CN103046157B - A kind of carbon nano tube/polyurethane/polypropylene conductive fiber and preparation method thereof - Google Patents

A kind of carbon nano tube/polyurethane/polypropylene conductive fiber and preparation method thereof Download PDF

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Publication number
CN103046157B
CN103046157B CN201210564030.6A CN201210564030A CN103046157B CN 103046157 B CN103046157 B CN 103046157B CN 201210564030 A CN201210564030 A CN 201210564030A CN 103046157 B CN103046157 B CN 103046157B
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polyurethane
polypropylene
carbon nano
conductive fiber
cnt
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CN103046157A (en
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潘玮
赵尧敏
张留学
刘红燕
孙亚丽
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Zhongyuan University of Technology
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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
    • D01F6/46—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 polyolefins
    • 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
    • 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
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a kind of carbon nano tube/polyurethane/polypropylene conductive fiber, described conductive fiber is made up of CNT, polyurethane, polypropylene, the mass percent of CNT is 1% ~ 10%, and the mass percent of polyurethane is 9% ~ 40%, and polyacrylic mass percent is 50% ~ 90%.This patent adopts conventional melt spining technology to prepare carbon nano tube/polyurethane/polypropylene conductive fiber, polyurethane and polypropylene are incompatible high polymer, owing to being subject to the effect such as shearing, stretching that continuous phase applies in spinning process, polyurethane forms in-situ micro-fibril in polypropylene matrix; Carboxyl and the polyurethane of the acidified process rear surface of CNT form hydrogen bond, and therefore it is optionally dispersed in polyurethane fento; Make carbon nano-tube/poly ammonia ester fento in polypropylene matrix, form continuous net chain fento conductive channel like this, obtain carbon nano tube/polyurethane/polypropylene conductive fiber.

Description

A kind of carbon nano tube/polyurethane/polypropylene conductive fiber and preparation method thereof
Technical field
The invention belongs to composite fibre and preparation field thereof, particularly a kind of carbon nano-tube/poly ammonia ester/polypropylene composite materials fiber and preparation method thereof.
Background technology
Chemical fibre is since appearance, and with the premium properties that its many natural fabric is incomparable, obtain and develop rapidly, market constantly expands.But simultaneously, producing and also exposing in use procedure an important common feature of their existence, be exactly that hygroscopicity is poor, in use easily produce electrostatic and bring harm to industrial production and people's lives thus, this makes the research of the electric conductivity of synthetic fiber more and more by people are paid close attention to.
The preparation method of conductive fiber has many kinds, and along with deepening continuously of research, according to final performance and the preparation technology of obtained fiber, people have progressively eliminated some preparation methods fallen behind.At present, the method being prepared into conductive fiber mainly contains three kinds; One is make fiber surface form the coat of metal at the textile surface physics such as fiber or chemical method, this method often makes the feel of fiber become thick and stiff due to the coat of metal formed, and be difficult to carry out textile process, and investment of production equipment is large, efficiency is low, and production cost is high; Two is chemically form semiconductor lamella at fiber surface, and chemical method technique is comparatively simple, and little on the physical and mechanical properties impact of fiber, electric conductivity is better, but conduction durability is poor; Three is that electrically conductive particles is mixed in spinning melt; made the conductive fiber of skin-core structure or island structure by composite spinning, Conductivity of Fiber electrical endurance obtained is in this way excellent, and less because adding conducting particles; do not damage the physical property of fiber, be thus subject to extensive concern.But the processing cost of this conductive fiber is higher, technique is also more complicated, this limits the production of conductive fiber to a certain extent, also limit the universal of use, therefore conductive fiber is mainly used in high-tech area at present, and is applied to civilian of less types.
Along with the raising of people's living standard and the enhancing to own health protective awareness, promoting the use of of civilian conductive fiber must become trend, and therefore the processing of conductive fiber should the future development of, low cost simple to technique.For taking for conductive fabric, under the prerequisite of giving fabric electric conductivity, also should Optimization Technology further, to keep original style of textiles, as color and luster, feel, drapability etc., take requirement to meet.The development of nanometer technology and the exploitation of series function nano material and market turn to the multi-functional textiles of development and bring opportunity.The plane being similar to graphite that CNT (CNTs) is made up of carbon hexatomic ring, by the nanoscale tubular structure that certain way is curling.CNT can be divided into again Single Walled Carbon Nanotube (SWNTs) and the large class of multi-walled carbon nano-tubes (MWNTs) two.The obvious quantum effect that CNT (CNTs) occurs under nano-scale, therefore CNT has unique texture and mechanics, electricity and chemical property.The accurate one dimension tracheary element structure of CNT uniqueness causes the interest of physics, chemistry, material science and nanosecond science and technology field scholar.
There are reports in the research of the various CNTs/high polymer conductive fiber using CNT as filler.Polyester, CNT and coupling agent mix by patent 200410033773.6, through to extrude and spinning process is prepared into conductive fiber.Patent CN101250770A utilizes wet spinning technology, uses CNT to carry out quick modification to the acrylic as-spun fibre being still in gel state, obtains antistatic acrylic fiber.Monomer, initator in ionic liquid, are then added wherein polymerization and obtain Polypropylene/Carbon Nanotube Composites stoste, adopt wet spinning or dry-jet wet spinning process to prepare polypropylene/carbon nano tube composite fibre by carbon nanotube dispersed by patent CN101864015A.Patent CN1569939A first by carbon nanotube dispersed in water, then carbon nano-tube aqueous solutions to be mixed with thermoplastic polymer, dry, granulation, is finally spun into conductive fiber.
A current trend uses multi-phase polymer co-mixing system to reduce the content of conductive filler in conduction high polymer, superpolymer blend be separated and inorganic conductive material be optionally distributed to a certain mutually in, the composite of high conductivity can be obtained when conductive agent consumption is lower, reasonable processing characteristics can be provided on the other hand, and effectively reduce the impact of the mechanical performance decline caused because filer content increases.Superpolymer blend be separated and inorganic conductive material to control the distribution of conducting particles in system and arrangement mode be the important channel of conductive fiber obtaining high-performance, low cost, be also the development trend of conductive polymer composite.This patent proposes to utilize configuration control method in blend polymer spinning process, makes decentralized photo original position become fento, and controls conducting particles and be selectively distributed in in-situ micro-fibril, thus the acquisition low cost of simple and effective, high performance conductive fiber.
Summary of the invention
The object of this invention is to provide a kind of preparation method of carbon nano tube/polyurethane/polypropylene conductive fiber.
Conductive fiber provided by the invention, be made up of CNT, polyurethane and polypropylene, the mass percent that CNT accounts for composite fibre is 1% ~ 10%, and polyurethane accounts for 9% ~ 40%, and polypropylene accounts for 50% ~ 90%.
The method of carbon nano tube/polyurethane/polypropylene conductive fiber of the present invention comprises the following steps:
(1) reflux CNT in the strong acid solution of mass fraction 70% ~ 98% 0.5-1.5 hour, dilute with deionized water, filter, and repeatedly rinse with deionized water, gained black solid is placed in vacuum drying oven and is dried to constant weight, obtain carboxylated CNT;
(2) carboxylic carbon nano-tube, polyurethane and polypropylene are put in high-speed mixer, control mixing temperature at 100 DEG C ~ 120 DEG C, mix; At double screw extruder or single screw extrusion machine, in the also system band granulation of 170 DEG C ~ 230 DEG C melt blendings, obtain carbon nano tube/polyurethane/polypropylene conductive section;
(3) conduction section melt spinning method is carried out spinning, obtain carbon nano-tube/poly ammonia ester/polypropylene and to come into being conductive fiber, spinning temperature 190 DEG C ~ 240 DEG C, spinning speed is 200m/min ~ 1000 m/min;
(4) will come into being conductive fiber through 70 DEG C ~ 120 DEG C hot gas spring, drafting multiple is 1.5 ~ 5 times, obtains carbon nano tube/polyurethane/polypropylene conductive fiber.
CNT used in the present invention is at least one in single armed CNT, multi-arm carbon nano-tube.
Strong acid of the present invention is at least one in nitric acid, sulfuric acid.
Described polypropylene is that conventional textile polypropylene fibre is cut into slices.
Described polyurethane is the section of fibre-grade polyurethane.
The invention has the beneficial effects as follows: the present invention adopts conventional melt spining technology to prepare carbon nano tube/polyurethane/polypropylene conductive fiber, polyurethane and polypropylene are incompatible high polymer, owing to being subject to the effect such as shearing, stretching that continuous phase applies in spinning process, polyurethane forms in-situ micro-fibril in polypropylene matrix; Carboxyl and the polyurethane of the acidified process rear surface of CNT form hydrogen bond, and therefore it is optionally dispersed in polyurethane fento; Make carbon nano-tube/poly ammonia ester fento in polypropylene matrix, form continuous net chain fento conductive channel like this, obtain conductive fiber.
This fiber not only have conduction or antistatic behaviour, and due in spinning process polymer flow know from experience make polyurethane fento along fiber axial orientation, thus play fento strengthen effect, greatly can improve the strength and modulus of synthetic fiber.The method is without the need to changing production line and the equipment of original polypropylene fibre, and technical process is easy, produces flexibly.The fiber produced not only has higher electrical conductivity, and has the features such as intensity is high, good hand touch, can meet the requirement of the later process such as weaving completely.With the conductive fiber that above-mentioned material and preparation method obtain, there is good electric conductivity, except can be used as semiconductor devices, electromagnetic shielding material and antistatic material, radar, infrared ray, ultraviolet etc. can also be absorbed, be applied to many special dimensions.
Detailed description of the invention
Embodiment 1
Multi-walled carbon nano-tubes puts into single port flask, 70% red fuming nitric acid (RFNA) is added under vigorous stirring, put into 140 DEG C of constant temperature oil bath backflows to take out after 1 hour, dilute with deionized water, filter, and repeatedly rinse with deionized water, finally gained black solid is placed in vacuum drying oven and is dried to constant weight in 50 DEG C, obtain carboxylated CNT;
Get the carboxylated CNT of 20g, the section of 380g polyurethane and the mixing of 600g polypropylene chip, put in high-speed mixer, control mixing temperature at 110 DEG C, in the also system band granulation of double screw extruder melt blending after mixing.Double screw extruder each district temperature is as follows:
Subregion One district 2nd district 3rd district 4th district 5th district
Temperature (DEG C) 190 200 205 210 220
By compound slice conveniently melt spinning method carry out spinning, drawing-off, spinning temperature 230 DEG C, spinning speed is 800 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 3 times.The mass fraction of this fibrous carbon nanotube is 2%, and the mass fraction of polyurethane is 38%, and polyacrylic mass fraction is 60%.The electrical conductivity of fiber is 10 -9s/cm, intensity is 2.85 cN/dtex.
Embodiment 2
Multi-walled carbon nano-tubes puts into single port flask, nitration mixture (volume ratio of 70% concentrated sulfuric acid and 98% red fuming nitric acid (RFNA) is 3:1) is added under vigorous stirring, put into 120 DEG C of constant temperature oil bath backflows to take out after 1 hour, dilute with deionized water, filter, and repeatedly rinse with deionized water, finally gained black solid is placed in vacuum drying oven and is dried to constant weight in 50 DEG C, obtain carboxylated CNT;
Get the carboxylated CNT of 30g, the section of 300g polyurethane and the mixing of 670g polypropylene chip, put in high-speed mixer, control mixing temperature at 110 DEG C, in the also system band granulation of double screw extruder melt blending after mixing.Double screw extruder each district temperature is as follows:
Subregion One district 2nd district 3rd district 4th district 5th district
Temperature (DEG C) 170 200 205 210 220
By compound slice conveniently melt spinning method carry out spinning, drawing-off, spinning temperature 225 DEG C, spinning speed is 600 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 4 times.The mass fraction of this fibrous carbon nanotube is 3%, and the mass fraction of polyurethane is 30%, and polyacrylic mass fraction is 67%.The electrical conductivity of fiber is 10 -6s/cm, intensity is 3.15 cN/dtex.
Embodiment 3
Multi-walled carbon nano-tubes puts into single port flask, nitration mixture (volume ratio of 70% concentrated sulfuric acid and 98% red fuming nitric acid (RFNA) is 3:1) is added under vigorous stirring, put into 120 DEG C of constant temperature oil bath backflows to take out after 1 hour, dilute with deionized water, filter, and repeatedly rinse with deionized water, finally gained black solid is placed in vacuum drying oven and is dried to constant weight in 50 DEG C, obtain carboxylated CNT;
Get the carboxylated CNT of 50g, the section of 300g polyurethane and the mixing of 650g polypropylene chip, put in high-speed mixer, control mixing temperature at 120 DEG C, in the also system band granulation of double screw extruder melt blending after mixing.Double screw extruder each district temperature is as follows:
Subregion One district 2nd district 3rd district 4th district 5th district
Temperature (DEG C) 190 210 215 215 225
By compound slice conveniently melt spinning method carry out spinning, drawing-off, spinning temperature 235 DEG C, spinning speed is 500 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 4 times.The mass fraction of this fibrous carbon nanotube is 5%, and the mass fraction of polyurethane is 30%, and polyacrylic mass fraction is 65%.The electrical conductivity of fiber is 10 -3s/cm, intensity is 3.26 cN/dtex.
Embodiment 4
Single armed wall carbon nano tube puts into single port flask, 98% concentrated sulfuric acid is added under vigorous stirring, put into 120 DEG C of constant temperature oil bath backflows to take out after 1.5 hours, dilute with deionized water, filter, and repeatedly rinse with deionized water, in vacuum drying oven, be dried to constant weight, obtain carboxylated single armed CNT;
Get the carboxylated single armed CNT of 80g, the section of 320g polyurethane and the mixing of 600g polypropylene chip, put in high-speed mixer, control mixing temperature at 110 DEG C, in the also system band granulation of double screw extruder melt blending after mixing.Double screw extruder each district temperature is as follows:
Subregion One district 2nd district 3rd district 4th district 5th district
Temperature (DEG C) 180 210 215 220 230
By compound slice conveniently melt spinning method carry out spinning, drawing-off, spinning temperature 240 DEG C, spinning speed is 500 m/min, and at 110 DEG C of hot gas spring, drafting multiple is 3.5 times.The mass fraction of this fibrous carbon nanotube is 8%, and the mass fraction of polyurethane is 32%, and the mass fraction of polyurethane is 60%.The electrical conductivity of fiber is 10 -2s/cm, intensity is 2.85 cN/dtex.
Embodiment 5
Multi-walled carbon nano-tubes puts into single port flask, nitration mixture (volume ratio of 70% concentrated sulfuric acid and 98% red fuming nitric acid (RFNA) is 3:1) is added under vigorous stirring, put into 120 DEG C of constant temperature oil bath backflows to take out after 1 hour, dilute with deionized water, filter, and repeatedly rinse with deionized water, finally gained black solid is placed in vacuum drying oven and is dried to constant weight in 50 DEG C, obtain carboxylated CNT;
Get the carboxylated CNT of 55g, the section of 400g polyurethane and the mixing of 545g polypropylene chip, put in high-speed mixer, control mixing temperature at 100 DEG C, in the also system band granulation of double screw extruder melt blending after mixing.Double screw extruder each district temperature is as follows:
Subregion One district 2nd district 3rd district 4th district 5th district
Temperature (DEG C) 170 200 205 215 225
By compound slice conveniently melt spinning method carry out spinning, drawing-off, spinning temperature 225 DEG C, spinning speed is 300 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 4 times.The mass fraction of this fibrous carbon nanotube is 5.5%, and the mass fraction of polyurethane is 40%, and polyacrylic mass fraction is 54.5%.The electrical conductivity of fiber is 10 -4s/cm, intensity is 2.94 cN/dtex.
Embodiment 6
Multi-walled carbon nano-tubes puts into single port flask, 70% red fuming nitric acid (RFNA) is added under vigorous stirring, put into 120 DEG C of constant temperature oil bath backflows to take out after 1 hour, dilute with deionized water, filter, and repeatedly rinse with deionized water, finally gained black solid is placed in vacuum drying oven and is dried to constant weight in 50 DEG C, obtain carboxylated CNT;
Get the carboxylated CNT of 20g, the section of 380g polyurethane and the mixing of 600g polypropylene chip, put in high-speed mixer, control mixing temperature at 110 DEG C, in the also system band granulation of double screw extruder melt blending after mixing.Double screw extruder each district temperature is as follows:
Subregion One district 2nd district 3rd district 4th district 5th district
Temperature (DEG C) 190 200 205 210 220
By compound slice conveniently melt spinning method carry out spinning, drawing-off, spinning temperature 230 DEG C, spinning speed is 800 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 3 times.The mass fraction of this fibrous carbon nanotube is 2%, and the mass fraction of polyurethane is 38%, and polyacrylic mass fraction is 60%.The electrical conductivity of fiber is 10 -9s/cm, intensity is 3.85 cN/dtex.
Embodiment 7
Multi-walled carbon nano-tubes puts into single port flask, 70% red fuming nitric acid (RFNA) is added under vigorous stirring, put into 120 DEG C of constant temperature oil bath backflows to take out after 1 hour, dilute with deionized water, filter, and repeatedly rinse with deionized water, finally gained black solid is placed in vacuum drying oven and is dried to constant weight in 50 DEG C, obtain carboxylated CNT;
Get the carboxylated CNT of 90g, the section of 400g polyurethane and the mixing of 510g polypropylene chip, put in high-speed mixer, control mixing temperature at 110 DEG C, in the also system band granulation of double screw extruder melt blending after mixing.Double screw extruder each district temperature is as follows:
Subregion One district 2nd district 3rd district 4th district 5th district
Temperature (DEG C) 190 200 215 220 230
By compound slice conveniently melt spinning method carry out spinning, drawing-off, spinning temperature 230 DEG C, spinning speed is 300 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 3 times.The mass fraction of this fibrous carbon nanotube is 9%, and the mass fraction of polyurethane is 40%, and polyacrylic mass fraction is 51%.The electrical conductivity of fiber is 10 -3s/cm, intensity is 2.74 cN/dtex.
In above-described embodiment, polypropylene chip is purchased from petrochemical industry, and the trade mark: 71735, melt index is 30 ~ 40g/10min (230 DEG C, 2.16Kg).Single armed CNT purchased from nanometer port, diameter < 2nm, length 5 ~ 15 μm, specific area 500 ~ 700 m 2/ g.Multi-arm carbon nano-tube purchased from nanometer port, diameter <10nm, length 5 ~ 15 μm, specific area 250 ~ 300 m 2/ g.Polyurethane section is fibre-grade, is space elastomer Co., Ltd purchased from Tianjin.

Claims (2)

1. a preparation method for carbon nano tube/polyurethane/polypropylene conductive fiber, is characterized in that its step is as follows:
(1) reflux CNT in the strong acid solution of mass fraction 70% ~ 98% 0.5-1.5 hour, dilute with deionized water, filter, and repeatedly rinse with deionized water, gained black solid is placed in vacuum drying oven and is dried to constant weight, obtain carboxylated CNT;
(2) carboxylic carbon nano-tube, polyurethane and polypropylene are put in high-speed mixer, control mixing temperature at 100 DEG C ~ 120 DEG C, mix; At double screw extruder or single screw extrusion machine, in the also system band granulation of 170 DEG C ~ 230 DEG C melt blendings, obtain carbon nano tube/polyurethane/polypropylene conductive section;
(3) conduction section melt spinning method is carried out spinning, obtain carbon nano-tube/poly ammonia ester/polypropylene and to come into being conductive fiber, spinning temperature 190 DEG C ~ 240 DEG C, spinning speed is 200m/min ~ 1000 m/min;
(4) will come into being conductive fiber through 70 DEG C ~ 120 DEG C hot gas spring, drafting multiple is 1.5 ~ 5 times, obtains carbon nano tube/polyurethane/polypropylene conductive fiber.
2. the preparation method of carbon nano tube/polyurethane/polypropylene conductive fiber according to claim 1, is characterized in that: described strong acid is at least one in nitric acid, sulfuric acid.
CN201210564030.6A 2012-12-24 2012-12-24 A kind of carbon nano tube/polyurethane/polypropylene conductive fiber and preparation method thereof Expired - Fee Related CN103046157B (en)

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CN106012093B (en) * 2016-05-23 2018-02-06 湖北华强科技有限责任公司 A kind of preparation method of composite conducting fiber
CN106868614A (en) * 2017-01-10 2017-06-20 烟台泰和新材料股份有限公司 A kind of conductive spandex fibre and preparation method thereof
CN107877893B (en) * 2017-11-24 2019-11-22 河南工程学院 A kind of preparation method being electromagnetically shielded PP film
CN109487367A (en) * 2018-11-15 2019-03-19 杨兴贵 A kind of polypropylene fiber silk band and preparation method thereof
CN110523142B (en) * 2019-08-23 2023-04-18 天津工业大学 Bark-imitated polypropylene/polycarbonate nanofiber melt-blown air filter material and preparation method thereof
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