CN116716732A - Functionalized terpolymer dispersion liquid and application thereof in textiles - Google Patents
Functionalized terpolymer dispersion liquid and application thereof in textiles Download PDFInfo
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- D—TEXTILES; PAPER
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
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- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
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- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
Description
技术领域Technical field
本发明涉及一种功能化的三元共聚物分散液及其在纺织品中的应用，属于功能材料领域。The invention relates to a functionalized terpolymer dispersion and its application in textiles, and belongs to the field of functional materials.
背景技术Background technique
随着社会的发展和人们生活水平的提高，人们对纺织品的功能化需求越来越多，要求也越来越高。而纤维、纱线和纺织品自身一般不具有功能性，要实现其功能，需要将功能材料引入到纤维、纱线和纺织品中，后处理是一种最直接有效的方式。With the development of society and the improvement of people's living standards, people have more and more functional needs for textiles, and their requirements are getting higher and higher. Fibers, yarns and textiles themselves generally do not have functionality. To realize their functions, functional materials need to be introduced into fibers, yarns and textiles. Post-processing is the most direct and effective way.
然而，功能材料一般为不溶不熔的无机或金属微/纳米填料，由于其直径小、比表面积大，易团聚，在溶剂中难以形成均匀的分散液，一般要用偶联剂等小分子物质对其进行表面化学处理，才能实现微/纳米功能填料在溶剂中的均匀分散。而且，功能材料和基材进行结合的时候还需要加入粘合剂，以实现功能填料与纤维、纱线或纺织品的结合，进一步增加了纤维、纱线和纺织品功能化的复杂性。However, functional materials are generally insoluble and infusible inorganic or metallic micro/nano fillers. Due to their small diameter and large specific surface area, they are easy to agglomerate and are difficult to form a uniform dispersion in solvents. Generally, small molecular substances such as coupling agents are used. Only through surface chemical treatment can the uniform dispersion of micro/nano functional fillers in the solvent be achieved. Moreover, when combining functional materials with substrates, adhesives need to be added to achieve the combination of functional fillers with fibers, yarns or textiles, further increasing the complexity of functionalization of fibers, yarns and textiles.
因此，寻找一种简单有效的方法，实现纤维、纱线和纺织品的功能化至关重要。Therefore, it is crucial to find a simple and effective method to functionalize fibers, yarns and textiles.
发明内容Contents of the invention
[技术问题][technical problem]
功能填料的分散通常需要添加分散剂，或者进行改性，才能实现分散。The dispersion of functional fillers usually requires the addition of dispersants or modification to achieve dispersion.
常规功能材料和基材进行结合需要粘合剂。Adhesives are required to bond conventional functional materials to substrates.
[技术方案][Technical solutions]
为了解决上述问题，本发明在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中添加功能填料制备得到了功能化的三元共聚物分散液；之后将其用于纺织品的功能整理，实现了功能纺织品的制备。本发明通过四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物实现了对于功能材料的良好分散，省略了分散剂添加以及改性的步骤；将其用于纺织品的功能整理不需要粘合剂，工艺更为简单。In order to solve the above problems, the present invention adds functional fillers to the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution to prepare a functionalized terpolymer dispersion; which is then used for functional finishing of textiles , realizing the preparation of functional textiles. The present invention achieves good dispersion of functional materials through the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer, omitting the steps of adding a dispersant and modifying it; using it for functional finishing of textiles does not require adhesion agent, the process is simpler.
本发明的第一个目的是提供一种制备功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液的方法，包括如下步骤：The first object of the present invention is to provide a method for preparing a functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion, which includes the following steps:
(1)将四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物和溶剂搅拌混合均匀，得到四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液；(1) Stir and mix the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer and the solvent evenly to obtain a tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution;
(2)在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中添加功能填料，搅拌，再超声振荡，得到所述的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液。(2) Add functional fillers to the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution, stir, and then ultrasonic oscillate to obtain the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution. Metacopolymer dispersion.
在本发明的一种实施方式中，步骤(1)所述的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物中氟含量小于70％；四氟乙烯、六氟丙烯和偏氟乙烯结构单元的重量百分比分别为45.8％、18.5％和35.7％。In one embodiment of the present invention, the fluorine content in the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer described in step (1) is less than 70%; tetrafluoroethylene, hexafluoropropylene and vinylidene fluoride The weight percentages of structural units are 45.8%, 18.5% and 35.7% respectively.
在本发明的一种实施方式中，步骤(1)所述的搅拌是磁力搅拌，具体是20℃-70℃下磁力搅拌10min-120min。In one embodiment of the present invention, the stirring in step (1) is magnetic stirring, specifically magnetic stirring at 20°C-70°C for 10min-120min.
在本发明的一种实施方式中，步骤(1)所述的溶剂为乙酸乙酯、丙酮、丁酮、四氢呋喃、二氯甲烷、三氯甲烷、1,4-二氧六环、N,N-二甲基甲酰胺和N,N-二甲基乙酰胺中的一种。In one embodiment of the present invention, the solvent described in step (1) is ethyl acetate, acetone, butanone, tetrahydrofuran, dichloromethane, chloroform, 1,4-dioxane, N,N -One of dimethylformamide and N,N-dimethylacetamide.
在本发明的一种实施方式中，步骤(1)所述的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液的浓度为5-200mg/mL。In one embodiment of the present invention, the concentration of the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution in step (1) is 5-200 mg/mL.
在本发明的一种实施方式中，步骤(2)所述的功能填料为市面上现有的不溶不熔的微/纳米粒子，具体包括炭黑、单壁碳纳米管、多壁碳纳米管、石墨烯、气相纳米碳纤维、硫化铜、硫化亚铜、碘化亚铜、光致变色微胶囊、相变微胶囊、银粉、银纳米线、氧化锌、二氧化钛、钒粉、铪粉、镁粉、锰粉、锆粉、铟粉、铬粉、铅粉、铋粉、锡粉、铌粉、钽粉、钛粉、钼粉、钨粉、镍粉、铝粉、铜粉、锌粉、铁粉、钴粉、镍粉、钨粉、钼粉、钛粉、钽粉、二氧化钒、氧化铟锡、氧化锡锑、氧化钨、氧化铋、氧化钼、氧化钴、氧化锡、氧化镁、四氧化三铁、氧化铁、氧化镍、氧化锆、氧化铝、氧化铜、二氧化硅、碳氮化钛、碳氮化铝、碳化铪、碳化钼、碳化铌、碳化钽、碳化钒、碳化铬、碳化钨、碳化硼、碳化锆、碳化钛、碳化硅、氮化镁、氮化铬、氮化锆、氮化硅、氮化硼、氮化钛、氮化铝、二硫化钼、二硫化钨、硼化硅、二硼化铪、六硼化钙、二硼化钛、六硼化镧、二硼化锆、硼粉、二硅化铪、二硅化锆、二硅化钼、氢化铪、氢化钛、氢化锆、氧化镝、氧化镨、氧化钕、氧化钆、氧化镧、氧化钐、氧化铈、氧化钇、MXene、纤维素纳米晶、甲壳素纳米晶、半导体量子点、钙钛矿量子点、富勒烯、碳点中的一种或几种。In one embodiment of the present invention, the functional filler in step (2) is an insoluble and infusible micro/nanoparticle currently available on the market, specifically including carbon black, single-walled carbon nanotubes, and multi-walled carbon nanotubes. , graphene, gas phase nanocarbon fiber, copper sulfide, cuprous sulfide, cuprous iodide, photochromic microcapsules, phase change microcapsules, silver powder, silver nanowires, zinc oxide, titanium dioxide, vanadium powder, hafnium powder, magnesium powder , manganese powder, zirconium powder, indium powder, chromium powder, lead powder, bismuth powder, tin powder, niobium powder, tantalum powder, titanium powder, molybdenum powder, tungsten powder, nickel powder, aluminum powder, copper powder, zinc powder, iron Powder, cobalt powder, nickel powder, tungsten powder, molybdenum powder, titanium powder, tantalum powder, vanadium dioxide, indium tin oxide, tin antimony oxide, tungsten oxide, bismuth oxide, molybdenum oxide, cobalt oxide, tin oxide, magnesium oxide, Iron tetroxide, iron oxide, nickel oxide, zirconium oxide, aluminum oxide, copper oxide, silicon dioxide, titanium carbonitride, aluminum carbonitride, hafnium carbide, molybdenum carbide, niobium carbide, tantalum carbide, vanadium carbide, carbide Chromium, tungsten carbide, boron carbide, zirconium carbide, titanium carbide, silicon carbide, magnesium nitride, chromium nitride, zirconium nitride, silicon nitride, boron nitride, titanium nitride, aluminum nitride, molybdenum disulfide, Tungsten sulfide, silicon boride, hafnium diboride, calcium hexaboride, titanium diboride, lanthanum hexaboride, zirconium diboride, boron powder, hafnium disilicide, zirconium disilicide, molybdenum disilicide, hafnium hydride, Titanium hydride, zirconium hydride, dysprosium oxide, praseodymium oxide, neodymium oxide, gadolinium oxide, lanthanum oxide, samarium oxide, cerium oxide, yttrium oxide, MXene, cellulose nanocrystals, chitin nanocrystals, semiconductor quantum dots, perovskite quantum dots One or more of dots, fullerenes, and carbon dots.
在本发明的一种实施方式中，步骤(2)所述的搅拌是磁力搅拌，具体是20-30℃下磁力搅拌10min-30min；超声振荡的时间为20min-180min。In one embodiment of the present invention, the stirring in step (2) is magnetic stirring, specifically magnetic stirring at 20-30°C for 10 min-30 min; the ultrasonic oscillation time is 20 min-180 min.
在本发明的一种实施方式中，步骤(2)所述的功能填料的粒径为5nm-5μm。In one embodiment of the present invention, the particle size of the functional filler in step (2) is 5 nm-5 μm.
在本发明的一种实施方式中，步骤(2)所述的功能填料在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中的浓度为0.05-30mg/mL。In one embodiment of the present invention, the concentration of the functional filler in step (2) in the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution is 0.05-30 mg/mL.
本发明的第二个目的是本发明所述的方法制备得到的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液。The second object of the present invention is the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion prepared by the method of the present invention.
本发明的第三个目的是提供一种基于本发明所述的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液制备功能化纺织品的方法，包括如下步骤：The third object of the present invention is to provide a method for preparing functional textiles based on the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion of the present invention, which includes the following steps:
将纺织品置于功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液中，在20-30℃下超声处理0.5-8min，取出，干燥，得到功能化纺织品。The textile is placed in the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion, ultrasonic treated at 20-30°C for 0.5-8 minutes, taken out, and dried to obtain functionalized textiles.
在本发明的一种实施方式中，所述的纺织品包括纤维、纱线、织物，具体包括涤纶、丙纶、维纶、腈纶、尼龙6、尼龙66、尼龙11、尼龙56、尼龙12、氯纶、聚乳酸纤维、聚对苯二甲酸丙二醇酯纤维、聚对苯二甲酸丁二醇酯纤维、聚对苯二甲酸丁二醇酯纤维、聚丁二酸丁二醇酯纤维、超高分子量聚乙烯纤维、芳纶1313、芳纶1414、聚酰亚胺纤维及其混纺的纱线、织物；织物包括针织物、机织物和非织造材料。In one embodiment of the present invention, the textiles include fibers, yarns, and fabrics, specifically including polyester, polypropylene, vinylon, acrylic, nylon 6, nylon 66, nylon 11, nylon 56, nylon 12, polyvinyl chloride, Polylactic acid fiber, polytrimethylene terephthalate fiber, polybutylene terephthalate fiber, polybutylene terephthalate fiber, polybutylene succinate fiber, ultra-high molecular weight polyethylene Fiber, aramid 1313, aramid 1414, polyimide fiber and its blended yarns and fabrics; fabrics include knitted fabrics, woven fabrics and non-woven materials.
在本发明的一种实施方式中，将纺织品置于功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液中是分散液能淹没纺织品即可。In one embodiment of the present invention, the textile is placed in the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion so that the dispersion can submerge the textile.
本发明的第四个目的是本发明所述的方法制备得到的功能化纺织品。The fourth object of the present invention is the functionalized textile prepared by the method of the present invention.
本发明的第五个目的是本发明所述的功能化纺织品在制备工业化纺织品中的应用。The fifth object of the present invention is the application of the functionalized textiles of the present invention in the preparation of industrial textiles.
[有益效果][beneficial effect]
(1)本发明采用的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物为含氟聚合物，当氟含量小于70％时，能溶于有机溶剂，且能够使不溶不熔的微/纳米粒子均匀地分散在溶剂中。(1) The tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer used in the present invention is a fluorine-containing polymer. When the fluorine content is less than 70%, it can be dissolved in organic solvents and can make insoluble and infusible microorganisms /Nanoparticles are evenly dispersed in the solvent.
(2)本发明采用的四氟乙烯结构单元含量较低的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物，对纤维及其制品具有较好的黏附性，因此，四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物可以作为粘合剂，和纺织品结合牢固，以增加纺织品的耐久性。(2) The tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer used in the present invention, which has a lower content of tetrafluoroethylene structural units, has good adhesion to fibers and their products. Therefore, tetrafluoroethylene- Hexafluoropropylene-vinylidene fluoride terpolymer can be used as an adhesive to bond firmly with textiles to increase the durability of textiles.
(3)本发明采用的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物为含氟聚合物，具有疏水性和阻燃性，除了能作为分散剂和粘合剂，还能增加纺织品的疏水性，降低其可燃性，特别在实现纺织品疏水性方面具有较好的效果。(3) The tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer used in the present invention is a fluorine-containing polymer, which is hydrophobic and flame retardant. In addition to being used as a dispersant and adhesive, it can also be added to textiles. It has good hydrophobicity and reduces its flammability, especially in achieving hydrophobicity of textiles.
(4)本发明采用的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物具有较好的弹性，经四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液处理后的纺织品回弹性不会降低。(4) The tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer used in the present invention has good elasticity. The textiles treated with the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution will return Elasticity will not be reduced.
具体实施方式Detailed ways
以下对本发明的优选实施例进行说明，应当理解实施例是为了更好地解释本发明，不用于限制本发明。Preferred embodiments of the present invention are described below. It should be understood that the embodiments are for the purpose of better explaining the present invention and are not intended to limit the present invention.
测试方法：Test Methods:
1、电导率测试方法：1. Conductivity test method:
用万用电表测试10cm长的纤维或纱线的电阻，根据电导率的公式计算出电导率。Use a multimeter to test the resistance of a 10cm long fiber or yarn, and calculate the conductivity based on the conductivity formula.
2、光致发热性能测试方法：2. Photoheating performance test method:
使用太阳光模拟器(模拟太阳光强度为1000W/m2)照射高效光热响应聚乳酸材料，同时用红外热成像仪记录样品的温度变化，照射时长为1min。A solar simulator (simulating sunlight intensity of 1000W/m 2 ) was used to irradiate the highly efficient photothermal response polylactic acid material, and an infrared thermal imager was used to record the temperature changes of the sample. The irradiation duration was 1 min.
3、光致变色性能测试方法：3. Photochromic performance test method:
采用Datacolor CI7800电脑测配色仪，在D65/10°下测试材料的色差。Use Datacolor CI7800 computer color matching instrument to test the color difference of the material at D65/10°.
4、抗菌性能测试方法：4. Antibacterial performance test method:
按照标准《GB/T 20944.3-2008纺织品抗菌性能的评价第3部分：振荡法》对材料的抗菌性能进行测试。The antibacterial properties of the materials were tested in accordance with the standard "GB/T 20944.3-2008 Evaluation of Antibacterial Properties of Textiles Part 3: Oscillation Method".
5、传感性能测试：5. Sensing performance test:
采用推拉力计(乐清市艾德堡仪器有限公司)调节施加压力大小，采用电化学工作站CME-660E(上海辰华仪器有限公司)获取实时的电流数据，测试电压为5V；A push-pull force meter (Yueqing Aidebao Instrument Co., Ltd.) was used to adjust the applied pressure, and an electrochemical workstation CME-660E (Shanghai Chenhua Instrument Co., Ltd.) was used to obtain real-time current data. The test voltage was 5V;
灵敏度的计算公式如下：The sensitivity is calculated as follows:
灵敏度S＝(ΔI/I0)/ΔP；Sensitivity S=(ΔI/I 0 )/ΔP;
其中，ΔI为电流变化值，I0为初始电流，ΔP为所施加的压强。Among them, ΔI is the current change value, I 0 is the initial current, and ΔP is the applied pressure.
6、疏水性的测试：6. Hydrophobicity test:
采用DSA25液滴形状分析仪(德国)，将10μL的水滴滴在表面上，测试水接触角。Using DSA25 droplet shape analyzer ( Germany), place 10 μL of water droplets on the surface and test the water contact angle.
7、水洗牢度的测试：7. Test of washing fastness:
将样品置于装有去离子水的烧杯中，用磁力搅拌器搅拌，转速为500rmp，处理5min，取出后用去离子水冲洗，然后烘干，对其对应的功能性进行测试。Place the sample in a beaker filled with deionized water, stir it with a magnetic stirrer at a rotation speed of 500 rpm, process it for 5 minutes, take it out, rinse it with deionized water, and then dry it to test its corresponding functionality.
实施例中采用的原料：Raw materials used in the examples:
四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物：四氟乙烯、六氟丙烯和偏氟乙烯结构单元的重量百分比分别为45.8％、18.5％和35.7％；Tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer: the weight percentages of tetrafluoroethylene, hexafluoropropylene and vinylidene fluoride structural units are 45.8%, 18.5% and 35.7% respectively;
多壁碳纳米管：直径为20～40nm、长度为5～15μm；Multi-walled carbon nanotubes: diameter 20~40nm, length 5~15μm;
红色光致变色微胶囊：型号为PMR01，平均粒径为3±1μm，购自广州盛色科技有限公司；Red photochromic microcapsules: model PMR01, average particle size 3±1μm, purchased from Guangzhou Shengse Technology Co., Ltd.;
碳化锆：平均粒径30nm，纯度99.9％，比表面积75m2/g，密度15.5g/cm3，购自上海攀田粉体材料有限公司；Zirconium carbide: average particle size 30nm, purity 99.9%, specific surface area 75m 2 /g, density 15.5g/cm 3 , purchased from Shanghai Pantian Powder Materials Co., Ltd.;
纳米银：平均粒径50nm，纯度99.9％，比表面积30m2/g，密度10.5g/cm3，购自上海攀田粉体材料有限公司；Nanosilver: average particle size 50nm, purity 99.9%, specific surface area 30m 2 /g, density 10.5g/cm 3 , purchased from Shanghai Pantian Powder Materials Co., Ltd.;
聚酰胺11长丝：聚酰胺11原料来源于法国阿科玛公司，型号为PA11 BMO TLD，对应的长丝为自制，直径为136.6μm；Polyamide 11 filament: The polyamide 11 raw material comes from the French Arkema company, the model is PA11 BMO TLD, the corresponding filament is self-made, and the diameter is 136.6 μm;
聚乳酸长丝：150D/144f FDY；Polylactic acid filament: 150D/144f FDY;
涤纶长丝：150D/144f FDY；Polyester filament: 150D/144f FDY;
涤棉混纺纱线：32S，T60/C30；Polyester-cotton blended yarn: 32S, T60/C30;
尼龙6基气流成网非织造材料：厚度为1.2cm，面密度为320g/m2；Nylon 6-based air-laid nonwoven material: thickness is 1.2cm, area density is 320g/m 2 ;
涤纶基气流成网非织造材料：厚度为1.0cm，面密度为250g/m2。Polyester-based air-laid nonwoven material: thickness is 1.0cm, area density is 250g/m 2 .
实施例1Example 1
一种基于功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液制备功能化尼龙6基气流成网非织造材料的方法，包括如下步骤：A method for preparing functionalized nylon 6-based air-laid nonwoven materials based on functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion, including the following steps:
(1)将四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物和乙酸乙酯混合，60℃下磁力搅拌60min，得到浓度为20mg/mL的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液；(1) Mix tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer and ethyl acetate, stir magnetically at 60°C for 60 minutes, and obtain tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride with a concentration of 20 mg/mL. Terpolymer solution;
(2)在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中添加多壁碳纳米管，使得其浓度为8mg/mL，在常温下磁力搅拌30min，再超声振荡120min，得到所述的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液；(2) Add multi-walled carbon nanotubes to the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution so that its concentration is 8 mg/mL, magnetically stir at room temperature for 30 minutes, and then ultrasonic oscillate for 120 minutes to obtain the result The above-mentioned functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion;
(3)将尼龙6基气流成网非织造材料常温浸渍在功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液中超声5min，再经过烘燥装置烘干，得到压阻式传感器。(3) Dip the nylon 6-based air-laid nonwoven material into the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion at room temperature and ultrasonicate for 5 minutes, and then dry it through a drying device to obtain the pressure Resistive sensor.
将得到的压阻式传感器进行性能测试，测试结构如下：The obtained piezoresistive sensor is tested for performance. The test structure is as follows:
压阻式传感器的灵敏度为1.26kPa-1，水接触角为153°。The piezoresistive sensor has a sensitivity of 1.26kPa -1 and a water contact angle of 153°.
实施例2Example 2
一种基于功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液制备功能化尼龙6基气流成网非织造材料的方法，包括如下步骤：A method for preparing functionalized nylon 6-based air-laid nonwoven materials based on functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion, including the following steps:
(1)将四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物和乙酸乙酯混合，60℃下磁力搅拌60min，得到浓度为20mg/mL的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液；(1) Mix tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer and ethyl acetate, stir magnetically at 60°C for 60 minutes, and obtain tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride with a concentration of 20 mg/mL. Terpolymer solution;
(2)在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中添加多壁碳纳米管，使得其浓度为4mg/mL，在常温下磁力搅拌30min，再超声振荡120min，得到所述的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液；(2) Add multi-walled carbon nanotubes to the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution so that its concentration is 4 mg/mL, magnetically stir at room temperature for 30 minutes, and then ultrasonic oscillate for 120 minutes to obtain the result The above-mentioned functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion;
(3)将尼龙6基气流成网非织造材料常温浸渍在功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液中超声5min，再经过烘燥装置烘干，得到压阻式传感器。(3) Dip the nylon 6-based air-laid nonwoven material into the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion at room temperature and ultrasonicate for 5 minutes, and then dry it through a drying device to obtain the pressure Resistive sensor.
将得到的压阻传感器进行性能测试，测试结构如下：The obtained piezoresistive sensor is tested for performance. The test structure is as follows:
压阻式传感器的灵敏度为0.83kPa-1，水接触角为152°。The piezoresistive sensor has a sensitivity of 0.83kPa -1 and a water contact angle of 152°.
实施例3Example 3
一种基于功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液制备涤纶基气流成网非织造材料的方法，包括如下步骤：A method for preparing polyester-based air-laid nonwoven materials based on functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion, including the following steps:
(1)将四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物和乙酸乙酯混合，60℃下磁力搅拌60min，得到浓度为20mg/mL的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液；(1) Mix tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer and ethyl acetate, stir magnetically at 60°C for 60 minutes, and obtain tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride with a concentration of 20 mg/mL. Terpolymer solution;
(2)在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中添加0.5μm的碳化锆，使得其浓度为8mg/mL，在常温下磁力搅拌30min，再超声振荡120min，得到所述的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液；(2) Add 0.5 μm zirconium carbide to the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution so that its concentration is 8 mg/mL, magnetically stir at room temperature for 30 min, and then ultrasonic oscillate for 120 min to obtain the result The above-mentioned functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion;
(3)将0.5μm的碳化锆常温浸渍在功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液中超声5min，再经过烘燥装置烘干，得到光致发热非织造材料。(3) Dip 0.5 μm zirconium carbide into the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion at room temperature and ultrasonic for 5 minutes, and then dry it through a drying device to obtain a photothermal nonwoven Material.
将得到的光致发热非织造材料进行性能测试，测试结构如下：The obtained photothermal nonwoven material was tested for performance. The test structure is as follows:
光致发热非织造材料的温度可达70℃，水接触角为154°。The temperature of photothermal nonwoven materials can reach 70°C, and the water contact angle is 154°.
实施例4Example 4
一种基于功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液制备功能化聚酰胺11长丝的方法，包括如下步骤：A method for preparing functionalized polyamide 11 filaments based on functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion, including the following steps:
(1)将四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物和乙酸乙酯混合，60℃下磁力搅拌60min，得到浓度为80mg/mL的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液；(1) Mix tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer and ethyl acetate, stir magnetically at 60°C for 60 minutes, and obtain tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride with a concentration of 80 mg/mL. Terpolymer solution;
(2)在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中添加多壁碳纳米管，使得其浓度为10mg/mL，在常温下磁力搅拌20min，再超声振荡60min，得到所述的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液；(2) Add multi-walled carbon nanotubes to the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution so that its concentration is 10 mg/mL, magnetically stir at room temperature for 20 minutes, and then ultrasonic oscillate for 60 minutes to obtain the result The above-mentioned functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion;
(3)将聚酰胺11长丝从筒子上退绕下来，之后常温浸渍在功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液中超声5min，再经过烘燥装置烘干，最后将处理后的聚酰胺11长丝以1m/min的速度卷绕到筒子上，制得聚酰胺11导电长丝。(3) Unwind the polyamide 11 filament from the bobbin, then immerse it in the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion at room temperature and sonicate for 5 minutes, and then dry it through a drying device Dry, and finally wind the treated polyamide 11 filament onto a bobbin at a speed of 1 m/min to prepare polyamide 11 conductive filament.
将得到的聚酰胺11导电长丝进行性能测试，测试结构如下：The obtained polyamide 11 conductive filament was tested for performance. The test structure is as follows:
聚酰胺11导电长丝的导电率为1.3S/m。The conductivity of polyamide 11 conductive filament is 1.3S/m.
实施例5Example 5
一种基于功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液制备功能化聚乳酸长丝的方法，包括如下步骤：A method for preparing functionalized polylactic acid filaments based on functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion, including the following steps:
(1)将四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物和乙酸乙酯混合，60℃下磁力搅拌60min，得到浓度为60mg/mL的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液；(1) Mix tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer and ethyl acetate, stir magnetically at 60°C for 60 minutes, and obtain tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride with a concentration of 60 mg/mL. Terpolymer solution;
(2)在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中添加红色光致变色微胶囊，使得其浓度为0.5mg/mL，在常温下磁力搅拌20min，再超声振荡60min，得到所述的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液；(2) Add red photochromic microcapsules to the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution so that its concentration is 0.5 mg/mL, magnetically stir at room temperature for 20 minutes, and then ultrasonic oscillate for 60 minutes. Obtain the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion;
(3)将聚乳酸长丝从筒子上退绕下来，之后常温浸渍在功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液中超声5min，再经过烘燥装置烘干，最后将处理后的聚乳酸长丝以2m/min的速度卷绕到筒子上，制得光致变色聚乳酸长丝。(3) Unwind the polylactic acid filament from the bobbin, then immerse it in the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion at room temperature and sonicate for 5 minutes, and then dry it through a drying device , and finally the treated polylactic acid filament is wound onto the bobbin at a speed of 2m/min to produce photochromic polylactic acid filament.
将得到的光致变色聚乳酸长丝进行性能测试，测试结构如下：The obtained photochromic polylactic acid filament was tested for performance. The test structure is as follows:
光致变色聚乳酸长丝的色差可达13.6。The color difference of photochromic polylactic acid filament can reach 13.6.
实施例6Example 6
一种基于功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液制备功能化涤纶长丝的方法，包括如下步骤：A method for preparing functional polyester filament based on functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion, including the following steps:
(1)将四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物和乙酸乙酯混合，60℃下磁力搅拌60min，得到浓度为40mg/mL的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液；(1) Mix tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer and ethyl acetate, stir magnetically at 60°C for 60 minutes, and obtain tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride with a concentration of 40 mg/mL. Terpolymer solution;
(2)在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中添加100nm的纳米银粉，使得其浓度为1mg/mL，在常温下磁力搅拌20min，再超声振荡60min，得到所述的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液；(2) Add 100 nm nanometer silver powder to the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution so that its concentration is 1 mg/mL, stir magnetically at room temperature for 20 minutes, and then ultrasonic oscillate for 60 minutes to obtain the above Functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion;
(3)将涤纶长丝从筒子上退绕下来，之后常温浸渍在功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液中超声5min，再经过烘燥装置烘干，最后将处理后的涤纶长丝以1m/min的速度卷绕到筒子上，制得抗菌涤纶长丝。(3) Unwind the polyester filament from the bobbin, then immerse it in the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion at room temperature and sonicate for 5 minutes, and then dry it through a drying device. Finally, the treated polyester filament is wound onto the bobbin at a speed of 1m/min to obtain antibacterial polyester filament.
将得到的抗菌涤纶长丝进行性能测试，测试结构如下：The obtained antibacterial polyester filament was tested for performance. The test structure is as follows:
抗菌涤纶长丝对金黄色葡萄球菌和大肠杆菌的抑菌率分别为99.3％和97.8％。The antibacterial rates of antibacterial polyester filament against Staphylococcus aureus and Escherichia coli are 99.3% and 97.8% respectively.
实施例7Example 7
一种基于功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液制备功能化涤棉混纺纱线的方法，包括如下步骤：A method for preparing functionalized polyester-cotton blended yarn based on functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion, including the following steps:
(1)将四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物和乙酸乙酯混合，60℃下磁力搅拌60min，得到浓度为80mg/mL的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液；(1) Mix tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer and ethyl acetate, stir magnetically at 60°C for 60 minutes, and obtain tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride with a concentration of 80 mg/mL. Terpolymer solution;
(2)在四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液中添加多壁碳纳米管，使得其浓度为10mg/mL，在常温下磁力搅拌20min，再超声振荡60min，得到所述的功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液；(2) Add multi-walled carbon nanotubes to the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution so that its concentration is 10 mg/mL, magnetically stir at room temperature for 20 minutes, and then ultrasonic oscillate for 60 minutes to obtain the result The above-mentioned functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion;
(3)将32S的涤棉混纺纱线(T60/C30)从筒子上退绕下来，之后常温浸渍在功能化的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物分散液中超声5min，再经过烘燥装置烘干，最后将处理后的涤棉混纺纱线以1m/min的速度卷绕到筒子上，制得导电涤棉混纺纱线。(3) Unwind the 32S polyester-cotton blended yarn (T60/C30) from the bobbin, and then immerse it in the functionalized tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer dispersion at room temperature and sonicate for 5 minutes. , and then dried by a drying device, and finally the treated polyester-cotton blended yarn was wound onto a bobbin at a speed of 1m/min to prepare conductive polyester-cotton blended yarn.
将得到的导电涤棉混纺纱线进行性能测试，测试结构如下：The obtained conductive polyester-cotton blended yarn was tested for performance. The test structure is as follows:
导电涤棉混纺纱线的导电率为0.9S/m。The conductivity of conductive polyester-cotton blended yarn is 0.9S/m.
对比例1Comparative example 1
将实施例1步骤(1)中的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物替换成聚丙烯酸，其他与实施例1保持一致，得到压阻式传感器。The tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer in step (1) of Example 1 was replaced with polyacrylic acid, and the other components were kept the same as Example 1 to obtain a piezoresistive sensor.
对比例2Comparative example 2
省略实施例1步骤(1)中的四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物，将多壁碳纳米管和乙酸乙酯混合得到分散液；之后将尼龙6基气流成网非织造材料常温浸渍在分散液中，其他与实施例1保持一致，得到压阻式传感器。The tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer in step (1) of Example 1 is omitted, and multi-walled carbon nanotubes and ethyl acetate are mixed to obtain a dispersion; then nylon 6-based air-laid non- The woven material was immersed in the dispersion liquid at room temperature, and other aspects were kept the same as in Example 1 to obtain a piezoresistive sensor.
实施例8Example 8
将实施例1步骤(1)中四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液的浓度调整为5mg/mL，其他与实施例1保持一致，得到压阻式传感器。The concentration of the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution in step (1) of Example 1 was adjusted to 5 mg/mL, and the others were kept consistent with Example 1 to obtain a piezoresistive sensor.
实施例9Example 9
将实施例1步骤(1)中四氟乙烯-六氟丙烯-偏氟乙烯三元共聚物溶液的浓度调整为50mg/mL，其他与实施例1保持一致，得到压阻式传感器。The concentration of the tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride terpolymer solution in step (1) of Example 1 was adjusted to 50 mg/mL, and the others were kept consistent with Example 1 to obtain a piezoresistive sensor.
将得到的压阻式传感器进行性能测试，测试结果如下表1：The obtained piezoresistive sensor was tested for performance. The test results are as follows in Table 1:
表1水洗前后材料的功能性Table 1 Functionality of materials before and after washing
虽然本发明已以较佳实施例公开如上，但其并非用以限定本发明，任何熟悉此技术的人，在不脱离本发明的精神和范围内，都可做各种的改动与修饰，因此本发明的保护范围应该以权利要求书所界定的为准。Although the present invention has been disclosed above in terms of preferred embodiments, they are not intended to limit the present invention. Anyone familiar with this technology can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, The protection scope of the present invention should be defined by the claims.
Claims (10)
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| DE10129194A1 (en) * | 2001-06-04 | 2002-12-05 | Johannes Fitz | Dirt- and water-repellent textile with low flammability for use, e.g. in vehicle seat covers, comprises fabric based on fibres of phosphorus-containing polyester coated with a layer of high-molecular weight fluoropolymer |
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| US5194322A (en) * | 1988-06-04 | 1993-03-16 | Scapa Group Plc | Coated textile materials |
| DE10129194A1 (en) * | 2001-06-04 | 2002-12-05 | Johannes Fitz | Dirt- and water-repellent textile with low flammability for use, e.g. in vehicle seat covers, comprises fabric based on fibres of phosphorus-containing polyester coated with a layer of high-molecular weight fluoropolymer |
| US20100184346A1 (en) * | 2009-01-21 | 2010-07-22 | Xerox Corporation | Superhydrophobic nano-fabrics and coatings |
| DE202009016833U1 (en) * | 2009-12-14 | 2010-02-25 | Fitz, Johannes | Weather resistant, flexible adhesive |
| US20130130003A1 (en) * | 2010-04-23 | 2013-05-23 | Kolon Industries, Inc. | Back sheet for solar cell module and manufacturing method thereof |
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