CN108385279A - 一种复合抗菌纤维膜的制备方法 - Google Patents

一种复合抗菌纤维膜的制备方法 Download PDF

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CN108385279A
CN108385279A CN201810087794.8A CN201810087794A CN108385279A CN 108385279 A CN108385279 A CN 108385279A CN 201810087794 A CN201810087794 A CN 201810087794A CN 108385279 A CN108385279 A CN 108385279A
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韩祥
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Pinghu Ivan House Bag Co Ltd
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Abstract

一种复合抗菌纤维膜及其制备方法，属于功能纺织材料领域。本发明通过在聚丙烯腈、铜氨再生纤维素中添加抗菌剂，采用静电纺丝技术制备了一种具有高效抗菌性能的聚丙烯腈抗菌纳米纤维膜。该纤维膜中的抗菌剂由2‑甲基‑2‑丙烯酸‑1,2‑丙二醇酯、甲基丙烯酸二甲氨基乙酯、烯基丙三乙氧基硅烷、锂皂石、纳米氧化钛聚合而成；将抗菌剂、纳米银、铜‑沸石分子筛微粉、纳米氧化锌溶胶加入聚丙烯腈、铜氨再生纤维素的混合溶液中混合均匀后，通过静电纺丝得到纤维膜，将纤维膜浸渍于含有氯化溴溶液中，取出并烘干，即得复合抗菌纤维膜。该抗菌纳米纤维膜能用于日用、纺织、产业和医药领域。

Description

一种复合抗菌纤维膜的制备方法
技术领域
本发明涉及功能纺织材料技术领域，尤其涉及一种复合抗菌纤维膜的制备方法。
背景技术
纳米纤维膜具有表面积大，孔隙率高，结构疏松，能够按照需要的功能预先设计组成，模拟细胞外基质，制备方法简单等优点而在很多领域有着巨大的应用潜能，现已在食品、医药、日化等领域有了很广泛的应用。尤其是以天然高聚物为纺丝液制备的纳米纤维膜，除了具有以上特点外，还具有优异的生物相容性，生物可降解性和可再生性等。
现有技术制得的载银纳米颗粒/复合纤维膜生物相容性差、制备过程有副产物产生造成纤维膜结构被破坏，使得抗菌纤维膜应用受限。而且由于纳米银呈颗粒状，粒度为纳米级别，往往只能聚集在石墨烯的特定部位，无法均匀分布在表面，从而影响的抗菌效果，限制了其进一步应用。为了解决上述问题，本专利发明了一种利用静电纺丝技术，制备复合抗菌纤维膜，使其具有高效抗菌功能。本发明充分利用了静电纺丝技术简单易操作，制备的功能纤维比表面积大、孔隙率高、稳定性好等优点，使得到的复合纤维膜与空气的接触面积大，吸附、催化以及抗菌效率高，并且易回收、无二次污染，可重复利用。
发明内容
基于背景技术存在的技术问题，本发明提出了一种复合抗菌纤维膜的制备方法，其过程简单，条件温和，得到的纤维膜抗菌性能好，机械强度和韧性高，使用寿命长。
本发明提出的一种复合抗菌纤维膜的制备方法，包括以下步骤：
S1、配制高分子聚合物的混合溶液：将聚丙烯腈溶于二甲基乙酰胺和丙酮的混合溶剂中，再将铜氨再生纤维素加入上述溶液中，在40℃下磁力搅拌12h使溶液得到充分溶解，得到混合溶液，其中二甲基乙酰胺和丙酮的体积比为3:7；
S2、制备抗菌剂：所述抗菌剂由2-甲基-2-丙烯酸-1,2-丙二醇酯、甲基丙烯酸二甲氨基乙酯、烯基丙三乙氧基硅烷、锂皂石、纳米氧化钛聚合而成；其制备工艺具体如下：将质量分数为20％的2-甲基-2-丙烯酸-1,2-丙二醇酯水溶液加入质量分数为15％的甲基丙烯酸二甲氨基乙酯水溶液中以80-150rmp搅拌混合均匀，然后加入烯基丙三乙氧基硅烷、锂皂石和纳米氧化钛，在热水浴加热下反应24h，取出后得到所述抗菌剂;
S3、制备复合抗菌纤维膜：将抗菌剂、纳米银、铜-沸石分子筛微粉、纳米氧化锌溶胶、抗氧化剂加入到步骤S2的混合溶液中，在100~300rpm搅拌下混合均匀，然后注入5ml注射器中，采用5号不锈钢针头，通过静电纺丝得到复合纤维膜；静电纺丝工艺参数为：直流高压电源为15~25kV，纺丝距离为10~30cm，纺丝溶液的流速为0.5-2mL/h；温度为30℃，相对湿度为35％；
S4、将上述复合纤维膜置于60℃的氯化溴溶液中进行浸泡，取出后室温真空干燥24h，除去残留溶剂，并在10℃干燥箱中保存。
优选地，在S1中，聚丙烯腈、铜氨再生纤维素的重量比为55-65:25-35。
优选地，在S2中，2-甲基-2-丙烯酸-1,2-丙二醇酯、甲基丙烯酸二甲氨基乙酯、烯基丙三乙氧基硅烷、锂皂石、纳米氧化钛的重量比为5-8:3-4:3-5:4-6:2-3。
优选地，在S3中，抗菌剂、纳米银、铜-沸石分子筛微粉、纳米氧化锌溶胶、抗氧化剂的重量比为3-8:2-4:1-2:2-6:0.3-1。
优选地，在S3中，所述抗氧化剂为N-苯基-2-萘胺、N,N-二苯基对苯二胺、N-苯基-N-异丙基对苯二胺等。
本发明在复合抗菌纤维膜的制备方法中，首先将聚丙烯腈溶于二甲基乙酰胺和丙酮的混合溶剂中，再将铜氨再生纤维素加入上述溶液中，制得混合溶液；再以2-甲基-2-丙烯酸-1,2-丙二醇酯、甲基丙烯酸二甲氨基乙酯、烯基丙三乙氧基硅烷、锂皂石、纳米氧化钛为原料，通过控制各物质的含量比例，使其发生聚合反应，制得抗菌剂，然后将其加入体系中，与纳米银、铜-沸石分子筛微粉、纳米氧化锌溶胶、抗氧化剂配合使用，赋予纤维膜优异的抗菌和防污性能，同时提高了纤维膜的机械性能和韧性，克服了单纯的聚丙烯腈分子旋转困难造成的机械强度和韧性差的缺陷，使得到的膜孔径均一、孔隙率高。
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。
本发明提出的一种复合抗菌纤维膜的制备方法，包括以下步骤：
实施例1
本发明提出的一种复合抗菌纤维膜的制备方法，包括以下步骤：
S1、配制高分子聚合物的混合溶液：将110份聚丙烯腈溶于二甲基乙酰胺和丙酮的混合溶剂中，再将70份铜氨再生纤维素加入上述溶液中，在40℃下磁力搅拌12h使溶液得到充分溶解，得到混合溶液，其中二甲基乙酰胺和丙酮的体积比为3:7；
S2、制备抗菌剂：所述抗菌剂由2-甲基-2-丙烯酸-1,2-丙二醇酯、甲基丙烯酸二甲氨基乙酯、烯基丙三乙氧基硅烷、锂皂石、纳米氧化钛聚合而成；其制备工艺具体如下：将25份质量分数为20％的2-甲基-2-丙烯酸-1,2-丙二醇酯水溶液加入15份质量分数为15％的甲基丙烯酸二甲氨基乙酯水溶液中以80-150rmp搅拌混合均匀，然后加入15份烯基丙三乙氧基硅烷、20份锂皂石和10份纳米氧化钛，在热水浴加热下反应24h，取出后得到所述抗菌剂;
S3、制备复合抗菌纤维膜：将30份抗菌剂、20份纳米银、10份铜-沸石分子筛微粉、20份纳米氧化锌溶胶、3份抗氧化剂加入到步骤S2的混合溶液中，在100~300rpm搅拌下混合均匀，然后注入5ml注射器中，采用5号不锈钢针头，通过静电纺丝得到复合纤维膜；静电纺丝工艺参数为：直流高压电源为15kV，纺丝距离为10cm，纺丝溶液的流速为0.5mL/h；温度为30℃，相对湿度为35％；
S4、将上述复合纤维膜置于60℃的氯化溴溶液中进行浸泡，取出后室温真空干燥24h，除去残留溶剂，并在10℃干燥箱中保存。
实施例2
本发明提出的一种复合抗菌纤维膜的制备方法，包括以下步骤：
S1、配制高分子聚合物的混合溶液：将130份聚丙烯腈溶于二甲基乙酰胺和丙酮的混合溶剂中，再将50铜氨再生纤维素加入上述溶液中，在40℃下磁力搅拌12h使溶液得到充分溶解，得到混合溶液，其中二甲基乙酰胺和丙酮的体积比为3:7；
S2、制备抗菌剂：所述抗菌剂由2-甲基-2-丙烯酸-1,2-丙二醇酯、甲基丙烯酸二甲氨基乙酯、烯基丙三乙氧基硅烷、锂皂石、纳米氧化钛聚合而成；其制备工艺具体如下：将40份质量分数为20％的2-甲基-2-丙烯酸-1,2-丙二醇酯水溶液加入20份质量分数为15％的甲基丙烯酸二甲氨基乙酯水溶液中以80-150rmp搅拌混合均匀，然后加入25份烯基丙三乙氧基硅烷、30份锂皂石和15份纳米氧化钛，在热水浴加热下反应24h，取出后得到所述抗菌剂;
S3、制备复合抗菌纤维膜：将40份抗菌剂、20份纳米银、10份铜-沸石分子筛微粉、30份纳米氧化锌溶胶、5份抗氧化剂加入到步骤S2的混合溶液中，在100~300rpm搅拌下混合均匀，然后注入5ml注射器中，采用5号不锈钢针头，通过静电纺丝得到复合纤维膜；静电纺丝工艺参数为：直流高压电源为25kV，纺丝距离为30cm，纺丝溶液的流速为2mL/h；温度为30℃，相对湿度为35％；
S4、将上述复合纤维膜置于60℃的氯化溴溶液中进行浸泡，取出后室温真空干燥24h，除去残留溶剂，并在10℃干燥箱中保存。
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 (5)

1.一种复合抗菌纤维膜的制备方法，其特征在于，依次包括以下步骤：
S1、配制高分子聚合物的混合溶液：将聚丙烯腈溶于二甲基乙酰胺和丙酮的混合溶剂中，再将铜氨再生纤维素加入上述溶液中，在40℃下磁力搅拌12h使溶液得到充分溶解，得到混合溶液，其中二甲基乙酰胺和丙酮的体积比为3:7；
S2、制备抗菌剂：所述抗菌剂由2-甲基-2-丙烯酸-1,2-丙二醇酯、甲基丙烯酸二甲氨基乙酯、烯基丙三乙氧基硅烷、锂皂石、纳米氧化钛聚合而成；其制备工艺具体如下：将质量分数为20％的2-甲基-2-丙烯酸-1,2-丙二醇酯水溶液加入质量分数为15％的甲基丙烯酸二甲氨基乙酯水溶液中以80-150rmp搅拌混合均匀，然后加入烯基丙三乙氧基硅烷、锂皂石和纳米氧化钛，在热水浴加热下反应24h，取出后得到所述抗菌剂;S3、制备复合抗菌纤维膜：将抗菌剂、纳米银、铜-沸石分子筛微粉、纳米氧化锌溶胶、抗氧化剂加入到步骤S2的混合溶液中，在100~300rpm搅拌下混合均匀，然后注入5ml注射器中，采用5号不锈钢针头，通过静电纺丝得到复合纤维膜；静电纺丝工艺参数为：直流高压电源为15~25kV，纺丝距离为10~30cm，纺丝溶液的流速为0.5-2mL/h；温度为30℃，相对湿度为35％；
S4、将上述复合纤维膜置于60℃的氯化溴溶液中进行浸泡，取出后室温真空干燥24h，除去残留溶剂，并在10℃干燥箱中保存。
2.根据权利要求1中所述复合抗菌纤维膜的制备方法，其特征在于，在S1中，聚丙烯腈、铜氨再生纤维素的重量比为55-65:25-35。
3.根据权利要求1-2任一项所述复合抗菌纤维膜的制备方法，其特征在于，在S2中，2-甲基-2-丙烯酸-1,2-丙二醇酯、甲基丙烯酸二甲氨基乙酯、烯基丙三乙氧基硅烷、锂皂石、纳米氧化钛的重量比为5-8:3-4:3-5:4-6:2-3。
4.根据权利要求1-2中任一项所述复合抗菌纤维膜的制备方法，其特征在于，在S3中，抗菌剂、纳米银、铜-沸石分子筛微粉、纳米氧化锌溶胶、抗氧化剂的重量比为3-8:2-4:1-2:2-6:0.3-1。
5.根据权利要求4所述复合抗菌纤维膜的制备方法，其特征在于，在S3中，所述抗氧化剂为N-苯基-2-萘胺、N,N-二苯基对苯二胺、N-苯基-N-异丙基对苯二胺等。
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