CN111576036B - 一种纳米防污、抑菌、透气的环保面料及其制备工艺 - Google Patents
一种纳米防污、抑菌、透气的环保面料及其制备工艺 Download PDFInfo
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Abstract
本发明提供一种纳米防污、抑菌、透气的环保面料制备工艺,将除杂后的棉绒纤维经过热碱处理,加捻、纺纱加工为纱线后通过硅烷偶联剂对纱线表面进行氨基化改性,再以环氧基封端的聚二甲基硅氧烷与纱线表面的氨基进行开环反应,将聚二甲基硅氧烷链在纱线表面接枝,显著降低了纱线的表面张力,再以表面改性的纱线织造成面料,不仅保留面料良好透气性,而且具有疏水防油的性能,同时,接枝的聚二甲基硅氧烷链可以在纱线表面建立薄层的空气膜,可以防止污染物和细菌的粘附,具有易清洁、抑菌的作用。
Description
技术领域
本发明涉及功能纤维面料领域,具体涉及一种纳米防污、抑菌、透气的环保面料及其制备工艺。
背景技术
随着经济的高速发展,我们所处的社会环境也越来越多样化复杂化。在日常生活中,我们总是会不可避免的碰到一些污渍,厨房的油污、饮料的滴溅、食物的掉落等,这些都是我们身边无形的服装杀手。需要一种能隔绝这些污渍的面料,而现有的疏水防污面料大多是通过直接在面料上设置涂层制备,其疏水防油性能较好,但直接在面料上设置涂层会极大地降低了面料的透气性,且手感较差。
发明内容
针对上述问题,本发明提供一种纳米防污、抑菌、透气的环保面料制备工艺。
本发明的目的采用以下技术方案来实现:
一种纳米防污、抑菌、透气的环保面料的制备工艺,包括以下步骤:
S1、纤维前处理
将除杂后的棉绒纤维浸入热的氢氧化钠溶液中浸泡清洗,浸泡完成后清水漂洗,70-90℃干燥,得到预处理的棉纤维;
S2、纱线的表面改性
将预处理的的棉纤维经加捻、纺纱加工为纱线后,以硅烷偶联剂进行纱线的氨丙基改性,得到表面改性纱线;
S3、中间体制备
数均分子量为4000-7500的氢封端聚甲基硅氧烷与烯丙基缩水甘油醚按摩尔比2.1:1混合,搅拌均匀后升温至80℃,加入反应物质量0.5-0.6%的1wt.%浓度的氯铂酸-异丙醇溶液,加入终浓度0.01%的对羟基苯甲醚,升温至85℃保温搅拌反应3h,产物经真空蒸馏后得到淡黄色的环氧基封端聚二甲基硅氧烷;
S4、纱线表面接枝改性
环氧基封端聚二甲基硅氧烷以异丙醇稀释,稀释比例为2-5:100,表面改性纱线移入反应釜中,加入稀释的环氧基封端聚二甲基硅氧烷溶液,液固比在50-100:1,密封反应釜后,在55-65℃下保温反应5h,反应完成后挤干,再以异丙醇漂洗,减压蒸除溶剂后,得到表面接枝改性纱线;
S5、面料织造
将所述表面接枝改性纱线织造为面料。
优选的,所述棉绒纤维是以长绒棉为原料,经过梳理提取的棉纤维。
优选的,步骤S1中所述氢氧化钠溶液的质量浓度在5-18%,溶液温度60-80℃,浸泡时间10-30min。
优选的,步骤S2中表面改性纱线由负载氨丙基改性纳米二氧化硅的棉纤维经加捻、纺纱加工为纱线得到,所述负载氨丙基改性纳米二氧化硅的棉纤维的制备方法为:
在200ml的无水乙醇中加入5ml去离子水,加入10ml的25%氨水,40-50℃恒温磁力搅拌1-2h,再加入12ml的硅酸四乙酯,继续保持恒温磁力搅拌10-12h,转速200-500rpm,反应完成后加入硅酸四乙酯质量10-30%的γ-氨丙基三甲氧基硅烷或γ-氨丙基三乙氧基硅烷,继续磁力搅拌3-4h,产物冷却后抽滤,无水乙醇洗涤5-8遍,再分散在200ml乙醇中,加入1g羟丙基纤维素,再加入预处理的棉纤维,液固比在50-100:1,将棉纤维减压蒸除溶剂,得到负载氨丙基改性纳米二氧化硅的棉纤维。
优选的,步骤S4中,所述反应釜的填充率为60-70%。
进一步优选的,步骤S4中,纱线以异丙醇漂洗后,再以清水漂洗,干燥后再次进行纱线的表面接枝改性。
本发明的有益效果为:
(1)本申请通过纱线表面改性,再以表面改性的纱线织造成面料,不仅保留面料良好透气性,而且具有疏水防油的性能。
(2)本申请通过硅烷偶联剂对纱线表面进行氨基化改性,再以环氧基封端的聚二甲基硅氧烷与纱线表面的氨基进行开环反应,将聚二甲基硅氧烷链在纱线表面接枝,显著降低了纱线的表面张力,所述纱线织造的面料保持透气同时具有疏水疏油的性能,同时,接枝的聚二甲基硅氧烷链可以在纱线表面建立薄层的空气膜,可以防止污染物和细菌的粘附,具有易清洁、抑菌的作用。
具体实施方式
结合以下实施例对本发明作进一步描述。
本申请的实施例涉及一种纳米防污、抑菌、透气的环保面料的制备工艺,包括以下步骤:
S1、纤维前处理
将除杂后的棉绒纤维浸入热的氢氧化钠溶液中浸泡清洗,所述氢氧化钠溶液质量浓度在5-18%,溶液温度60-80℃,浸泡时间10-30min,浸泡完成后清水漂洗,70-90℃干燥,得到预处理的棉纤维;
S2、纱线的表面改性
配制质量浓度3-5%的γ-氨丙基三甲氧基硅烷或γ-氨丙基三乙氧基硅烷的乙醇溶液,得到偶联剂溶液,将预处理的的棉纤维经加捻、纺纱加工为纱线后,加入配制的偶联剂溶液,在温度50℃以下进行纱线的氨丙基改性,其中,棉纤维与偶联剂的质量比为2-3:1,浸泡改性时间2-6h,改性完成后挤去水分,以清水漂洗,70-90℃干燥,得到表面改性纱线;
S3、中间体制备
数均分子量为4000-7500的氢封端聚甲基硅氧烷与烯丙基缩水甘油醚按摩尔比2.1:1混合,搅拌均匀后升温至80℃,加入反应物质量0.5-0.6%的1wt.%浓度的氯铂酸-异丙醇溶液,加入终浓度0.01%的对羟基苯甲醚,升温至85℃保温搅拌反应3h,产物经真空蒸馏后得到淡黄色的环氧基封端聚二甲基硅氧烷;
S4、纱线表面接枝改性
环氧基封端聚二甲基硅氧烷以异丙醇稀释,稀释比例为2-5:100,表面改性纱线移入反应釜中,加入稀释的环氧基封端聚二甲基硅氧烷溶液,液固比在50-100:1,反应釜填充率60-70%,密封反应釜后,在55-65℃下保温反应5h,反应完成后挤干,再以异丙醇漂洗,减压蒸除溶剂后,得到表面接枝改性纱线;
S5、面料织造
将所述表面接枝改性纱线织造为面料。
现有的疏水防污面料大多是通过直接在面料上设置涂层制备,其疏水防油性能较好,但直接在面料上设置涂层会极大地降低了面料的透气性,本申请通过纱线表面改性,再以表面改性的纱线织造成面料,不仅保留面料良好透气性,而且具有疏水防油的性能。
棉纤维的主要成分是纤维素,耐碱性能较好,经热碱溶液处理后,可以除去纤维表面污染,也可以使纤维的天然转曲伸直,并具有一定的光泽度,同时对纤维强度的提高也具有积极作用。
本申请通过硅烷偶联剂对纱线表面进行氨基化改性,再以环氧基封端的聚二甲基硅氧烷与纱线表面的氨基进行开环反应,将聚二甲基硅氧烷链在纱线表面接枝,基于聚二甲基硅氧烷链的位阻效应和链间排斥作用,聚二甲基硅氧烷链被拉伸并向表面垂直的方向伸展,在纱线表面形成无数的“触须”,聚二甲基硅氧烷链具有良好的生理惰性和化学稳定性,且表面张力较小,具有良好的疏水性、防水性和柔顺性,因此,接枝的聚二甲基硅氧烷链显著降低了纱线的表面张力,所述纱线织造的面料保持透气同时具有疏水疏油的性能,触感良好,耐久度强;另一方面,较于直接设置涂层的方法,本申请接枝的聚二甲基硅氧烷链可以在纱线表面建立薄层的空气膜,可以防止污染物和细菌的粘附,具有易清洁、抑菌的作用,所述可应用于防污抗菌服装领域。
优选的,所述棉绒纤维是以长绒棉为原料,经过梳理提取的棉纤维。
优选的,步骤S2中表面改性纱线由负载氨丙基改性纳米二氧化硅的棉纤维经加捻、纺纱加工为纱线得到,所述负载氨丙基改性纳米二氧化硅的棉纤维的制备方法为:
在200ml的无水乙醇中加入5ml去离子水,加入10ml的25%氨水,40-50℃恒温磁力搅拌1-2h,再加入12ml的硅酸四乙酯,继续保持恒温磁力搅拌10-12h,转速200-500rpm,反应完成后加入硅酸四乙酯质量10-30%的γ-氨丙基三甲氧基硅烷或γ-氨丙基三乙氧基硅烷,继续磁力搅拌3-4h,产物冷却后抽滤,无水乙醇洗涤5-8遍,再分散在200ml乙醇中,加入1g羟丙基纤维素,再加入预处理的棉纤维,液固比在50-100:1,将棉纤维减压蒸除溶剂,得到负载氨丙基改性纳米二氧化硅的棉纤维;
聚二甲基硅氧烷在纱线表面的均匀接枝虽然可以获得良好的疏水防油性能,但覆盖式的接枝方法极大地影响了纤维本身的光泽度,作为进一步的改进,本申请以纳米二氧化硅为连接体,将聚二甲基硅氧烷链接枝在纱线上的纤维间形成的沟槽,以减少接枝改性对纱线光泽度的影响,具体的,以硅酸四乙酯为硅源合成纳米二氧化硅,以硅烷偶联剂对二氧化硅进行氨基化改性,羟丙基纤维素有助于二氧化硅在纤维表面的负载,表面负载二氧化硅的棉纤维经加捻纺纱后容易发生脱载,而纤维间沟槽内的纳米二氧化硅则被进一步固载,形成沟槽定向氨基化的表面改性纱线,经接枝改性后在纱线沟槽内接枝聚二甲基硅氧烷链。
进一步优选的,步骤S4中,纱线以异丙醇漂洗后,再以清水漂洗,干燥后再次进行纱线的表面接枝改性。
以纳米二氧化硅为连接体虽可以减少接枝对纤维光泽度的影响,但局部集中的接枝链形成的空间位阻,以及链间排斥影响了链的进一步接枝,接枝率较低,本申请通过以强极性的水对第一次接枝改性后的纱线进行漂洗,使得相邻间的聚二甲基硅氧烷链间聚集缠结,降低空间位阻,暴露出更多的活性接枝位点,从而提高接枝率。
实施例1
一种纳米防污、抑菌、透气的环保面料的制备工艺,包括以下步骤:
S1、纤维前处理
将除杂后的棉绒纤维浸入热的氢氧化钠溶液中浸泡清洗,所述棉绒纤维是以长绒棉为原料,经过梳理提取的棉纤维,所述氢氧化钠溶液质量浓度在5-18%,溶液温度60-80℃,浸泡时间10-30min,浸泡完成后清水漂洗,70-90℃干燥,得到预处理的棉纤维;
S2、纱线的表面改性
配制质量浓度3-5%的γ-氨丙基三甲氧基硅烷或γ-氨丙基三乙氧基硅烷的乙醇溶液,得到偶联剂溶液,将预处理的的棉纤维经加捻、纺纱加工为纱线后,加入配制的偶联剂溶液,在温度50℃以下进行纱线的氨丙基改性,其中,棉纤维与偶联剂的质量比为2-3:1,浸泡改性时间2-6h,改性完成后挤去水分,以清水漂洗,70-90℃干燥,得到表面改性纱线;
S3、中间体制备
数均分子量为4000-7500的氢封端聚甲基硅氧烷与烯丙基缩水甘油醚按摩尔比2.1:1混合,搅拌均匀后升温至80℃,加入反应物质量0.5-0.6%的1wt.%浓度的氯铂酸-异丙醇溶液,加入终浓度0.01%的对羟基苯甲醚,升温至85℃保温搅拌反应3h,产物经真空蒸馏后得到淡黄色的环氧基封端聚二甲基硅氧烷;
S4、纱线表面接枝改性
环氧基封端聚二甲基硅氧烷以异丙醇稀释,稀释比例为2-5:100,表面改性纱线移入反应釜中,加入稀释的环氧基封端聚二甲基硅氧烷溶液,液固比在50-100:1,反应釜填充率60-70%,密封反应釜后,在55-65℃下保温反应5h,反应完成后挤干,以异丙醇漂洗,减压蒸除溶剂,得到表面接枝改性纱线;
S5、面料织造
将所述表面接枝改性纱线织造为面料。
实施例2
一种纳米防污、抑菌、透气的环保面料的制备工艺,包括以下步骤:
S1、纤维前处理
将除杂后的棉绒纤维浸入热的氢氧化钠溶液中浸泡清洗,所述棉绒纤维是以长绒棉为原料,经过梳理提取的棉纤维,所述氢氧化钠溶液质量浓度在5-18%,溶液温度60-80℃,浸泡时间10-30min,浸泡完成后清水漂洗,70-90℃干燥,得到预处理的棉纤维;
S2、纱线的表面改性
在200ml的无水乙醇中加入5ml去离子水,加入10ml的25%氨水,40-50℃恒温磁力搅拌1-2h,再加入12ml的硅酸四乙酯,继续保持恒温磁力搅拌10-12h,转速200-500rpm,反应完成后加入硅酸四乙酯质量10-30%的γ-氨丙基三甲氧基硅烷或γ-氨丙基三乙氧基硅烷,继续磁力搅拌3-4h,产物冷却后抽滤,无水乙醇洗涤5-8遍,再分散在200ml乙醇中,加入1g羟丙基纤维素,再加入预处理的棉纤维,液固比在50-100:1,将棉纤维减压蒸除溶剂,得到表面改性纱线;
S3、中间体制备
数均分子量为4000-7500的氢封端聚甲基硅氧烷与烯丙基缩水甘油醚按摩尔比2.1:1混合,搅拌均匀后升温至80℃,加入反应物质量0.5-0.6%的1wt.%浓度的氯铂酸-异丙醇溶液,加入终浓度0.01%的对羟基苯甲醚,升温至85℃保温搅拌反应3h,产物经真空蒸馏后得到淡黄色的环氧基封端聚二甲基硅氧烷;
S4、纱线表面接枝改性
环氧基封端聚二甲基硅氧烷以异丙醇稀释,稀释比例为2-5:100,表面改性纱线移入反应釜中,加入稀释的环氧基封端聚二甲基硅氧烷溶液,液固比在50-100:1,反应釜填充率60-70%,密封反应釜后,在55-65℃下保温反应5h,反应完成后挤干,以异丙醇漂洗,减压蒸除溶剂,得到表面接枝改性纱线;
S5、面料织造
将所述表面接枝改性纱线织造为面料。
实施例3
一种纳米防污、抑菌、透气的环保面料的制备工艺,包括以下步骤:
S1、纤维前处理
将除杂后的棉绒纤维浸入热的氢氧化钠溶液中浸泡清洗,所述棉绒纤维是以长绒棉为原料,经过梳理提取的棉纤维,所述氢氧化钠溶液质量浓度在5-18%,溶液温度60-80℃,浸泡时间10-30min,浸泡完成后清水漂洗,70-90℃干燥,得到预处理的棉纤维;
S2、纱线的表面改性
在200ml的无水乙醇中加入5ml去离子水,加入10ml的25%氨水,40-50℃恒温磁力搅拌1-2h,再加入12ml的硅酸四乙酯,继续保持恒温磁力搅拌10-12h,转速200-500rpm,反应完成后加入硅酸四乙酯质量10-30%的γ-氨丙基三甲氧基硅烷或γ-氨丙基三乙氧基硅烷,继续磁力搅拌3-4h,产物冷却后抽滤,无水乙醇洗涤5-8遍,再分散在200ml乙醇中,加入1g羟丙基纤维素,再加入预处理的棉纤维,液固比在50-100:1,将棉纤维减压蒸除溶剂,得到表面改性纱线;
S3、中间体制备
数均分子量为4000-7500的氢封端聚甲基硅氧烷与烯丙基缩水甘油醚按摩尔比2.1:1混合,搅拌均匀后升温至80℃,加入反应物质量0.5-0.6%的1wt.%浓度的氯铂酸-异丙醇溶液,加入终浓度0.01%的对羟基苯甲醚,升温至85℃保温搅拌反应3h,产物经真空蒸馏后得到淡黄色的环氧基封端聚二甲基硅氧烷;
S4、纱线表面接枝改性
环氧基封端聚二甲基硅氧烷以异丙醇稀释,稀释比例为2-5:100,表面改性纱线移入反应釜中,加入稀释的环氧基封端聚二甲基硅氧烷溶液,液固比在50-100:1,反应釜填充率60-70%,密封反应釜后,在55-65℃下保温反应5h,反应完成后挤干,分别以异丙醇、去离子水漂洗,干燥后再次进行纱线的表面接枝改性,异丙醇漂洗后减压蒸除溶剂,得到表面接枝改性纱线;
S5、面料织造
将所述表面接枝改性纱线织造为面料。
测试实验:
1、三防功能性
测定实施例1-3所制备的面料的三防等级,其中,
防水性能测试方法参照GB/T4745—2012《纺织品防水性能的检测和评价沾水法》
防油等级测试方法参照GB/T19977—2014《纺织品拒油性抗碳氢化合物试验》
易去污性能测试方法参照FZ/T14021-2011《防水、防油、易去污、免烫印染布》
产品的品等按FZ/T14021-2011《防水、防油、易去污、免烫印染布》的规定分等,为一等品,具体测试结果如下:
2、抑菌测试
以未处理棉面料为对照,以金黄色葡萄球菌ATCC6538和大肠杆菌ATCC25922为测试菌种,菌种培养至OD600=0.3,试样面料灭菌后放置与24孔培养板中,每个孔中接入等量菌液,培养24h,无菌缓冲液漂洗表面,再超声震荡将黏附的细菌震落,测量所得悬液的OD600值,结果如下:
3、透气性测试
以YG(B)461D型数字式织物透气量仪测定,喷嘴孔径8mm,两侧压差100Pa,透气面积20cm2,以未处理棉面料为对照,测定透气值,结果如下:
对照 | 实施例1 | 实施例2 | 实施例3 | |
透气值/mm·s<sup>-1</sup> | 367 | 355 | 360 | 358 |
最后应当说明的是,以上实施例仅用以说明本发明的技术方案,而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细地说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (4)
1.一种纳米防污、抑菌、透气的环保面料的制备工艺,其特征在于,包括以下步骤:
S1、纤维前处理
将除杂后的棉绒纤维浸入热的氢氧化钠溶液中浸泡清洗,所述氢氧化钠溶液的质量浓度在5-18%,溶液温度60-80℃,浸泡时间10-30min,浸泡完成后清水漂洗,70-90℃干燥,得到预处理的棉纤维;
S2、纱线的表面改性
将负载氨丙基改性纳米二氧化硅的棉纤维经加捻、纺纱加工为纱线,得到表面改性纱线;
所述负载氨丙基改性纳米二氧化硅的棉纤维的制备方法为:
在200ml的无水乙醇中加入5ml去离子水,加入10ml的25%氨水,40-50℃恒温磁力搅拌1-2h,再加入12ml的硅酸四乙酯,继续保持恒温磁力搅拌10-12h,转速200-500rpm,反应完成后加入硅酸四乙酯质量10-30%的γ-氨丙基三甲氧基硅烷或γ-氨丙基三乙氧基硅烷,继续磁力搅拌3-4h,产物冷却后抽滤,无水乙醇洗涤5-8遍,再分散在200ml乙醇中,加入1g羟丙基纤维素,再加入预处理的棉纤维,液固比在50-100:1,将棉纤维减压蒸除溶剂,得到负载氨丙基改性纳米二氧化硅的棉纤维;
S3、中间体制备
数均分子量为4000-7500的氢封端聚甲基硅氧烷与烯丙基缩水甘油醚按摩尔比2.1:1混合,搅拌均匀后升温至80℃,加入反应物质量0.5-0.6%的1wt.%浓度的氯铂酸-异丙醇溶液,加入终浓度0.01%的对羟基苯甲醚,升温至85℃保温搅拌反应3h,产物经真空蒸馏后得到淡黄色的环氧基封端聚二甲基硅氧烷;
S4、纱线表面接枝改性
环氧基封端聚二甲基硅氧烷以异丙醇稀释,稀释比例为2-5:100,表面改性纱线移入反应釜中,加入稀释的环氧基封端聚二甲基硅氧烷溶液,液固比在50-100:1,密封反应釜后,在55-65℃下保温反应5h,反应完成后挤干,再以异丙醇漂洗,将以异丙醇漂洗后的纱线,先以清水漂洗,干燥后再次进行步骤S4的表面接枝改性,减压蒸除溶剂后,得到表面接枝改性纱线;
S5、面料织造
将所述表面接枝改性纱线织造为面料。
2.根据权利要求1所述的一种纳米防污、抑菌、透气的环保面料的制备工艺,其特征在于,所述棉绒纤维是以长绒棉为原料,经过梳理提取的棉纤维。
3.根据权利要求1所述的一种纳米防污、抑菌、透气的环保面料的制备工艺,其特征在于,步骤S4中,所述反应釜的填充率为60-70%。
4.根据权利要求1-3任一所述制备工艺制备的面料在服装上的应用。
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