CN112626857A - 一种自清洁抗菌无纺布及其制备方法 - Google Patents
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Abstract
本发明提出了一种自清洁抗菌无纺布及其制备方法,所述无纺布包括聚丙烯无纺布的基材以及接枝在聚丙烯无纺布基材表面的壳聚糖和纳米二氧化钛。本发明提出的一种自清洁抗菌无纺布及其制备方法,通过在聚丙烯无纺布上有效接枝了壳聚糖和纳米二氧化钛,并以壳聚糖为抑菌成膜剂,二氧化钛为光催化剂,从而提升了聚丙烯无纺布的自清洁和抗菌性能。
Description
技术领域
本发明涉及功能无纺布技术领域,尤其涉及一种自清洁抗菌无纺布及其制备方法。
背景技术
聚丙烯(PP)无纺布由于其优异的机械强度和物理、化学稳定性,在许多领域都有广泛的应用。但是由于其分子结构中仅存在规整排列的甲基基团,缺乏更多的官能团和极性基团,容易引起细菌、蛋白等物质的粘附,因此聚丙烯无纺布存在耐老化性不足、抗菌能力差等缺陷。
壳聚糖因为其良好的亲水性、成膜性、能抑制微生物生长繁殖以及可降解可食用、无抗原作用等优点而被广泛应用于生物医药、水处理、纺织工业、农业、果蔬的贮藏保鲜等领域。而二氧化钛光催化活性高,且纳米二氧化钛无毒,化学性质稳定,光催化降解污染物效果好,无二次污染,成为光催化中常用的催化剂。现有技术中将二氧化钛负载在纺织品、玻璃、陶瓷等物质上,从而制备出具有自清洁功能的材料,这些材料可以清除灰尘、污迹、细菌,同时也可以降解有害物质,从而达到自清洁的目的。
因此通过将壳聚糖和二氧化钛与聚丙烯无纺布结合,综合利用壳聚糖的成膜抑菌和二氧化钛的自清洁功能,具有重要的意义,但目前由于聚丙烯无纺布表面无活性基团,目前尚无方法能够在聚丙烯无纺布表明有效负载壳聚糖和二氧化钛。
发明内容
基于背景技术存在的技术问题,本发明提出了一种自清洁抗菌无纺布及其制备方法。通过在聚丙烯无纺布上有效接枝了壳聚糖和纳米二氧化钛,并以壳聚糖为抑菌成膜剂,二氧化钛为光催化剂,从而提升了聚丙烯无纺布的自清洁和抗菌性能。
本发明提出的一种自清洁抗菌无纺布,所述无纺布包括聚丙烯无纺布的基材以及接枝在聚丙烯无纺布基材表面的壳聚糖和纳米二氧化钛。
优选地,所述聚丙烯无纺布基材的表面还黏附有聚多巴胺层。
优选地,所述纳米二氧化钛均匀分布在壳聚糖表面。
本发明提一种自清洁抗菌无纺布的制备方法,包括如下步骤:
S1、将多巴胺在聚丙烯无纺布表面进行氧化自聚反应,得到表面黏附有聚多巴胺层的无纺布;
S2、将壳聚糖与表面黏附有聚多巴胺层的无纺布进行接枝反应,得到接枝有壳聚糖的无纺布;
S3、将钛酸四丁酯在接枝有壳聚糖的无纺布的表面进行原位水解反应,得到同时负载有壳聚糖和TiO2的无纺布,即为所述自清洁抗菌无纺布。
优选地,步骤S1具体包括:将盐酸多巴胺和氧化剂、交联剂按照摩尔比1:1-3:1-4加入溶剂中,配置得到多巴胺溶液,再将聚丙烯无纺布浸泡在所述多巴胺溶液中,常温震荡反应1-3h,即得到表面黏附有聚多巴胺层的无纺布。
优选地,所述氧化剂为过硫酸盐,所述交联剂为二元有机胺。
优选地,步骤S2具体包括:将壳聚糖加入醋酸溶液中,配置得到含量为0.5-1.5wt%的壳聚糖溶液,再将表面黏附有聚多巴胺层的无纺布浸泡在所述壳聚糖溶液中,40-50℃下震荡反应12-16h,即得到接枝有壳聚糖的无纺布。
优选地,所述壳聚糖的脱乙酰度≥80%。
优选地,步骤S3具体包括:将钛酸四丁酯加入乙醇中,配置得到含量为4-10wt%的钛酸四丁酯乙醇溶液,再将接枝有壳聚糖的无纺布浸泡在所述钛酸四丁酯乙醇溶液中,50-60℃下加水并震荡反应4-8h,得到表面同时负载有壳聚糖和TiO2的无纺布,即为所述自清洁抗菌无纺布。
优选地,所述水的添加量为钛酸四丁酯质量的30-50倍。
本发明中,利用多巴胺在弱碱性条件下发生氧化自聚反应,再通过共价键、非共价键和氢键的作用牢固地黏附在材料表面,形成聚多巴胺层;该聚多巴胺层所含的邻苯二酚基团可以与壳聚糖上的氨基发生反应,从而将壳聚糖接枝在无纺布表面;由于壳聚糖存在-NH2官能团,在酸性溶液中质子化后会使无纺布表面形成季铵盐的结构,由于该季铵盐结构可以对钛酸四丁酯形成吸附,因此可以使得钛酸四丁酯水解后的TiO2均布在壳聚糖表面,最终使得原本难以吸附壳聚糖和二氧化钛的聚丙烯无纺布表面能够有效地接枝壳聚糖和二氧化钛,最终赋予聚丙烯无纺布以优异的抗菌性能,同时可以催化降解有机污染物,获得自清洁功能。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明,但是应该明确提出这些实施例用于举例说明,但是不解释为限制本发明的范围。
实施例1
一种自清洁抗菌无纺布,其制备方法包括如下步骤:
S1、将聚丙烯无纺布(30g/m2)裁剪成10cm×5cm大小,在乙醇中超声处理30min以去除表面灰尘,用去离子水反复冲洗后烘干待用;将盐酸多巴胺加入三羟甲基氨基甲烷缓冲液(pH=8.5)中搅拌溶解,配置成浓度为30mmol/L的溶液,再加入与盐酸多巴胺等摩尔量的过硫酸铵和乙二胺,得到多巴胺溶液;将上述聚丙烯无纺布按照浴比(g/mL)1:40浸泡在上述多巴胺溶液中,在25℃恒温水浴摇床中震荡反应2h后取出,用去离子水冲洗,烘干,得到表面黏附有聚多巴胺层的无纺布;
S2、将壳聚糖(脱乙酰度≥80%)加入醋酸溶液(2wt%)中搅拌溶解,配置成浓度为1wt%的壳聚糖溶液,用5wt%的氢氧化钠溶液调节pH值为6.0;将上述表面黏附有聚多巴胺层的无纺布按照浴比(g/mL)1:30浸泡在上述壳聚糖溶液中,在40℃恒温水浴摇床中震荡反应14h后取出,用去离子水冲洗,烘干,得到接枝有壳聚糖的无纺布;
S3、将钛酸四丁酯加入无水乙醇中搅拌溶解,配置成浓度为8wt%的钛酸四丁酯乙醇溶液;将上述接枝有壳聚糖的无纺布按照浴比(g/mL)1:30浸泡在上述钛酸四丁酯乙醇溶液中,在60℃水浴下,逐滴滴加水,水的添加量是钛酸四丁酯重量的40倍,并震荡反应6h后取出,用乙醇冲洗,烘干,得到表面同时负载有壳聚糖和TiO2的无纺布,即为所述自清洁抗菌无纺布。
实施例2
一种自清洁抗菌无纺布,其制备方法包括如下步骤:
S1、将聚丙烯无纺布(30g/m2)裁剪成10cm×5cm大小,在乙醇中超声处理30min以去除表面灰尘,用去离子水反复冲洗后烘干待用;将盐酸多巴胺加入三羟甲基氨基甲烷缓冲液(pH=8.5)中搅拌溶解,配置成浓度为30mmol/L的溶液,再加入盐酸多巴胺2倍摩尔量的过硫酸铵和盐酸多巴胺3倍摩尔量的乙二胺,得到多巴胺溶液;将上述聚丙烯无纺布按照浴比(g/mL)1:40浸泡在上述多巴胺溶液中,在25℃恒温水浴摇床中震荡反应1h后取出,用去离子水冲洗,烘干,得到表面黏附有聚多巴胺层的无纺布;
S2、将壳聚糖(脱乙酰度≥80%)加入醋酸溶液(2wt%)中搅拌溶解,配置成浓度为0.5wt%的壳聚糖溶液,用5wt%的氢氧化钠溶液调节pH值为6.0;将上述表面黏附有聚多巴胺层的无纺布按照浴比(g/mL)1:30浸泡在上述壳聚糖溶液中,在50℃恒温水浴摇床中震荡反应12h后取出,用去离子水冲洗,烘干,得到接枝有壳聚糖的无纺布;
S3、将钛酸四丁酯加入无水乙醇中搅拌溶解,配置成浓度为10wt%的钛酸四丁酯乙醇溶液;将上述接枝有壳聚糖的无纺布按照浴比(g/mL)1:30浸泡在上述钛酸四丁酯乙醇溶液中,在60℃水浴下,逐滴滴加水,水的添加量是钛酸四丁酯重量的50倍,并震荡反应8h后取出,用乙醇冲洗,烘干,得到表面同时负载有壳聚糖和TiO2的无纺布,即为所述自清洁抗菌无纺布。
实施例3
一种自清洁抗菌无纺布,其制备方法包括如下步骤:
S1、将聚丙烯无纺布(30g/m2)裁剪成10cm×5cm大小,在乙醇中超声处理30min以去除表面灰尘,用去离子水反复冲洗后烘干待用;将盐酸多巴胺加入三羟甲基氨基甲烷缓冲液(pH=8.5)中搅拌溶解,配置成浓度为30mmol/L的溶液,再加入盐酸多巴胺3倍摩尔量的过硫酸铵和盐酸多巴胺4倍摩尔量的乙二胺,得到多巴胺溶液;将上述聚丙烯无纺布按照浴比(g/mL)1:40浸泡在上述多巴胺溶液中,在25℃恒温水浴摇床中震荡反应3h后取出,用去离子水冲洗,烘干,得到表面黏附有聚多巴胺层的无纺布;
S2、将壳聚糖(脱乙酰度≥80%)加入醋酸溶液(2wt%)中搅拌溶解,配置成浓度为1.5wt%的壳聚糖溶液,用5wt%的氢氧化钠溶液调节pH值为6.0;将上述表面黏附有聚多巴胺层的无纺布按照浴比(g/mL)1:30浸泡在上述壳聚糖溶液中,在40℃恒温水浴摇床中震荡反应16h后取出,用去离子水冲洗,烘干,得到接枝有壳聚糖的无纺布;
S3、将钛酸四丁酯加入无水乙醇中搅拌溶解,配置成浓度为4wt%的钛酸四丁酯乙醇溶液;将上述接枝有壳聚糖的无纺布按照浴比(g/mL)1:30浸泡在上述钛酸四丁酯乙醇溶液中,在60℃水浴下,逐滴滴加水,水的添加量是钛酸四丁酯重量的30倍,并震荡反应4h后取出,用乙醇冲洗,烘干,得到表面同时负载有壳聚糖和TiO2的无纺布,即为所述自清洁抗菌无纺布。
对比例1
一种自清洁抗菌无纺布,其制备方法包括如下步骤:
S1、将聚丙烯无纺布(30g/m2)裁剪成10cm×5cm大小,在乙醇中超声处理30min以去除表面灰尘,用去离子水反复冲洗后烘干待用;将盐酸多巴胺加入三羟甲基氨基甲烷缓冲液(pH=8.5)中搅拌溶解,配置成浓度为30mmol/L的溶液,再加入与盐酸多巴胺等摩尔量的过硫酸铵和乙二胺,得到多巴胺溶液;将上述聚丙烯无纺布按照浴比(g/mL)1:40浸泡在上述多巴胺溶液中,在25℃恒温水浴摇床中震荡反应2h后取出,用去离子水冲洗,烘干,得到表面黏附有聚多巴胺层的无纺布;
S2、将壳聚糖(脱乙酰度≥80%)加入醋酸溶液(2wt%)中搅拌溶解,配置成浓度为1wt%的壳聚糖溶液,用5wt%的氢氧化钠溶液调节pH值为6.0;将上述表面黏附有聚多巴胺层的无纺布按照浴比(g/mL)1:30浸泡在上述壳聚糖溶液中,在40℃恒温水浴摇床中震荡反应14h后取出,用去离子水冲洗,烘干,得到接枝有壳聚糖的无纺布;
S3、将接枝有壳聚糖的无纺布按照浴比(g/mL)1:30浸泡在浓度为20g/L的TiO2乙醇溶液中,在60℃恒温水浴摇床中震荡反应6h后取出,用去离子水冲洗,烘干,得到所述自清洁抗菌无纺布。
对比例2
一种自清洁抗菌无纺布,其制备方法包括如下步骤:
S1、将聚丙烯无纺布(30g/m2)裁剪成10cm×5cm大小,在乙醇中超声处理30min以去除表面灰尘,用去离子水反复冲洗后烘干待用;将盐酸多巴胺加入三羟甲基氨基甲烷缓冲液(pH=8.5)中搅拌溶解,配置成浓度为30mmol/L的溶液,再加入与盐酸多巴胺等摩尔量的过硫酸铵和乙二胺,得到多巴胺溶液;将上述聚丙烯无纺布按照浴比(g/mL)1:40浸泡在上述多巴胺溶液中,在25℃恒温水浴摇床中震荡反应2h后取出,用去离子水冲洗,烘干,得到表面黏附有聚多巴胺层的无纺布;
S2、将钛酸四丁酯加入无水乙醇中搅拌溶解,配置成浓度为8wt%的钛酸四丁酯乙醇溶液;将上述表面黏附有聚多巴胺层的无纺布按照浴比(g/mL)1:30浸泡在上述钛酸四丁酯乙醇溶液中,在60℃水浴中,逐滴滴加水,水的添加量是钛酸四丁酯重量的40倍,并震荡反应6h后取出,用乙醇冲洗,烘干,得到表面同时负载有TiO2的无纺布,即为所述自清洁抗菌无纺布。
将实施例和对比例获得的自清洁抗菌无纺布进行下述性能测试,结果参照表1、表2所示。
抗菌性能:参照GB/T20944.3-2008《纺织品抗菌性能的评价》,以振荡法测定抗菌性能,所用菌种为大肠杆菌(ATCC 8099)、金黄色葡萄球菌(ATCC 6538)、白色念珠菌(ATCC10231),抗菌性能以其抑菌率来表征。
表1实施例和对比例所得自清洁抗菌无纺布的抑菌率
参照表1可知,本发明所述抗菌无纺布对金黄色葡萄球菌、大肠杆菌以及白色念珠菌具有有效的抑制作用,而对比例所述抗菌无纺布虽然有一定的抑菌作用,但是由于TiO2无法对聚丙烯无纺布形成有效结合,即便单纯依赖壳聚糖也不能达到很好的抗菌效果。
光降解性能:将实施例和对比例获得的自清洁抗菌无纺布放入100mg/L的甲基橙溶液中完全浸泡,在40W的紫外灯下进行光降解反应,1h后取样离心取上清液,用紫外-可见分光光度计测试其吸光度,光降解性能以降解效率来表征。
表2实施例和对比例所得自清洁抗菌无纺布的降解率
实施例1 | 实施例2 | 实施例3 | 对比例1 | 对比例2 | |
降解率% | 98.2 | 98.7 | 97.9 | 66.1 | 39.2 |
同上原因,对比例所述抗菌无纺布虽然有一定的光降解性能,但是由于TiO2无法对聚丙烯无纺布形成有效结合,因此其光降解效果不佳。本发明所得到的聚丙烯无纺布则具有优良的光降解性能。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种自清洁抗菌无纺布,其特征在于,所述无纺布包括聚丙烯无纺布的基材以及接枝在聚丙烯无纺布基材表面的壳聚糖和纳米二氧化钛。
2.根据权利要求1所述自清洁抗菌无纺布,其特征在于,所述聚丙烯无纺布基材的表面还黏附有聚多巴胺层。
3.根据权利要求1或2所述自清洁抗菌无纺布,其特征在于,所述纳米二氧化钛均匀分布在壳聚糖表面。
4.一种权利要求1-3任一项所述自清洁抗菌无纺布的制备方法,其特征在于,包括如下步骤:
S1、将多巴胺在聚丙烯无纺布表面进行氧化自聚反应,得到表面黏附有聚多巴胺层的无纺布;
S2、将壳聚糖与表面黏附有聚多巴胺层的无纺布进行接枝反应,得到接枝有壳聚糖的无纺布;
S3、将钛酸四丁酯在接枝有壳聚糖的无纺布的表面进行原位水解反应,得到同时负载有壳聚糖和TiO2的无纺布,即为所述自清洁抗菌无纺布。
5.根据权利要求4所述自清洁抗菌无纺布的制备方法,其特征在于,步骤S1具体包括:将盐酸多巴胺和氧化剂、交联剂按照摩尔比1:1-3:1-4加入溶剂中,配置得到多巴胺溶液,再将聚丙烯无纺布浸泡在所述多巴胺溶液中,常温震荡反应1-3h,即得到表面黏附有聚多巴胺层的无纺布。
6.根据权利要求5所述自清洁抗菌无纺布的制备方法,其特征在于,所述氧化剂为过硫酸盐,所述交联剂为二元有机胺。
7.根据权利要求4-6任一项所述自清洁抗菌无纺布的制备方法,其特征在于,步骤S2具体包括:将壳聚糖加入醋酸溶液中,配置得到含量为0.5-1.5wt%的壳聚糖溶液,再将表面黏附有聚多巴胺层的无纺布浸泡在所述壳聚糖溶液中,40-50℃下震荡反应12-16h,即得到接枝有壳聚糖的无纺布。
8.根据权利要求7所述自清洁抗菌无纺布的制备方法,其特征在于,所述壳聚糖的脱乙酰度≥80%。
9.根据权利要求4-8任一项所述自清洁抗菌无纺布的制备方法,其特征在于,步骤S3具体包括:将钛酸四丁酯加入乙醇中,配置得到含量为4-10wt%的钛酸四丁酯乙醇溶液,再将接枝有壳聚糖的无纺布浸泡在所述钛酸四丁酯乙醇溶液中,50-60℃下加水并震荡反应4-8h,得到表面同时负载有壳聚糖和TiO2的无纺布,即为所述自清洁抗菌无纺布。
10.根据权利要求9所述自清洁抗菌无纺布的制备方法,其特征在于,所述水的添加量为钛酸四丁酯质量的30-50倍。
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