CN107216694B - 一种主客体自修复抗菌薄膜的制备方法 - Google Patents
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Abstract
本发明公开了一种主客体自修复抗菌薄膜的制备方法,该方法包括以下步骤:步骤一、在基底上重复顺次沉积修饰有β环糊精的支化聚乙烯亚胺及修饰有金刚烷的聚丙烯酸,沉积数次周期后,得到金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(PAA‑AD/PEI‑βCD)主客体薄膜;步骤二、旋涂MoS2溶液,制备得到MoS2/金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(MoS2/PAA‑AD/PEI‑βCD)主客体自修复抗菌薄膜。本发明提供的方法简单有效,操作简便,且所需时间较短。
Description
技术领域
本发明涉及一种MoS2/金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(MoS2/PAA-AD/PEI-βCD)主客体自修复抗菌薄膜的制备方法,属于MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜制备技术领域与应用。
背景技术
食品中含有丰富的营养成分,在适宜的温度和湿度条件下,微生物可大量生长繁殖。而食品包装可以保障食品品质,防止食品在生产、运输、储存、销售等过程中受到微生物或其他物质污染,减少食品氧化等反应发生率,延长货架期。今年来,食品包装新材料和新技术的开发应用与日俱增,人们对食品包装的要求也随之提高。消费者普遍希望购买到口感良好、品质安全且不含防腐剂的食品,因此,抗菌包装材料的作用显得尤为重要。一方面,抗菌材料可以保障食品品质,减少微生物污染;另一方面,可以有效减少食品中防腐剂的添加,满足消费者的购买需要。
在以往的研究工作中,抗菌材料如抗菌塑料、抗菌膜、抗菌纸等,虽然它们具有卫生自洁功能,并能有效地防止细菌交叉感染,但其易被磨损或者破裂,减少了材料的使用寿命,从而导致食品保鲜周期降低。随着材料科学与技术的发展,仿生材料逐渐进入人们的视野,如果能够模仿人类皮肤及骨骼的自愈合现象,制备出具有自修复效果的抗菌涂层材料,那么将从一个新的角度极大程度的延长材料的使用寿命。
层层自组装技术(Layer-by-Layer self-assembly)是近年来发展起来的制备有序薄膜的方法。它利用有机或无机阴阳离子的静电吸附特性,通过反离子体系的交替分子沉积形成薄膜。1991年D.Decher等人用层层吸附技术对构造有序薄膜进行了开创性研究。他们用两亲性有机阴阳离子(或者聚电解质)在离子化基片表面交替吸附制备多层膜。到目前为止,很多种材料比如碳纳米管、蛋白质、核酸、磷脂和有机及无机颗粒都被成功的用来构造具有特定组成,厚度和性质的多层有序膜,孙俊奇课题组在层层自组装制备自修复薄膜方面做了很多杰出的工作。
目前,关于通过层层自组装技术的主体客体相互作用的MoS2自愈合抗菌涂层的相关研究尚未有报道。本专利制备了这样多功能的自修复薄膜,填补了现有技术中的空缺。
发明内容
技术问题:本发明的目的是提供一种主客体自修复抗菌薄膜的制备方法,该方法利用层层自组装技术将MoS2,β环糊精修饰的支化聚乙烯亚胺和金刚烷修饰的聚丙烯酸组装到基底表面,制备MoS2/金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(MoS2/PAA-AD/PEI-βCD)自修复抗菌薄膜;本方法简单有效,操作简便,且所需时间较短。
技术方案:MoS2/金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(MoS2/PAA-AD/PEI-βCD)表示“MoS2”复合“金刚烷的聚丙烯酸”复合“β环糊精的支化聚乙烯亚胺”。
本发明的一种主客体自修复抗菌薄膜的制备方法包括如下步骤:
步骤一、在预处理过的基底上重复顺次沉积修饰有β环糊精的支化聚乙烯亚胺及修饰有金刚烷的聚丙烯酸,沉积数次周期后,得到金刚烷的聚丙烯酸-β环糊精的支化聚乙烯亚胺PAA-AD/PEI-βCD主客体薄膜;
步骤二、在步骤一得到的PAA-AD/PEI-βCD主客体薄膜上旋涂MoS2溶液,制备得到MoS2/金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜。
其中:
所述预处理过的基底,其预处理的方法为:将玻璃片先后浸入丙酮溶液和乙醇溶液中超声振荡,之后浸入H2SO4-H2O2混合溶液中浸泡,取出后氮气吹干得到预处理过的基底。
所述的超声振荡,超声振荡的时间30~60min,超声频率为90~100Hz。
所述的H2SO4-H2O2混合溶液中H2SO4:H2O2的体积比为3:7~1:3,所述浸泡时间为4~12h。
所述得到金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺PAA-AD/PEI-βCD主客体薄膜具体过程为:首先将预处理后的玻璃片浸泡在浓度为4~8mg/mlβ环糊精的支化聚乙烯亚胺溶液中15~30min,取出用水冲洗后浸泡在金刚烷修饰的聚丙烯酸溶液中15~30min,取出用水冲洗,再浸泡在浓度为4~8mg/ml刚烷的聚丙烯酸溶液中15~30min,取出用水冲洗,上述步骤重复15~30周期,制得金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺PAA-AD/PEI-βCD主客体薄膜。
所述的制备得到MoS2/金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜的过程为:旋转速度1000~3000rpm,旋涂浓度为10mg/L~18mg/L MoS2溶液,得到MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜。
有益效果:本发明与现有技术相比,具有以下优点:
1、本发明以层层自组装法制备MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜,通过支化聚乙烯亚胺侧链上β环糊精的和聚丙烯酸上的金刚烷之间的可逆性主客体连接实现薄膜的自修复能力;
2、MoS2的添加,实现薄膜的抗菌能力;
3、本发明方法简单有效,操作简便,且所需时间较短;
4、本发明制备装置简单,不需要特殊的设备;
5、本发明制备MoS2/PAA-AD/PEI-βCD主客体自修复透明抗菌薄膜,不仅本身具有很好的抗菌效应,在紫外照射下,可以达到完全的抗菌效果,具有广泛的应用前景。
附图说明
图1是实施例1制备出MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜对大肠杆菌抑制图。
具体实施方式
下面结合实施例对本发明做更进一步地解释,下列实施例仅用于说明本发明,但并不用来限定本发明的实施范围。
本发明的MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜的制备方法包括如下步骤:
步骤一、将玻璃片浸入丙酮溶液超声振荡30~60min,之后再浸入乙醇溶液中超声振荡30~60min;最后浸入体积比为3:7~1:3的H2SO4-H2O2混合溶液中浸泡4~12h,N2吹干得到清洗干净的玻璃片。
步骤二、将处理后的玻璃片浸泡在浓度为4~8mg/mlβ环糊精的支化聚乙烯亚胺溶液中15~30min,取出用水冲洗后浸泡在金刚烷修饰的聚丙烯酸溶液中15~30min,取出用水冲洗,再浸泡在浓度为4~8mg/ml金刚烷的聚丙烯酸溶液中15~30min,取出用水冲洗,上述步骤重复15~30周期,制得金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(PAA-AD/PEI-βCD)主客体薄膜。
步骤三、旋转速度1000~3000rpm,旋涂浓度为10mg/L~18mg/L MoS2溶液,得到MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜。
实施例1
1)将玻璃片浸入丙酮溶液超声振荡30min,之后再浸入乙醇溶液中超声振荡30min;最后浸入体积比为3:7的H2SO4-H2O2混合溶液中浸泡4h,氮气吹干得到清洗干净的玻璃片。
2)将清洗干净的玻璃片浸泡在4mg/mlβ环糊精修饰的支化聚乙烯亚胺溶液15min,用水冲洗洗去物理吸附的聚合物;然后再浸入到4mg/ml金刚烷修饰的聚丙烯酸溶液中15min后用水冲洗;上述步骤重复15周期,制得金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(PAA-AD/PEI-βCD)主客体薄膜。
3)旋转速度1000rpm,旋涂浓度为10mg/L MoS2溶液,得到MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜。
图1是实施例1制备出MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜对大肠杆菌抑制图。
实施例2
1)将玻璃片浸入丙酮溶液超声振荡40min,之后再浸入乙醇溶液中超声振荡40min;最后浸入体积比为3:8的H2SO4-H2O2混合溶液中浸泡6h,N2吹干得到清洗干净的硅片片。
2)将清洗干净的玻璃片浸泡在5mg/mlβ环糊精修饰的支化聚乙烯亚胺溶液20min,用水冲洗洗去物理吸附的聚合物;然后再浸入到5mg/ml金刚烷修饰的聚丙烯酸溶液中20min后用水冲洗;上述步骤重复20周期,制得金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(PAA-AD/PEI-βCD)主客体薄膜。
3)旋转速度1500rpm,旋涂浓度为13mg/L MoS2溶液,得到MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜。
实施例3
1)将玻璃片浸入丙酮溶液超声振荡50min,之后再浸入乙醇溶液中超声振荡50min;最后浸入体积比为2:5的H2SO4-H2O2混合溶液中浸泡8h,氮气吹干得到清洗干净的金属合金片。
2)将清洗干净的玻璃片浸泡在6mg/mlβ环糊精修饰的支化聚乙烯亚胺溶液25min,用水冲洗洗去物理吸附的聚合物;然后再浸入到6mg/ml金刚烷修饰的聚丙烯酸溶液中25min后用水冲洗;上述步骤重复25周期,制得金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(PAA-AD/PEI-βCD)主客体薄膜。
3)旋转速度2000rpm,旋涂浓度为16mg/L MoS2溶液,得到MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜。
实施例4
1)将玻璃片浸入丙酮溶液超声振荡60min,之后再浸入乙醇溶液中超声振荡60min;最后浸入体积比为1:3的H2SO4-H2O2混合溶液中浸泡12h,氮气吹干得到清洗干净的玻璃片。
2)将清洗干净的玻璃片浸泡在8mg/mlβ环糊精修饰的支化聚乙烯亚胺溶液30min,用水冲洗洗去物理吸附的聚合物;然后再浸入到8mg/ml金刚烷修饰的聚丙烯酸溶液中30min后用水冲洗;上述步骤重复30周期,制得金刚烷的聚丙烯酸/β环糊精的支化聚乙烯亚胺(PAA-AD/PEI-βCD)主客体薄膜。
3)旋转速度3000rpm,旋涂浓度为18mg/L MoS2溶液,得到MoS2/PAA-AD/PEI-β CD主客体自修复抗菌薄膜。
Claims (3)
1.一种主客体自修复抗菌薄膜的制备方法,其特征在于:该方法包括如下步骤:
步骤一、在预处理过的基底上重复顺次沉积修饰有β环糊精的支化聚乙烯亚胺及修饰有金刚烷的聚丙烯酸,沉积数次周期后,得到金刚烷修饰的聚丙烯酸/β环糊精修饰的支化聚乙烯亚胺PAA-AD/PEI-βCD主客体薄膜;
步骤二、在步骤一得到的PAA-AD/PEI-βCD主客体薄膜上旋涂MoS2溶液,制备得到MoS2/金刚烷修饰的聚丙烯酸/β环糊精修饰的支化聚乙烯亚胺MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜;
制备得到金刚烷修饰的聚丙烯酸/β环糊精修饰的支化聚乙烯亚胺PAA-AD/PEI-βCD主客体薄膜的具体过程为:首先将预处理后的玻璃片浸泡在浓度为4~8mg/mlβ环糊精修饰的支化聚乙烯亚胺溶液中15~30min,取出用水冲洗后再浸泡在浓度为4~8mg/ml金刚烷修饰的聚丙烯酸溶液中15~30min,取出用水冲洗,上述步骤重复15~30周期,制得金刚烷修饰的聚丙烯酸/β环糊精修饰的支化聚乙烯亚胺PAA-AD/PEI-βCD主客体薄膜;
制备得到MoS2/金刚烷修饰的聚丙烯酸/β环糊精修饰的支化聚乙烯亚胺MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜的过程为:旋转速度1000~3000rpm,旋涂浓度为10mg/L~18mg/L的MoS2溶液,得到MoS2/PAA-AD/PEI-βCD主客体自修复抗菌薄膜;
所述预处理过的基底,其预处理的方法为:将玻璃片先后浸入丙酮溶液和乙醇溶液中超声振荡,之后浸入H2SO4-H2O2混合溶液中浸泡,取出后氮气吹干得到预处理过的基底。
2.如权利要求1所述的一种主客体自修复抗菌薄膜的制备方法,其特征在于:所述的超声振荡,超声振荡的时间30~60min,超声频率为90~100Hz。
3.如权利要求1所述的一种主客体自修复抗菌薄膜的制备方法,其特征在于:所述的H2SO4-H2O2混合溶液中H2SO4:H2O2的体积比为3:7~1:3,所述浸泡时间为4~12h。
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