CN107524011B - 一种超疏水防紫外线纺织品的制备方法 - Google Patents
一种超疏水防紫外线纺织品的制备方法 Download PDFInfo
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- 239000004753 textile Substances 0.000 title claims abstract description 70
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- -1 polysiloxanes Polymers 0.000 claims abstract description 75
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 74
- 239000004744 fabric Substances 0.000 claims abstract description 42
- 239000002131 composite material Substances 0.000 claims abstract description 40
- 238000009988 textile finishing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 150000001875 compounds Chemical class 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 18
- 239000003431 cross linking reagent Substances 0.000 claims description 17
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000000835 fiber Substances 0.000 claims description 11
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 claims description 7
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 7
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 5
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- 239000011593 sulfur Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical group CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
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- 229920002647 polyamide Polymers 0.000 claims description 3
- QHQNYHZHLAAHRW-UHFFFAOYSA-N 2-trimethoxysilylethanamine Chemical compound CO[Si](OC)(OC)CCN QHQNYHZHLAAHRW-UHFFFAOYSA-N 0.000 claims description 2
- 229920004933 Terylene® Polymers 0.000 claims description 2
- ODWXUNBKCRECNW-UHFFFAOYSA-M bromocopper(1+) Chemical compound Br[Cu+] ODWXUNBKCRECNW-UHFFFAOYSA-M 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 2
- 150000005846 sugar alcohols Polymers 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims 1
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- 230000006750 UV protection Effects 0.000 abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 abstract 5
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 abstract 1
- 239000010949 copper Substances 0.000 abstract 1
- 238000004073 vulcanization Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 11
- 229920004934 Dacron® Polymers 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000004224 protection Effects 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000009738 saturating Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 239000002023 wood Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
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- 238000002604 ultrasonography Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000010919 dye waste Substances 0.000 description 2
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- PUVRBXSPPBNRHE-UHFFFAOYSA-N C(C)[Si](OCC)(OCC)OCC.N Chemical compound C(C)[Si](OCC)(OCC)OCC.N PUVRBXSPPBNRHE-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- PTVDYARBVCBHSL-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu] PTVDYARBVCBHSL-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
本发明涉及一种超疏水防紫外线纺织品的制备方法,包括聚硅氧烷/花状CuS复合材料的制备、纺织品整理。将花状硫化铜与聚硅氧烷混合制得聚硅氧烷/花状硫化铜复合材料,并将其对纺织品整理,通过聚硅氧烷低表面能特性与CuS花状层级多孔微观粗糙结构的协同,并结合花状CuS的紫外屏蔽性能及聚硅氧烷对CuS粒子、纺织品的粘结作用,获得超疏水防紫外线功能复合纺织品。本发明制备工艺简单,整理纺织品同时具有优异的超疏水及防紫外功能,使纺织品附加值大大提高,并具有广泛的应用领域。
Description
技术领域
本发明属于纺织品功能整理领域,尤其是涉及一种超疏水防紫外线纺织品的制备方法。
背景技术
目前我国纺织行业正处于产业转型升级的关键阶段,纺织品的功能整理已经不仅仅局限于单一功能整理,而多功能纺织品已明确成为纺织行业未来发展的重要趋势之一。近年来超疏水纺织品,即水滴在纺织品表面的接触角大于150°,具有独特的抗污、易洁等性能以及纺织材料的柔韧、透气、轻质等优异特性。随着科技的飞速发展,超疏水防紫外线复合功能纺织品作为重要的户外保护用品,在工业、医疗、军事和日常生活中具有广泛的应用领域,日益受到人们的极大关注和喜爱,吸引了越来越多的学者关注。
国内市场上已有防水和抗紫外线复合功能纺织产品,但是这些产品主要是采用传统的防水涂层方法,达不到超疏水性能,且织物手感厚重,透气性差,大多是采用有机紫外线屏蔽剂实现纺织品抗紫外功能,而大部分有机紫外线屏蔽剂对人体有害,也会造成环境污染,不利于环保。制备超疏水纺织品的关键技术包括微纳粗糙结构的构筑和低表面能物质疏水化修饰。表面微观结构粗糙化可通过引入无机纳米材料来实现,如SiO2、TiO2、ZnO、碳纳米管、银粒子等,低表面能物质包括有机硅、有机氟等有机物。此外,无机物质如纳米TiO2、纳米ZnO等还具有较强的紫外线吸收能力。
采用纳米TiO2、纳米ZnO等具有较强的紫外线吸收能力的无机材料在纺织品表面用于构建微纳粗糙结构,再通过低表面能物质修饰可以实现超疏水防紫外线复合功能纺织品的制备。然而,在充分利用纳米TiO2、纳米ZnO等纳米材料构建微纳粗糙结构及其紫外线吸收性能的同时,必须考虑纳米TiO2、纳米ZnO优异的光催化作用对纤维基体及附于纳米粒子表面的低表面能物质的降解效应,大大降低其超疏水性能。目前文献报道有效的方法是在TiO2、ZnO表面包覆一层不具有光催化活性的物质,如二氧化硅、氧化铝等,屏蔽光催化作用,将被二氧化硅包覆的TiO2、ZnO负载织物表面并进行疏水化整理得到具有超疏水和防紫外线复合功能纺织品。但这些方法工艺复杂、条件苛刻,且大多都存在超疏水稳定性不好的缺点。
中国专利CN106082303A公开了一种花状结构的CuS材料及其制备方法和应用,将含二价铜的化合物和溶剂混合,在一定温度下充分搅拌得到均相溶液;在强烈搅拌下,将含硫化合物缓慢加入均相溶液中,然后保温处理;将上述溶液转移至水热反应釜中,在一定温度下密封加热反应,然后降温至室温,过滤,收集,洗涤产物,再进行过滤,真空干燥,研磨得到黑色产物即为花状结构的CuS材料,可以在光催化降解染料废水中应用。但是该专利制备的花状CuS微球直径为3-6μm,尺寸相对较大,属于微米级尺寸,较大的花状CuS微球不利于在柔性纺织品表面固着,且该专利制备的花状CuS比表面积为15.7884m2/g,仅涉及光催化降解染料废水中的应用,应用具有局限性。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种超疏水防紫外线纺织品的制备方法,采用聚硅氧烷/花状CuS复合材料在超声空化辅助及焙烘作用下在纺织品表面构建有机无机复合花状层级多孔微观结构,同时实现超疏水防紫外线复合功能,避免了先用SiO2包覆TiO2或ZnO后再负载织物表面最后进行疏水化整理的复杂工艺,成本较低,安全环保,制备工艺简单,制备的超疏水防紫外线纺织品其附加值和档次大大提高,应用领域也明显拓宽。
本发明的目的可以通过以下技术方案来实现:
一种超疏水防紫外线纺织品的制备方法,采用以下步骤:
(1)聚硅氧烷/花状CuS复合材料的制备:将花状CuS与聚硅氧烷及其交联剂混合在溶剂中,在20-60℃下,超声分散得到聚硅氧烷/花状CuS复合材料。其中所用的花状CuS的制备步骤为:将含二价铜的化合物(氯化铜、溴化铜、醋酸铜或硫酸铜)和溶剂(水或多元醇类化合物)混合,含二价铜的化合物在溶剂中的浓度为3~16wt%,在75~150℃下充分搅拌15~60min后,再加入含硫化合物(硫脲、硫化钠、硫化钾、二甲基亚砜、二硫化碳或硫代乙酰胺),含二价铜的化合物与含硫化合物的摩尔比为10:1~3:1,保温处理30~60min,然后将上述溶液转移至水热反应釜中,在135~200℃下密封加热反应3~30h,降温至室温,过滤,收集和洗涤产物过滤,真空干燥,研磨得到花状CuS。
(2)纺织品整理:在超声波条件下,将纺织品浸渍在聚硅氧烷/花状CuS复合材料中,再经烘干、焙烘得到超疏水防紫外线纺织品。
步骤(1)中,制备得到的花状CuS形貌为六方相花状,尺寸直径0.1-1.5μm。上述尺寸较小,而比表面积更大,可达18.32m2/g以上,这非常有利于花状CuS与纺织纤维的牢固结合,具有较大比表面积和多孔结构的纳米级花状CuS提供了超疏水表面构建所必需的微观粗糙结构及粗糙结构间的空气垫,且本申请将聚硅氧烷与花状CuS复合,加固和增强了CuS花状层级多孔骨架结构,而不影响花状CuS高比表面积和多孔的优良特性及其优异的紫外线吸收性能,同时聚硅氧烷对花状CuS的“包裹”能够有效隔离花状CuS对纤维基底的光催化降解,并结合聚硅氧烷较低的表面能及其对花状CuS与纺织品之间的粘结作用,实现高性能超疏水防紫外线多功能柔性纺织品的制备,大大拓宽了花状CuS的应用领域。
步骤(1)中,所述的聚硅氧烷为聚二甲基硅氧烷、氨乙基聚硅氧烷或氨丙基聚硅氧烷,所述的交联剂为氨丙基三甲氧基硅烷、氨丙基三乙氧基硅烷、氨乙基三甲氧基硅烷或氨乙基三乙氧基硅烷,所述的溶剂为四氢呋喃、二氯甲烷、三氯甲烷或异丙醇。花状CuS的用量为0.25-10wt%,聚硅氧烷的用量为0.1-8wt%,交联剂的用量为聚硅氧烷用量的5-15wt%。超声分散时间为10-100min。超声分散的时间对制备的聚硅氧烷/花状CuS复合材料的分散稳定性有一定影响,超声分散的时间必须为10-100min,才能使花状CuS不易团聚分散均匀,并促使聚硅氧烷在所有花状CuS微球表面较好地结合,大大有利于分散稳定的聚硅氧烷/花状CuS复合材料的形成,以致使整理后纺织品具有优异的超疏水防紫外线多功能性。超声分散的时间如果不在上述范围内,会导致花状CuS部分团聚,使部分花状CuS未与聚硅氧烷结合,进而造成整理织物表面部分部位缺少低表面能物质聚硅氧烷而难以实现均匀的纺织品超疏水性。
步骤(2)中所述的纺织品为涤纶、锦纶、腈纶或其混纺机织物或针织物。浸渍时间为10~80min,烘干温度为80~100℃,烘干时间为3-12min;焙烘温度是120~200℃,焙烘时间为5~90min。上述工艺条件对最终整理织物的超疏水防紫外线性能有重要影响。浸渍时间必须充分,在上述工艺条件范围内才能保证聚硅氧烷/花状CuS复合材料在织物纤维表面以分散状态均匀附着;经烘干后随着溶剂的挥发,纤维表面的聚硅氧烷/花状CuS复合材料逐步靠拢并紧密排列,烘干温度和烘干时间在上述工艺条件范围内才能保证溶剂全部挥发;焙烘处理使纤维表面的聚硅氧烷/花状CuS复合材料相互聚结,聚硅氧烷分子链相互扩散、缠绕,聚硅氧烷含有的活性基团与交联剂形成共价交联反应并粘结在纤维表面,而CuS仍保持花状微球形,最终在织物表面形成牢固的聚硅氧烷/花状CuS复合低表面能粗糙膜,实现纺织品超疏水防紫外线多功能性。如果不在上述工艺条件的范围内,难以保证聚硅氧烷/花状CuS复合材料在织物纤维表面均匀附着并牢固结合,无法实现聚硅氧烷/花状CuS复合低表面能粗糙膜的形成,进而无法得到具有优异超疏水防紫外线多功能纺织品。
本发明将具有优异固化交联粘结性的聚硅氧烷与花状CuS复合,制备聚硅氧烷/花状CuS复合材料,并对纺织品一步法浸渍焙烘整理,获得超疏水防紫外线复合功能纺织品,可使织物保持基本物理机械性能,如柔软的手感、强力等,具有十分广阔的应用前景。
本发明将聚硅氧烷/花状CuS复合材料在纺织品表面构建有机无机花状层级多孔微观结构。具有较大的比表面积的花状CuS相互交叉的纳米片间开放的孔状结构满足了超疏水表面构建所需要的微观结构及粗糙结构间的空气垫,且将聚硅氧烷与花状CuS复合,加固和增强了CuS花状层级多孔骨架结构,而不影响花状CuS高比表面积和多孔的优良特性及其优异的紫外线吸收性能,此外聚硅氧烷对花状CuS的“包裹”能够有效隔离花状CuS对纤维基底的光催化降解,同时聚硅氧烷中的Si-O键能为460kJ/mol,键能较大,能够抵御花状CuS(禁带宽度1.46eV)光催化降解,也可以抵御(紫外光314-419kJ/mol)的降解。聚硅氧烷优异的低表面能特性大大降低了织物表面自由能,通过聚硅氧烷低表面能特性与花状CuS层级多孔微观粗糙结构的协同效应,同时结合花状CuS优异的紫外线吸收性能,制备稳定性超疏水防紫外线复合功能纺织品。此外,本发明将聚硅氧烷/花状CuS复合材料对纺织品在超声空化条件下浸渍处理再通过焙烘制备超疏水防紫外线纺织品,利用超声空化效应使聚硅氧烷/花状CuS复合材料向即织物空隙处聚集,有效提高了织物多孔结构对聚硅氧烷/花状CuS复合材料的收集和固着吸附能力。焙烘条件下一方面进一步增强聚硅氧烷/花状CuS复合材料在纺织品纤维孔隙的固着吸附作用,另一方面使聚硅氧烷含有的活性基团与所用交联剂形成共价交联反应,增强花状CuS与纺织品之间的交联粘结作用,提高超疏水防紫外线纺织品表面的耐久稳定性。
与现有技术相比,本发明具有以下优点:
(1)本发明的超疏水防紫外线纺织品的制备,方法简单、安全环保、成本低,超疏水、防紫外线性能优异。不同于目前先用SiO2包覆TiO2或ZnO后再负载织物表面最后低表面能修饰制备超疏水防紫外线纺织品的复杂方法,在纺织品表面同时引入低表面能聚硅氧烷与花状CuS层级多孔微观粗糙结构,并结合花状CuS优异的紫外线吸收性能,协同实现了超疏水防紫外线纺织品的制备;
(2)本发明的超疏水防紫外线纺织品的制备,利用聚硅氧烷优异的交联固化粘结作用实现对花状CuS的“包裹”加固和增强了CuS花状层级多孔骨架结构,而不影响CuS花状层级多孔的优良特性及其优异的紫外线吸收性能,并增强花状层级多孔微观结构与纤维基底之间的结合牢度,同时聚硅氧烷对花状CuS的“包裹”能够有效隔离花状CuS对纤维基底的光催化降解,且低表面能物质聚硅氧烷能够抵御花状CuS光催化降解,大大增强超疏水防紫外线纺织品的耐久稳定性。
(3)满足开发高档超疏水防紫外线多功能纺织品的需要。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例1
将尺寸直径为0.2-0.3μm的2%花状CuS与3%聚二甲基硅氧烷及其交联剂(聚硅氧烷用量的9%,氨丙基三甲氧基硅烷)混合在溶剂异丙醇50mL中,在30℃下,经超声分散50min得到聚硅氧烷/花状CuS复合材料。在超声波空化条件下,将涤纶织物浸渍在聚硅氧烷/花状CuS复合材料中,浸渍30min,80℃烘干5min,180℃焙烘10min,得到超疏水防紫外线涤纶织物。
使用Kruss DSA30型视频接触角测量仪进行接触角测试,水量为5μL,水滴与织物接触60s后读数,在同一样品不同位置测量5次,取平均值。织物表面抗湿性根据AATCC 22-2005《拒水性:喷淋试验》进行测试。利用Labsphere UV1000F紫外线防护系数测试仪,对每个织物样品的五个不同部位分别测试其紫外线防护系数UPF、紫外线UVA(320-420nm)的透过率T(UVA),取平均值。测得整理后涤纶织物的接触角为156°,表面抗湿性评分95,UPF为246,T(UVA)为1.96%,紫外线照射24h后涤纶织物的接触角为153°,表面抗湿性评分95。
实施例2
将尺寸直径为0.5-0.6μm的4%花状CuS与4%氨乙基聚硅氧烷及其交联剂(聚硅氧烷用量的10%,氨丙基三乙氧基硅烷)混合在溶剂异丙醇50mL中,在30℃下,经超声分散40min得到聚硅氧烷/花状CuS复合材料。在超声空化条件下,将涤纶织物浸渍在聚硅氧烷/花状CuS复合材料中,浸渍40min,85℃烘干5min,185℃焙烘10min,得到超疏水防紫外线涤纶织物。
使用Kruss DSA30型视频接触角测量仪进行接触角测试,水量为5μL,水滴与织物接触60s后读数,在同一样品不同位置测量5次,取平均值。织物表面抗湿性根据AATCC 22-2005《拒水性:喷淋试验》进行测试。利用Labsphere UV1000F紫外线防护系数测试仪,对每个织物样品的五个不同部位分别测试其紫外线防护系数UPF、紫外线UVA(320-420nm)的透过率T(UVA),取平均值。测得整理后涤纶织物的接触角为159°,表面抗湿性评分100,UPF为368,T(UVA)为1.62%,紫外线照射24h后涤纶织物的接触角为154°,表面抗湿性评分95。
实施例3
将尺寸直径为0.6-0.7μm的3%花状CuS与4%聚二甲基硅氧烷及其交联剂(聚硅氧烷用量的10%,氨丙基三甲氧基硅烷)混合在溶剂异丙醇50mL中,在40℃下,经超声分散30min得到聚硅氧烷/花状CuS复合材料。在超声空化条件下,将锦纶织物浸渍在聚硅氧烷/花状CuS复合材料中,浸渍30min,90℃烘干5min,190℃焙烘20min,得到超疏水防紫外线锦纶织物。
使用Kruss DSA30型视频接触角测量仪进行接触角测试,水量为5μL,水滴与织物接触60s后读数,在同一样品不同位置测量5次,取平均值。织物表面抗湿性根据AATCC 22-2005《拒水性:喷淋试验》进行测试。利用Labsphere UV1000F紫外线防护系数测试仪,对每个织物样品的五个不同部位分别测试其紫外线防护系数UPF、紫外线UVA(320-420nm)的透过率T(UVA),取平均值。测得整理后锦纶织物的接触角为160°,表面抗湿性评分100,UPF为326,T(UVA)为1.58%,紫外线照射24h后锦纶织物的接触角为154°,表面抗湿性评分95。
实施例4
将尺寸直径为0.7-0.8μm的4%花状CuS与5%氨丙基聚硅氧烷及其交联剂(聚硅氧烷用量的8%,氨丙基三乙氧基硅烷)混合在溶剂异丙醇50mL中,在40℃下,经超声分散30min得到聚硅氧烷/花状CuS复合材料。在超声空化条件下,将腈纶织物浸渍在聚硅氧烷/花状CuS复合材料中,浸渍30min,90℃烘干5min,190℃焙烘20min,得到超疏水防紫外线腈纶织物。
使用Kruss DSA30型视频接触角测量仪进行接触角测试,水量为5μL,水滴与织物接触60s后读数,在同一样品不同位置测量5次,取平均值。织物表面抗湿性根据AATCC 22-2005《拒水性:喷淋试验》进行测试。利用Labsphere UV1000F紫外线防护系数测试仪,对每个织物样品的五个不同部位分别测试其紫外线防护系数UPF、紫外线UVA(320-420nm)的透过率T(UVA),取平均值。测得整理后腈纶织物的接触角为160°,表面抗湿性评分100,UPF为326,T(UVA)为1.58%,紫外线照射24h后腈纶织物的接触角为154°,表面抗湿性评分95。
实施例5
一种超疏水防紫外线纺织品的制备方法,采用以下步骤:
(1)聚硅氧烷/花状CuS复合材料的制备:将花状CuS与聚二甲基硅氧烷及氨丙基三甲氧基硅烷交联剂混合在四氢呋喃溶剂中,花状CuS的用量为0.25wt%,聚硅氧烷的用量为0.1wt%,交联剂的用量为聚硅氧烷用量的5wt%,在20℃下,超声分散10min,得到聚硅氧烷/花状CuS复合材料。其中所用的花状CuS的制备步骤为:将氯化铜和水混合,配制得到浓度为3wt%的溶液,在75℃下充分搅拌60min后,再加入硫脲,氯化铜与硫脲的摩尔比为10:1,保温处理60min,然后将上述溶液转移至水热反应釜中,在135℃下密封加热反应30h,降温至室温,过滤,收集和洗涤产物过滤,真空干燥,研磨得到形貌为六方相花状,尺寸平均直径0.1μm的CuS。
(2)纺织品整理:在超声波条件下,将涤纶纺织品浸渍在聚硅氧烷/花状CuS复合材料中10min,控制烘干温度为80℃,烘干时间为12min,焙烘温度120℃,焙烘时间为90min,通过烘干、焙烘得到超疏水防紫外线纺织品。
实施例6
一种超疏水防紫外线纺织品的制备方法,采用以下步骤:
(1)聚硅氧烷/花状CuS复合材料的制备:将花状CuS与氨乙基聚硅氧烷及氨乙基三甲氧基硅烷交联剂混合在二氯甲烷溶剂中,花状CuS的用量为5wt%,聚硅氧烷的用量为5wt%,交联剂的用量为聚硅氧烷用量的10wt%,在30℃下,超声分散50min,得到聚硅氧烷/花状CuS复合材料。其中所用的花状CuS的制备步骤为:将醋酸铜和乙醇混合,配制得到浓度为10wt%的溶液,在100℃下充分搅拌30min后,再加入硫化钠,醋酸铜与硫化钠的摩尔比为5:1,保温处理60min,然后将上述溶液转移至水热反应釜中,在150℃下密封加热反应12h,降温至室温,过滤,收集和洗涤产物过滤,真空干燥,研磨得到形貌为六方相花状,尺寸平均直径1μm的CuS。
(2)纺织品整理:在超声波条件下,将锦纶纺织品浸渍在聚硅氧烷/花状CuS复合材料中30min,控制烘干温度为90℃,烘干时间为10min,焙烘温度150℃,焙烘时间为30min,通过烘干、焙烘得到超疏水防紫外线纺织品。
实施例7
一种超疏水防紫外线纺织品的制备方法,采用以下步骤:
(1)聚硅氧烷/花状CuS复合材料的制备:将花状CuS与氨丙基聚硅氧烷及氨乙基三乙氧基硅烷交联剂混合在异丙醇溶剂中,花状CuS的用量为10wt%,聚硅氧烷的用量为8wt%,交联剂的用量为聚硅氧烷用量的15wt%,在60℃下,超声分散100min,得到聚硅氧烷/花状CuS复合材料。其中所用的花状CuS的制备步骤为:将硫酸铜和正丙醇混合,配制得到浓度为16wt%的溶液,在150℃下充分搅拌15min后,再加入硫代乙酰胺,硫酸铜与硫代乙酰胺的摩尔比为3:1,保温处理30min,然后将上述溶液转移至水热反应釜中,在200℃下密封加热反应3h,降温至室温,过滤,收集和洗涤产物过滤,真空干燥,研磨得到形貌为六方相花状,尺寸平均直径1.5μm的CuS。
(2)纺织品整理:在超声波条件下,将腈纶纺织品浸渍在聚硅氧烷/花状CuS复合材料中80min,控制烘干温度为100℃,烘干时间为3min,焙烘温度200℃,焙烘时间为5min,通过烘干、焙烘得到超疏水防紫外线纺织品。
以上对本发明的具体实施例进行了描述。需要理解的是,本发明并不局限于上述特定实施方式,本领域技术人员可以在权利要求的范围内做出各种变形或修改,这并不影响本发明的实质内容。
Claims (8)
1.一种超疏水防紫外线纺织品的制备方法,其特征在于,该方法采用以下步骤:
(1)聚硅氧烷/花状CuS复合材料的制备:将花状CuS与聚硅氧烷及其交联剂混合在溶剂中,花状CuS的用量为0.25-10wt%,聚硅氧烷的用量为0.1-8wt%,交联剂的用量为聚硅氧烷用量的5-15wt%,在20-60℃下,超声分散得到聚硅氧烷/花状CuS复合材料,所述的花状CuS形貌为六方相花状,尺寸直径0.1-1.5μm,比表面积大于18.32m2/g,具有花状层级多孔微观结构;
(2)纺织品整理:在超声波条件下,将纺织品浸渍在聚硅氧烷/花状CuS复合材料中,再经烘干、焙烘得到超疏水防紫外线纺织品。
2.根据权利要求1中所述的一种超疏水防紫外线纺织品的制备方法,其特征在于,步骤(1)中所述的花状CuS采用以下方法制备得到:
将含二价铜的化合物和溶剂混合,在75~150℃下充分搅拌15~60min后,再加入含硫化合物,保温处理30~60min,然后将上述溶液转移至水热反应釜中,在135~200℃下密封加热反应3~30h,降温至室温,过滤,收集和洗涤产物过滤,真空干燥,研磨得到花状CuS。
3.根据权利要求2中所述的一种超疏水防紫外线纺织品的制备方法,其特征在于,所述的含二价铜的化合物为氯化铜、溴化铜、醋酸铜或硫酸铜,所述的溶剂为水或多元醇类化合物,所述的含硫化合物为硫脲、硫化钠、硫化钾、二甲基亚砜、二硫化碳或硫代乙酰胺。
4.根据权利要求2中所述的一种超疏水防紫外线纺织品的制备方法,其特征在于,所述的含二价铜的化合物与含硫化合物的摩尔比为10:1~3:1,含二价铜的化合物在溶剂中的浓度为3~16wt%。
5.根据权利要求1所述的一种超疏水防紫外线纺织品的制备方法,其特征在于,步骤(1)中,所述的聚硅氧烷为聚二甲基硅氧烷、氨乙基聚硅氧烷或氨丙基聚硅氧烷,所述的交联剂为氨丙基三甲氧基硅烷、氨丙基三乙氧基硅烷、氨乙基三甲氧基硅烷或氨乙基三乙氧基硅烷,所述的溶剂为四氢呋喃、二氯甲烷、三氯甲烷或异丙醇。
6.根据权利要求1所述的一种超疏水防紫外线纺织品的制备方法,其特征在于,步骤(1)中,超声分散时间为10-100min。
7.根据权利要求1所述的一种超疏水防紫外线纺织品的制备方法,其特征在于,步骤(2)中所述的纺织品为涤纶、锦纶、腈纶或其混纺机织物或针织物。
8.根据权利要求1所述的一种超疏水防紫外线纺织品的制备方法,其特征在于,步骤(2)中浸渍时间为10~80min,烘干温度为80~100℃,烘干时间为3-12min;焙烘温度是120~200℃,焙烘时间为5~90min。
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