CN106337276B - 一种基于石墨烯泡沫改性的壳聚糖面料的制备方法 - Google Patents
一种基于石墨烯泡沫改性的壳聚糖面料的制备方法 Download PDFInfo
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Abstract
本发明提供一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,包括以下步骤:将壳聚糖纤维和壳寡糖纤维混纺形成混纺纱,将混纺纱浸入含3‑氯‑2‑羟丙基三甲基氯化铵的溶液中,加热搅拌,乙醇水洗,烘干得到季铵盐改性的壳聚糖和壳寡糖混纺纤维;将步季铵盐改性的壳聚糖和壳寡糖混纺纤维作为原料,经织造形成壳聚糖面料;将壳聚糖面料浸入氧化石墨烯溶液中,振荡,取出,烘干固化,再浸入含还原剂和纳米二氧化钛的整理液中,加热反应,取出,真空干燥,水洗去除表面结合不牢的物质,烘干,得到基于石墨烯泡沫改性的壳聚糖面料。
Description
技术领域
本发明属于纺织材料技术领域,具体涉及一种基于石墨烯泡沫改性的壳聚糖面料的制备方法。
背景技术
随着人们健康和保健意识的增强,多功能的绿色环保面料越来越受到消费者的亲睐。多糖是一种天然高分子化合物,甲壳素是一种从虾蟹外壳、真菌剂藻类植物细胞壁中提取的天然多糖,壳聚糖是脱乙酰的甲壳素,壳聚糖具有较高的生物活性,而壳寡糖又名壳低聚糖,壳寡糖是低聚合度的壳聚糖,随着分子量的降低,壳寡糖除了具备壳聚糖的一些类特性外,还表现出更加优异的水溶性、吸湿锁水性和抗菌抑菌等性能,因子基于壳聚糖及其衍生物的面料产品的开发较多。中国文献(“壳聚糖多组分功能性针织面料的开发”,杨立敬,针织工业,2013年11期,第1-3页)公开了将壳聚糖混纺纱与低温氨纶弹性纤维作为原料,纬平针组织作为组织结构,在单面开幅织布机上织造形成针织面料。中国专利CN 104757724A公开的一种吸湿速干壳聚糖棉针织面料,将棉纤维与壳聚糖纤维混纺形成混纺纱,再与丙纶原液色纺纤维作为原料,经织造形成吸湿速干的针织面料。由上述现有技术可知,目前壳聚糖纤维多是作为原料之一,与天然纤维或者化学纤维混纺或者混织制备形成功能性面料,但是针对纯壳聚糖面料改性方面的研究并不多见。
石墨烯是目前研究较为热点的纳米材料之一,石墨烯是一种新型的碳纳米轻质材料,具有超高的强度、电导率、热导率等性能。石墨烯及其衍生物在纺织品改性方面的应用也较多。中国专利CN 104328653B公开的一种氧化石墨烯衍生物用于纺织品多功能整理的方法,将氧化石墨烯及其衍生物与阴离子表面活性剂、含氮化合物混合形成混合溶液,将混合溶液经紫外线照射反应形成氮掺杂氧化石墨烯及其衍生物混合液,将织物浸渍其中,再进行还原,继而得到导电、抗紫外和拒水的织物。中国专利CN 103603081B公开的一种石墨烯增强聚合物多孔海绵纤维的制备方法,将石墨烯溶液与聚合物溶液混合,经湿法纺丝成纤,在经水洗、还原、水洗、冷冻干燥或者超临界干燥得到石墨烯增强聚合物多孔海绵纤维。有上述现有技术可知,石墨烯在纺织方面的应用多以薄膜的形态附着于纤维的表面,或者与混合物混纺形成纤维,但是石墨烯的难分散易聚合的问题将会难以控制石墨烯在纤维内部和表面的用量,难以均匀分散和量化。
发明内容
本发明要解决的技术问题是提供一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,采用壳聚糖和壳寡糖混纺纤维作为原料制备形成面料,将面料先后经氧化石墨烯、还原剂和纳米二氧化钛处理,得到基于石墨烯泡沫改性的壳聚糖面料。本发明制备的基于石墨烯泡沫改性的壳聚糖面料表面附着石墨烯泡沫和纳米二氧化钛,制备的面料不仅绿色安全,抗菌,还具有抗紫外,自清洁,抗静电等功能。
为解决上述技术问题,本发明的技术方案是:
一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,包括以下步骤:
(1)将壳聚糖纤维和壳寡糖纤维,以60-80:40-20的比例混纺形成混纺纱,将混纺纱浸入含3-氯-2-羟丙基三甲基氯化铵的溶液中,加热搅拌,乙醇水洗,烘干得到季铵盐改性的壳聚糖和壳寡糖混纺纤维;
(2)将步骤(1)制备的季铵盐改性的壳聚糖和壳寡糖混纺纤维作为原料,经织造形成壳聚糖面料;
(3)将步骤(2)制备的壳聚糖面料浸入氧化石墨烯溶液中,振荡,取出,烘干固化,再浸入含还原剂和纳米二氧化钛的整理液中,加热反应,取出,真空干燥,水洗去除表面结合不牢的物质,烘干,得到基于石墨烯泡沫改性的壳聚糖面料。
作为上述技术方案的优选,所述步骤(1)中,混纺纱的线密度为16.7-20.4tex。
作为上述技术方案的优选,所述步骤(1)中,含3-氯-2-羟丙基三甲基氯化铵的溶液中含有3-氯-2-羟丙基三甲基氯化铵、异丙醇和去离子水,含3-氯-2-羟丙基三甲基氯化铵的溶液中3-氯-2-羟丙基三甲基氯化铵的质量分数为25-30%。
作为上述技术方案的优选,所述步骤(1)中,含3-氯-2-羟丙基三甲基氯化铵的溶液的pH值为8-8.5。
作为上述技术方案的优选,所述步骤(2)中,壳聚糖面料为无纺布、机织面料或者针织面料。
作为上述技术方案的优选,所述步骤(3)中,氧化石墨烯溶液的质量分数为5-8%,浴比为1:30。
作为上述技术方案的优选,所述步骤(3)中,还原剂为水合肼,含还原剂和纳米二氧化钛的整理液中水合肼的质量分数为15-20%,纳米二氧化钛的质量分数为5-10%。
作为上述技术方案的优选,所述步骤(3)中,含还原剂和纳米二氧化钛的整理液中还含有助剂,所述助剂为表面活性剂十二烷基苯磺酸钠。
与现有技术相比,本发明具有以下有益效果:
(1)本发明制备的基于石墨烯泡沫改性的壳聚糖面料主要原料为壳聚糖纤维和壳寡糖纤维,壳聚糖纤维和壳寡糖纤维基本结构单元相同,但聚合度不同,壳寡糖的分子量较小,具有独特的生物活性和生理功能,水溶性好,保湿抑菌,将壳寡糖纤维与壳聚糖纤维混纺形成混饭纱,在不降低纤维机械性能的同时,显著提高混纺纱的抗菌吸湿保湿等性能,因此制备的面料具有舒适柔软,吸湿透气,绿色抗菌等功能。
(2)本发明制备的基于石墨烯泡沫改性的壳聚糖面料表面附着石墨烯泡沫和纳米二氧化钛,石墨烯泡沫具有优异的纳米特性,还具有良好的导电、吸附性能,可以将纳米二氧化钛牢固的吸附在面料的表面,提高面料的使用性能,此外还赋予面料抗紫外,自清洁,抗静电等功能。
(3)本发明制备的基于石墨烯泡沫改性的壳聚糖面料制备方法简便,可操控性强,面料的功能性好,性能多且稳定,面料的经济价值高。
具体实施方式
下面将结合具体实施例来详细说明本发明,在此本发明的示意性实施例以及说明用来解释本发明,但并不作为对本发明的限定。
实施例1:
(1)将壳聚糖纤维和壳寡糖纤维,以60:40的比例混纺形成16.7tex的混纺纱,将混纺纱,以浴比1:40,浸入质量分数为25%的3-氯-2-羟丙基三甲基氯化铵的异丙醇水溶液中,pH值为8,在60℃下加热搅拌30min,用乙醇充分水洗,烘干得到季铵盐改性的壳聚糖和壳寡糖混纺纤维。将季铵盐改性的壳聚糖和壳寡糖混纺纤维作为原料,经织造形成壳聚糖机织面料。
(2)将水合肼、纳米二氧化钛和十二烷基苯磺酸钠加入水溶液中充分搅拌形成整理液中,其中水合肼的质量分数为15%,纳米二氧化钛的质量分数为5%。
(3)将壳聚糖面料,以浴比为1:30,先浸入质量分数为5%的氧化石墨烯溶液中,在45℃下振荡30min,取出,烘干固化,再以浴比为1:30浸入整理液中,150℃下加热反应4h,取出,真空干燥,水洗去除表面结合不牢的物质,烘干,得到基于石墨烯泡沫改性的壳聚糖面料。
实施例2:
(1)将壳聚糖纤维和壳寡糖纤维,以80:20的比例混纺形成20.4tex的混纺纱,将混纺纱,以浴比1:50,浸入质量分数为30%的3-氯-2-羟丙基三甲基氯化铵的异丙醇水溶液中,pH值为8.5,在80℃下加热搅拌30min,用乙醇充分水洗,烘干得到季铵盐改性的壳聚糖和壳寡糖混纺纤维。将季铵盐改性的壳聚糖和壳寡糖混纺纤维作为原料,经织造形成壳聚糖无纺布。
(2)将水合肼、纳米二氧化钛和十二烷基苯磺酸钠加入水溶液中充分搅拌形成整理液中,其中水合肼的质量分数为20%,纳米二氧化钛的质量分数为10%。
(3)将壳聚糖面料,以浴比为1:30,先浸入质量分数为8%的氧化石墨烯溶液中,在60℃下振荡30min,取出,烘干固化,再以浴比为1:30浸入整理液中,160℃下加热反应6h,取出,真空干燥,水洗去除表面结合不牢的物质,烘干,得到基于石墨烯泡沫改性的壳聚糖面料。
实施例3:
(1)将壳聚糖纤维和壳寡糖纤维,以70:30的比例混纺形成18.2tex的混纺纱,将混纺纱,以浴比1:45,浸入质量分数为28%的3-氯-2-羟丙基三甲基氯化铵的异丙醇水溶液中,pH值为8.2,在70℃下加热搅拌30min,用乙醇充分水洗,烘干得到季铵盐改性的壳聚糖和壳寡糖混纺纤维。将季铵盐改性的壳聚糖和壳寡糖混纺纤维作为原料,经织造形成壳聚糖针织面料。
(2)将水合肼、纳米二氧化钛和十二烷基苯磺酸钠加入水溶液中充分搅拌形成整理液中,其中水合肼的质量分数为18%,纳米二氧化钛的质量分数为8%。
(3)将壳聚糖面料,以浴比为1:30,先浸入质量分数为6%的氧化石墨烯溶液中,在50℃下振荡30min,取出,烘干固化,再以浴比为1:30浸入整理液中,155℃下加热反应5h,取出,真空干燥,水洗去除表面结合不牢的物质,烘干,得到基于石墨烯泡沫改性的壳聚糖面料。
实施例4:
(1)将壳聚糖纤维和壳寡糖纤维,以65:35的比例混纺形成17.2tex的混纺纱,将混纺纱,以浴比1:40,浸入质量分数为30%的3-氯-2-羟丙基三甲基氯化铵的异丙醇水溶液中,pH值为8.3,在65℃下加热搅拌30min,用乙醇充分水洗,烘干得到季铵盐改性的壳聚糖和壳寡糖混纺纤维。将季铵盐改性的壳聚糖和壳寡糖混纺纤维作为原料,经织造形成壳聚糖无纺布。
(2)将水合肼、纳米二氧化钛和十二烷基苯磺酸钠加入水溶液中充分搅拌形成整理液中,其中水合肼的质量分数为20%,纳米二氧化钛的质量分数为5%。
(3)将壳聚糖面料,以浴比为1:30,先浸入质量分数为8%的氧化石墨烯溶液中,在45℃下振荡30min,取出,烘干固化,再以浴比为1:30浸入整理液中,155℃下加热反应5h,取出,真空干燥,水洗去除表面结合不牢的物质,烘干,得到基于石墨烯泡沫改性的壳聚糖面料。
实施例5:
(1)将壳聚糖纤维和壳寡糖纤维,以75:25的比例混纺形成19.8tex的混纺纱,将混纺纱,以浴比1:40,浸入质量分数为30%的3-氯-2-羟丙基三甲基氯化铵的异丙醇水溶液中,pH值为8,在65℃下加热搅拌30min,用乙醇充分水洗,烘干得到季铵盐改性的壳聚糖和壳寡糖混纺纤维。将季铵盐改性的壳聚糖和壳寡糖混纺纤维作为原料,经织造形成壳聚糖机织面料。
(2)将水合肼、纳米二氧化钛和十二烷基苯磺酸钠加入水溶液中充分搅拌形成整理液中,其中水合肼的质量分数为18%,纳米二氧化钛的质量分数为10%。
(3)将壳聚糖面料,以浴比为1:30,先浸入质量分数为7%的氧化石墨烯溶液中,在55℃下振荡30min,取出,烘干固化,再以浴比为1:30浸入整理液中,160℃下加热反应4h,取出,真空干燥,水洗去除表面结合不牢的物质,烘干,得到基于石墨烯泡沫改性的壳聚糖面料。
实施例6:
(1)将壳聚糖纤维和壳寡糖纤维,以80:20的比例混纺形成20.4tex的混纺纱,将混纺纱,以浴比1:40,浸入质量分数为25%的3-氯-2-羟丙基三甲基氯化铵的异丙醇水溶液中,pH值为8.5,在65℃下加热搅拌30min,用乙醇充分水洗,烘干得到季铵盐改性的壳聚糖和壳寡糖混纺纤维。将季铵盐改性的壳聚糖和壳寡糖混纺纤维作为原料,经织造形成壳聚糖无纺布。
(2)将水合肼、纳米二氧化钛和十二烷基苯磺酸钠加入水溶液中充分搅拌形成整理液中,其中水合肼的质量分数为20%,纳米二氧化钛的质量分数为5%。
(3)将壳聚糖面料,以浴比为1:30,先浸入质量分数为7%的氧化石墨烯溶液中,在55℃下振荡30min,取出,烘干固化,再以浴比为1:30浸入整理液中,160℃下加热反应6h,取出,真空干燥,水洗去除表面结合不牢的物质,烘干,得到基于石墨烯泡沫改性的壳聚糖面料。
经检测,实施例1-6制备的基于石墨烯泡沫改性的壳聚糖面料的克重、抗菌性、抗静电、抗紫外和透气性的结果如下所示:
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | |
克重(g/m2) | 168 | 189 | 172 | 169 | 180 | 173 |
抗菌率(%) | 76 | 84 | 81 | 83 | 79 | 80 |
织物表面电阻率(×106Ω) | 3.2 | 2.1 | 2.9 | 2.4 | 3.0 | 2.8 |
紫外线屏蔽率(%) | 65 | 67 | 64 | 68 | 64 | 63 |
透气量(L/m2·S) | 1526 | 1734 | 1698 | 1593 | 1648 | 1599 |
由上表可见,本发明制备的基于石墨烯泡沫改性的壳聚糖面料具有轻薄透气、抗菌、抗紫外、抗静电的性能。
上述实施例仅例示性说明本发明的原理及其功效,而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下,对上述实施例进行修饰或改变。因此,举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变,仍应由本发明的权利要求所涵盖。
Claims (8)
1.一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,其特征在于,包括以下步骤:
(1)将壳聚糖纤维和壳寡糖纤维,以60-80:40-20的比例混纺形成混纺纱,将混纺纱浸入含3-氯-2-羟丙基三甲基氯化铵的溶液中,加热搅拌,乙醇水洗,烘干得到季铵盐改性的壳聚糖和壳寡糖混纺纤维;
(2)将步骤(1)制备的季铵盐改性的壳聚糖和壳寡糖混纺纤维作为原料,经织造形成壳聚糖面料;
(3)将步骤(2)制备的壳聚糖面料浸入氧化石墨烯溶液中,振荡,取出,烘干固化,再浸入含还原剂和纳米二氧化钛的整理液中,加热反应,取出,真空干燥,水洗去除表面结合不牢的物质,烘干,得到基于石墨烯泡沫改性的壳聚糖面料。
2.根据权利要求1所述的一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,其特征在于:所述步骤(1)中,混纺纱的线密度为16.7-20.4tex。
3.根据权利要求1所述的一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,其特征在于:所述步骤(1)中,含3-氯-2-羟丙基三甲基氯化铵的溶液中含有3-氯-2-羟丙基三甲基氯化铵、异丙醇和去离子水,含3-氯-2-羟丙基三甲基氯化铵的溶液中3-氯-2-羟丙基三甲基氯化铵的质量分数为25-30%。
4.根据权利要求1所述的一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,其特征在于:所述步骤(1)中,含3-氯-2-羟丙基三甲基氯化铵的溶液的pH值为8-8.5。
5.根据权利要求1所述的一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,其特征在于:所述步骤(2)中,壳聚糖面料为无纺布、机织面料或者针织面料。
6.根据权利要求1所述的一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,其特征在于:所述步骤(3)中,氧化石墨烯溶液的质量分数为5-8%,浴比为1:30。
7.根据权利要求1所述的一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,其特征在于:所述步骤(3)中,还原剂为水合肼,含还原剂和纳米二氧化钛的整理液中水合肼的质量分数为15-20%,纳米二氧化钛的质量分数为5-10%。
8.根据权利要求1所述的一种基于石墨烯泡沫改性的壳聚糖面料的制备方法,其特征在于:所述步骤(3)中,含还原剂和纳米二氧化钛的整理液中还含有助剂,所述助剂为表面活性剂十二烷基苯磺酸钠。
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