CN102808327B - Method for preparing nylon-PEDOT (poly(3,4-ethylenedioxythiophene)) compound conductive fabric through in-situ polymerization - Google Patents
Method for preparing nylon-PEDOT (poly(3,4-ethylenedioxythiophene)) compound conductive fabric through in-situ polymerization Download PDFInfo
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- CN102808327B CN102808327B CN201210303170.8A CN201210303170A CN102808327B CN 102808327 B CN102808327 B CN 102808327B CN 201210303170 A CN201210303170 A CN 201210303170A CN 102808327 B CN102808327 B CN 102808327B
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- 239000004744 fabric Substances 0.000 title claims abstract description 64
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 13
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 12
- 150000001875 compounds Chemical class 0.000 title 1
- 229920001778 nylon Polymers 0.000 claims abstract description 42
- 239000004677 Nylon Substances 0.000 claims abstract description 38
- 239000002131 composite material Substances 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims abstract description 13
- 239000004753 textile Substances 0.000 claims abstract description 11
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 229940059939 kayexalate Drugs 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000004900 laundering Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000004043 dyeing Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000007598 dipping method Methods 0.000 abstract 2
- 238000005096 rolling process Methods 0.000 abstract 2
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 229940006186 sodium polystyrene sulfonate Drugs 0.000 abstract 1
- 229920001940 conductive polymer Polymers 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- -1 poly 3,4-ethylenedioxy thiophene Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 241001044369 Amphion Species 0.000 description 1
- 229920000144 PEDOT:PSS Polymers 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明涉及一种原位聚合制备尼龙/PEDOT复合导电织物的方法，包括：（1）将尼龙织物用酸溶液进行预处理，二浸二轧，浸渍时间为5～15min，轧余率60%～90%；（2）将上述尼龙织物浸入含氯化铁、聚苯乙烯磺酸钠和3,4-乙撑二氧噻吩EDOT的混合溶液中，反应温度30-90℃，反应时间1-20h，反应结束后，取出织物，洗涤、烘干，即得。本发明方法结合染整常用的浸轧工艺，使PEDOT快速进入尼龙纤维内部，缩短了反应时间，环境污染较小；应用于纺织品化学传感、生物修复材料、电磁屏蔽材料等方面。The invention relates to a method for preparing nylon/PEDOT composite conductive fabric by in-situ polymerization, including: (1) pretreating the nylon fabric with an acid solution, two dipping and two rolling, the dipping time is 5 to 15 minutes, and the rolling ratio is 60% ~90%; (2) Immerse the above nylon fabric in the mixed solution containing ferric chloride, sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene EDOT, the reaction temperature is 30-90°C, and the reaction time is 1- After 20 hours, after the reaction is over, take out the fabric, wash and dry it. The method of the invention combines the padding process commonly used in dyeing and finishing, so that PEDOT quickly enters the interior of nylon fibers, shortens the reaction time, and causes less environmental pollution; it is applied to textile chemical sensing, bioremediation materials, electromagnetic shielding materials, and the like.
Description
Technical field
The invention belongs to the preparation field of composite conductive fabric, particularly a kind of in-situ polymerization is prepared the method for nylon/PEDOT composite conductive fabric.
Background technology
Conducting polymer composite, because of unique chemistry and chemical property, all has wide practical use in fields such as conductive coating, secondary cell, opto-electronic device, gas sensor and electromagnetic shielding, anti-corrosion of metal and stealth technologies.
Conductive polymer poly 3,4-ethylenedioxy thiophene (being called for short PEDOT), owing to thering is high electrical conductivity, preferably environmental stability and the film transparency and paid close attention to widely, and aspect antistatic coating, photodiode, sensor, also showing wide application prospect, but because the insoluble, not molten of PEDOT makes its processing difficult treatment, thereby limited its business application.
Polystyrolsulfon acid (PSS) thus as adulterant, introducing PEDOT makes the sulphur on thiophene be connected with adulterant, effect due to hydrophilic functional group, what make that PEDOT long-chain can unfold opens, make the PEDOT can be water-soluble by a certain proportion of mixing with PSS, form the PEDOT:PSS aqueous solution that homogeneous disperses, change the valence state of PEDOT simultaneously, and then improved electric conductivity.
Nylon is typical polarity crystalline polymer polymer.In macromolecular main chain repetitive, contain polar group amido link (CONH-).In neutral solution, nylon with amphion structure (
+nH
3-nylon-COO-) exist.Under acid condition, Carboxylic Acid Ions is protonated, and nylon fiber exists with end amido form, and polarity increases, and nylon can adsorb PEDOT-PSS well.
Using textiles as base material, utilize " scene " adsorpting polymerization method, using conducting polymer as conductive covering layer, be adsorbed in matrix fiber surface and can make it possess electric conductivity.The fiber of producing by the method had both had electric conductivity, had again the physical and mechanical properties of matrix fiber, in intelligent textile field, made great progress, and was widely used in the aspects such as textiles chemical sensitisation, bioprosthetic material, electromagnetic shielding material.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that in-situ polymerization is prepared nylon/PEDOT composite conductive fabric, the method is in conjunction with the conventional impregnation technology of dyeing and finishing, make PEDOT enter fast nylon fiber inside, improved the electrical conductivity of composite fabric, and cost is lower, the less pollution to environment; The composite conductive fabric sheet resistance making is 0.20～2.75K Ω/, powerful variation not quite, and there is good antistatic and electro-magnetic screen function.
A kind of in-situ polymerization of the present invention is prepared the method for nylon/PEDOT composite conductive fabric, comprising:
(1) nylon fabrics is carried out to preliminary treatment with acid solution, two soak two rolls, and dip time is 5～15min, pick-up 60%～90%;
(2) above-mentioned nylon fabrics is immersed in the mixed solution of chloride containing iron, kayexalate and 3,4-ethylene dioxythiophene EDOT, reaction temperature is 30-90 ℃, and reaction time 1-20h, after reaction finishes, takes out fabric, and washing, oven dry, obtain; Wherein the concentration of iron chloride is 0.05mol/L-0.3mol/L, and kayexalate concentration is 5-30g/L, and the mol ratio of EDOT and iron chloride is 1:2.
Acid solution in described step (1) is acetic acid, hydrochloric acid or the sulfuric acid of pH value 3-4.
Kayexalate mean molecule quantity 5000-60000 in described step (2).
Fabric washing in described step (2) is specially first and washes away surperficial attachment with deionized water, then uses soaked in absolute ethyl alcohol laundering of textile fabrics colourless to cleaning solution.
Bake out temperature in described step (2) is 40-60 ℃.
In described step (2), nylon/PEDOT composite conductive fabric sheet resistance of gained is 0.20～2.75K Ω/.
beneficial effect
The present invention prepares the method for nylon/PEDOT composite conductive fabric by situ aggregation method, the method in conjunction with dyeing and finishing conventional pad technique, make PEDOT enter fast nylon fiber inside, improved the electrical conductivity of composite fabric, and cost is lower, the less pollution to environment; The composite conductive fabric sheet resistance making can reach 0.20～2.75K Ω/, powerful variation not quite, and there is good anti-flammability, WATER REPELLENCY, antibiotic property, antistatic and electro-magnetic screen function.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
First nylon fabrics is processed with the hydrochloric acid solution of pH=4, two soak two rolls, and dip time is 10min, pick-up 70%; Then the nylon fabrics of processing being immersed to EDOT concentration is 0.1mol/L, and ferric chloride concn is 0.2mol/L, in 20g/L kayexalate solution.Reaction temperature is 70 ℃, reaction time 10h.After reaction finishes, take out fabric.First with deionized water, wash away surperficial attachment, then use soaked in absolute ethyl alcohol laundering of textile fabrics colourless to cleaning solution, 60 ℃ of oven dry, obtain nylon/PEDOT composite conductive fabric.Conductive fabric sheet resistance is 0.20K Ω/.
Embodiment 2
First nylon fabrics is processed with the hydrochloric acid solution of pH=4, two soak two rolls, and dip time is 5min, pick-up 70%; Then the nylon fabrics of processing being immersed to EDOT concentration is 0.1mol/L, and ferric chloride concn is 0.2mol/L, in 15g/L kayexalate solution.Reaction temperature is 70 ℃, reaction time 15h.After reaction finishes, take out fabric.First with deionized water, wash away surperficial attachment, then use soaked in absolute ethyl alcohol laundering of textile fabrics colourless to cleaning solution, 60 ℃ of oven dry, obtain nylon/PEDOT composite conductive fabric.Conductive fabric sheet resistance is 1.89K Ω/.
Embodiment 3
First nylon fabrics is processed with the hydrochloric acid solution of pH=4, two soak two rolls, and dip time is 10min, pick-up 70%; Then the nylon fabrics of processing being immersed to EDOT concentration is 0.1mol/L, and ferric chloride concn is 0.2mol/L, in 20g/L kayexalate solution.Reaction temperature is 60 ℃, reaction time 10h.After reaction finishes, take out fabric.First with deionized water, wash away surperficial attachment, then use soaked in absolute ethyl alcohol laundering of textile fabrics colourless to cleaning solution, 60 ℃ of oven dry, obtain nylon/PEDOT composite conductive fabric.Conductive fabric sheet resistance is 2.75K Ω/.
Embodiment 4
First nylon fabrics is processed with the hydrochloric acid solution of pH=4, two soak two rolls, and dip time is 5min, pick-up 70%; Then the nylon fabrics of processing being immersed to EDOT concentration is 0.1mol/L, and ferric chloride concn is 0.2mol/L, in 10g/L kayexalate solution.Reaction temperature is 70 ℃, reaction time 8h.After reaction finishes, take out fabric.First with deionized water, wash away surperficial attachment, then use soaked in absolute ethyl alcohol laundering of textile fabrics colourless to cleaning solution, 60 ℃ of oven dry, obtain nylon/PEDOT composite conductive fabric.Conductive fabric sheet resistance is 1.35K Ω/.
Embodiment 5
First nylon fabrics is processed with the hydrochloric acid solution of pH=4, two soak two rolls, and dip time is 5min, pick-up 70%; Then the nylon fabrics of processing being immersed to EDOT concentration is 0.20mol/L, and ferric chloride concn is 0.40mol/L, in 10g/L kayexalate solution.Reaction temperature is 70 ℃, reaction time 10h.After reaction finishes, take out fabric.First with deionized water, wash away surperficial attachment, then use soaked in absolute ethyl alcohol laundering of textile fabrics colourless to cleaning solution, 60 ℃ of oven dry, obtain nylon/PEDOT composite conductive fabric.Conductive fabric sheet resistance is 0.99K Ω/.
Claims (6)
1. in-situ polymerization is prepared a method for nylon/PEDOT composite conductive fabric, comprising:
(1) nylon fabrics is carried out to preliminary treatment with acid solution, two soak two rolls, and dip time is 5～15min, and pick-up is 60%～90%;
(2) above-mentioned nylon fabrics is immersed in the mixed solution of chloride containing iron, kayexalate and 3,4-ethylene dioxythiophene EDOT, reaction temperature is 30-90 ℃, and the reaction time is 1-20h, after reaction finishes, takes out fabric, and washing, oven dry, obtain; Wherein the concentration of iron chloride is 0.05mol/L-0.3mol/L, and the concentration of kayexalate is 5-30g/L, and the mol ratio of EDOT and iron chloride is 1:2.
2. a kind of in-situ polymerization according to claim 1 is prepared the method for nylon/PEDOT composite conductive fabric, it is characterized in that: the acid solution in described step (1) is acetic acid, hydrochloric acid or the sulfuric acid of pH value 3-4.
3. a kind of in-situ polymerization according to claim 1 is prepared the method for nylon/PEDOT composite conductive fabric, it is characterized in that: the mean molecule quantity of the kayexalate in described step (2) is 5000-60000.
4. a kind of in-situ polymerization according to claim 1 is prepared the method for nylon/PEDOT composite conductive fabric, it is characterized in that: in described step (2), fabric washing is specially the attachment that first washes away fabric face with deionized water, then uses soaked in absolute ethyl alcohol laundering of textile fabrics colourless to cleaning solution.
5. a kind of in-situ polymerization according to claim 1 is prepared the method for nylon/PEDOT composite conductive fabric, it is characterized in that: the bake out temperature in described step (2) is 40-60 ℃.
6. a kind of in-situ polymerization according to claim 1 is prepared the method for nylon/PEDOT composite conductive fabric, it is characterized in that: in described step (2), nylon/PEDOT composite conductive fabric sheet resistance of gained is 0.20～2.75K Ω/.
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| CN201210303170.8A CN102808327B (en) | 2012-08-23 | 2012-08-23 | Method for preparing nylon-PEDOT (poly(3,4-ethylenedioxythiophene)) compound conductive fabric through in-situ polymerization |
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| CN201210303170.8A CN102808327B (en) | 2012-08-23 | 2012-08-23 | Method for preparing nylon-PEDOT (poly(3,4-ethylenedioxythiophene)) compound conductive fabric through in-situ polymerization |
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| FR3063501A1 (en) * | 2017-03-03 | 2018-09-07 | Association Pour La Recherche Et Le Developpement De Methodes Et Processus Industriels "Armines" | SYNTHESIS OF FIBERS AND ELECTRONIC TEXTILES BASED ON CONDUCTIVE POLYMERS |
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| CN103469578B (en) * | 2013-09-23 | 2015-06-03 | 青岛大学 | Preparation method of ultraviolet-proof anti-electromagnetic radiation textile fabric |
| CN103753926B (en) * | 2014-01-16 | 2016-03-16 | 中科院广州化学有限公司 | Polythiophene conductive coating of a kind of high conductivity and preparation method thereof and application |
| CN106367969A (en) * | 2015-07-22 | 2017-02-01 | 上海工程技术大学 | Polysulfone amide/PEDOT electric conduction composite yarn and preparation method thereof |
| CN107059408B (en) * | 2017-01-13 | 2019-06-11 | 华北科技学院 | A kind of high conductive PEDOT coating material and preparation method thereof |
| CN108193499A (en) * | 2017-12-20 | 2018-06-22 | 苏州禾川化学技术服务有限公司 | A kind of fiber metallizing treatment process |
| CN108589270B (en) * | 2018-05-10 | 2021-06-01 | 武汉纺织大学 | Fiber-based PEDOT:PSS nanoflowers and preparation method and application thereof |
| CN110656497A (en) * | 2019-09-05 | 2020-01-07 | 浙江省检验检疫科学技术研究院 | Preparation method of poly (3, 4-ethylenedioxythiophene)/cotton composite fabric |
| CN113215814A (en) * | 2020-01-21 | 2021-08-06 | 天津工业大学 | Low-temperature interfacial polymerization organic textile thermoelectric material and preparation method thereof |
| CN111809385B (en) * | 2020-07-09 | 2022-08-23 | 吴江福华织造有限公司 | Preparation method of polyamide fabric with lasting antibacterial effect |
| CN112898767A (en) * | 2021-01-25 | 2021-06-04 | 江阴市宏丰塑业有限公司 | High-temperature-resistant antistatic modified polyamide and preparation method thereof |
| CN113417144B (en) * | 2021-05-31 | 2022-05-24 | 苏州大学 | A kind of polythiophene composite nylon conductive fiber and preparation method thereof |
| CN116535707B (en) * | 2023-05-22 | 2024-08-20 | 陕西科技大学 | Ultrathin aramid nanofiber-based electromagnetic shielding composite film and preparation method thereof |
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| CN101704958A (en) * | 2009-10-23 | 2010-05-12 | 北京化工大学 | Method for preparing flexible poly(3,4-ethylenedioxythiophene) composite conductive thin film |
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| JP5256454B2 (en) * | 2006-02-28 | 2013-08-07 | 国立大学法人山梨大学 | Method for treating conductive polymer |
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| CN101704958A (en) * | 2009-10-23 | 2010-05-12 | 北京化工大学 | Method for preparing flexible poly(3,4-ethylenedioxythiophene) composite conductive thin film |
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| 李昕等.聚(3 4-乙撑二氧噻吩)导电织物的制备、结构及其电致变色性能.《高等学校化学学报》.2009 |
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| FR3063501A1 (en) * | 2017-03-03 | 2018-09-07 | Association Pour La Recherche Et Le Developpement De Methodes Et Processus Industriels "Armines" | SYNTHESIS OF FIBERS AND ELECTRONIC TEXTILES BASED ON CONDUCTIVE POLYMERS |
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