congo red as modifying agent, two-dimensional material is sonicated, the two-dimentional material of realization under the intermolecular conjugation of π-π
Expect removing and dispersion in water isopolarity solvent, obtains high concentration two-dimensional material dispersion liquid (> 10mg/mL).It as follows will be to this
Technical solution, its implementation process and principle etc. are further explained.
As shown in Fig. 2, a kind of high-concentration biological base two-dimensional material dispersion liquid that the one aspect of the embodiment of the present invention provides
Preparation method comprising:
Modifying agent is provided, the modifying agent includes Congo red；
Two-dimensional material, modifying agent and solvent are uniformly mixed, and are ultrasonically treated, two-dimensional material lamella and the Congo are passed through
The intermolecular conjugation of π-π between red molecule phenyl ring removes two-dimensional material, later centrifugal treating, obtains high-concentration biological base two
Tie up material dispersion liquid.
In some embodiments, the modifying agent and the mass ratio of two-dimensional material are 1:0.01~1:1.
In some embodiments, the two-dimensional material includes in graphite, boron nitride, molybdenum disulfide and tungsten disulfide etc.
Any one or two or more combinations, but not limited to this.
Further, the two-dimensional material is preferably graphite, and graphite removing preparation is converted into graphene and its graphene
Dispersion, graphene dispersing solution maximum concentration are 50mg/mL.
In some embodiments, the solvent includes water, ethyl alcohol, methanol, acetone and methylene chloride isopolarity solvent, but
It is without being limited thereto.
The present invention using it is Congo red be modifying agent and dispersing agent, the two-dimensional materials such as graphite are sonicated, pass through graphite
Etc. π-π effect between two-dimensional materials lamella and Congo red molecules phenyl ring realize the removings of the two-dimensional materials such as graphene, finally by
The hydrophilic radicals such as carboxyl, amido realize the high concentrations of the two-dimensional materials in water isopolarity solvent such as graphene in Congo red molecules
Dispersion obtains the good two-dimensional material dispersion liquid of high-concentration and stable.
Congo red is diphenyl -4,4'- bis- (azo -2-) -1- amino naphthalenes -4- sodium sulfonate, is brown-red powder, is a kind of
Reproducible biomass material.It is Congo red negatively charged in water ,-the SO being had on phenyl ring3,-NH2With-N=N- group in altogether
Yoke planar structure (referring to Fig. 1).Strong π-π effect and-NH between Benzene Molecule2, electric charge transfer acts between-N=N- group Molecule
It is considered as the major impetus for leading to the removing of the two-dimensional materials such as graphene.In addition ,-the SO on phenyl ring3Group has been to confer to stone
The two-dimensional materials such as black alkene in polar solvent there is superelevation to disperse energy.Therefore, it can firmly be adsorbed in as modifying agent is Congo red
Realize its removing and non-covalent modification to two-dimensional materials such as graphenes in the two-dimensional materials such as graphene upper surface.
Further, the time of the ultrasonic treatment is 1~72h, and temperature is 20~40 DEG C.
Further, the ultrasonic power used that is ultrasonically treated is 20~650W.
Further, the centrifuge speeds that the centrifugal treating uses for 500~2000rpm, the time be 30~
90min。
One of preferably, the preparation method further include: with filter membrane to the high-concentration biological base two dimension material
Material dispersion liquid is filtered, and obtains biology base two-dimensional material.
Further, the aperture of the filter membrane is 0.01~0.45 μm.
The other side of the embodiment of the present invention additionally provides the high-concentration biological base two-dimensional material prepared by preceding method
Dispersion liquid comprising modified two-dimensional material, modifying agent and solvent, the modifying agent include Congo red.
In some embodiments, the two-dimensional material of the modification includes graphene, boron nitride, molybdenum disulfide and curing
Any one in tungsten etc. or two or more combinations, but not limited to this.
Further, the graphene includes graphene nanometer sheet.
Further, the average diameter of the graphene nanometer sheet is 0.5~15 μm.
In some embodiments, the solvent includes water, ethyl alcohol, methanol, acetone and methylene chloride isopolarity solvent, but
It is without being limited thereto.
Further, the concentration of the high-concentration biological base two-dimensional material dispersion liquid is 0.01~50mg/mL.
The other side of the embodiment of the present invention additionally provides high-concentration biological base two-dimensional material dispersion liquid above-mentioned and is making
Purposes in the conductive and heat-conductives films such as standby energy-storage battery, supercapacitor, graphene or polymer composites.
In conclusion preparation method of the invention is simple, high production efficiency, obtained two-dimensional material dispersion liquid with concentration compared with
High, method in energy-storage battery, supercapacitor, conductive and heat-conductive film, is gathered simply and with characteristics such as excellent storage stabilities
The fields such as compound composite material have excellent application prospect, also, it is bio-based materials that modifying agent used in the present invention is Congo red,
Its is from a wealth of sources, no pollution to the environment, prepared by the extensive high yield that this method is suitable for two-dimensional material.
Below by way of several embodiments and in conjunction with the attached drawing technical solution that present invention be described in more detail.However, selected
Embodiment be merely to illustrate the present invention, and do not limit the scope of the invention.
Embodiment 1
By the Congo red aqueous solution for being add to deionized water configuration 0.1mg/mL, then it is with graphite according to Congo red
The graphite powder that diameter is 50 μm is added in 0.1:10 mass ratio.By mixed liquor under conditions of 25 DEG C, ultrasound removing 12h, ultrasonic function
Rate is 200W.By product with the centrifugation rate of 1500rpm, centrifugal treating 30min.Separate 2/3 solution of upper layer, as graphene point
Dispersion liquid, wherein the average diameter of graphene nanometer sheet is 5 μm.Measuring its concentration is 5mg/mL, and graphene dispersing solution is used hole
The polytetrafluoroethylene film vacuum filter that diameter is 0.22 μm, is washed with deionized water to colourless.
Embodiment 2
It is then 0.1 with graphite according to Congo red by the Congo red ethanol solution for being added to configuration 0.1mg/mL in ethyl alcohol:
The graphite powder that diameter is 80 μm is added in 5 mass ratioes.By mixed liquor under conditions of 30 DEG C, ultrasound removes 48h, and ultrasonic power is
100W.By product with the centrifugation rate of 2000rpm, centrifugal treating 45min.Separate 2/3 solution of upper layer, as graphene dispersion
Liquid, wherein the average diameter of graphene nanometer sheet is 0.5 μm.Measuring its concentration is 20mg/mL, and graphene dispersing solution is used hole
The polytetrafluoroethylene film vacuum filter that diameter is 0.45 μm, is washed with deionized water to colourless.
Embodiment 3
By the Congo red aqueous solution for being add to deionized water configuration 0.1mg/mL, then it is with graphite according to Congo red
The graphite powder that diameter is 60 μm is added in 0.1:10 mass ratio.By mixed liquor under conditions of 40 DEG C, ultrasound removing 72h, ultrasonic function
Rate is 300W.By product with the centrifugation rate of 2000rpm, centrifugal treating 90min.Separate 2/3 solution of upper layer, as graphene point
Dispersion liquid, wherein the average diameter of graphene nanometer sheet is 15 μm.Measuring its concentration is 50mg/mL, and graphene dispersing solution is used
The polytetrafluoroethylene film vacuum filter that aperture is 0.45 μm, is washed with deionized water to colourless.
By gained filter cake in embodiment 3,50 DEG C of dryings are for 24 hours in a vacuum drying oven.Filter cake is ground to it is broken, according to 2-
The concentration of 50mg/mL is add to deionized water, and ultrasound 30min, obtains the graphene dispersing solution of various concentration at 25 DEG C, will be divided
After dispersion liquid is stored for 24 hours at 25 DEG C of room temperature, apparent precipitating is not observed and (as shown in Figure 3) occurs in flocculation.
The transmission scanning electron microscope figure of the obtained graphene of the present embodiment as shown in fig. 4 a, atomic force scanning electron microscope (SEM) photograph such as Fig. 4 b institute
Show.The optical microscope of the obtained graphene redisperse liquid of the present embodiment is as shown in Figure 5.Fig. 6 shows graphite powder and this implementation
Example obtains the XPS figure of removing graphene.
Embodiment 4
By the Congo red methanol solution for being added to configuration 0.1mg/mL in methanol, then it is with boron nitride according to Congo red
The boron nitride powder that diameter is 50 μm is added in 0.1:1 mass ratio.By mixed liquor under conditions of 20 DEG C, ultrasound removing 72h, ultrasonic function
Rate is 300W.By product with the centrifugation rate of 500rpm, centrifugal treating 90min.Separate 2/3 solution of upper layer, as boron nitride point
Dispersion liquid.Measuring its concentration is 20mg/mL, uses aperture for 0.35 μm of polytetrafluoroethylene film vacuum mistake boron nitride dispersion
Filter, is washed till colourless with methanol.
Embodiment 5
By the Congo red acetone soln for being added to configuration 0.1mg/mL in acetone, then it is with molybdenum disulfide according to Congo red
The molybdenum disulphide powder that diameter is 50 μm is added in 1:1 mass ratio.By mixed liquor under conditions of 40 DEG C, ultrasound removing 1h, ultrasonic function
Rate is 650W.By product with the centrifugation rate of 2000rpm, centrifugal treating 30min.Separate 2/3 solution of upper layer, as molybdenum disulfide
Dispersion liquid.Measuring its concentration is 0.01mg/mL, uses aperture for 0.01 μm of polytetrafluoroethylene film vacuum boron nitride dispersion
Filtering, is washed till colourless with acetone.
Embodiment 6
By the dichloromethane solution of Congo red adding into dichloromethane configuration 0.1mg/mL, then according to Congo red with two
Tungsten sulfide is the curing tungsten powder that 0.5:1 mass ratio is added that diameter is 50 μm.By mixed liquor under conditions of 30 DEG C, ultrasound removing
60h, ultrasonic power 20W.By product with the centrifugation rate of 1000rpm, centrifugal treating 50min.2/3 solution of upper layer is separated, i.e.,
For tungsten disulfide dispersion liquid.Measuring its concentration is 10mg/mL, uses aperture for 1 μm of polytetrafluoroethylene (PTFE) boron nitride dispersion
Film vacuum filter is washed till colourless with methylene chloride.
Comparative example
This comparative example uses the identical method of embodiment 3, and graphite is removed and dispersed with different modifying agent, ties
Fruit is shown in Table 1.
Pass through the comparison of embodiment 1-6 and comparative example 1, it can be seen that, selection is Congo red to be used as modifying agent and dispersing agent, can
To obtain, stability is good, be uniformly dispersed, concentration is high, the biology base two-dimensional material dispersion liquid with excellent storage stability.
In addition, inventor also refers to the mode of embodiment 1- embodiment 6, with the other raw materials listed in this specification
It is tested with condition etc., and the biology base two-dimensional material dispersion liquid of high concentration, high stability has equally been made.
In conclusion having concentration higher, square by the two-dimensional material dispersion liquid that above-mentioned technical proposal of the invention obtains
Method is simple and has the characteristics such as excellent storage stability, multiple in energy-storage battery, supercapacitor, conductive and heat-conductive film, polymer
The fields such as condensation material have excellent application prospect, also, it is bio-based materials, source that modifying agent used in the present invention is Congo red
Extensively, prepared by no pollution to the environment, the extensive high yield that this method is suitable for two-dimensional material.
It should be understood that the technical concepts and features of above-described embodiment only to illustrate the invention, ripe its object is to allow
The personage for knowing technique cans understand the content of the present invention and implement it accordingly, and protection model of the invention can not be limited with this
It encloses.Any equivalent change or modification in accordance with the spirit of the invention should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of high-concentration biological base two-dimensional material dispersion liquid, characterized by comprising:
Modifying agent is provided, the modifying agent includes Congo red；
Two-dimensional material, modifying agent and solvent are uniformly mixed, and are ultrasonically treated, two-dimensional material lamella and Congo red point are passed through
The intermolecular conjugation of π-π between sub- phenyl ring removes two-dimensional material, later centrifugal treating, obtains high-concentration biological base two dimension material
Expect dispersion liquid.
2. preparation method according to claim 1, it is characterised in that: the modifying agent and the mass ratio of two-dimensional material are 1:
0.01~1:1.
3. preparation method according to claim 1, it is characterised in that: the two-dimensional material includes graphite, boron nitride, two sulphur
Change any one in molybdenum and tungsten disulfide or two or more combinations.
4. preparation method according to claim 1, it is characterised in that: the solvent includes polar solvent；Preferably, described
Polar solvent includes any one or two or more combinations in water, ethyl alcohol, methanol, acetone and methylene chloride.
5. preparation method according to claim 1, it is characterised in that: the time of the ultrasonic treatment is 1~72h, temperature
It is 20~40 DEG C；And/or the ultrasonic power used that is ultrasonically treated is 20~650W.
6. preparation method according to claim 1, it is characterised in that: the centrifuge speeds that the centrifugal treating uses for
500~2000rpm, time are 30~90min.
7. preparation method according to claim 1 to 6, it is characterised in that further include: with filter membrane to the height
Concentration biology base two-dimensional material dispersion liquid is filtered, and obtains biology base two-dimensional material；Preferably, the aperture of the filter membrane is
0.01~0.45 μm.
8. the high-concentration biological base two-dimensional material dispersion liquid prepared by any one of claim 1-7 the method, feature exist
In including modified two-dimensional material, modifying agent and solvent, the modifying agent includes Congo red.
9. high-concentration biological base two-dimensional material dispersion liquid according to claim 8, it is characterised in that: the two dimension of the modification
Material includes any one or two or more combinations in graphene, boron nitride, molybdenum disulfide and tungsten disulfide；Preferably,
The graphene includes graphene nanometer sheet；Especially preferred, the average diameter of the graphene nanometer sheet is 0.5~15 μm；
And/or the solvent includes polar solvent；Preferably, the polar solvent includes water, ethyl alcohol, methanol, acetone and dichloro
Any one in methane or two or more combinations；
And/or the concentration of the high-concentration biological base two-dimensional material dispersion liquid is 0.01~50mg/mL.
10. the high-concentration biological base two-dimensional material dispersion liquid as described in any one of claim 8-9 is preparing energy-storage battery, is surpassing
Purposes in grade capacitor, conductive and heat-conductive film or polymer composites.
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Application publication date: 20190924 |