CN103255502B - A kind of preparation method of the light composite conducting fiber containing nano ATO - Google Patents
A kind of preparation method of the light composite conducting fiber containing nano ATO Download PDFInfo
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- CN103255502B CN103255502B CN201310194460.8A CN201310194460A CN103255502B CN 103255502 B CN103255502 B CN 103255502B CN 201310194460 A CN201310194460 A CN 201310194460A CN 103255502 B CN103255502 B CN 103255502B
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Abstract
The invention discloses a kind of preparation method of the light composite conducting fiber containing nano ATO, its step is as follows: nano ATO and silane coupler are stirred rear drying by (1) in organic solvent, obtain hydride modified nano ATO; (2) hydride modified nano ATO, polypropylene chip, poliester chip mix after carrying out vacuumize respectively, melt spinning, spinning temperature 260-300 DEG C, and spinning speed is 200-1000 m/min, obtain nascent conductive fiber; (3) by nascent conductive fiber just hot gas spring under the condition of 70 DEG C-120 DEG C, drafting multiple is 1.5-4 times, obtains the preparation method of the light composite conducting fiber containing nano ATO.The present invention utilizes 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 composite conducting fiber.
Description
Technical field
The invention belongs to composite fibre and preparation field thereof, particularly one is containing nano ATO light color composite conducting fiber and preparation method thereof.
Background technology
Synthetic fiber, compared with natural fabric, have the advantages such as intensity is high, wear-resisting, are widely used in every field.In processing or use procedure, easily produce electrostatic due to friction, when the electrostatic gathered is higher than 500V, spark can be produced, cause fire because of electric discharge, during higher than 8000V, then can produce shock phenomenon.Therefore, since synthetic fiber come out, people are just devoted to each research about antistatic aspect always.Especially nearly ten years, the progress of polymer chemistry Application Areas developmental research, all makes some progress in raising antistatic behaviour and durability.
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; it is make fiber surface form the coat of metal at the textile surface physics such as fiber or chemical method that the method being prepared into conductive fiber mainly contains three kinds: one; this method due to formed the coat of metal often make the feel of fiber become thick and stiff; 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 when adopting this technique to prepare antistatic fibre, usual used conductive filler particles size mostly is a μm level, does not have the characteristic of nano material, and in molding process, often increases the weight of the loss of equipment, be unfavorable for reducing production cost.Meanwhile, because the antistatic additive of major part itself is with color, cause aft-loaded airfoil (the when especially dyeing) difficulty of fiber.Therefore, development cost conductive fiber that is low, function admirable just seems particularly important.
Nanometer antimony-doped stannic oxide (Antimony Doped Tin Oxide is called for short ATO) is a kind of N-type semiconductor material.Compared with traditional anti-static material, nano ATO conductive powder body has obvious advantage, is mainly manifested in good electric conductivity, light-coloured transparent, good weatherability and the aspect such as stability and low infrared emittance are the extremely potential Multifunction conductive materials of one.Under many application conditions, the color of conductive fiber and transparency be there are certain requirements, the conventional conductive such as carbon black and metal filler then inevitably have impact on the quality of final products, the light-coloured transparent feature of nanosize metal oxide powder just in time fills up this blank, can obtain the conductive fiber of light color, the high grade of transparency.
There is researcher in recent years by nano ATO conducting powder for the preparation of antistatic fibre, as CN186991A adopts nano-powder ATO powder to be antistatic additive, with polymine (PEI) for dispersant, nano ATO stable and uniform is scattered in deionized water, and using the pre-heating bath of this suspension as polyacrylonitrile fibre spinning process, improve the antistatic behaviour of fiber, this method added in the later stage of spinning process, there is the problem that conducting function is lasting not.Patent CN1765951A discloses a kind of antistatic terylene nanometer composite material and preparation method thereof, for raw material with phthalic acid, ethylene glycol, nano ATO, catalyst and stabilizing agent, the method of In-situ reaction polymerization is adopted to obtain, this method nano ATO can be dispersed, antistatic property is lasting, but complex technical process.A kind of conducting fibre master batch and preparation method thereof disclosed in patent CN101085845A, this conductive agglomerate take polypropylene as matrix, take ATO as conductive agent, melt blending granulation is adopted to obtain, this preparation method's technique is simply with low cost, but need the conductive powder body adding more than 18%, the excessive various performances that will affect matrix material itself of conductive powder body addition.
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.
Summary of the invention
The object of this invention is to provide a kind of preparation method of the light composite conducting fiber containing nano ATO.
Containing a preparation method for the light composite conducting fiber of nano ATO, its step is as follows:
(1) nano ATO and silane coupler are stirred rear drying in organic solvent, the quality of silane coupler is the 0.5-4% of nano ATO quality, and the ratio of silane coupler and organic solvent is 1g:10-30ml, obtains hydride modified nano ATO;
(2) hydride modified nano ATO, polypropylene chip, poliester chip mix after carrying out vacuumize respectively, the mass fraction of hydride modified nano ATO is 5-15%, the mass fraction of polyethylene terephthalate is 20-35%, surplus is polypropylene, melt spinning, spinning temperature 260-300 DEG C, spinning speed is 200-1000 m/min, obtains nascent conductive fiber;
(3) by nascent conductive fiber just hot gas spring under the condition of 70-120 DEG C, drafting multiple is 1.5-4 times, obtains the preparation method of the light composite conducting fiber containing nano ATO.
Silane coupler in described step (1) is KH550, KH560 or KH570.
Organic solvent in described step (1) is ethanol, ethylene glycol, chloroform, oxolane or acetone.
The invention has the beneficial effects as follows: the present invention adopts conventional melt spining technology to prepare nano ATO// polyethylene terephthalate/polypropylene conductive fiber, polyethylene terephthalate and polypropylene are incompatible high polymer, owing to being subject to the effect such as shearing, stretching that continuous phase applies in spinning process, polyethylene terephthalate forms in-situ micro-fibril in polypropylene matrix; Nano ATO is optionally dispersed in polyethylene terephthalate fento; Nano ATO// polyethylene terephthalate fento forms continuous net chain fento conductive channel in polypropylene matrix, obtains composite conducting fiber.This method can keep the physical and mechanical properties of matrix material itself while of reducing conductive filler content, the raising electric conductivity of material.To equipment without particular/special requirement.Simultaneously this patent provide the process route economy preparing conductive fiber, easy, can suitability for industrialized production.
The present invention utilizes 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 composite conducting fiber.Can improve the adding of nano ATO that PP/PET two is alternate answers compatibility, the dispersion size of PET in PP be reduced, is more evenly distributed, improves fiber spinnability.The present invention selects light color nanometer ATO conducting powder as conductive agent, be easy to dyeing, at civilian clothes, interior decoration, carpet, household textiles and have more wide application prospect in microelectronics, medicine (containing aseptic, cleanness clothing), food, precision instrument, biotechnology field.
Detailed description of the invention
Embodiment 1
Nano ATO is placed in together with KH570 ethanol and stirs rear drying, obtain the nano ATO of coupling agent treatment.KH570 consumption is 1% of composite nano ATO quality, and every 1g coupling agent uses ethanol 20ml.Get nano ATO that 50g coupling agent treatment crosses, 350gPET section and 600g polypropylene chip to mix after vacuumize respectively, conveniently melt spinning method carries out spinning, drawing-off.Spinning temperature 270 DEG C, spinning speed is 500 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 3 times.In this fiber, the mass fraction of the mass fraction of nano ATO to be the mass fraction of 5%, PET be 35%, PP is 60%.The electrical conductivity of fiber is 10
-8s/cm, intensity is 3.05 cN/dtex.
Embodiment 2
Nano ATO is placed in together with KH570 ethanol and stirs rear drying, obtain the nano ATO of coupling agent treatment.KH570 consumption is 1% of composite nano ATO quality, and every 1g coupling agent uses ethanol 20ml.Get nano ATO that 100g coupling agent treatment crosses, 300gPET section and 600g polypropylene chip to mix after vacuumize respectively, conveniently melt spinning method carries out spinning, drawing-off.Spinning temperature 270 DEG C, spinning speed is 500 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 3 times.In this fiber, the mass fraction of the mass fraction of nano ATO to be the mass fraction of 10%, PET be 30%, PP is 60%.The electrical conductivity of fiber is 10
-6s/cm, intensity is 2.89 cN/dtex.
Embodiment 3
Nano ATO is placed in together with KH560 ethanol and stirs rear drying, obtain the nano ATO of coupling agent treatment.KH570 consumption is 2% of composite nano ATO quality, and every 1g coupling agent uses acetone 15ml.Get nano ATO that 150g coupling agent treatment crosses, 250gPET section and 600g polypropylene chip to mix after vacuumize respectively, conveniently melt spinning method carries out spinning, drawing-off.Spinning temperature 280 DEG C, spinning speed is 400 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 2.5 times.In this fiber, the mass fraction of the mass fraction of nano ATO to be the mass fraction of 15%, PET be 25%, PP is 60%.The electrical conductivity of fiber is 10
-4s/cm, intensity is 2.70 cN/dtex.
Embodiment 4
Nano ATO is placed in together with KH560 ethanol and stirs rear drying, obtain the nano ATO of coupling agent treatment.KH560 consumption is 2% of composite nano ATO quality, and every 1g coupling agent uses acetone 30ml.Get nano ATO that 100g coupling agent treatment crosses, 200gPET section and 700g polypropylene chip to mix after vacuumize respectively, conveniently melt spinning method carries out spinning, drawing-off.Spinning temperature 270 DEG C, spinning speed is 800 m/min, and at 100 DEG C of hot gas spring, drafting multiple is 3.5 times.In this fiber, the mass fraction of the mass fraction of nano ATO to be the mass fraction of 10%, PET be 20%, PP is 70%.The electrical conductivity of fiber is 10
-6s/cm, intensity is 3.14 cN/dtex.
Embodiment 5
Nano ATO is placed in together with KH560 ethanol and stirs rear drying, obtain the nano ATO of coupling agent treatment.KH560 consumption is 1% of composite nano ATO quality, and every 1g coupling agent uses acetone 15ml.Get nano ATO that 50g coupling agent treatment crosses, 200gPET section and 750g polypropylene chip to mix after vacuumize respectively, conveniently melt spinning method carries out spinning, drawing-off.Spinning temperature 270 DEG C, spinning speed is 900 m/min, and at 110 DEG C of hot gas spring, drafting multiple is 4.5 times.In this fiber, the mass fraction of the mass fraction of nano ATO to be the mass fraction of 5%, PET be 20%, PP is 75%.The electrical conductivity of fiber is 10
-9s/cm, intensity is 3.36 cN/dtex.
Embodiment 6
Nano ATO is placed in together with KH560 ethanol and stirs rear drying, obtain the nano ATO of coupling agent treatment.KH560 consumption is 2% of composite nano ATO quality, and every 1g coupling agent uses acetone 20ml.Get nano ATO that 80g coupling agent treatment crosses, 300gPET section and 620g polypropylene chip to mix after vacuumize respectively, conveniently melt spinning method carries out spinning, drawing-off.Spinning temperature 280 DEG C, spinning speed is 600 m/min, and at 110 DEG C of hot gas spring, drafting multiple is 3 times.In this fiber, the mass fraction of the mass fraction of nano ATO to be the mass fraction of 8%, PET be 30%, PP is 62%.The electrical conductivity of fiber is 10
-6s/cm, intensity is 2.93 cN/dtex.
Embodiment 7
Nano ATO is placed in together with KH570 ethanol and stirs rear drying, obtain the nano ATO of coupling agent treatment.KH570 consumption is 2% of composite nano ATO quality, and every 1g coupling agent uses acetone 20ml.Get nano ATO that 120g coupling agent treatment crosses, 200gPET section and 680gPP to cut into slices after vacuumize respectively and mix, conveniently melt spinning method carries out spinning, drawing-off.Spinning temperature 280 DEG C, spinning speed is 800 m/min, and at 90 DEG C of hot gas spring, drafting multiple is 4.5 times.In this fiber, the mass fraction of the mass fraction of nano ATO to be the mass fraction of 12%, PET be 20%, PP is 68%.The electrical conductivity of fiber is 10
-7s/cm, intensity is 2.98 cN/dtex.
Embodiment 8
Containing a preparation method for the light composite conducting fiber of nano ATO, its step is as follows:
(1) dry after nano ATO and Silane coupling agent KH550 being stirred in organic solvent ethanol, the quality of silane coupler is 0.5% of nano ATO quality, and the ratio of silane coupler and organic solvent is 1g:10ml, obtains hydride modified nano ATO;
(2) hydride modified nano ATO, polypropylene chip, poliester chip mix after carrying out vacuumize respectively, the mass fraction of hydride modified nano ATO is 5%, the mass fraction of polyethylene terephthalate is 20%, surplus is polypropylene, melt spinning, spinning temperature 260 DEG C, spinning speed is 200 m/min, obtains nascent conductive fiber;
(3) by nascent conductive fiber just hot gas spring under the condition of 70 DEG C, drafting multiple is 1.5 times, obtains the preparation method of the light composite conducting fiber containing nano ATO.
Embodiment 9
Containing a preparation method for the light composite conducting fiber of nano ATO, its step is as follows:
(1) dry after nano ATO and silane coupler KH570 being stirred in organic solvent tetrahydrofuran, the quality of silane coupler is 4% of nano ATO quality, and the ratio of silane coupler and organic solvent is 1g:30ml, obtains hydride modified nano ATO;
(2) hydride modified nano ATO, polypropylene chip, poliester chip mix after carrying out vacuumize respectively, the mass fraction of hydride modified nano ATO is 15%, the mass fraction of polyethylene terephthalate is 35%, surplus is polypropylene, melt spinning, spinning temperature 300 DEG C, spinning speed is 1000 m/min, obtains nascent conductive fiber;
(3) by nascent conductive fiber just hot gas spring under the condition of 120 DEG C, drafting multiple is 4 times, obtains the preparation method of the light composite conducting fiber containing nano ATO.
Embodiment 10
Containing a preparation method for the light composite conducting fiber of nano ATO, its step is as follows:
(1) dry after nano ATO and silane coupler KH560 being stirred in organic solvent-acetone, the quality of silane coupler is 2% of nano ATO quality, and the ratio of silane coupler and organic solvent is 1g:20ml, obtains hydride modified nano ATO;
(2) hydride modified nano ATO, polypropylene chip, poliester chip mix after carrying out vacuumize respectively, the mass fraction of hydride modified nano ATO is 10%, the mass fraction of polyethylene terephthalate is 30%, surplus is polypropylene, melt spinning, spinning temperature 280 DEG C, spinning speed is 500 m/min, obtains nascent conductive fiber;
(3) by nascent conductive fiber just hot gas spring under the condition of 100 DEG C, drafting multiple is 2 times, obtains the preparation method of the light composite conducting fiber containing nano ATO.
In above-described embodiment, polypropylene chip purchased from oil of SPC limited company, fibre-grade, melt index: 16g/10min (230 DEG C, 2.16Kg); Poliester chip purchased from Jiangsu Hengli Chemical Fiber Co., Ltd., fibre-grade, inherent viscosity: 0.678(d1/g); Nano ATO purchased from Shanghai Huzheng Nano-Tech Co., Ltd., SnO
2: Sb
2o
3=95:5.
Claims (2)
1., containing a preparation method for the light composite conducting fiber of nano ATO, it is characterized in that, its step is as follows:
(1) nano ATO and silane coupler are stirred rear drying in organic solvent, the quality of silane coupler is the 0.5-4% of nano ATO quality, the ratio of silane coupler and organic solvent is 1g:10-30ml, obtain hydride modified nano ATO, described silane coupler is KH550, KH560 or KH570;
(2) hydride modified nano ATO, polypropylene chip, poliester chip mix after carrying out vacuumize respectively, the mass fraction of hydride modified nano ATO is 5-15%, the mass fraction of polyethylene terephthalate is 20-35%, surplus is polypropylene, melt spinning, spinning temperature 260-300 DEG C, spinning speed is 200-1000 m/min, obtains nascent conductive fiber;
(3) by nascent conductive fiber just hot gas spring under the condition of 70-120 DEG C, drafting multiple is 1.5-4 times, obtains the preparation method of the light composite conducting fiber containing nano ATO.
2. the preparation method of the light composite conducting fiber containing nano ATO according to claim 1, is characterized in that: the organic solvent in described step (1) is ethanol, ethylene glycol, chloroform, oxolane or acetone.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103966691B (en) * | 2014-04-29 | 2016-04-13 | 中原工学院 | A kind of preparation method of nano ATO/cellulose diacetate composite conducting fiber |
| CN104593890B (en) * | 2015-02-06 | 2017-02-01 | 江苏盛虹科技股份有限公司 | Attapulgite hybrid conductive fibers and preparation method thereof |
| CN105063794B (en) * | 2015-09-02 | 2018-04-24 | 四川大学 | The method for promoting the dispersed phase in incompatible polymer blend to form stable fibers |
| CN115012056B (en) * | 2022-06-30 | 2023-09-26 | 江南大学 | Polyamide 56 antistatic fiber and preparation method thereof |
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