CN106637924B - 一种抗菌纺织品及其制备方法 - Google Patents
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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
- D06M11/73—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
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Abstract
本发明提供一种抗菌纺织品及其制备方法,纺织品经改性后,于氧化石墨烯和聚乙烯吡咯烷酮等N‑乙烯基酰胺类聚合物水溶液中浸渍生成氧化石墨烯‑N‑乙烯基酰胺类聚合物膜,然后与碘自组装,得到抗菌纺织品,该抗菌纺织品一方面克服氧化石墨烯在织物表面的结合量少和不牢固的缺点,另一方面充分发挥氧化石墨烯、聚乙烯吡咯烷酮等N‑乙烯基酰胺类聚合物和碘三者的生物相容性优良特性,借助优良的抗菌性用于医护用品的开发和使用。
Description
技术领域
本发明属于纺织品功能整理技术领域,特别涉及一种氧化石墨烯/碘复合抗菌纺织品的制备方法。
背景技术
石墨烯是21世纪的新型“材料之王”,具有着强度高、韧性好,透明和导电等多种优良特性,被广泛用于材料、医学、电学、纺织等各领域的研究。石墨烯在纺织品功能整理方面应用较多,借助自身的优良性能,对整理织物的导电、阻燃、拒水、抗紫外线等影响显著。近年来,石墨烯与织物结合用于柔性电极的制备已有初步成果,石墨烯在电池,导电纺织品、内暖融等方面也正在加紧实现量产化。
氧化石墨烯(GO)是石墨烯经氧化剥离生成的衍生物,表面具有较多的羟基、羧基等含氧官能团,为石墨烯在纺织行业的应用提供了契机。GO在织物表面的粘附成膜只需要通过简单的浸渍、沉积或静电结合的方法实现,还原剂又进一步促进了石墨烯在织物表面形成较为牢固的薄膜结构。为了更多地吸附GO分子,超声法、真空过滤沉积法、抽滤法、层层自组装技术等都均有研究,此外,采用阳离子型表面改性剂对织物进行预处理或GO表面阳离子改性都较好地提高了织物与GO的结合量。最新的科学研究表明,溶液状态下的GO能够通过细菌细胞膜破坏、OH-氧化和表面接触作用多种方式致死细菌,其溶液在较低浓度的情况下抑菌率达99%以上。然而,片层状的GO未能充分发挥抗菌性能,一方面由于GO的亲水性导致与织物不能牢固结合,另一方面,相互键合作用减少了分子结构中的含氧官能团的存在,从而减弱了GO的抗菌效果。
聚乙烯吡咯烷酮(PVP)是N-乙烯基酰胺类非离子型高分子化合物,可由单体乙烯基吡咯烷酮(NVP)为原料,通过本体聚合、溶液聚合等方法得到。PVP具有优良的生物相容性,而且成膜性、粘结性较好,在研究中常用于人体相容性材料、生物薄膜等的添加剂。在纺织行业,PVP则较多地作为一种染整助剂或前处理复配溶剂使用。PVP对碘的吸附络合是一大特色,在医学领域聚维酮碘已广泛用于清洁杀菌的特效药物,碘络合不但可以充分发挥两者的细胞相容性特征,而且抗菌效果也比较显著。此外,PVP还能与GO以氢键键合,表现出较好的粘结效果。
专利CN201410554360.6采用GO及其衍生物水溶液浸渍的方式即可用于多种织物的功能整理,并赋予织物导电、拒水、抗紫外等多种优良性能。青岛大学曲丽君教授在阳离子改性预处理织物表面采用层层自组装技术,成功地将GO整理到织物上,在与其他特性物质复配的基础上使织物在抗紫外线、导电、运红外发射、电磁屏蔽性、电热性能等方面都获得显助提升。Surajit Some等直接利用超声混合的方法制得氧化石墨烯碘(GO-I)复合薄膜(Some S,Sohn J S,Kim J,et al.Scientific reports,2016,6.),不仅具有较低的抑菌浓度和明显的抑菌圈效果,而且人体细胞在该膜存在条件下成活率高达98%,显出极好的人体相容性。
然而,印染整理过程中通过直接浸渍超声的方式能够在织物表面聚集的GO量非常有限;采用浸轧法则对Hummers法所制备的GO溶液来说,杂质的存在尤为明显;对织物的阳离子改性处理局限于GO在织物表面的絮凝结合,未能有如期的牢度效果。生活常用的碘酒、碘伏等消毒杀菌液较多地用于外伤口感染的简单处理,且遇到棉织物其抗菌性会受到影响而降低,作为一种极易挥发的物质,碘的应用还要依赖具有络合性能的高分子化合物才能发挥理想的效果。氧化石墨烯作为一种新型的高效抗菌剂,其在纺织行业的应用也会对医疗用品的发展起着较为重要的影响,因此解决这些问题具有重大的意义。
发明内容
为解决上述技术问题,本发明的目的是提供一种抗菌纺织品的制备方法。
本发明的一种抗菌纺织品的制备方法(制备方法中提及到的所有水溶液,溶剂优选去离子水),包括以下步骤:
(1)采用Hummers法制备氧化石墨烯(GO),具体如下:
氧化石墨烯的合成采用典型的低温、中温和高温三步骤进行:低温反应时,将浓硫酸与石墨烯和硝酸钠在容器中搅拌混合均匀,并放入冰浴(0-5℃)中反应15-30min,优选20min;中温反应时,移去冰浴并将容器转入35℃下,加入高锰酸钾,搅拌反应1-2h,优选1.5h,然向缓慢加入蒸馏水;高温反应时,将容器转入95℃下搅拌反应25-40min,优选30min,最后,加入蒸馏水终止反应,加入30%的H2O2去除过量的高锰酸钾,用足量的稀盐酸(体积比1:10)清洗2-3次去除MnO2杂质,再用大量的蒸馏水洗至溶液呈中性为止,抽滤烘干,得到氧化石墨烯,称取一定量的GO溶于水中超声处理约30min制得GO水溶液。
(2)将纺织品浸渍于浴比(指纺织品与染液等的重量比例)为1:50阳离子改性剂(如阳离子聚电解质水溶液)水溶液中,在75-98℃下处理30-90min,得到阳离子改性的纺织品。
(3)将步骤(2)中得到的阳离子改性的纺织品依次浸渍于氧化石墨烯水溶液和N-乙烯基酰胺类聚合物(分子式(C6H9NO)n)水溶液中,分别处理15-40min,将阳离子改性的纺织品浸渍于氧化石墨烯水溶液中处理后,先在25-60℃下干燥,然后再浸渍于N-乙烯基酰胺类聚合物水溶液中,最后25-60℃下干燥,温度过高会导致氧化石墨烯的热还原,从而失去抗菌性而成为具有导电性能的石墨烯,得到含有氧化石墨烯-N-乙烯基酰胺类聚合物膜的纺织品。
(4)将步骤(3)中得到的含有氧化石墨烯-N-乙烯基酰胺类聚合物膜的纺织品浸渍于碘离子溶液(溶剂为水或乙醇)中1-6h,以保证碘离子的充分接触络合,达到预期的效果,碘离子充分接触络合到氧化石墨烯-N-乙烯基酰胺类聚合物膜的表面和内部,得到所述抗菌纺织品。
进一步的,所述纺织品为棉、麻、蚕丝、羊毛纤维、涤纶及腈纶等的纯纺、混纺及交织织物,也同样适用于无纺布。
进一步的,所述N-乙烯基酰胺类聚合物为聚乙烯吡咯烷酮(PVP)等。
进一步的,步骤(2)中,所述阳离子改性剂为十六烷基三甲基溴化铵(CTAB)、聚乙烯亚胺(PEI)、聚二甲基二烯丙基氯化铵(PDM)、邻苯二甲酸二乙二醇二丙烯酸酯(PDDA)和聚乙烯胺中的一种或几种。
进一步的,步骤(2)中,所述阳离子改性剂的浓度为1-10g/L。
进一步的,步骤(3)中,所述氧化石墨烯水溶液中氧化石墨烯的浓度为0.5-12mg/ml。
进一步的,步骤(3)中,所述N-乙烯基酰胺类聚合物水溶液中N-乙烯基酰胺类聚合物的质量百分数为3-12%,优选3-10%,以提高氧化石墨烯-N-乙烯基酰胺类聚合物膜在织物上的耐久性和更多地促进I3 -和I5 -粒子的络合,进一步提升纺织品的对细菌真菌的抗性和促进人体细胞的生长。
进一步的,步骤(4)中,所述碘离子溶液为碘-碘化钾溶液或碘的乙醇溶液中的一种或组合,碘-碘化钾溶液或碘的乙醇溶液均可用于碘离子的吸附络合,碘-碘化钾溶液或碘的乙醇溶液中碘单质的质量百分数为0.1-1.2%,由于碘的溶解性较低,而且较易损失,这也是用量较低的原因,而纺织品中氧化石墨烯-N-乙烯基酰胺类聚合物膜对碘的络合可以通过延长作用时间来实现,不但节约材料而且避免因含量过高而超出含量而对人体健康产生不利的影响。
进一步的,步骤(4)中,碘离子与氧化石墨烯-聚乙烯吡咯烷酮等N-乙烯基酰胺类聚合物膜络合的温度为40-60℃,避免温度过低或过高而导致有效碘浓度的降低。
本发明的一种抗菌纺织品,由上述方法制得,该纺织品为氧化石墨烯-碘(GO-I)复合整理的抗菌纺织品,一方面克服GO在织物表面的结合量少和不牢固的缺点,另一方面充分发挥GO、PVP和I三者的生物相容性优良特性,借助优良的抗菌性用于医护用品的开发和使用。
借由上述方案,本发明至少具有以下优点:
本发明采用层层自组装技术,借助物质之间的静电吸引或其他键合方式,达到GO、PVP、I三者与纺织品的牢固结合,方法简单易行而且分布均匀。反应过程中不涉及到高温、强酸碱环境和其他化学物质的添加辅助作用,环境友好且健康完全。此外,新型GO材料和广谱杀菌剂聚维酮碘的优良抗菌性和生物相容性可以协同提升而发挥较好的作用。在此基础上,该处理方式可以适应多种材料的要求,在医用敷料领域可以更好地发挥敷料的增生、抗菌和保护等作用。
上述说明仅是本发明技术方案的概述,为了能够更清楚了解本发明的技术手段,并可依照说明书的内容予以实施,以下以本发明的较佳实施例并配合附图详细说明如后。
附图说明
图1是本发明的实施例1中制备方法的流程示意图。
具体实施方式
下面结合附图和实施例,对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明,但不用来限制本发明的范围。
采用Hummers法制备氧化石墨烯(GO),将浓硫酸与石墨烯和硝酸钠在容器中搅拌混合均匀,并放入冰浴中反应20min;移去冰浴并将容器转入35℃下,加入高锰酸钾,搅拌反应1.5h,然向缓慢加入蒸馏水;将容器转入95℃下搅拌反应30min,最后,加入蒸馏水终止反应,加入30%的H2O2去除过量的高锰酸钾,用足量的稀盐酸(体积比1:10)清洗3-5次去除MnO2杂质,再用大量的蒸馏水洗至溶液呈中性为止,抽滤烘干,得到氧化石墨烯。
实施例1:抗菌棉织物的制备方法,流程图如图1所示,包括以下步骤:
(1)称取上述制备的氧化石墨烯于水中超声处理约30min制得浓度为5g/L GO水溶液,使用前将该溶液于超声清洗器中在300w功率的条件下清洗30min。
(2)剪取棉织物(尺寸大小为10cm*5cm)浸润到3g/L的CTAB溶液中改性处理约1h,处理过程温度为85℃,处理完毕置于70℃热风烘燥机烘干即可,得到阳离子改性的棉织物。
(3)阳离子表面改性的棉织物经烘干后直接常温浸渍5g/L的GO水溶液20min,取出后在60℃条件下烘干10min,并再次浸入质量分数为3%的PVP水溶液中,20min后将样品取出置于60℃烘箱烘干10min,得到含有氧化石墨烯-聚乙烯吡咯烷酮膜的棉织物。
(4)最后将含有氧化石墨烯-聚乙烯吡咯烷酮膜的棉织物于50℃条件下、在质量分数为0.5%的碘钾溶液中浸渍处理60min,取出棉织物浸渍于碘钾溶液中以除去未络合的碘,最后室温晾干,得到抗菌棉织物。
实施例2
本实施例与实施例1的步骤相同,其区别在于:步骤(1)中GO水溶液浓度为2g/L;步骤(4)中碘钾溶液中碘质量分数提高到1%,处理过程中,实验现象说明GO水溶液的浓度对整理效果的影响不及碘浓度影响大。
实施例3
本实施例与实施例1的步骤相同,其区别在于:步骤(1)中,5g/L GO水溶液在600w功率的条件下清洗30min;步骤(2)中,精练漂白后的机织疏麻织物在80℃条件下处理30min;步骤(3)中,浸渍于质量分数为5%的PVP水溶液中20min;步骤(4)中,将疏麻织物放入碘钾溶液中处理90min,处理完毕后用碘钾溶液浸渍10min以除去未络合的碘。
以上所述仅是本发明的优选实施方式,并不用于限制本发明,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和变型,这些改进和变型也应视为本发明的保护范围。
Claims (9)
1.一种抗菌纺织品的制备方法,其特征在于,包括以下步骤:
(1)将纺织品浸渍于阳离子改性剂水溶液中进行改性处理,得到阳离子改性的纺织品;
(2)将步骤(1)中得到的阳离子改性的纺织品依次浸渍于氧化石墨烯水溶液和N-乙烯基酰胺类聚合物水溶液中处理,得到含有氧化石墨烯-N-乙烯基酰胺类聚合物膜的纺织品;所述N-乙烯基酰胺类聚合物为聚乙烯吡咯烷酮;
(3)将步骤(2)中得到的含有氧化石墨烯-N-乙烯基酰胺类聚合物膜的纺织品浸渍于碘离子溶液中,使碘离子与氧化石墨烯-N-乙烯基酰胺类聚合物膜络合,得到所述抗菌纺织品。
2.根据权利要求1所述的制备方法,其特征在于:所述纺织品为棉、麻、蚕丝、羊毛纤维、涤纶、腈纶中的一种或几种制成的织物。
3.根据权利要求1所述的制备方法,其特征在于:步骤(1)中,所述阳离子改性剂为十六烷基三甲基溴化铵、聚乙烯亚胺、聚二甲基二烯丙基氯化铵、邻苯二甲酸二乙二醇二丙烯酸酯和聚乙烯胺中的一种或几种。
4.根据权利要求1所述的制备方法,其特征在于:步骤(1)中,所述阳离子改性剂的浓度为1-10g/L。
5.根据权利要求1所述的制备方法,其特征在于:步骤(2)中,所述氧化石墨烯水溶液中氧化石墨烯的浓度为0.5-12mg/mL。
6.根据权利要求1所述的制备方法,其特征在于:步骤(2)中,所述N-乙烯基酰胺类聚合物水溶液中N-乙烯基酰胺类聚合物的质量百分数为3-12%。
7.根据权利要求1所述的制备方法,其特征在于:步骤(3)中,所述碘离子溶液为碘-碘化钾溶液或碘的乙醇溶液中的一种或组合。
8.根据权利要求1所述的制备方法,其特征在于:步骤(3)中,碘离子与氧化石墨烯-N-乙烯基酰胺类聚合物膜络合的温度为40-60℃。
9.一种由权利要求1-8中任一所述的制备方法制得的抗菌纺织品。
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