CN106245139B - A kind of conduction selfreparing fiber and preparation method thereof - Google Patents
A kind of conduction selfreparing fiber and preparation method thereof Download PDFInfo
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- CN106245139B CN106245139B CN201610710900.4A CN201610710900A CN106245139B CN 106245139 B CN106245139 B CN 106245139B CN 201610710900 A CN201610710900 A CN 201610710900A CN 106245139 B CN106245139 B CN 106245139B
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- carbon nanotube
- selfreparing
- fiber
- sodium polyacrylate
- conductive
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/52—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated carboxylic acids or unsaturated esters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
Abstract
The present invention relates to a kind of conductive selfreparing fiber and preparation method thereof, the fiber is the composite fibre of lauryl sodium sulfate modified multiwalled carbon nanotube and Sodium Polyacrylate composition；Wherein, multi-walled carbon nanotube and the mass ratio of lauryl sodium sulfate are 2~4:1~4；The mass ratio of multi-walled carbon nanotube and Sodium Polyacrylate is 0.5~10：5~30.Preparation method includes：Multi-walled carbon nanotube and lauryl sodium sulfate are dissolved in solvent, cell pulverization, obtain modified multiwalled carbon nanotube dispersion liquid, be added Sodium Polyacrylate, mixing obtains modified multiwalled carbon nanotube/Sodium Polyacrylate gel spinning solution, wet spinning to get.The method of the present invention is simple, of low cost, is easy to industrialization；Obtained conductive selfreparing fiber quality is high, has preferable electric conductivity, stable mechanical property, and in flexible electronic component, the fields such as flexible energy storage device and senser element have huge application prospect.
Description
Technical field
The invention belongs to composite fibre and its preparation field, more particularly to a kind of conductive selfreparing fiber and its preparation side
Method.
Background technology
Carbon nanotube has as monodimension nanometer material and connects perfect hexagonal structure, and light weight, has preferable
Mechanics, electricity and chemical property.Goed deep into its wide application prospect with carbon nanotube and nano materials research in recent years
Also it constantly shows.For multi-walled carbon nanotube compared with single-walled carbon nanotube, production cost is low, can produce on a large scale etc. excellent
Gesture is more conducive to its commercialization.Multi-walled carbon nanotube is applied to some products on a large scale as basis material or additive
In, for example, high-performance carbon nanotube fiber prepared by dry spinning, the composite material of intelligent driving, photoelectric device flexible,
Composite materials such as the functional film for disperseing or detaching etc..
One-dimensional material of the fiber as macroscopic view can be constructed two-dimentional, three-dimensional by some special braidings and design
Macroscopic material and product.Because its distinctive performance is by scientific research scholars widely concern, they have conductive non-metallic fibers
Have the advantages that light, flexibility is good, there is prodigious advantage in fields such as intelligent clothing, flexible sensings.Wherein with carbon nanotube
It is made great progress for the fiber research of conductive additive.In the early time, the Baughman of UT Dallas, R.H.
Professor obtains the carbon with superior electrical conductivity energy by the way that the carbon nanotube aligned to be wound up on the IR fiber of elasticity
Nanotube/rubber composite fibre, resistance does not increase (Liu Z.F., Baughman substantially when stretching reaches 1000%
R.H.,et al.Science,2015,349,400)；The Kim S.J. of Han Yang University are prepared for carbon nanotube by dry spinning
Yarn, adjustment load boric acid on yarn and have the function of detecting glucose concentration, and can generate actuating to environmental stimuli
Deformation can be used for artificial muscle (Lee J.h., Kim S.J., et al.Small, 2016,12,2085) etc..
Currently, in practical applications some conductive fibers due to fatigue, aging will produce fracture, influencing electronic circuit just
It is often used.Therefore, preparing a kind of conductive and energy selfreparing fibrous material has important practical value.
Invention content
Technical problem to be solved by the invention is to provide a kind of conductive selfreparing fiber and preparation method thereof, party's legal systems
Standby obtained conductive selfreparing fiber, has good electric conductivity, can be used as light-weight conductor；Conductive selfreparing fiber has good
Good flexibility can be used for preparing flexible electronic component.
A kind of conductive selfreparing fiber of the present invention, the fiber be lauryl sodium sulfate modified multiwalled carbon nanotube with
The composite fibre of Sodium Polyacrylate composition；Wherein, multi-walled carbon nanotube and the mass ratio of lauryl sodium sulfate are 2~4:1~
4；The mass ratio of multi-walled carbon nanotube and Sodium Polyacrylate is 0.5~10：5~30.
A kind of preparation method of conductive selfreparing fiber of the present invention, including：
(1) multi-walled carbon nanotube and lauryl sodium sulfate are dissolved in solvent, cell pulverization, obtain modified multi wall carbon and receives
Mitron dispersion liquid；Wherein, multi-walled carbon nanotube and lauryl sodium sulfate mass ratio are 2~4:1~4；
(2) Sodium Polyacrylate is added in the modified multiwalled carbon nanotube dispersion liquid in step (1), mixing is changed
Property multi-walled carbon nanotube/Sodium Polyacrylate gel spinning solution；Wherein, the mass ratio of multi-walled carbon nanotube and Sodium Polyacrylate
It is 0.5~10：5~30；
(3) spinning solution in step (2) is subjected to wet spinning, obtains conductive selfreparing fiber.
A concentration of 0.5~10mg/mL of modified multiwalled carbon nanotube dispersion liquid in the step (1).
Solvent is deionized water in the step (1).
The time of cell pulverization is 3~7h, preferably 5h in the step (1).
The mode of mixing is in the step (2)：The time of whirlpool blending instrument processing is 5~10h.
The ratio of Sodium Polyacrylate and modified multiwalled carbon nanotube dispersion liquid is 5~30mg in the step (2):1mL.
The condition of wet spinning is in the step (3)：It is placed in coagulating bath to take out after 10~60min and dry；Spinning mouth
A diameter of 0.3~2mm；Spinning speed is 3~12mL/h；Wherein, coagulating bath is to be saturated calcium chloride solution at room temperature.
The present invention obtains modified multi wall carbon by the way that Sodium Polyacrylate and modified multiwalled carbon nanotube dispersion liquid to be sufficiently mixed
The gelatinous spinning solution of nanotube/Sodium Polyacrylate, and be injected into saturation calcium chloride coagulation bath by wet spinning technology,
Not only had conductivity but can selfreparing modified multiwalled carbon nanotube/Sodium Polyacrylate composite fibre, this method is easy to operate,
It is at low cost, it is with a wide range of applications.
By adjust gel spinning solution in the ratio of Sodium Polyacrylate and multi-walled carbon nanotube be prepared electric conductivity,
The conductive selfreparing fiber that complex velocity speed is different and intensity is different is reviewed one's lessons by oneself, when multi-walled carbon nanotube content is more, the conduction is certainly
The selfreparing effect of repairing fiber is deteriorated, when modified multiwalled carbon nanotube dispersion liquid a concentration of is more than 10mg/mL, the modification
Multi-walled carbon nanotube/Sodium Polyacrylate composite fibre is difficult to achieve the effect that selfreparing.
Advantageous effect
(1) operating method of the invention is simple, preparation process fast and easy；
(2) the prepared modified multiwalled carbon nanotube/Sodium Polyacrylate composite conducting selfreparing fiber of invention has excellent
Mechanical property, have well elasticity, arbitrarily can bend and weave；
(3) modified multiwalled carbon nanotube/Sodium Polyacrylate composite conducting selfreparing fiber prepared by the present invention is preferable
Electric conductivity and good self-healing properties, can be used as lightweight conductive material, deformable electronic component, flexible energy storage device and
Sensor etc. has broad application prospects.
Description of the drawings
Fig. 1 is (a) before the conductive selfreparing fiber prepared in embodiment 1 blocks, after blocking (b), after selfreparing (c), from
Repair the digital photograph of post-tensioning (d)；
Fig. 2 be embodiment 1 in prepare conductive selfreparing fiber reset condition, block and repair after I-V diagram；
Fig. 3 is the I-V diagram of the conductive selfreparing fiber prepared in embodiment 2；
Fig. 4 is the I-V diagram of the conductive selfreparing fiber prepared in embodiment 3.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) at room temperature, multi-walled carbon nanotube 50mg and lauryl sodium sulfate 25mg are weighed respectively, are placed in 100mL's
In beaker, the mixed liquor that deionized water 50mL is made into a concentration of 1mg/mL of multi-walled carbon nanotube is then added, then by mixed liquor
Cell pulverization handles 5h, obtains dispersed modified multiwalled carbon nanotube solution 50mL well；
(2) 500mg Sodium Polyacrylates are added into above-mentioned multi-walled carbon nanotube dispersion liquid, 10h is handled with whirlpool blending instrument,
Form the gelatinous spinning solution of modified multiwalled carbon nanotube/Sodium Polyacrylate；
(3) the gelatinous spinning solution loading 10mL of modified multiwalled carbon nanotube/Sodium Polyacrylate is connected with internal diameter
In syringe for 500 μm of polytetrafluoroethylene (PTFE) micro-pipes, on the propeller that fltting speed is 10mL/h, modified multi-wall carbon nano-tube
Pipe/polyacrylic acid sodium gel is through in the orderly extrusion of micro-pipe to the culture dish for filling saturation calcium chloride (at room temperature), and placing
It takes out and dries after 30min, obtain modified multiwalled carbon nanotube/Sodium Polyacrylate conduction selfreparing fiber, be denoted as sample 1；
Fig. 1 is macroscopical digital photograph of conductive selfreparing fiber prepared by this example：Wherein (a) is before the fiber blocks
Photo；(b) it is digital photograph after being blocked with scissors；(c) it is photo by pressing lightly on rear fiber selfreparing；(d) it is certainly
The digital photograph after post-tensioning 100% is repaired, from the stretching picture it is found that good mechanical properties after the fiber selfreparing.Fig. 2 is
Conduction selfreparing fiber reset condition manufactured in the present embodiment, block and repair after I-V diagram, it can be seen that：It is prepared by the example
Electric conductivity of the conductive fiber after blocking and repairing and it is original have almost no change, illustrate electric conductivity after fiber selfreparing
Well.
Embodiment 2
(1) at room temperature, multi-walled carbon nanotube 100mg and lauryl sodium sulfate 50mg are weighed respectively, are placed in 100mL's
In beaker, the mixed liquor that deionized water 50mL is made into a concentration of 2mg/mL of multi-walled carbon nanotube is then added, then by mixed liquor
Cell pulverization handles 5h, obtains dispersed modified multiwalled carbon nanotube solution 50mL well；
(2) 500mg Sodium Polyacrylates are added into above-mentioned multi-walled carbon nanotube dispersion liquid, 10h is handled with whirlpool blending instrument,
Form the gelatinous spinning solution of modified multiwalled carbon nanotube/Sodium Polyacrylate；
(3) the gelatinous spinning solution loading 10mL of modified multiwalled carbon nanotube/Sodium Polyacrylate is connected with internal diameter
In syringe for 500 μm of polytetrafluoroethylene (PTFE) micro-pipes, on the propeller that fltting speed is 10mL/h, modified multi-wall carbon nano-tube
Pipe/polyacrylic acid sodium gel is through in the orderly extrusion of micro-pipe to the culture dish for filling saturation calcium chloride (at room temperature), and placing
It is taken out after 30min and dries to obtain modified multiwalled carbon nanotube/Sodium Polyacrylate conduction selfreparing fiber, be denoted as sample 2；
Fig. 3 is the I-V diagram of conductive selfreparing fiber manufactured in the present embodiment, it can be seen that its slope is more than in example 1
The slope of I-V diagram illustrates that the conductivity of conductive selfreparing fiber prepared by the example is more than the fiber prepared in example 1.
Embodiment 3
(1) at room temperature, multi-walled carbon nanotube 150mg and lauryl sodium sulfate 75mg are weighed respectively, are placed in 100mL's
In beaker, the mixed liquor that deionized water 50mL is made into a concentration of 3mg/mL of multi-walled carbon nanotube is then added, then by mixed liquor
Cell pulverization handles 5h, obtains dispersed modified multiwalled carbon nanotube solution 50mL well；
(2) 500mg Sodium Polyacrylates are added into above-mentioned modified multiwalled carbon nanotube dispersion liquid, are handled with whirlpool blending instrument
10h forms the gelatinous spinning solution of modified multiwalled carbon nanotube/Sodium Polyacrylate；
(3) the gelatinous spinning solution loading 10mL of modified multiwalled carbon nanotube/Sodium Polyacrylate is connected with internal diameter
In syringe for 500 μm of polytetrafluoroethylene (PTFE) micro-pipes, on the propeller that fltting speed is 10mL/h, modified multi-wall carbon nano-tube
Pipe/polyacrylic acid sodium gel is through in the orderly extrusion of micro-pipe to the culture dish for filling saturation calcium chloride (at room temperature), and placing
It takes out and dries after 30min, obtain modified multiwalled carbon nanotube/Sodium Polyacrylate conduction selfreparing fiber, be denoted as sample 3；
Fig. 4 is the I-V diagram of conductive selfreparing fiber manufactured in the present embodiment, and it is real to can be seen that it is more than from the slope in figure
Example 1 and 2 corresponding I-V diagram slopes, it may thus be appreciated that：As the multi-walled carbon nanotube/Sodium Polyacrylate composite conducting selfreparing is fine
Content of carbon nanotubes increases in dimension, and the conductivity of the fiber increases.
Claims (3)
1. a kind of preparation method of conduction selfreparing fiber, including：
(1) multi-walled carbon nanotube and lauryl sodium sulfate are dissolved in deionized water, cell pulverization, obtain a concentration of 0.5~
The modified multiwalled carbon nanotube dispersion liquid of 10mg/mL；Wherein, multi-walled carbon nanotube and lauryl sodium sulfate mass ratio be 2~
4:1~4；
(2) Sodium Polyacrylate is added in the modified multiwalled carbon nanotube dispersion liquid in step (1), mixing, it is more obtains modification
Wall carbon nano tube/Sodium Polyacrylate gel spinning solution；Wherein, the mass ratio of multi-walled carbon nanotube and Sodium Polyacrylate is
0.5~10：5~30；
(3) spinning solution in step (2) is subjected to wet spinning, obtains conductive selfreparing fiber；Wherein, the item of wet spinning
Part is：It is placed in coagulating bath to take out after 10~60min and dry；A diameter of 0.3~the 2mm of spinning mouth；Spinning speed is 3~12mL/
h；Wherein coagulating bath is to be saturated calcium chloride solution at room temperature.
2. a kind of preparation method of conductive selfreparing fiber according to claim 1, which is characterized in that the step (1)
The time of middle cell pulverization is 3~7h.
3. a kind of preparation method of conductive selfreparing fiber according to claim 1, which is characterized in that the step (2)
The mode of middle mixing is：The time of whirlpool blending instrument processing is 5~10h.
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| CN110359128B (en) * | 2018-04-09 | 2020-12-25 | 中国科学技术大学 | Fiber material, fiber gel, stretchable conductive composite fiber with superelasticity and frost resistance and preparation method thereof |
| CN109448889A (en) * | 2018-12-05 | 2019-03-08 | 业成科技（成都）有限公司 | Selfreparing conductive structure and preparation method thereof |
| CN114561718B (en) * | 2022-02-28 | 2023-06-16 | 中国科学技术大学 | Composite fiber material, preparation method thereof and high-stretchability fibrous supercapacitor |
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| EP2698457A2 (en) * | 2011-03-15 | 2014-02-19 | IUCF-HYU (Industry-University Cooperation Foundation Hanyang University) | Hybrid polymer composite fiber including graphene and carbon nanotube, and method for manufacturing same |
| CN104894692A (en) * | 2015-06-03 | 2015-09-09 | 东华大学 | Preparation method of high-strength graphene fibers |
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| US20030188879A1 (en) * | 2001-08-08 | 2003-10-09 | Easter Mark R. | Self-healing cables |
| JP4797121B2 (en) * | 2003-04-24 | 2011-10-19 | 三星電子株式会社 | Conductive carbon nanotube / polymer composite |
| KR20060077982A (en) * | 2004-12-30 | 2006-07-05 | 주식회사 효성 | Method of preparing carbon nanotube fibers and fibers prepared by the method |
| US8691178B2 (en) * | 2010-06-03 | 2014-04-08 | The Regents Of The University Of Michigan | Purification of carbon nanotubes using agarose column and density gradient ultracentrifugation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2698457A2 (en) * | 2011-03-15 | 2014-02-19 | IUCF-HYU (Industry-University Cooperation Foundation Hanyang University) | Hybrid polymer composite fiber including graphene and carbon nanotube, and method for manufacturing same |
| CN104894692A (en) * | 2015-06-03 | 2015-09-09 | 东华大学 | Preparation method of high-strength graphene fibers |
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| "基于非共价键的本征型自修复聚合物材料及其应用";龚征宇 等;《高分子通报》;20150415(第4期);第1-11页 * |
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