CN1569939A - Carbon nanotube electrically conductive fibre and method for making same - Google Patents
Carbon nanotube electrically conductive fibre and method for making same Download PDFInfo
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- CN1569939A CN1569939A CN 200410017918 CN200410017918A CN1569939A CN 1569939 A CN1569939 A CN 1569939A CN 200410017918 CN200410017918 CN 200410017918 CN 200410017918 A CN200410017918 A CN 200410017918A CN 1569939 A CN1569939 A CN 1569939A
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Abstract
The invention provides a carbon nanotube electrically conductive fibre and method for making same, wherein the conductive fiber comprises a carbon nano tube, dispersing agent and thermoplastic polymeric compound, the preparation comprises dispersing the carbon nano tube into water at the presence of the dispersing agent, mixing the carbon nano tube aqueous solution with thermoplastic polymer, drying, granulating and spinning.
Description
Technical field
The present invention relates to a kind of electro-conductive fiber and preparation method thereof, particularly relating to a kind of is electro-conductive fiber of conductive component and preparation method thereof with carbon nanotube or carbon nano fiber.
Background technology
Most macromolecular materials are insulating material, and the man-made fiber by macromolecular material is made equally also has insulativity as terylene, polypropylene fibre, polyamide fibre, acrylic fibers etc.These man-made fiber in use static constantly accumulate, and electric charge can't discharge, and finally have than higher electromotive force.Man-made fiber with static bring serious threat can for the safety in production of service station, oil depot and some special occasions.The man-made fiber clothes also can bring disadvantageous effect to HUMAN HEALTH owing to often have static.
Solve the disadvantageous effect that this class man-made fiber static brings, at present main way is to manage to allow originally nonconducting Polymer Synthesizing fiber conduction, being about to a certain proportion of conductive component joins in the fiber, mainly comprise following two kinds of methods: the one,, conductive component is invested fiber surface, as Chinese patent " method for formulating of electro-conductive fiber and conductive fabric " (application number is 92108939.2) disclose electrolytic copper, pure tungsten, nickel prepared electrolysis by a certain percentage after, fiber and the cloth that cleaned is carried out electric plating method.This method is carried out antistatic treatment to it after man made fiber fabric is shaped, weak point is that the antistatic textile washing resistance performance for preparing is relatively poor.Ultrafine metal fibers sneaked in yarn or the textiles also has obvious effects to eliminating man-made fiber static, but this kind fabric feel is relatively poor, weaves also relatively difficulty.The 2nd,, conducting particles adds in the polymkeric substance, prepares electro-conductive fiber through spinning.Conducting particles at present commonly used is conductive carbon black, metal oxide etc., could form conductive network but must add a large amount of conductive component (often surpass 20%, even 40%) in fiber, gives the fiber conductivity.A large amount of carbon black particles or metal oxide particle add the preparation technology's more complicated that causes electro-conductive fiber in the polymkeric substance to, and high-load carbon black has destroyed the spinning rheological property of polymkeric substance in the product, make fibre-forming performance, the mechanical property variation of polymkeric substance.The electro-conductive fiber of this high carbon black content is carried out spinning then need to adopt composite spinning technology.So-called composite spinning technology is to contain the polymkeric substance of a large amount of carbon blacks as a component, the polymkeric substance that does not contain carbon black is as another component, preparation core-skin type (or tangerine lobe type) structure, use the twin screw spinning machine equipment to carry out spinning, this causes the business equipment input to increase, processing parameter increases, and the controllable quality difficulty is increased.
Carbon nanotube is the type material that the nineties develops, and obtains common concern both domestic and external, and the preparation method is multiple, large-scale production is all arranged at present, but it is at industrial application and development ground zero both at home and abroad.Carbon nanotube is divided into Single Walled Carbon Nanotube and multi-walled carbon nano-tubes: Single Walled Carbon Nanotube single tube diameter is about 1nm, and length-to-diameter ratio is 50～2000; Multi-walled carbon nano-tubes is looked the how much different of wall, and diameter has bigger length-to-diameter ratio generally less than 100nm.Simultaneously, carbon nano fiber also has similar characteristic.Because the diameter of carbon nanotube is also littler than the diameter of conducting particles, and length-to-diameter ratio is bigger, very little addition (0.1%～2%) just can form conductive channel in polymkeric substance, obtain electro-conductive fiber behind spinning technique, and do not need composite spinning technology.Because the various effects of nano material make that carbon nanotube is very easy to assemble, so scattering problem is the key of preparation carbon nanotube composite conducting fiber.
Summary of the invention
Technical problem to be solved of the present invention is to provide a kind of carbon nanotube conducting fiber and preparation method thereof, with solve the conductive effect that exists in the prior art poor, be difficult for that spinning, washing resistance performance are poor, shortcoming such as complex process, feel are relatively poor.
One of purpose of the present invention provides a kind of carbon nanotube conducting fiber, and this carbon nanotube conducting fiber is made up of carbon nanotube, dispersion agent and thermoplastic polymer, and its mass percent consists of:
Carbon nanotube 0.1～5
Dispersion agent 0.1～5
Thermoplastic polymer 100
And the mass ratio of carbon nanotube and dispersion agent sum and polymkeric substance was less than 5.1: 100.
Described carbon nanotube is one or more in Single Walled Carbon Nanotube, multi-walled carbon nano-tubes and the carbon nano fiber.
Described dispersion agent is alkylbenzene sulfonate CH
3(CH
2)
nC
6H
4SO
3X, or alkylsurfuric acid hydrochlorate CH
3(CH
2)
nSO
4Among the X one or more, n=0～15 wherein, X=Li, Na, Mg, Ca, NH
4
Described thermoplastic polymer is one or more in polyethylene, polypropylene, polyester, polymeric amide, polyvinyl alcohol, polyacrylonitrile or the Mierocrystalline cellulose.
Described electro-conductive fiber preparation method comprises the steps:
A joins carbon nanotube and dispersion agent in the container that water is housed, and concussion disperses, and removes the precipitation part, prepares carbon nano-tube aqueous solutions.
B is with carbon nano-tube aqueous solutions and thermoplastic polymer mixing, and drying is prepared the carbon nano-tube/polymer composite granule.
C carries out spinning, stretching preparation electro-conductive fiber with the carbon nano-tube/polymer composite granule through spining technology.
Carbon nanotube described in the electro-conductive fiber preparation process a and dispersion agent are added to the water in no particular order; The quality of dispersion agent and carbon nanotube accounts for 0.1～5% of this aqueous solution; The mass ratio of dispersion agent and carbon nanotube is 0.1～10: 1.
Carbon nano-tube aqueous solutions described in the electro-conductive fiber preparation process b mixes with polymer machinery, comprises polymkeric substance joined in the carbon nano-tube aqueous solutions mixing, and the carbon nano-tube aqueous solutions spray is attached to polymer surfaces.
Spining technology described in the electro-conductive fiber preparation process c is one or more in melt-spinning technology, wet-spinning technology or the dry-wet spinning technology.
The invention has the beneficial effects as follows: described electro-conductive fiber and preparation method thereof technology is simple, production efficiency is high, and the fiber conductive effect of preparation is good.It is conductive component that the present invention has adopted carbon nanomaterial, and it still is good strongthener, and the mechanical property of fiber is played the influence in front, has higher technology content.Described electro-conductive fiber can carry out spinning by enough single extruder type spinning machines, has reduced the input of enterprise's spinning equipment, has simplified the production technique of electro-conductive fiber.
Electro-conductive fiber provided by the invention can be used as antistatic material and electromagnetic shielding material in fields such as clothes, bunting, transport tapes.
Embodiment
Below in conjunction with embodiment the present invention is elaborated.
Embodiment 1
0.2 gram Single Walled Carbon Nanotube is joined in the 100 gram water, and mechanically mixing is even, 1 gram lithium dodecyl sulfate is joined in the above solution again, and ultrasonic oscillation disperses, and whizzer is centrifugal, removes the precipitation part, obtains the finely dispersed aqueous solution of carbon nanotube.
Polypropylene powder is poured in the carbon nano-tube aqueous solutions of preparation, mechanical stirring is even, heats up moisture evaporation is fallen, and obtains the composite powder that polypropylene surface is attached with carbon nanotube.Obtain can be used for the section of spinning through the screw extrusion press granulation.Adopt melt spinning method to obtain the carbon nanotube/polypropylene composite conducting fiber.Wherein the mass content of carbon nanotube in fiber is 1%, and specific conductivity is 5 * 10
-5S/cm.
Embodiment 2-8
Shown carbon nano-tube aqueous solutions and preparation method thereof is identical with embodiment 1, and other condition sees Table 1.Wherein add method (Disp+H
2O)+and CNT represents and earlier dispersion agent is added to the water, and after the dissolving, conductive component joined in the above solution again, and other is identical.
Table 1 embodiment 2-8
| Embodiment | Conductive component (gram) | Dispersion agent (gram) | Water (gram) | The adding method |
| ????2 | Single Walled Carbon Nanotube 1 | Heptane base benzene sulfonic acid sodium salt 4 | 100 | (Disp+H 2O)+CNT |
| ????3 | Single Walled Carbon Nanotube 1 | Sodium lauryl sulphate 0.1 | 100 | (Disp+CNT)+H 2O |
| ????4 | Multi-walled carbon nano-tubes 0.1 | Butylbenzene sulfanilic acid 0.5 | 100 | (CNT+H 2O)+Disp |
| ????5 | Multi-walled carbon nano-tubes 0.4 | Toluene sulfonic acide magnesium 4 | 100 | (Disp+H 2O)+CNT |
| ????6 | Multi-walled carbon nano-tubes 2 | Sodium lauryl sulphate 1 | 100 | (CNT+H 2O)+Disp |
| ????7 | Carbon nano fiber 2 | Heptane base Lithium Sulphate 3 | 100 | (Disp+CF)+H 2O |
| ????8 | Carbon nano fiber 4 | Hexadecyl Phenylsulfonic acid calcium 1 | 100 | (Disp+H 2O)+CF |
Wherein:
The polyacrylonitrile powder is poured in the carbon nano-tube aqueous solutions of embodiment 2 preparations, mechanical stirring is even, heats up moisture evaporation is fallen, and obtains the composite powder that the polyacrylonitrile surface attachment has carbon nanotube.Composite powder is dissolved in the solvent of polyacrylonitrile in (as dimethyl formamide, N,N-DIMETHYLACETAMIDE or sulphur hydracid sodium water solution), the preparation spinning slurry adopts wet-spinning technology spinning to obtain carbon nanotube/polypropylene nitrile composite conducting fiber.Wherein the mass content of carbon nanotube in fiber is 0.5%, and specific conductivity is 8 * 10
-6S/cm.
Pva powder is poured in the carbon nano-tube aqueous solutions of embodiment 2 preparations, mechanical stirring is even, in carbon nano-tube aqueous solutions in the polyvinyl alcohol dissolving, obtain spinning slurry, adopt wet-spinning technology spinning to obtain carbon nanotube/polypropylene nitrile composite conducting fiber.Wherein the mass content of carbon nanotube in fiber is 3%, and specific conductivity is 2 * 10
-2S/cm.
The carbon nano-tube aqueous solutions of embodiment 3 preparations evenly is sprayed at the polyamide 66 powder surface with atomizer, heats up afterwards moisture evaporation is fallen, and obtains the composite powder that the polyamide 66 surface attachment has carbon nanotube.Obtain can be used for the section of spinning through the screw extrusion press granulation.Adopt melt spinning method to obtain the carbon nanotube/polypropylene composite conducting fiber.Wherein the mass content of carbon nanotube in fiber is 0.1%, and specific conductivity is 3 * 10
-7S/cm.
Polyester powder is poured in the carbon nano-tube aqueous solutions of embodiment 6 preparations, mechanical stirring is even, heats up moisture evaporation is fallen, and obtains the composite powder that surface of polyester is attached with carbon nanotube.Obtain can be used for the section of spinning through the screw extrusion press granulation.Adopt melt spinning method to obtain carbon nano-tube/poly ester composite conducting fiber.Wherein the mass content of carbon nanotube in fiber is 3%, and specific conductivity is 2 * 10
-3S/cm.
Be dissolved in polyvinyl alcohol in the water earlier, the carbon nano fiber aqueous solution with embodiment 8 preparations drips in the aqueous solution of polyvinyl alcohol again, mechanical stirring evenly obtains spinning slurry, adopts wet-spinning technology spinning to obtain carbon nano fiber/polyvinyl alcohol composite conducting fiber.Wherein the mass content of carbon nano fiber in fiber is 4%, and specific conductivity is 5 * 10
-3S/cm.
Claims (8)
1. carbon nanotube conducting fiber is characterized in that this carbon nanotube conducting fiber is made up of carbon nanotube, dispersion agent and thermoplastic polymer, and its mass ratio is
Carbon nanotube 0.1～5
Dispersion agent 0.1～5
Thermoplastic polymer 100;
And the mass ratio of carbon nanotube and dispersion agent sum and polymkeric substance was less than 5.1: 100.
2. carbon nanotube conducting fiber according to claim 1 is characterized in that described carbon nanotube is one or more in Single Walled Carbon Nanotube, multi-walled carbon nano-tubes or the carbon nano fiber.
3. carbon nanotube conducting fiber according to claim 1 is characterized in that described dispersion agent is alkylbenzene sulfonate CH
3(CH
2)
nC
6H
4SO
3X or alkyl-sulphate CH
3(CH
2)
nSO
4Among the X one or more,
N=0～15 wherein, X=Li, Na, Mg, Ca, NH
4
4. carbon nanotube conducting fiber according to claim 1 is characterized in that described thermoplastic polymer is one or more in polyethylene, polypropylene, polyester, polymeric amide, polyvinyl alcohol, polyacrylonitrile or the Mierocrystalline cellulose.
5. one kind as each described carbon nanotube conducting fiber preparation method of claim 1～4, it is characterized in that this method in turn includes the following steps:
A joins carbon nanotube and dispersion agent in the container that water is housed, and concussion disperses, and removes the precipitation part, prepares carbon nano-tube aqueous solutions.
B is with carbon nano-tube aqueous solutions and thermoplastic polymer mixing, and drying is prepared the carbon nano-tube/polymer composite granule.
C carries out spinning, stretching preparation electro-conductive fiber with the carbon nano-tube/polymer composite granule through spining technology.
6. carbon nanotube conducting fiber preparation method according to claim 5 is characterized in that carbon nanotube described in the step a and dispersion agent are added to the water in no particular order; The mass percent in this aqueous solution of dispersion agent and carbon nanotube is 0.1～5%; The mass ratio of dispersion agent and carbon nanotube is 0.1～10: 1.
7. carbon nanotube conducting fiber preparation method according to claim 5, it is characterized in that described carbon nano-tube aqueous solutions and mixed with polymers, comprise polymer powder joined in the carbon nano-tube aqueous solutions and mix, or the carbon nano-tube aqueous solutions spray is attached to polymer surfaces.
8. carbon nanotube conducting fiber preparation method according to claim 5 is characterized in that described spining technology is one or more in melt-spinning technology, wet-spinning technology or the dry-wet spinning technology.
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| WO2007096479A1 (en) * | 2006-02-23 | 2007-08-30 | Panipol Oy | Novel compositions and methods for the production thereof |
| CN1760269B (en) * | 2004-10-13 | 2010-06-09 | 上海扬泽纳米新材料有限公司 | Electric polymer and preparation method |
| CN1869291B (en) * | 2005-05-23 | 2010-09-08 | 中国科学院化学研究所 | Fibre structure of polyester/carbone nanotube nano composite and its preparation method |
| CN102025018A (en) * | 2009-09-17 | 2011-04-20 | 深圳富泰宏精密工业有限公司 | Antenna and wireless communication device using same |
| CN101586259B (en) * | 2009-06-23 | 2011-06-22 | 东华大学 | Method for preparing polyvinyl alcohol spin dope added with carbon nano-tube |
| CN102304786A (en) * | 2011-07-18 | 2012-01-04 | 东华大学 | Method for preparing CNT (carbon nano tube)-polyacrylonitrile fibre by melting spinning |
| CN102731994A (en) * | 2012-07-03 | 2012-10-17 | 金发科技股份有限公司 | Nylon composite, preparation method, application thereof and plastic product of nylon composite |
| CN102953137A (en) * | 2011-08-18 | 2013-03-06 | 香港理工大学 | High-elasticity conductive fiber and preparation method thereof |
| CN101403721B (en) * | 2008-11-03 | 2013-05-08 | 东华大学 | Flexible penetration sensor used for military uniform |
| CN103183327A (en) * | 2013-03-18 | 2013-07-03 | 江苏苏美仑智能科技有限公司 | Treating agent for carbon nano tube and preparation method of water-soluble carbon nano tube |
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| CN1869291B (en) * | 2005-05-23 | 2010-09-08 | 中国科学院化学研究所 | Fibre structure of polyester/carbone nanotube nano composite and its preparation method |
| WO2007096479A1 (en) * | 2006-02-23 | 2007-08-30 | Panipol Oy | Novel compositions and methods for the production thereof |
| CN101403721B (en) * | 2008-11-03 | 2013-05-08 | 东华大学 | Flexible penetration sensor used for military uniform |
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| CN102025018A (en) * | 2009-09-17 | 2011-04-20 | 深圳富泰宏精密工业有限公司 | Antenna and wireless communication device using same |
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| CN102953137A (en) * | 2011-08-18 | 2013-03-06 | 香港理工大学 | High-elasticity conductive fiber and preparation method thereof |
| CN102953137B (en) * | 2011-08-18 | 2014-08-27 | 香港理工大学 | High-elasticity conductive fiber and preparation method thereof |
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