CN107010614A - Aqueous liquid dispersion of carbon nanomaterial and preparation method thereof - Google Patents
Aqueous liquid dispersion of carbon nanomaterial and preparation method thereof Download PDFInfo
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- CN107010614A CN107010614A CN201710272712.2A CN201710272712A CN107010614A CN 107010614 A CN107010614 A CN 107010614A CN 201710272712 A CN201710272712 A CN 201710272712A CN 107010614 A CN107010614 A CN 107010614A
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Abstract
The present invention relates to a kind of aqueous liquid dispersion of carbon nanomaterial, it includes carbon nanomaterial, surfactant, reducing sugar and deionized water.The aqueous liquid dispersion of above-mentioned carbon nanomaterial, due to the addition of reducing sugar, reducing sugar has free aldehyde or ketone group so that its is water-soluble and be dispersed in system.Reducing sugar is intermolecular easily with Hydrogenbond, can be with the uniform and stable presence of whole dispersion.In addition, reducing sugar molecule is due to electron conjugated effect, shape tends to be spherical, and volume is much smaller than carbon nanomaterial, and lubrication is served to whole system；The dispersion of high dispersive concentration can to sum up be formed.The aqueous liquid dispersion of above-mentioned carbon nanomaterial, is aqueous liquid dispersion, and organic solvent system and super acid system are not used, environmental protection, and expands the application of carbon nanomaterial.The invention also discloses a kind of preparation method of the aqueous liquid dispersion of carbon nanomaterial.
Description
Technical field
The present invention relates to carbon nanomaterial technical field, the aqueous liquid dispersion of more particularly to a kind of carbon nanomaterial and its
Preparation method.
Background technology
Nano material is inhaled due to Van der Waals for larger between huge specific surface area, particle, electrostatic force and capillary
The factors such as power, very easily reunite, so as to have a strong impact on the using effect in later stage.Carbon nanomaterial is in the liquid phase in theory
The possibility reunited will be less than pure powder, so carbon nanomaterial in the liquid phase can stable dispersion, so as to obtain scattered
The property dispersion liquid that good, stability is high and solid content is big, enters but promotes the development of carbon nanomaterial downstream application.
At present, the dispersion of traditional carbon nanomaterial mainly has three kinds：
The first：Aqueous surfactant solution；The system cost is low, easy to operate；But carbon nanomaterial is scattered dense
Degree is very low, it is impossible to meet the demand of carbon nanomaterial application development.
Second：Organic solvent；Compared to the first, although the system can obtain the scattered dense of higher carbon nanomaterial
Degree；But, organic solvent cost is high, boiling point is higher and the later stage is difficult to remove；In addition, organic solvent more or less has poison in itself
The hazard properties such as property, inflammability and environmental hazard, under higher and higher environmental requirement, it has not been adapted under the new situation
Demand for development.
The third：Super acid；Super acid is by the redox with carbon nanomaterial, grafting, modification, so must reach good
Dispersibility.The system can obtain current highest dispersion concentration.But, the system have highly acid, it is high to equipment requirement,
And significant care is needed in operating process, with higher potential potential safety hazard, while the waste liquor contamination such as strong acid situation is still
Cause anxiety.
Especially in the coating of carbon nanomaterial most application prospect, conductive film, electric heating thermal insulation equipment, energy storage storage lamp
It is that close use occasion is being contacted with people mostly, organic solvent and super acid can not meet what is increasingly improved etc. technical field
Environmental requirement, so as to limit the application of carbon nanomaterial.
Therefore, a kind of dispersion liquid for forming high dispersive concentration and the carbon nanomaterial of environmental protection is needed badly.
The content of the invention
Based on this, it is necessary to for existing carbon nanomaterial dispersion or dispersion concentration it is low or not environmentally the problem of,
A kind of aqueous liquid dispersion for forming high dispersive concentration and the carbon nanomaterial of environmental protection is provided.
A kind of aqueous liquid dispersion of carbon nanomaterial, including carbon nanomaterial, surfactant, reducing sugar and go from
Sub- water.
The aqueous liquid dispersion of above-mentioned carbon nanomaterial, due to the addition of reducing sugar, reducing sugar have free aldehyde or
Ketone group is so that its is water-soluble and be dispersed in system.Reducing sugar it is intermolecular easily with Hydrogenbond, can with it is whole
Dispersion is uniform and stable to be present.In addition, reducing sugar molecule is due to electron conjugated effect, shape tends to be spherical, and volume is far small
In carbon nanomaterial, lubrication is served to whole system；The dispersion of high dispersive concentration can to sum up be formed.Above-mentioned carbon is received
The aqueous liquid dispersion of rice material, is aqueous liquid dispersion, organic solvent system and super acid system is not used, environmental protection, and is expanded
The application of carbon nanomaterial.
In one of the embodiments, the carbon nanomaterial is CNT or graphene.
In one of the embodiments, a diameter of 5nm~40nm of the CNT, wall thickness be 1 layer~10 layers, length
For 1 μm~20 μm.
In one of the embodiments, the reducing sugar is selected from glucose, fructose, galactolipin, lactose or maltose
It is one or more of.
In one of the embodiments, the surfactant includes nonionic surface active agent and second surface is lived
Property agent；The second surface activating agent be selected from sterol and its salt-forming compound, bile acid and its salt-forming compound or bilichol and
One or more in its salt-forming compound.
In one of the embodiments, the nonionic surface active agent is selected from polyvinyl alcohol and its derivative or poly-
One or more in oxygen vinyl acetate and its derivative.
In one of the embodiments, the second surface activating agent be selected from sodium taurocholate, NaTDC, neocholan,
One or more in natrium dehydrocholicum, cupreol or cholesterol.
In one of the embodiments, including following component：
Present invention also offers a kind of preparation method of the aqueous liquid dispersion of above-mentioned carbon nanomaterial.
A kind of preparation method of the aqueous liquid dispersion of carbon nanomaterial, including by carbon nanomaterial, surfactant, reduction
Property sugar and deionized water mix.
Above-mentioned preparation method, the aqueous liquid dispersion of obtained carbon nanomaterial, its dispersion concentration is high and environmentally friendly.
In one of the embodiments, comprise the following steps：
The deionized water of carbon nanomaterial, the surfactant of a part and Part I is sanded or ball milling mixing, obtained
To the first mixed liquor；
First mixed liquor is mixed with the deionized water of Part II in static mixer, the second mixing is obtained
Liquid；
Second mixed liquor, remaining surfactant and remaining deionized water are mixed in static mixer,
Obtain the aqueous liquid dispersion of carbon nanomaterial.
In one of the embodiments, the deionized water of the Part I accounts for 70~80wt% of ion water inventory；
The deionized water of the Part II accounts for 5~15wt% of ion water inventory.
Brief description of the drawings
Fig. 1 is dispersion liquid A1 electron-microscope scanning figure.
Fig. 2 is dispersion liquid D1 electron-microscope scanning figure.
Fig. 3 is dispersion liquid B1 electron-microscope scanning figure.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with embodiment
The present invention is further elaborated.It should be appreciated that embodiment described herein is only to explain the present invention,
It is not intended to limit the present invention.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The implication that technical staff is generally understood that is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein " and/or " including one or more
The arbitrary and all combination of related Listed Items.
A kind of aqueous liquid dispersion of carbon nanomaterial, including carbon nanomaterial, surfactant, reducing sugar and go from
Sub- water.
Wherein, nano-carbon material refers generally in the dispersed phase yardstick at least one-dimensional carbon material less than 100nm.Preferably,
Carbon nanomaterial is selected from CNT or graphene.
It is highly preferred that a diameter of 5nm~40nm of CNT, wall thickness is 1 layer~10 layers, length is 1 μm~20 μm.Adopt
Above-mentioned CNT is used, with good electrology characteristic, it is to avoid electric property loss reduction, CNT is microcosmic to be twined while reducing
Knot is more conducive to scattered.
Wherein, reducing sugar refers to the carbohydrate with reproducibility.Reducing sugar be generally in molecule containing free aldehyde or
Disaccharides containing free aldehyde in the monose or molecule of ketone group.
Preferably, reducing sugar is selected from the one or more of glucose, fructose, galactolipin, lactose or maltose.
Wherein, the main function of surfactant is to promote carbon nanomaterial to disperse in deionized water.
Preferably, surfactant includes nonionic surface active agent and second surface activating agent.Second surface is lived
Property agent in sterol and its salt-forming compound, bile acid and its salt-forming compound or bilichol and its salt-forming compound one
Plant or several.Dispersion effect is further improved using nonionic surface active agent and second surface activating agent compounding.
It is highly preferred that second surface activating agent is selected from sodium taurocholate, NaTDC, neocholan, natrium dehydrocholicum, β-paddy
One or more in sterol or cholesterol.
It is, of course, understood that the second surface activating agent of the present invention is not limited to above-claimed cpd, it can also be
Other ionic surfactants.Such as ET-500, SORPOL 7948.
Wherein, nonionic surface active agent, refers to the surfactant for not producing ion in aqueous.
Preferably, nonionic surface active agent is selected from polyvinyl alcohol and its derivative or polyoxyethylene ester and its derivative
One or more in thing.It so can further improve dispersion effect.
It is, of course, understood that the nonionic surface active agent of the present invention is not limited to above-claimed cpd, may be used also
To be other nonionic surface active agent.Such as polyoxyethylene alkyl ether and its derivative, P.O.E glyceride, polyethylene glycol
Fatty acid ester, Crodaret, polyethylene glycol etc..
Preferably, the aqueous liquid dispersion of carbon nanomaterial includes following component：
It is highly preferred that the aqueous liquid dispersion of carbon nanomaterial includes following component：
The aqueous liquid dispersion of carbon nanomaterial provided by the present invention, due to the addition of reducing sugar, reducing sugar has
Free aldehyde or ketone group are so that its is water-soluble and be dispersed in system.Reducing sugar is intermolecular easily with hydrogen bond knot
Close, can be with the uniform and stable presence of whole dispersion.In addition, reducing sugar molecule is due to electron conjugated effect, shape tends to ball
Shape, volume is much smaller than carbon nanomaterial, and lubrication is served to whole system；The dispersion of high dispersive concentration can to sum up be formed
System, so as to be conducive to the application of carbon nanomaterial.The aqueous liquid dispersion of above-mentioned carbon nanomaterial, is aqueous liquid dispersion, does not use
Organic solvent system and super acid system, so as to avoid the not environmentally problem that organic solvent and super acid are brought, and are expanded
The application of carbon nanomaterial.
The aqueous liquid dispersion of carbon nanomaterial provided by the present invention, also with good film performance, in film former-free
Adhesive force is higher than other aqueous liquid dispersions in the case of addition, and the surface resistivity uniformity is obviously improved.
Present invention also offers a kind of preparation method of the aqueous liquid dispersion of above-mentioned carbon nanomaterial.
A kind of preparation method of the aqueous liquid dispersion of carbon nanomaterial, including by carbon nanomaterial, surfactant, reduction
Property sugar and deionized water mix.
Preferably, mixing comprises the following steps：By going for carbon nanomaterial, a part of surfactant and Part I
Ionized water is sanded or ball milling mixing, obtains the first mixed liquor；The deionized water of first mixed liquor and Part II is mixed in static state
Mixed in clutch, obtain the second mixed liquor；By the second mixed liquor, remaining surfactant and remaining deionized water in quiet
Mixed in state blender, obtain the aqueous liquid dispersion of carbon nanomaterial.
It is highly preferred that the deionized water of carbon nanomaterial, ionic surfactant and Part I is sanded or ball milling
Mixing, obtains the first mixed liquor；First mixed liquor is mixed with the deionized water of Part II in static mixer, is obtained
Two mixed liquors；Second mixed liquor, nonionic surfactant and remaining deionized water are mixed in static mixer, obtained
To the aqueous liquid dispersion of carbon nanomaterial.So make carbon in one layer of second surface activating agent of carbon nanomaterial Surface coating first
Nano material is changed into hydrophilic；Then by being dissolved in the nonionic surface active agent of water, give carbon nanomaterial aqueous point
The certain space steric effect of granular media system, reduces and suppresses the reunion of carbon nanomaterial, long-term steady so as to further reach
Surely the effect disperseed.
It is highly preferred that the deionized water of Part I accounts for 70~80wt% of ion water inventory；Part II go from
Sub- water accounts for 5~15wt% of ion water inventory.So further carbon nanomaterial is promoted to be uniformly dispersed.
Above-mentioned preparation method, the aqueous liquid dispersion of obtained carbon nanomaterial, its dispersion concentration is high and environmentally friendly.
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment 1-1
Carbon nanomaterial：4g carbon nanotube dusts (average diameter 10nm, 3~5 layers, 5~20 μm of length)；
Nonionic surfactant：1.2g PVA；
Second surface activating agent：0.5g NaTDCs；
Reducing sugar：1g galactolipins；
Deionized water：It is 100g (93.3g) added to gross weight；
1h is sanded in the deionized water of carbon nanotube dust, second surface activating agent and total amount 75% in sand mill,
Obtain the first mixed liquor.
In the first mixed liquor, the deionized water of reducing sugar and total amount 10% is added, and mixed in static mixer
After 10min, the second mixed liquor is obtained.
In the second mixed liquor, nonionic surfactant and remaining 15% deionized water are added, in static mixing
20min is mixed in device.The aqueous liquid dispersion of carbon nanomaterial is obtained, A1 is denoted as.
Embodiment 1-2
Carbon nanomaterial：4g carbon nanotube dusts (average diameter 10nm, 3~5 layers, 5~20 μm of length)；
Nonionic surfactant：1g PVA；
Second surface activating agent：0.2g NaTDCs；
Reducing sugar：1.5g galactolipin；
Deionized water：It is 100g added to gross weight；
1h is sanded in the deionized water of carbon nanotube dust, ionic surface active agent and total amount 75% in sand mill,
Obtain the first mixed liquor.
In the first mixed liquor, the deionized water of reducing sugar and total amount 10% is added, and mixed in static mixer
After 10min, the second mixed liquor is obtained.
In the second mixed liquor, nonionic surfactant and remaining 15% deionized water are added, in static mixing
20min is mixed in device.The aqueous liquid dispersion of carbon nanomaterial is obtained, A2 is denoted as.
Embodiment 1-3
Carbon nanomaterial：4g carbon nanotube dusts (average diameter 10nm, 3~5 layers, 5~20 μm of length)；
Nonionic surfactant：1g PVA；
Second surface activating agent：1.25g sodium taurocholates and 0.6g cupreols；
Reducing sugar：0.8g galactolipins；
Deionized water：It is 100g added to gross weight；
1h is sanded in the deionized water of carbon nanotube dust, ionic surface active agent and total amount 75% in sand mill,
Obtain the first mixed liquor.
In the first mixed liquor, the deionized water of reducing sugar and total amount 10% is added, and mixed in static mixer
After 10min, the second mixed liquor is obtained.
In the second mixed liquor, nonionic surfactant and remaining 15% deionized water are added, in static mixing
20min is mixed in device.The aqueous liquid dispersion of carbon nanomaterial is obtained, A3 is denoted as.
Embodiment 1-4
Carbon nanomaterial：4g carbon nanotube dusts (average diameter 10nm, 3~5 layers, 5~20 μm of length)；
Surfactant：1.5g PVP；
Reducing sugar：0.73g galactolipins；
Deionized water：It is 100g added to gross weight；
1h is sanded in the deionized water of carbon nanotube dust, surfactant and total amount 75% in sand mill, is obtained
First mixed liquor.
In the first mixed liquor, the deionized water of reducing sugar and total amount 10% is added, and mixed in static mixer
After 10min, the second mixed liquor is obtained.
In the second mixed liquor, remaining 15% deionized water is added, 20min is mixed in static mixer.Obtain
The aqueous liquid dispersion of carbon nanomaterial, is denoted as A4.
Embodiment 1-5
Carbon nanomaterial：4g carbon nanotube dusts (average diameter 10nm, 3~5 layers, 5~20 μm of length)；
Surfactant：1.28g natrium dehydrocholicum；
Reducing sugar：0.6g galactolipins；
Deionized water：It is 100g added to gross weight；
1h is sanded in the deionized water of carbon nanotube dust, surfactant and total amount 75% in sand mill, is obtained
First mixed liquor.
In the first mixed liquor, the deionized water of reducing sugar and total amount 10% is added, and mixed in static mixer
After 10min, the second mixed liquor is obtained.
In the second mixed liquor, remaining 15% deionized water is added, 20min is mixed in static mixer.Obtain
The aqueous liquid dispersion of carbon nanomaterial, is denoted as A5.
Comparative example 1-1
With embodiment 1-1 except that, without reducing sugar.
Other parts are identical with embodiment 1-1.
The aqueous liquid dispersion of carbon nanomaterial is obtained, D1 is denoted as.
Embodiment 2-1
Carbon nanomaterial：4g graphenes (3-5 layers of the number of plies)；
Nonionic surfactant：1.42g PVA；
Second surface activating agent：0.35g sodium taurocholates and 0.1g cupreols；
Reducing sugar：1.08g maltose
Deionized water：It is 100g added to gross weight；
1h is sanded in the deionized water of carbon nanotube dust, ionic surface active agent and total amount 75% in sand mill,
Obtain the first mixed liquor.
In the first mixed liquor, the deionized water of reducing sugar and total amount 10% is added, and mixed in static mixer
After 10min, the second mixed liquor is obtained.
In the second mixed liquor, nonionic surfactant and remaining 15% deionized water are added, in static mixing
20min is mixed in device.The aqueous liquid dispersion of carbon nanomaterial is obtained, B1 is denoted as.
Comparative example 2-1
With embodiment 2-1 except that, without reducing sugar.
Other parts are identical with embodiment 2-1.
The aqueous liquid dispersion of carbon nanomaterial is obtained, D2 is denoted as.
Embodiment 3-1
Carbon nanomaterial：4g carbon nanotube dusts (average diameter 10nm, 3~5 layers, 5~20 μm of length)；
Nonionic surfactant：1.2g PVA；
Second surface activating agent：0.5g NaTDCs；
Reducing sugar：0.5g galactolipins；
Deionized water：It is 100g added to gross weight；
1h is sanded in the deionized water of carbon nanotube dust, second surface activating agent and total amount 75% in sand mill,
Obtain the first mixed liquor.
In the first mixed liquor, the deionized water of reducing sugar and total amount 10% is added, and mixed in static mixer
After 10min, the second mixed liquor is obtained.
In the second mixed liquor, nonionic surfactant and remaining 15% deionized water are added, in static mixing
20min is mixed in device.The aqueous liquid dispersion of carbon nanomaterial is obtained, C1 is denoted as.
Embodiment 3-2
With embodiment 3-1 except that, reducing sugar be 1g galactolipins.
Other parts are identical with embodiment 3-1.
The aqueous liquid dispersion of carbon nanomaterial is obtained, C2 is denoted as.
Embodiment 3-2
With embodiment 3-1 except that, reducing sugar be 1.5g galactolipins.
Other parts are identical with embodiment 3-1.
The aqueous liquid dispersion of carbon nanomaterial is obtained, C3 is denoted as.
Embodiment 3-2
With embodiment 3-1 except that, reducing sugar be 2g galactolipins.
Other parts are identical with embodiment 3-1.
The aqueous liquid dispersion of carbon nanomaterial is obtained, C4 is denoted as.
Comparative example 3-1
With embodiment 3-1 except that, without reducing sugar.
Other parts are identical with embodiment 3-1.
The aqueous liquid dispersion of carbon nanomaterial is obtained, D3 is denoted as.
Performance test：
Electron-microscope scanning：
Aqueous liquid dispersion A1, D1 and B1 of carbon nanomaterial are subjected to electron-microscope scanning, obtain scanning figure see respectively Fig. 1,
Fig. 2 and Fig. 3.
With respect to Fig. 2, the agglomeration in Fig. 1 greatly reduces, and this explanation adds the aqueous of the carbon nanomaterial of reducing sugar
Dispersion liquid, it is more uniformly scattered.
Referring to Fig. 3, graphene does not observe agglomeration substantially in Fig. 3, and this explanation present invention can also disperse well
Graphene.
Film electric resistance standard deviation is tested：
The aqueous liquid dispersion C1-C4 and D3 of carbon nanomaterial are used into bar method film, size 8*15cm respectively2；Often apply
One layer, five resistance (using four detecting probe surface resistance instrument) thereon are surveyed after each film white drying, test result is shown in Table 1.
Table 1
As it can be seen from table 1 relative to dispersion liquid D3 film forming, no matter film layer number, the resistance standard of dispersion liquid C1-C4 film forming
Difference is smaller, and the distribution of resistance of this explanation dispersion liquid C1-C4 film forming is obtained evenly, is further related to：Relative to dispersion liquid D3, disperse
CNT is scattered evenly in liquid C1-C4.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned
The all possible combination of each technical characteristic in embodiment is all described, as long as however, the combination of these technical characteristics
In the absence of contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of aqueous liquid dispersion of carbon nanomaterial, it is characterised in that including carbon nanomaterial, surfactant, reproducibility
Sugar and deionized water.
2. the aqueous liquid dispersion of carbon nanomaterial according to claim 1, it is characterised in that the carbon nanomaterial is carbon
Nanotube or graphene.
3. the aqueous liquid dispersion of carbon nanomaterial according to claim 2, it is characterised in that the reducing sugar is selected from Portugal
Grape sugar, fructose, galactolipin, the one or more of lactose or maltose.
4. the aqueous liquid dispersion of the carbon nanomaterial according to claim any one of 1-3, it is characterised in that live on the surface
Property agent include nonionic surface active agent and second surface activating agent；The second surface activating agent be selected from sterol and its into
One or more in salt compound, bile acid and its salt-forming compound or bilichol and its salt-forming compound.
5. the aqueous liquid dispersion of carbon nanomaterial according to claim 4, it is characterised in that the non-ionic surface is lived
One or more of the property agent in polyvinyl alcohol and its derivative or polyoxyethylene ester and its derivative.
6. the aqueous liquid dispersion of carbon nanomaterial according to claim 4, it is characterised in that the second surface activating agent
One or more in sodium taurocholate, NaTDC, neocholan, natrium dehydrocholicum, cupreol or cholesterol.
7. the aqueous liquid dispersion of carbon nanomaterial according to claim 1, it is characterised in that including following component：
8. a kind of preparation method of the aqueous liquid dispersion of carbon nanomaterial, it is characterised in that including carbon nanomaterial, surface are lived
Property agent, reducing sugar and deionized water mix.
9. the preparation method of the aqueous liquid dispersion of carbon nanomaterial according to claim 8, it is characterised in that including as follows
Step：
The deionized water of carbon nanomaterial, the surfactant of a part and Part I is sanded or ball milling mixing, the is obtained
One mixed liquor；
First mixed liquor is mixed with the deionized water of Part II in static mixer, the second mixed liquor is obtained；
Second mixed liquor, remaining surfactant and remaining deionized water are mixed in static mixer, obtained
The aqueous liquid dispersion of carbon nanomaterial.
10. the preparation method of the aqueous liquid dispersion of carbon nanomaterial according to claim 9, it is characterised in that described
The deionized water of a part accounts for 70~80wt% of ion water inventory；It is total that the deionized water of the Part II accounts for ionized water
5~15wt% of amount.
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| CN108975314A (en) * | 2018-09-17 | 2018-12-11 | 苏州纳磐新材料科技有限公司 | Dispersion, preparation method and its system containing carbon nanomaterial |
| CN109199399A (en) * | 2018-09-05 | 2019-01-15 | 苏州纳磐新材料科技有限公司 | Fingerprint manifestation agent and preparation method thereof |
| CN110963483A (en) * | 2019-12-31 | 2020-04-07 | 新材料与产业技术北京研究院 | Aqueous carbon nanotube dispersion and preparation method thereof |
| CN115521663A (en) * | 2022-09-29 | 2022-12-27 | 安徽宇航派蒙健康科技股份有限公司 | Conductive ink, conductive film and preparation method |
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