CN107501476B - 一种光交联抗菌性聚乙烯醇复合膜的制备方法 - Google Patents
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Abstract
本发明涉及一种光交联抗菌性聚乙烯醇复合膜的制备方法，包括：将PVA在90℃下搅拌溶于去离子水中，加入季铵盐单体甲基丙烯酰氧乙基二甲基十二烷基溴化铵(DMAEMA‑DB)和N,N‑亚甲基双丙烯酰胺(MBA)，经紫外光引发DMAEMA‑DB和MBA发生交联反应，季铵盐被固定在PVA基体中，得到光交联抗菌性PVA复合膜，这种复合膜具有优异的抗菌性能和稳定性，并且在使用过程中不会释放抗菌剂，使其在活性包装领域的应用成为可能。
Description
技术领域
本发明涉及一种光交联抗菌性聚乙烯醇复合膜的制备方法，特别是加入季铵盐得到抗菌性光固化复合材料，属于高分子复合材料领域。
背景技术
近年来伴随着频发的公共安全卫生事件，如何有效控制和消灭有害细菌及病毒的生长和传播，依然是一项与人类健康息息相关的重要课题。抗菌制品被公认为是具有广泛发展前景的新型健康产品之一，抗菌塑料、抗菌陶瓷、抗菌纤维以及抗菌涂料等抗菌产品可以广泛的应用在家用电器、日用品、纺织服装和建筑材料等领域。研制新型高效的抗菌材料对保持民众健康以及增强卫生制品的防护效果意义重大。基于此，新型抗菌材料的研发引起越来越多研究者的兴趣。
聚乙烯醇(PVA)是由聚醋酸乙烯水解得到的一种水溶性聚合物，结构式为-CH2CH(OH)n-。性能介于塑料和橡胶之间，一般用于纤维和非纤维两大类。PVA分子主链为碳链，每一个重复单元上均含有一个羟基，由于羟基尺寸小，极性强，容易形成氢键，其化学性质稳定，具有足够的热稳定性、高度的亲水性和水溶性；同时它还具有良好的成膜性和粘接力，有卓越的耐油脂、耐溶剂性能和良好的物理化学稳定性，广泛应用于纺织、食品、医药、建筑、木材加工、造纸、印刷、高分子化工等领域。目前，国内外已有学者以PVA树脂作为基材制备出功能性PVA薄膜，主要是向PVA中添加抗菌剂来制备抗菌性PVA复合材料。
常用的抗菌剂主要有无机类、有机小分子类、天然分子类和高分子类抗菌材料。其中，季铵盐类抗菌剂是研究较多的一类有机抗菌剂。对于小分子季铵盐抗菌剂的抗菌活性已经有了较多的研究，但是小分子抗菌剂存在着易挥发、不易加工、化学稳定性差等缺点。有研究发现带有长链烷基的季铵盐经交联后能够被固定在聚合物基体中，且具有很好的抗菌性能，同时在使用过程中季铵盐抗菌剂不会释放到环境中，还具有比小分子抗菌剂更好的抗菌性能和稳定性。
发明内容
本发明的目的是在PVA中加入季铵盐单体(DMAEMA-DB)、光交联剂(MBA)、光引发剂(I2959)，在紫外光辐射下季铵盐发生交联反应，被固定在PVA基体，以提供一种光交联抗菌性聚乙烯醇复合膜及其制备方法，提高聚乙烯醇薄膜的使用性能和适用范围。
本发明的目的是通过下述技术方案实现：一种光交联抗菌性聚乙烯醇复合膜的制备方法，包含下述步骤：
(1)PVA水溶液的制备：将2g PVA在90℃下搅拌溶于25ml去离子水中，得到均匀的PVA水溶液；
(2)季铵盐复合液的制备：将季铵盐单体、光交联剂、光引发剂溶于乙醇/水的混合溶液中，超声分散20min，得到季铵盐复合液；
(3)PVA复合膜的制备：将上述步骤(1)中的PVA水溶液置于60℃的磁力搅拌器上，60℃下遮光搅拌20min，后加入上述步骤(2)的季铵盐复合液，60℃下遮光搅拌60min，在室温下静置消泡后，浇铸到玻璃模具中，室温放置12h，60℃下烘干，得到PVA复合膜；
(4)光交联PVA复合膜的制备：将上述步骤(3)PVA复合膜暴露在紫外灯下辐射1min，得到光交联PVA复合膜。
步骤(2)中所述的季铵盐单体选自甲基丙烯酰氧乙基二甲基苄基氯化铵(DMAEMA-BC)、甲基丙烯酰氧乙基二甲基丁基溴化铵(DMAEMA-BB)、甲基丙烯酰氧乙基二甲基辛基溴化铵(DMAEMA-OB)、甲基丙烯酰氧乙基二甲基十二烷基溴化铵(DMAEMA-DB)、甲基丙烯酰氧乙基二甲基十六烷基溴化铵(DMAEMA-HB)其用量为PVA的1％～10％。
步骤(2)中所述的光交联剂为一种水溶性光交联剂N,N-亚甲基双丙烯酰胺(MBA)，其用量为QAS的1％～3％。
步骤(2)中所述的光引发剂为一种水溶性光引发剂2959，其用量为QAS的1％～3％。
步骤(2)中所述乙醇/水溶液中乙醇和水的体积比为2:8。
与现有的技术相比，本发明具有如下优点和有益效果：PVA分子链含有大量羟基(-OH)，使其具有良好的水溶性，选择具有优异抗菌性能的甲基丙烯酰氧乙基二甲基十二烷基溴化铵(DMAEMA-DB)为抗菌活性单体，再加入水溶性的光交联剂和光引发剂，经紫外光引发，季铵盐单体发生交联反应，最终被固定在PVA基体中，避免了在使用过程中抗菌剂释放到环境中。改性后的PVA复合膜具有优异的抗菌性能和力学性能，使其在活性包装领域的应用成为可能。
附图说明：
图1为实施例1中光交联前后的傅里叶红外光谱(FTIR)图。
图2为实施例1和对比例1中所制备PVA复合膜的抑菌实验图。
具体实施方式
为了更好地解释本发明，下面结合具体实施例对本发明进一步详细解释，但本发明的实施方式不限于此。
实施例1
(1)PVA水溶液的制备：将2g PVA在90℃下搅拌溶于25ml去离子水中，得到均匀的PVA水溶液；
(2)季铵盐复合液的制备：将0.1g季铵盐单体(DMAEMA-DB)、0.003g光交联剂(MBA)、0.003g光引发剂2959(2-羟基-4’-(2-羟基乙氧基)-2-甲基苯)溶于5mL乙醇/水(V乙醇:V水＝2:8)的混合溶液中，超声分散20min，得到季铵盐复合液；
(3)PVA复合膜的制备：将上述步骤(1)中的PVA水溶液趁热置于60℃的磁力搅拌器上，60℃下搅拌20min，后加入上述步骤(2)的季铵盐复合液，60℃下遮光搅拌60min，在室温下静置消泡后，浇铸到玻璃模具中，室温放置12h，60℃下烘干，得到PVA复合膜；
(4)光交联PVA复合膜的制备：将上述步骤(3)PVA复合膜暴露在紫外灯下1min，得到光交联PVA复合膜。
将上述实施例1中制备的改性PVA复合膜裁剪成15mm×15mm的正方形，后置于10mL浓度为106～107CFU/mL的金黄色葡萄球菌液中，37℃下振荡4h，后取100μL菌液，在固体培养基上涂覆并在37℃下恒温培养12h，观察固体培养基上的细菌生长情况。
Claims (2)
1.一种光交联抗菌性聚乙烯醇复合膜的制备方法：
(1)PVA水溶液的制备：将2g PVA在90℃下搅拌溶于25ml去离子水中，得到均匀的PVA水溶液；
(2)季铵盐复合液的制备：将季铵盐单体、光交联剂、光引发剂溶于乙醇/水的混合溶液中，超声分散20min，得到季铵盐复合液，其中季铵盐单体选自甲基丙烯酰氧乙基二甲基苄基氯化铵(DMAEMA-BC)、甲基丙烯酰氧乙基二甲基丁基溴化铵(DMAEMA-BB)、甲基丙烯酰氧乙基二甲基辛基溴化铵(DMAEMA-OB)、甲基丙烯酰氧乙基二甲基十二烷基溴化铵(DMAEMA-DB)、甲基丙烯酰氧乙基二甲基十六烷基溴化铵(DMAEMA-HB)，其用量为PVA的1％～10％，光交联剂为一种水溶性光交联剂N,N-亚甲基双丙烯酰胺(MBA)，其用量为季铵盐单体(QAS)的1％～3％，光引发剂为一种水溶性光引发剂2959，其用量为QAS的1％～3％；
(3)PVA复合膜的制备：将上述步骤(1)中的PVA水溶液置于60℃的磁力搅拌器上，60℃下遮光搅拌20min，后加入上述步骤(2)的季铵盐复合液，60℃下遮光搅拌60min，在室温下静置消泡后，浇铸到玻璃模具中，室温放置12h，60℃下烘干，得到PVA复合膜；
(4)光交联PVA复合膜的制备：将上述步骤(3)PVA复合膜暴露在紫外灯下辐射1min，得到光交联PVA复合膜。
2.根据权利要求1所述一种光交联抗菌性聚乙烯醇复合膜的制备方法，其特征在于步骤(2)中所述乙醇/水溶液中乙醇和水的体积比为2:8。
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