CN109455696A - A kind of aqueous carbon nano tube paste and preparation method thereof - Google Patents
A kind of aqueous carbon nano tube paste and preparation method thereof Download PDFInfo
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- CN109455696A CN109455696A CN201811235809.7A CN201811235809A CN109455696A CN 109455696 A CN109455696 A CN 109455696A CN 201811235809 A CN201811235809 A CN 201811235809A CN 109455696 A CN109455696 A CN 109455696A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
- B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
- B01F31/83—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations comprising a supplementary stirring element
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/83—Mixing plants specially adapted for mixing in combination with disintegrating operations
- B01F33/831—Devices with consecutive working receptacles, e.g. with two intermeshing tools in one of the receptacles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8361—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating
- B01F33/83613—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating by grinding or milling
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Abstract
The invention discloses a kind of aqueous carbon nano tube pastes and preparation method thereof, include the following steps: the 10-20% for a) reserving deionized water gross mass, remaining deionized water and dispersant A, dispersant B, wetting agent, moisturizer are mixed into dispersion in dispersion machine, obtain premix；B) carbon nanotube is added in the premix that step a) is obtained and is dispersed, using dispersion machine to be higher than 200 revs/min of Rate Dispersion not less than 30 minutes, and the deionized water reserved in step a) is added in dispersion process, obtain pre-dispersed carbon nano tube paste；C) the pre-dispersed carbon nano tube paste for obtaining step b) carries out grinding distribution 3-10 times in grinder, then carries out obtaining aqueous carbon nano tube paste in ultrasonic wave decentralized processing 0.5-2 hours.
Description
Technical field
The present invention relates to a kind of aqueous carbon nano tube pastes, belong to field of fine chemical.
Background technique
Carbon nanotube because its with unique nanostructure and due to excellent machinery, electricity, magnetics and optical property by
Extensive concern.However carbon nano tube surface defect is few, lacks active group, the dispersibility in water and in solvent is lower；Separately
Mainly with SP between carbon atom in outer carbon nanotube2Hybrid form forms the delocalized big pi bond of height, cause carbon nanotube it
Between there are stronger Van der Waals forces, while the specific surface area of carbon nanotube and major diameter are bigger, seriously affect point in a solvent
It dissipates, dispersibility especially in water is bad.Under normal circumstances, it is mutually intertwined between carbon nanotube with agglomerate morphology
In the presence of, affect carbon nanotube physical property itself, largely limit its battery conductive agent, paint field (it is conductive/
Antistatic, heat dissipation, anti-corrosion), the application in the fields such as rubber and latex, cement, polymer coating and weaving.
In the fields such as conductive coating, electrically conductive ink of the carbon nanotube as function additive, uniformly and stably by carbon nanotube
Dispersion is in a solvent the critical problem of urgent need to resolve especially in water.A variety of disperse aqueous carbon nanotubes are disclosed in recent years
Method, have the physical methods such as ultrasonic wave, mechanical stirring, ball milling, as United States Patent (USP) US2006039848 discloses a kind of use
At least method that ultrasonic wave decentralized processing prepares single-walled carbon nanotube dispersion under the high frequency of 20KHZ；But ultrasonic wave distributing
It sets small scale and is only suitable for laboratory preparation, be not suitable for large-scale industrial production and use.Common ultrasonic wave needs to use media filler,
To the small volume of ultrasonic disperse substance, set as United States Patent (USP) US6438998 discloses a kind of ultrasonic disperse for Silica hydrogel
Standby, Silica hydrogel carries out ultrasonic disperse processing by the pipeline of bending.Existing ultrasonic disperse device is suitble to point of low viscosity material
Mixing is dissipated, the high feed liquid content low-flow of viscosity is bad, is unfavorable for the transmitting of ultrasonic wave, and it is super to improve promotion by equipment
The important channel of sound dispersion effect, Chinese patent CN201610763172.3 disclose a kind of highly viscous slurry ultrasonic wave strength point
It is casually arranged with standby, including ultrasonic wave distributing device, autoclave, homogenizer and low pressure kettle.
Another method of disperse aqueous carbon nano tube paste is surface modification method, and the method for surface modification is divided into covalently
Key modification and non-covalent bond modification, wherein the mode of non-covalent bond modification is due to that will not cause brokenly the structure of carbon nanotube itself
Badly become main method.Studies have shown that can preferably make carbon nanotube uniform using physical dispersion and surface modification simultaneously
Dispersion.Chinese patent CN201310350352.5 discloses a kind of using naphthalene sulfonic acids-styrenesulfonic-maleic acid anhydride polymer
Lithium salts or sodium salt make dispersing agent, and defoaming agent and suspension thickener is added, and are prepared aqueous carbon using stirring or sanding method and are received
The method of mitron slurry；Chinese patent CN201410114650.9 discloses a kind of carbon nanotube conducting slurry of ground preparation
Method, use common dispersing agent: polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, sodium carboxymethylcellulose, 12
At least one of sodium alkyl sulfonate, neopelex.
There are still certain defects for the aqueous carbon nano tube paste of prior art preparation, in a short time such as carbon nano tube paste
The problems such as will appear sedimentation, aggregation, the performances such as Stability of Slurry are difficult to reach customer requirement.
Summary of the invention
To overcome above-mentioned technological deficiency, the present invention provides a kind of aqueous carbon nano tube paste and preparation method thereof, the party
Method carries out non-covalent modification to carbon nanotube by using two kinds of dispersing agents, and the carbon in phenyl ring and carbon nanotube in dispersing agent is former
There is very strong attraction, so that dispersing agent and carbon nanotube be made to combine between son；Sulfonate in dispersing agent has very
Good water solubility, keeps dispersing agent and the combination of carbon nanotube fully dispersed in water.In addition dispersant A is polymethylene
Hexichol bis ether sulfonate has excellent surface-active, while having good dispersibility and wetability again.Gather in dispersant B
Ethylene oxide ether segment is dispersed in water for carbon nanotube and plays good transition, and phenyl ring and sulfonate is made to play a role alone.
The ultrasonic wave distributing device that dispersing Nano carbon tubes slurry uses is arranged in multilayer, and every layer by multiple supersonic generators in an orderly manner
By multiple supersonic generator equidistant arrangements, the scale ultrasonic wave dispersion of carbon nano tube paste is realized, it can ultrasonic disperse height
The carbon nano tube paste of viscosity.Aqueous carbon nanometer of this method using two kinds of dispersing agents by grinding and ultrasonic disperse processing preparation
Pipe slurry has good storage stability.
The technical scheme is that
A kind of aqueous carbon nano tube paste, including following each components:
The carbon nanotube of carbon nano tube paste gross mass percentage 2-10% is accounted for,
The dispersant A of carbon nanotube mass percentage 20-80% is accounted for,
The dispersant B of carbon nanotube mass percentage 5-50% is accounted for,
The wetting agent of carbon nanotube mass percentage 0.1-5.0% is accounted for,
The moisturizer of carbon nano tube paste gross mass percentage 2-20% is accounted for,
The defoaming agent of carbon nano tube paste gross mass percentage 0.1-0.5% is accounted for,
Surplus is deionized water；
The general structure of the dispersant A are as follows:
R1It is linear or branched alkyl group containing carbon number between 1~20, a be integer, M between 1~10 is H, K, Na, NH4
One or more of；
The dispersant B is alkyl phenol polyoxyethylene ether sulfonate or plant polyphenol polyethenoxy ether sulphonate, wherein alkane
The general structure of base phenol polyethenoxy ether sulfonate are as follows:
R2It is linear or branched alkyl group containing carbon number between 1~10, b be integer, M between 1~30 is H, K, Na, NH4
One or more of.
Further, the carbon nanotube is the mixing of one or both of single-walled carbon nanotube, multi-walled carbon nanotube.
Further, the wetting agent is at least one of phosphatidyl choline, Dodecyl Glucoside.
Further, the moisturizer is at least one of ethylene glycol, propylene glycol, glycerine and diglycol.
Further, the defoaming agent is at least one of polysiloxanes ether copolymer, polyether compound.
A kind of preparation method of aqueous carbon nano tube paste, which is characterized in that include the following steps:
A) 10-20% for reserving deionized water gross mass, by remaining deionized water and dispersant A, dispersant B, wetting agent,
Moisturizer mixes dispersion in dispersion machine, obtains premix；
B) will disperse in the obtained premix of carbon nanotube addition step a), using dispersion machine be higher than 200 turns/
The Rate Dispersion of minute is not less than 30 minutes, and the deionized water reserved in step a) is added in dispersion process, obtains pre- point
Dissipate carbon nano tube paste；
C) the pre-dispersed carbon nano tube paste for obtaining step b) carries out grinding distribution 3-10 times in grinder, then into
Row ultrasonic wave decentralized processing obtains aqueous carbon nano tube paste in 0.5-2 hours.
Further, defoaming agent is added in step c) process of lapping.
A kind of ultrasound wave distributing device, multiple supersonic generator layers including ordered arrangement.
Further, supersonic generator layer is formed by multiple supersonic generator equidistant arrangements.
Compared with prior art, the method have the benefit that: the present invention provides a kind of aqueous carbon nanotubes to starch
Material and preparation method thereof, this method carry out non-covalent modification to carbon nanotube by using two kinds of dispersing agents, the benzene in dispersing agent
There is very strong attraction, so that dispersing agent and carbon nanotube be made to combine between carbon atom in ring and carbon nanotube；Point
Sulfonate in powder has water solubility well, keeps dispersing agent and the combination of carbon nanotube fully dispersed in water.
The ultrasonic wave distributing device that dispersing Nano carbon tubes slurry uses is arranged in multilayer, and every layer by multiple supersonic generators in an orderly manner
By multiple supersonic generator equidistant arrangements, realize the scale ultrasonic disperse of carbon nano tube paste, can ultrasonic disperse height it is viscous
The carbon nano tube paste of degree.Have by the aqueous carbon nano tube paste that mixing dispersion, grinding, ultrasonic wave decentralized processing obtain good
Good storage stability, preparation method is high-efficient to realize scale automation serialization and integration production.
Detailed description of the invention
Fig. 1 is the schematic diagram of disperse aqueous carbon nano tube paste equipment of the present invention.
Fig. 2 is ultrasonic wave distributing device cross sectional shape schematic diagram.
1 dispersion machine, 2 first delivery pumps, 3 grinders, 4 second delivery pumps, 5 ultrasonic wave distributing devices, 5-1 ultrasonic wave occur
Device, 6 third delivery pumps, 7 liquid storage cylinders.
Specific embodiment
Present invention is further described in detail with reference to the accompanying drawings and examples:
Embodiment and comparative example use the preparation method comprises the following steps:
A) 10-20% for reserving deionized water gross mass, by remaining deionized water and dispersant A, dispersant B, wetting agent,
Moisturizer mixes dispersion in dispersion machine 1, obtains premix；
B) carbon nanotube is added in the premix that step a) is obtained and is dispersed, using dispersion machine 1 to be higher than 200
Rev/min Rate Dispersion be not less than 30 minutes, and in dispersion process be added step a) in reserve deionized water, obtain pre-
Dispersing Nano carbon tubes slurry；
C) the pre-dispersed carbon nano tube paste that the first delivery pump 2 obtains step b) carries out grinding distribution in grinder 3
3-10 times, the second delivery pump 4 be passed to ultrasonic wave distributing device 5 obtain within ultrasonic wave decentralized processing 0.5-2 hours it is aqueous
Carbon nano tube paste, third delivery pump 6 send aqueous carbon nano tube paste to liquid storage cylinder 7.
In order to reduce the bubble generated in process of lapping, defoaming agent is added in step c) process of lapping.
In order to improve ultrasonic wave dispersion effect, multiple ultrasonic waves of setting ordered arrangement occur in ultrasonic wave distributing device 5
Device layer, supersonic generator layer are formed by multiple supersonic generator 5-1 equidistant arrangements.
The dispersant A and B used in embodiment and comparative example specifically:
The general structure of dispersant A are as follows:
In dispersant A 1, R1For C10H21-, a 6, M Na；
In dispersant A 2, R1For CH3-, a 10, M K；
In dispersant A 3, R1For C20H41-, a 1, M NH4。
Dispersant B is alkyl phenol polyoxyethylene ether sulfonate or plant polyphenol polyethenoxy ether sulphonate, wherein alkyl phenol
The general formula of polyethenoxy ether sulphonate are as follows:
In dispersant B 1, R2For C5H11-, b 15, M Na；
In dispersant B 2, R2For C10H21-, b 30, M H；
Dispersant B 3 is catechol polyethenoxy ether sulphonate.
It is specific:
Embodiment 1
10 parts of deionized waters are reserved, by 68.82 parts of deionized waters, 3 parts of 1,1.8 part of dispersant A, 1,0.18 part of dispersant B phosphorus
Phosphatidylcholine, 10 parts of ethylene glycol disperse in dispersion machine, obtain premix；Premix is added in 6 parts of multi-walled carbon nanotubes
In dispersed, using dispersion machine Rate Dispersion 40 minutes of 600 revs/min, and be added in dispersion process 10 parts it is reserved
Deionized water, obtain pre-dispersed carbon nano tube paste；Pre-dispersed carbon nano tube paste is carried out in grinder grinding point
It dissipates 8 times, adds 0.2 part of polysiloxanes ether copolymer during the grinding process, then the processing of progress ultrasonic disperse obtains aqueous for 1 hour
Carbon nano tube paste.
Embodiment 2
15 parts of deionized waters are reserved, by 78.2 parts of deionized waters, 1.6 parts of 2,1 parts of dispersant A, 2,0.1 part 12 of dispersant Bs
Alkyl glycosides, 2 parts of glycerine disperse in dispersion machine, obtain premix；2 parts of single-walled carbon nanotubes are added in premix
Dispersed, using dispersion machine Rate Dispersion 50 minutes of 500 revs/min, and be added in dispersion process 15 parts it is reserved
Deionized water obtains pre-dispersed carbon nano tube paste；Pre-dispersed carbon nano tube paste is carried out grinding distribution 3 in grinder
Time, 0.1 part of polyether compound is added during the grinding process, is then carried out ultrasonic disperse processing and is obtained aqueous carbon nanotube in 2 hours
Slurry.
Embodiment 3
10 parts of deionized waters are reserved, by 53.49 parts of deionized waters, 2 parts of 3,4 parts of dispersant A, 3,0.005 parts of dispersant B phosphorus
Phosphatidylcholine and 0.005 part of Dodecyl Glucoside, 20 parts of diglycols disperse in dispersion machine, obtain premix；By 6
Part multi-walled carbon nanotube and 4 parts of single-walled carbon nanotubes are added in premixs and are dispersed, using dispersion machine at 200 revs/min
Rate Dispersion 60 minutes, and in dispersion process be added 10 parts of reserved deionized waters, obtain pre-dispersed carbon nano tube paste；
Pre-dispersed carbon nano tube paste is carried out grinding distribution 10 times in grinder, adds 0.2 part of poly- silicon oxygen during the grinding process
Then alkane ether copolymer and 0.3 part of polyether compound carry out ultrasonic disperse processing and obtain aqueous carbon nano tube paste in 0.5 hour.
Embodiment 4
10 parts of deionized waters are reserved, by 66.25 parts of deionized waters, 3 parts of dispersant As, 1,0.15 part of dispersant B 2 and 0.1 part
3,0.2 parts of phosphatidyl cholines of dispersant B, 10 parts of ethylene glycol and 5 parts of propylene glycol are dispersed in dispersion machine, obtain premix；By 5
Part multi-walled carbon nanotube, which is added in premix, to be dispersed, using dispersion machine Rate Dispersion 30 minutes of 400 revs/min,
And 10 parts of reserved deionized waters are added in dispersion process, obtain pre-dispersed carbon nano tube paste；Pre-dispersed carbon nanometer
Pipe slurry carries out grinding distribution 6 times in grinder, adds 0.3 part of polyether compound during the grinding process, then carries out ultrasound
Obtain aqueous carbon nano tube paste within decentralized processing 1.5 hours.
Comparative example 1
10 parts of deionized waters are reserved, by 70.62 parts of deionized waters, 3 parts of dispersant As, 1,0.18 part of phosphatidyl choline, 10 parts
Ethylene glycol disperses in dispersion machine, obtains premix；6 parts of multi-walled carbon nanotubes are added in premix and are dispersed, are made
With dispersion machine Rate Dispersion 40 minutes of 600 revs/min, and 10 parts of reserved deionized waters are added in dispersion process, obtain
To pre-dispersed carbon nano tube paste；Pre-dispersed carbon nano tube paste is carried out grinding distribution 8 times in grinder, ground
0.2 part of polysiloxanes ether copolymer is added in journey, is then carried out ultrasonic disperse processing and is obtained aqueous carbon nano tube paste in 1 hour.
Comparative example 2
10 parts of deionized waters are reserved, by 71.82 parts of deionized waters, 1.8 parts of dispersant Bs 1,0.18 part of phosphatidyl choline, 10
Part ethylene glycol disperses in dispersion machine, obtains premix；6 parts of multi-walled carbon nanotubes are added in premix and are dispersed,
Using dispersion machine Rate Dispersion 40 minutes of 600 revs/min, and 10 parts of reserved deionized waters are added in dispersion process,
Obtain pre-dispersed carbon nano tube paste；Pre-dispersed carbon nano tube paste is carried out grinding distribution 8 times in grinder, is being ground
0.2 part of polysiloxanes ether copolymer is added in the process, is then carried out ultrasonic disperse processing and is obtained within 1 hour aqueous carbon nanotube slurry
Material.
Comparative example 3
Reserve 10 parts of deionized waters, by 68.82 parts of deionized waters, 3 parts of dispersant As, 1,1.8 part of neopelex,
0.18 part of phosphatidyl choline, 10 parts of ethylene glycol disperse in dispersion machine, obtain premix；6 parts of multi-walled carbon nanotubes are added
Dispersed in premix, using dispersion machine Rate Dispersion 40 minutes of 600 revs/min, and is added in dispersion process
10 parts of reserved deionized waters, obtain pre-dispersed carbon nano tube paste；Pre-dispersed carbon nano tube paste in grinder into
Row grinding distribution 8 times, 0.2 part of polysiloxanes ether copolymer is added during the grinding process, is then carried out ultrasonic disperse and is handled 1 hour
Obtain aqueous carbon nano tube paste.
Comparative example 4
Reserve 10 parts of deionized waters, by 70.5 parts of deionized waters, 3 parts of neopelexes, 1.8 parts of dispersant Bs 1,
0.18 part of phosphatidyl choline, 10 parts of ethylene glycol disperse in dispersion machine, obtain premix；6 parts of multi-walled carbon nanotubes are added
Dispersed in premix, using dispersion machine Rate Dispersion 40 minutes of 600 revs/min, and is added in dispersion process
10 parts of reserved deionized waters, obtain pre-dispersed carbon nano tube paste；Pre-dispersed carbon nano tube paste in grinder into
Row grinding distribution 8 times, 0.2 part of polysiloxanes ether copolymer is added during the grinding process, is then carried out ultrasonic disperse and is handled 1 hour
Obtain aqueous carbon nano tube paste.
Comparative example 5
10 parts of deionized waters are reserved, by 70.5 parts of deionized waters, 3 parts of naphthalene sulfonic acids-styrenesulfonic-maleic acid anhydride polymer
Sodium salt, 0.18 part of phosphatidyl choline, 10 parts of ethylene glycol disperse in dispersion machine, obtain premix；By 6 parts of multi-wall carbon nano-tubes
Pipe, which is added in premix, to be dispersed, using dispersion machine Rate Dispersion 40 minutes of 600 revs/min, and in dispersion process
10 parts of reserved deionized waters of middle addition, obtain pre-dispersed carbon nano tube paste；Pre-dispersed carbon nano tube paste is being ground
It is carried out in machine grinding distribution 8 times, adds 0.2 part of polysiloxanes ether copolymer during the grinding process, then carried out at ultrasonic disperse
Reason obtains aqueous carbon nano tube paste in 1 hour.
Comparative example 6
10 parts of deionized waters are reserved, by 68.82 parts of deionized waters, 3 parts of neopelexes, 1.8 parts of polyethylene pyrroles
It coughs up ketone, 0.18 part of phosphatidyl choline, 10 parts of ethylene glycol to disperse in dispersion machine, obtains premix；By 6 parts of multi-walled carbon nanotubes
It is added in premix and is dispersed, using dispersion machine Rate Dispersion 40 minutes of 600 revs/min, and in dispersion process
10 parts of reserved deionized waters are added, obtain pre-dispersed carbon nano tube paste；Pre-dispersed carbon nano tube paste in grinder
0.2 part of polysiloxanes ether copolymer is added in middle progress grinding distribution 8 times during the grinding process, then carries out ultrasonic disperse processing 1
Hour obtains aqueous carbon nano tube paste.
The stability test of aqueous carbon nano tube paste
It usesThe aqueous carbon nanotube of analysis of stability analyzer testing example 1-4 and comparative example 1-6 preparation
The clarification index (instability index) of slurry, test condition are 25 DEG C, and 2000 revs/min of speed is centrifuged 250 points
Clock, clarification index is smaller, shows that stability is better.Table 1 is test result, and it is smaller that embodiment 1-4 clarifies index after centrifugation, table
The good stability of bright dispersion stabilization is almost unchanged；It is higher that comparative example 1-6 clarifies index after centrifugation, show centrifugal stability compared with
Difference.
The clarification index of the aqueous carbon nano tube paste of table 1.
As can be seen from Table 1, at the same joined dispersant A and the aqueous carbon nano tube paste of B clarification index it is obviously good
In a kind of clarification index for the aqueous carbon nano tube paste that dispersant A or B and other dispersing agents is added, show water of the invention
The stability of property carbon nano tube paste is preferable.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.It is all not
The simple deformation or modification made in the case where being detached from core of the present invention each fall within protection scope of the present invention.
Claims (9)
1. a kind of aqueous carbon nano tube paste, which is characterized in that including following each components:
The carbon nanotube of carbon nano tube paste gross mass percentage 2-10% is accounted for,
The dispersant A of carbon nanotube mass percentage 20-80% is accounted for,
The dispersant B of carbon nanotube mass percentage 5-50% is accounted for,
The wetting agent of carbon nanotube mass percentage 0.1-5.0% is accounted for,
The moisturizer of carbon nano tube paste gross mass percentage 2-20% is accounted for,
The defoaming agent of carbon nano tube paste gross mass percentage 0.1-0.5% is accounted for,
Surplus is deionized water；
The general structure of the dispersant A are as follows:
R1It is linear or branched alkyl group containing carbon number between 1~20, a be integer, M between 1~10 is H, K, Na, NH4In
It is one or more of；
The dispersant B is alkyl phenol polyoxyethylene ether sulfonate or plant polyphenol polyethenoxy ether sulphonate, wherein alkyl phenol
The general structure of polyethenoxy ether sulphonate are as follows:
R2It is linear or branched alkyl group containing carbon number between 1~10, b be integer, M between 1~30 is H, K, Na, NH4In
It is one or more of.
2. a kind of aqueous carbon nano tube paste according to claim 1, which is characterized in that the carbon nanotube is single wall carbon
The mixing of one or both of nanotube, multi-walled carbon nanotube.
3. a kind of aqueous carbon nano tube paste according to claim 1, which is characterized in that the wetting agent is phosphatidyl gallbladder
At least one of alkali, Dodecyl Glucoside.
4. a kind of aqueous carbon nano tube paste according to claim 1, which is characterized in that the moisturizer be ethylene glycol,
At least one of propylene glycol, glycerine and diglycol.
5. a kind of aqueous carbon nano tube paste according to claim 1, which is characterized in that the defoaming agent is polysiloxanes
At least one of ether copolymer, polyether compound.
6. a kind of preparation method of aqueous carbon nano tube paste according to claim 1-5, which is characterized in that packet
Include following step:
A) 10-20% for reserving deionized water gross mass, by remaining deionized water and dispersant A, dispersant B, wetting agent, moisturizing
Agent mixes dispersion in dispersion machine, obtains premix；
B) carbon nanotube is added in the premix that step a) is obtained and is dispersed, using dispersion machine to be higher than 200 revs/min
Rate Dispersion be not less than 30 minutes, and in dispersion process be added step a) in reserve deionized water, obtain pre-dispersed carbon
Nanotube slurry；
C) the pre-dispersed carbon nano tube paste for obtaining step b) carries out grinding distribution 3-10 times in grinder, is then surpassed
Obtain aqueous carbon nano tube paste within sound wave decentralized processing 0.5-2 hours.
7. a kind of preparation method of aqueous carbon nano tube paste according to claim 6, which is characterized in that ground in step c)
Defoaming agent is added during mill.
8. a kind of ultrasonic wave distributing device used such as claim 6, which is characterized in that multiple ultrasonic waves including ordered arrangement
Generator layer.
9. a kind of ultrasonic wave distributing device according to claim 8, which is characterized in that supersonic generator layer is by multiple super
Sonic generator equidistant arrangement forms.
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| CN110247051A (en) * | 2019-05-29 | 2019-09-17 | 常熟理工学院 | A kind of carbon nanotube mill base and preparation method thereof and the application in lithium battery |
| CN110669342A (en) * | 2019-10-14 | 2020-01-10 | 江西铜业技术研究院有限公司 | Carbon nanotube pre-dispersion for modified silicone rubber and preparation method thereof |
| CN113421695A (en) * | 2021-06-17 | 2021-09-21 | 苏州汉纳材料科技有限公司 | Aqueous carbon nanotube dispersion liquid, conductive slurry and preparation method thereof |
| CN113784468A (en) * | 2021-09-10 | 2021-12-10 | 四川普利司德高分子新材料有限公司 | Heating material and application thereof, conductive heating film and manufacturing method thereof |
| CN114307791A (en) * | 2021-12-31 | 2022-04-12 | 无锡东恒新能源科技有限公司 | Dispersing system of carbon nano tube |
| CN114773897A (en) * | 2022-03-29 | 2022-07-22 | 江苏索普聚酯科技有限公司 | Large-scale preparation method of graded porous carbon water-based slurry with ultrahigh conductivity and high dispersibility |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080260616A1 (en) * | 2004-07-29 | 2008-10-23 | William Marsh Rice University | Bulk Separation of Carbon Nanotubes by Bandgap |
| CN202122928U (en) * | 2011-05-17 | 2012-01-25 | 冯晶 | Ultrasonic dispersion machine |
| US20130187084A1 (en) * | 2006-04-14 | 2013-07-25 | Samsung Electronics Co., Ltd. | Dispersed solution of carbon nanotubes and method of preparing the same |
| CN103400991A (en) * | 2013-08-13 | 2013-11-20 | 天奈(镇江)材料科技有限公司 | Water-based carbon nanotube slurry and preparation method thereof |
| CN105271175A (en) * | 2015-11-16 | 2016-01-27 | 中南大学 | Dispersion method of carbon nano tube |
| CN108102041A (en) * | 2017-12-21 | 2018-06-01 | 上海三瑞高分子材料股份有限公司 | A kind of Carbon nano-tube dispersant and preparation method thereof |
-
2018
- 2018-10-24 CN CN201811235809.7A patent/CN109455696B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080260616A1 (en) * | 2004-07-29 | 2008-10-23 | William Marsh Rice University | Bulk Separation of Carbon Nanotubes by Bandgap |
| US20130187084A1 (en) * | 2006-04-14 | 2013-07-25 | Samsung Electronics Co., Ltd. | Dispersed solution of carbon nanotubes and method of preparing the same |
| CN202122928U (en) * | 2011-05-17 | 2012-01-25 | 冯晶 | Ultrasonic dispersion machine |
| CN103400991A (en) * | 2013-08-13 | 2013-11-20 | 天奈(镇江)材料科技有限公司 | Water-based carbon nanotube slurry and preparation method thereof |
| CN105271175A (en) * | 2015-11-16 | 2016-01-27 | 中南大学 | Dispersion method of carbon nano tube |
| CN108102041A (en) * | 2017-12-21 | 2018-06-01 | 上海三瑞高分子材料股份有限公司 | A kind of Carbon nano-tube dispersant and preparation method thereof |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110247051A (en) * | 2019-05-29 | 2019-09-17 | 常熟理工学院 | A kind of carbon nanotube mill base and preparation method thereof and the application in lithium battery |
| CN110669342A (en) * | 2019-10-14 | 2020-01-10 | 江西铜业技术研究院有限公司 | Carbon nanotube pre-dispersion for modified silicone rubber and preparation method thereof |
| CN110669342B (en) * | 2019-10-14 | 2021-10-22 | 江西铜业技术研究院有限公司 | Carbon nanotube pre-dispersion for modified silicone rubber and preparation method thereof |
| CN113421695A (en) * | 2021-06-17 | 2021-09-21 | 苏州汉纳材料科技有限公司 | Aqueous carbon nanotube dispersion liquid, conductive slurry and preparation method thereof |
| CN113421695B (en) * | 2021-06-17 | 2022-05-17 | 苏州汉纳材料科技有限公司 | Aqueous carbon nanotube dispersion liquid, conductive slurry and preparation method thereof |
| CN113784468A (en) * | 2021-09-10 | 2021-12-10 | 四川普利司德高分子新材料有限公司 | Heating material and application thereof, conductive heating film and manufacturing method thereof |
| CN113784468B (en) * | 2021-09-10 | 2024-03-12 | 四川普利司德高分子新材料有限公司 | Heating material and application thereof, conductive heating film and manufacturing method thereof |
| CN114307791A (en) * | 2021-12-31 | 2022-04-12 | 无锡东恒新能源科技有限公司 | Dispersing system of carbon nano tube |
| CN114307791B (en) * | 2021-12-31 | 2023-02-24 | 无锡东恒新能源科技有限公司 | Dispersing system of carbon nano tube |
| CN114773897A (en) * | 2022-03-29 | 2022-07-22 | 江苏索普聚酯科技有限公司 | Large-scale preparation method of graded porous carbon water-based slurry with ultrahigh conductivity and high dispersibility |
| CN114773897B (en) * | 2022-03-29 | 2023-06-30 | 江苏索普聚酯科技有限公司 | Large-scale preparation method of hierarchical porous carbon aqueous slurry with ultrahigh conductivity and high dispersibility |
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