CN108545718A - A kind of dispersing method of carbon nanotube - Google Patents
A kind of dispersing method of carbon nanotube Download PDFInfo
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- CN108545718A CN108545718A CN201810335724.XA CN201810335724A CN108545718A CN 108545718 A CN108545718 A CN 108545718A CN 201810335724 A CN201810335724 A CN 201810335724A CN 108545718 A CN108545718 A CN 108545718A
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- 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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Abstract
The invention discloses a kind of dispersing methods of carbon nanotube, are related to the field of dispersions of superfine powder.The process of the dispersing method is：Firstly the need of the gas removal that carbon nano tube surface is adsorbed, liquid is facilitated to moisten；Then pass through the grinding of the mill ball of specific bulky grain, collision, the place cut-out that carbon nanotube is interconnected, it uses smaller grinding bead instead again and carries out dispersion flow with smaller grinding rate, you can obtain the carbon nano tube dispersion liquid of the preferable higher concentration of electric conductivity.Improve the structure and specific surface of carbon nanotube using the method for the present invention, reduces agglomeration so that high conductivity, high intensity and its unique texture of carbon nanotube are widely used in various conductive materials and composite material.
Description
Technical field
The present invention relates to a kind of field of dispersions of superfine powder, and in particular to a kind of dispersion side of carbon nanotube in a liquid
Method.
Background technology
Carbon nanotube is nanoscale hollow tube made of being crimped by graphene layer, is the 1-dimention nano material with high length-diameter ratio
Material.Carbon nanotube is also because its high conductivity, high intensity and its unique texture are widely used various conductive materials and composite wood
Expect carbon nanotube, but due to the structure of carbon nanotube and prodigious specific surface, the agglomeration strong influence property of carbon pipe
The application of carbon pipe can be limited.Carbon pipe is easy to reunite the reason is that, the axial geometry of carbon nanotube high length-diameter ratio first is
The reunion of carbon pipe provides the contact of large area so that carbon pipe is easy to reunion tied up in knots；Secondly carbon nanotube is insoluble in exhausted
Most of solvent；The high polarization of the p electronics of last carbon pipe graphene layer causes powerful Van der Waals between carbon nanotube to be inhaled
Gravitation can be up to 500eV so that hydrophobic carbon pipe in water can be in system for contacting Van der Waals combination between every micron of carbon pipe
Entropy acutely increase, single-walled carbon nanotube is even more serious compared to multi-walled carbon nanotube agglomeration, one side single
Pipe tends to be gathered into the carbon nano-tube bundle being made of 50-200 carbon nanotube；Another aspect single-walled carbon nanotube caliber smaller
It is more easily wrapped around one another, therefore be more difficult to disperse.Because the application to carbon nanotube is to carry out it in a liquid first
Good dispersion, so it is very urgent to find suitable dispersing method.
Method has ball milling in a liquid for the dispersion of carbon nanotube at present, ultrasound, the methods of surface treatment.Such as《Ball milling disperses
The influence that technique disperses carbon nanotube》, material Leader, P35-38 (in November, 2013 album 22 of volume 27), but due to ball
The energy density of mill is low, and mill ball is huge（Centimeter Level）, ground in a manner of impact merely, be easily destroyed the knot of carbon nanotube
Structure, dispersion effect are bad.Such as patent《A kind of dispersing method of carbon nanotube》, the method for patent publication No. CN102500255A,
Using specific dispersant, dispersion liquid is obtained with the method for ultrasound by grinding, this method is used dispersion solution and divided
The limitation of powder, is unable to extensive utilization.Patent《The manufacturing method of carbon nanotube aggregate dispersion liquid, patent publication No.
CN103189311A》With《A kind of physical dispersion method of carbon nanotube, patent publication No. CN105771762A》Spy is used
Fixed dispersant carrys out Aided Physical dispersing method, but the two patents due to cannot abundant dispersing Nano carbon tubes first, dispersion
Agent also has no way of being inserted between all carbon nanotubes, therefore its dispersion effect cannot still reach optimal effect.
It is the purpose of the present invention to improve nanotube dispersion, and the specific surface for being primarily due to carbon nanotube is very big, adsorption
Many gases, so carbon nanotube is difficult to be wet in a liquid, liquid is hard to reach the surface of carbon nanotube, so being to be difficult
Dispersion process is carried out, the draw ratio of second carbon nanotube is very long, is easy to tangle mutually, is difficult dispersion in a liquid, so this
The method of invention is that carbon nanotube is moistened first, then cuts off carbon by the powerful shearing of larger grinding bead and impact force and receives
The tie point of mitron, especially carbon nanotube, shorter pipe are less likely to tangle and are arranged in aggregation.By being ground with smaller
The more mild shearing of pearl is ground, impact etc. disperses carbon nanotube, but is unlikely to the pipe assembling structure of destroying carbon nanometer tube, to make
Standby well dispersed, the carbon nano tube dispersion liquid of structural integrity.Wherein in dispersion process, stirred using medium without using ball milling
Mill, the definition of ball milling be cylinder rotation drive it is internal grind ball rotation, inside does not have an agitating shaft action of forced stirring mill ball, and medium
The cylinder of Ball-stirring mill does not rotate, and there are agitating shaft and corresponding mixing component in inside, can be with action of forced stirring mill ball, medium stirring
Mill has higher energy density than ball milling（The input energy of unit volume）Smaller mill ball can carry out carbon nanotube
It is good dispersion and it is smaller to the destruction of carbon nanotube.
Invention content
In order to overcome the disadvantages mentioned above and deficiency of the prior art, the purpose of the present invention is to provide a kind of points of carbon nanotube
Dissipate method.
The purpose of the present invention can be realized by following technical solution.
A kind of dispersing method of carbon nanotube, includes the following steps：（1）It is pre-dispersed：Carbon nanotube is added equipped with pure
In the agitator tank of water, vacuum suction excludes gas in agitator tank, that is, removes the gas of carbon nano tube surface absorption, forms carbon and receives
The pre-dispersed slurry of mitron；（2）Grinding distribution：The carbon nanotube of dispersion will be obtained by grinding distribution by pre-dispersed slurry
Slurry.
Further, step（1）The pre-dispersed agitator tank used is closed structure, has pumping to fill above agitator tank
It sets, vacuum pump and mating valve, gas-filtering device, tank lower part have liquid feed pipe, discharge nozzle and pump, feed pipe, discharge nozzle
Cyclic process is formed with pump, carbon nanotube enters by way of feeding effective pumping in agitator tank；Carbon nanotube also by into
The online High shear device of expects pipe, inside carbon nanotube sucking agitator tank.
Further, step（2）The grinding distribution includes two-stage grinding distribution process, and first order dispersion uses grinding bead
The milling apparatus that diameter is 3-5 millimeters cuts off the tie point of carbon nanotube aggregate by the collision of grinding bead；Second
Grade dispersion uses grinding bead diameter for 0.6-1.2 millimeters of milling apparatus, with the stirring at low speed linear velocity of 3-12 metre per second (m/s)s
With the agitation energy of 0.6-2.0kw per kilogram slurries, the carbon nanotube by cut-out is disperseed, the carbon nanometer of dispersion is obtained
Pipe slurry.
Further, the milling apparatus of first order dispersion is horizontal medium stirring mill.
Further, the milling apparatus of second level dispersion is the medium stirring mill of either in a horizontal or vertical.
Further, it is additionally added dispersant during grinding distribution.If the slurries for long-term preservation by dispersion, root
According to need be added dispersant carry out stable slurry, in other field, the conductive additive such as carbon nanotube as lithium battery
When, dispersant is not added in selection, gives full play to the electric conductivity of carbon nanotube.
Since dispersion effect is preferable, the carbon nano tube dispersion liquid of the more conventional method dispersion of viscosity of carbon nano tube dispersion liquid
Viscosity wants low, therefore carbon nanotube can be dispersed in higher concentration in liquid.The viscosity generally allowed is in 1-5%, part carbon
Nanotube（The dispersion performance of the product of different carbon nanotube producers is different）Dispersion liquid concentration can reach 10% a left side
It is right.
Compared with prior art, the invention has the advantages that and technique effect：By vacuum suction, removal is adsorbed on carbon
The gas of nanotube surface improves the ability of carbon nanotube adsorption liquid；It is ground by two-stage, both protects carbon nanotube
Pipe assembling structure, and improve the dispersibility of carbon nanotube in a liquid so that the high conductivity of carbon nanotube, high intensity and
Its unique texture is widely used in various conductive materials and composite material.
Description of the drawings
Fig. 1 shows carbon nanotube dispersion process implementing procedure figure.
Fig. 2 is indicated in pre-dispersing operation, and the process that carbon nanotube dust introduces inside agitator tank is illustrated by pumping
Figure.
Fig. 3 is indicated in pre-dispersing operation, by High shear device the mistake inside carbon nanotube dust introducing agitator tank
Journey schematic diagram.
Specific implementation mode
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.It is noted that if the following process or symbol for having not special detailed description, is that those skilled in the art can refer to
The prior art realize or understand.
The present invention is the manufacturing method of the carbon nano tube dispersion liquid with following characteristics.
The dispersing method of carbon nanotube is according to following two steps：
（1）First before dispersion, need there are one pre-dispersed process, this process is that carbon nanotube is added to advance dress
Have in the closed agitator tank of pure water, and by way of agitator tank vacuum suction, gas in tank is excluded, and then carbon is received
The gas removal of nanotube surface absorption is easy to be soaked by liquid by carbon nanotube after the step.What pre-dispersing operation used
Agitator tank is the structure of totally-enclosed, and air extractor can connect the equipment such as vacuum pump in the top of jar, and liquid is arranged at jar lower part
Feed pipe and discharge nozzle, carbon nanotube can be entered by way of feeding effective pumping in agitator tank, and carbon nanotube can lead to
It crosses feed pipe with online high shear dispersion equipment suck inside agitator tank carbon nanotube, and passes through discharge nozzle and pump shape
At cyclic process, carbon nanotube can be added on liquid circulating pipe road.In view of in pre-dispersing operation, possible carbon nanotube is starched
The viscosity change of material is larger, it may be considered that uses impeller pump, peristaltic pump, diaphragm pump either single-screw (single screw) pump Quimby pump or more
Screw pump, online high shear dispersion equipment can be selected using the module series of IKA or the similar production of Ystal companies
Product and the similar products of other companies.
（2）Dispersion is obtained by the grinding distribution process of the different size of grinding bead of two-stage by pre-dispersed slurries
Carbon nanotube slurry.Specifically, it is preferred to use the dispersion flow of two-stage：Pass through the grinding of the different size of grinding bead of two-stage
Dispersion process can obtain the carbon nanotube slurry of fine dispersion.First order dispersion uses the grinding of the grinding bead of larger particles
Equipment, the abradant grinding bead diameter of the first order are 3-5 millimeters, and the abradant milling apparatus of the first order is horizontal medium
Ball-stirring mill；The abradant grinding bead diameter in the second level is 0.6-1.2 millimeters, by the collision of grinding bead carbon nanotube group
The tie point of aggressiveness is cut off, and then uses the milling apparatus of smaller grinding bead, with lower mixing speed, the carbon that process is cut off
Nanotube is disperseed, and the abradant milling apparatus in the second level is the medium stirring mill of either in a horizontal or vertical, is ground using lower
Mill speed ensures that carbon nano tube structure is not broken, and the general maximum line velocity for grinding mixing component is no more than 15 metre per second (m/s)s, warp
The low speed grinding distribution process for spending certain time, can obtain good carbon nanotube dispersed paste, and sand mill can select moral
State is resistance to speed or the horizontal sand mill product of Burl Corp.
Fig. 1 shows the sequence of above-mentioned operating process and main points.
Embodiment
With reference to embodiment, the present invention will be further described, it should be noted that embodiment is not constituted to this
Invent the limitation of desired protection.
Embodiment one
Fig. 1 shows carbon nanotube dispersion process implementing procedure figure.
The schematic diagram of the pre-dispersing operation device of Fig. 1 is Fig. 2, and pre-dispersing device above connects vacuum pump using sealing agitator tank,
First pure water is added in agitator tank, vacuum degree control in tank is used by vacuum pump by the Z- of YSTRAL in 0.1Mpa
Then Inline Disperser equipment is added 1% as powder sucking and size circulations pump by online high shear dispersion equipment
（Weight percent）Carbon nanotube, and be uniformly mixed with liquid, pre-dispersed slurry viscosity is 2200cps or so.
First order process of lapping in Fig. 1 is as follows：Pre-dispersed 20kg slurries are passed through, speeded using resistance to（Shanghai）Mechanical instrument
The LMZ10 sand mills of device Co., Ltd carry out first order dispersion, use 3 millimeters of the grinding that pearl is sanded and carries out 50 minutes, stirring
Speed is 300rpm, and linear velocity is 10 metre per second (m/s)s, and slurry final viscosity is 350cps or so.Grinding spindle input energy is
0.8kw per kilogram slurries.
Second level process of lapping in Fig. 1 is as follows：20 kilograms of slurries by first order dispersion, speeded using resistance to（Shanghai）
The LMZ10 sand mills of mechanical device Co., Ltd carry out second level dispersion, use 0.8 millimeter of point that pearl is sanded and carries out 40 minutes
Grinding, mixing speed 300rpm are dissipated, slurry final viscosity is 350cps.Grinding stirring linear velocity be 10 metre per second (m/s)s, second
Grade grinding energy input is 0.6kw per kilogram slurries.
Fig. 2 indicates the pre-dispersing device schematic diagram of the present embodiment 1.
It is detected by Hegman grind gage, whole granularities are less than 10 microns or less.
Embodiment two
Fig. 1 carbon nanotubes indicate the sequence and main points of following operating process in the implementing procedure figure of dispersion process.
Pre-dispersing operation schematic device is Fig. 3, and pre-dispersing device above connects vacuum pump, first pure using sealing agitator tank
Water purification is added in agitator tank, and vacuum degree control is used the single-screw (single screw) pump equipment of Japanese HEISHIN in 0.2Mpa by vacuum pump
As powder sucking and size circulations pump.Then liquid circulation is got up by pumping, by drainage, gradually carbon nanotube
A mixing bowl is added, and is uniformly mixed with liquid, finally premixes a concentration of 5%（Weight percent）The pre-dispersed slurry of carbon nanotube
Expect that viscosity is 6700cps or so.
First order process of lapping in Fig. 1 is as follows：Pre-dispersed 20kg slurries are passed through, Burl Corp of Switzerland is used
Macromedia sand mills carry out first order dispersion, use 5 millimeters of the grinding that pearl is sanded and carries out 30 minutes, 8 meters of mixing speed
Per second, slurry viscosity is 3500cps or so.
Second level process of lapping in Fig. 1 is as follows：5 kilograms of slurries by first order dispersion, strangled using Switzerland's cloth public
The Micormedia X1 sand mills of department carry out second level dispersion, and the dispersion carried out 50 minutes using 0.6 millimeter of sand milling pearl is ground
Mill, mixing speed 600rpm, the linear velocity for grinding stirring are 12 metre per second (m/s)s, and grinding energy input in the second level is 2.0kw per public
Jin slurry, slurry final viscosity are 150cps.
It is detected by Hegman grind gage, whole granularities are less than 10 microns or less.
Fig. 1 shows the sequence of above-mentioned operating process and main points.
Fig. 3 indicates the pre-dispersing device schematic diagram of the present embodiment 2.
Embodiment three
Pre-dispersing device is Fig. 3, and pre-dispersing device is above connect vacuum pump, agitator tank first is added in pure water using sealing agitator tank
It is interior, by vacuum pump vacuum degree control in 0.1Mpa, using the Quimby pump equipment of Japanese HEISHIN as powder sucking and
Size circulations pump.Then liquid circulation is got up by pumping, by drainage, a mixing bowl gradually is added in carbon nanotube, and
It is uniformly mixed with liquid, finally premixes a concentration of 6%（Weight percent）The pre-dispersed slurry viscosity of carbon nanotube be
8200cps or so.
First order process of lapping is as follows：Pre-dispersed 5kg slurries are passed through, speeded using resistance to（Shanghai）The limited public affairs of mechanical device
The Labstar Laboratary type sand mills of department carry out first order dispersion, use 4 millimeters of the grinding that pearl is sanded and carries out 10 minutes, slurry
Expect that viscosity is 2600cps or so.
Second level process of lapping is as follows：5 kilograms of slurries by first order dispersion, resistance to resistance to speed of speeding is used（Shanghai）Machinery
The Labstar sand mills of Instrument Ltd. carry out second level dispersion, use 1.2 millimeters of the dispersion that pearl is sanded and carries out 40 minutes
Grinding, mixing speed 1000rpm, stirring linear velocity are 5 metre per second (m/s)s, and slurry final viscosity is 350cps.Grind energy in the second level
Amount input is 0.9kw per kilogram slurries.
It is detected by Hegman grind gage, whole granularities are less than 10 microns or less.
Fig. 1 shows the sequence of above-mentioned operating process and main points.
Fig. 3 indicates the pre-dispersing device schematic diagram of the present embodiment 3.
Example IV
Pre-dispersing device is Fig. 3, and pre-dispersing device above connects vacuum pump, vacuum degree control makes in 0.2Mpa using sealing agitator tank
It uses the single-screw (single screw) pump equipment for using Japanese HEISHIN as powder sucking and size circulations pump, agitator tank first is added in pure water
It is interior, then 1% is added by pumping（Weight percent）Carbon nanotube and 0.5% polyvinylpyrrolidone as dispersant
（PVP）K30 powder.And be uniformly mixed with liquid, pre-dispersed slurry viscosity is 2300cps or so.
First order process of lapping is as follows：Pre-dispersed 5kg slurries are passed through, speeded using resistance to（Shanghai）The limited public affairs of mechanical device
The Labstar Laboratary type sand mills of department carry out first order dispersion, use 4 millimeters of the grinding that pearl is sanded and carries out 10 minutes, slurry
Expect that viscosity is 1000cps or so.
Second level process of lapping is as follows：5 kilograms of slurries by first order dispersion, resistance to resistance to speed of speeding is used（Shanghai）Machinery
The Labstar sand mills of Instrument Ltd. carry out second level dispersion, use 1.2 millimeters of the dispersion that pearl is sanded and carries out 50 minutes
Grinding, mixing speed 600rpm, stirring linear velocity are 3 metre per second (m/s)s, and slurry final viscosity is 280cps.Second level grinding energy
Input is 1.0kw per kilogram slurries
It is detected by Hegman grind gage, whole granularities are less than 10 microns or less.
Claims (6)
1. a kind of dispersing method of carbon nanotube, which is characterized in that include the following steps：（1）It is pre-dispersed：Carbon nanotube is added
In agitator tank equipped with pure water, vacuum suction excludes gas in agitator tank, that is, removes the gas of carbon nano tube surface absorption,
Form the pre-dispersed slurry of carbon nanotube；（2）Grinding distribution：The pre-dispersed slurry of carbon nanotube is disperseed by grinding distribution
Carbon nano tube paste.
2. a kind of dispersing method of carbon nanotube according to claim 1, which is characterized in that step（1）It is pre-dispersed to use
Agitator tank is closed structure, there is air extractor, vacuum pump and mating valve, gas-filtering device above agitator tank, under tank
Portion has liquid feed pipe, discharge nozzle and pump, feed pipe, discharge nozzle and pump to form cyclic process, and carbon nanotube is effective by feeding
The mode of pumping enters in agitator tank；Carbon nanotube also by the online High shear device of feed pipe, sucks carbon nanotube
Inside agitator tank.
3. a kind of dispersing method of carbon nanotube according to claim 1, which is characterized in that step（2）The grinding distribution
Including two-stage grinding distribution process, first order dispersion uses grinding bead diameter for 3-5 millimeters of milling apparatus, passes through grinding
The tie point of carbon nanotube aggregate is cut off in the collision of pearl；Second level dispersion uses grinding bead diameter for 0.6-1.2 millis
The milling apparatus of rice, with the agitation energy of the stirring at low speed linear velocity and 0.6-2.0kw per kilogram slurries of 3-12 metre per second (m/s)s, passing through
The carbon nanotube for crossing cut-out is disperseed, and the carbon nano tube paste of dispersion is obtained.
4. a kind of dispersing method of carbon nanotube according to claim 3, which is characterized in that the grinding of first order dispersion is set
Standby is horizontal medium stirring mill.
5. a kind of dispersing method of carbon nanotube according to claim 3, which is characterized in that the grinding of second level dispersion is set
Standby is the medium stirring mill of either in a horizontal or vertical.
6. a kind of dispersing method of carbon nanotube according to claim 1, which is characterized in that be additionally added during grinding distribution
Dispersant.
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| CN111020270A (en) * | 2019-12-19 | 2020-04-17 | 陕西科技大学 | CNTs reinforced magnesium-based composite material and preparation method thereof |
| CN111408468A (en) * | 2020-02-24 | 2020-07-14 | 东莞职业技术学院 | Grinding method for nonporous nano material |
| CN114516630A (en) * | 2022-03-17 | 2022-05-20 | 无锡东恒新能源科技有限公司 | Method for improving dispersibility of carbon nano tube |
| CN115304056A (en) * | 2022-07-21 | 2022-11-08 | 青岛泰联新材料有限公司 | Granular carbon nano tube and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111020270A (en) * | 2019-12-19 | 2020-04-17 | 陕西科技大学 | CNTs reinforced magnesium-based composite material and preparation method thereof |
| CN111020270B (en) * | 2019-12-19 | 2021-04-23 | 陕西科技大学 | CNTs reinforced magnesium-based composite material and preparation method thereof |
| CN111408468A (en) * | 2020-02-24 | 2020-07-14 | 东莞职业技术学院 | Grinding method for nonporous nano material |
| CN111408468B (en) * | 2020-02-24 | 2021-10-08 | 东莞职业技术学院 | Grinding method for nonporous nano material |
| CN114516630A (en) * | 2022-03-17 | 2022-05-20 | 无锡东恒新能源科技有限公司 | Method for improving dispersibility of carbon nano tube |
| CN114516630B (en) * | 2022-03-17 | 2023-09-01 | 无锡东恒新能源科技有限公司 | Method for improving dispersibility of carbon nano tube |
| CN115304056A (en) * | 2022-07-21 | 2022-11-08 | 青岛泰联新材料有限公司 | Granular carbon nano tube and preparation method thereof |
| CN115304056B (en) * | 2022-07-21 | 2024-01-26 | 青岛泰联新材料有限公司 | Granular carbon nano tube and preparation method thereof |
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Application publication date: 20180918 |