CN107082895A - 可降解的纳米抑菌薄膜的制备方法 - Google Patents
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Abstract
本发明提供了一种可降解的纳米抑菌薄膜的制备方法,其包括如下步骤:制备纳米Si‑TiO2;将纳米Si‑TiO2、分散剂加入可降解聚合物水溶液中,混合均匀,脱气后得到制膜液;将所述制膜液进行流延成膜,得到所述可降解的纳米抑菌薄膜;其中,所述纳米Si‑TiO2的制备方法为:将纳米TiO2与硅烷偶联剂分散在丙酮中,在超声的条件下进行偶联,经过滤、水洗、真空干燥、研磨后制备成纳米Si‑TiO2。与现有技术相比,本发明具有如下的有益效果:本发明工艺步骤简单、包装材料的抑菌(大肠杆菌和金黄色葡萄球菌)效果显著;本发明的包装材料具有机械性强、渗透性小等优点;本发明工艺操作安全、高效无毒、绿色环保、易于推广等优点。
Description
技术领域
本发明涉及一种可降解的纳米抑菌薄膜的制备方法,属于食品包装材料技术领域。
背景技术
目前,食品安全已经成为公众关注的焦点。除了食品链中的有害物质带来的食品安全问题之外,食品包装导致的食品安全问题也日益引起重视。为了进一步提高食品包装的安全和品质,我们必须从包装材料本身寻求突破,来逾越包装技术遇到的屏障。为了节约能源、保护环境、实现可持续发展,开发新型的可生物降解材料是食品包装的必由之路。
从材料上分,现有的食品包装有普通塑料包装(聚乙烯、聚丙烯、聚氯乙烯等),以及新型可降解包装(可降解聚合物,聚乳酸等)。可生物降解高分子可降解聚合物(PVA)安全无毒,具有优异的气体阻隔性、拉伸强度和机械强度,是良好的包装材料,但是单纯的PVA包装材料并不具有抑菌作用,且其耐水性较差,限制了其在食品包装中的应用。纳米包装材料主要是指运用纳米技术,通过对包装材料进行纳米合成、纳米添加、纳米改性,使其具有某一特性或功能的一类包装材料。纳米材料由于其结构的特殊性,如大比表面、小尺寸效应、界面效应、量子效应和量子隧道效应,因而表现出许多不同于传统材料的独特性能:较高的机械性能(强韧性,耐磨性和可塑性)、优异的物理化学性能(高阻隔性、光泽和透明度、抗磁防爆特性)、较好的生物活性(抑菌性、固定化酶、生物传感)。纳米TiO2安全无毒,已被美国食品药品监督管理局批准用于食品、药品、化妆品、以及与食品直接接触的物体表面,除了纳米材料的共性以外,纳米TiO2所具有的超亲水性在应用于包装时具有自清洁和防雾效果。因此,将纳米TiO2与可生物降解的PVA交联复合,不仅使包装材料具有抑菌性能,而且能够改善PVA的耐水性和力学性能。此外为了使TiO2在聚合物基质中更好的分散,将TiO2与硅烷偶联改性,此方法引入的Si-O键对CO2和O2具有吸附、溶解、扩散、释放作用,以上特性,恰好是对可生物降解高分子材料性能缺陷的弥补,使其用于食品包装成为可能。
然而,现有报道中还未见有可降解PVA/纳米Si-TiO2包装材料的任何报道,也未见其在抑菌方面的任何报道。
发明内容
本发明目的在于提供一种可降解纳米抑菌包装材料及其制备方法,与市面上现有的普通塑料包装(聚乙烯、聚丙烯、聚氯乙烯等)和传统可降解包装相比,可降解PVA/纳米Si-TiO2包装材料具有制备工艺简单、抑菌显著、机械性优、渗透性小、操作安全、高效无毒、绿色环保、易于推广等优点。
本发明是通过以下技术方案实现的:
本发明提供了一种可降解的纳米抑菌薄膜的制备方法,其包括如下步骤:
制备纳米Si-TiO2;
将纳米Si-TiO2、分散剂加入可降解聚合物水溶液中,混合均匀,脱气后得到制膜液;
将所述制膜液进行流延成膜,得到所述可降解的纳米抑菌薄膜;
其中,所述纳米Si-TiO2的制备方法为:将纳米TiO2与硅烷偶联剂分散在丙酮中,在超声的条件下进行偶联,经过滤、水洗、真空干燥、研磨后制备成纳米Si-TiO2。
作为优选方案,所述纳米Si-TiO2的粒径为60~100nm。
作为优选方案,所述超声的功率为500~700W。超声功率过小,则会影响二氧化钛在PVA中的溶解,同时延长超声时间,功率过大则会造成能耗过大。
作为优选方案,所述纳米Si-TiO2和分散剂的总质量与可降解聚合物的质量比为(1~5):100。
作为优选方案,所述硅烷偶联剂为氨丙基三乙氧基硅烷,所述分散剂为聚乙二醇;所述可降解聚合物选自聚乙烯醇、聚维酮、淀粉、聚乳酸中的至少一种。
作为优选方案,所述聚乙二醇的平均分子量为400,聚乙烯醇为1797型,指的是聚合度为1700,醇解度为97%的聚乙烯醇。
作为优选方案,所述纳米TiO2与硅烷偶联剂的质量比为100:(5~20),纳米TiO2与丙酮的质量体积比为1g:100mL。
作为优选方案,所述可降解聚合物水溶液的制备方法为:
将3g可降解聚合物粉末加入97mL水中,在95℃下进行搅拌,得到质量分数为3%的可降解聚合物水溶液。
作为优选方案,所述流延成膜的温度为25℃,相对湿度为50%。
与现有技术相比,本发明具有如下的有益效果:
1、本发明工艺步骤简单、包装材料的抑菌(大肠杆菌和金黄色葡萄球菌)效果显著;
2、本发明的包装材料具有机械性强、渗透性小等优点;
3、本发明工艺操作安全、高效无毒、绿色环保、易于推广等优点。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例1
本实施例涉及一种可降解的纳米抑菌薄膜的制备方法,其包括如下步骤:
硅烷偶联剂改性纳米TiO2:0.1g纳米TiO2(粒径为100nm)与0.01g硅烷偶联剂(氨丙基三乙氧基硅烷,APS)加入至10mL丙酮溶液中,在超声功率为600W的条件下超声偶联30分钟,纯水洗涤2次,过滤,真空干燥4h,干燥物研磨后即成改性纳米TiO2(Si-TiO2)。聚乙烯醇/纳米Si-TiO2包装材料的制备:3g聚乙烯醇(1797型)粉末加入97mL纯水中,于95℃下加热搅拌2小时,冷却得到3%聚乙烯醇水溶液。将0.06g纳米Si-TiO2和0.06g分散剂聚乙二醇400(PEG400)加入上述聚乙烯醇(PVA)水溶液中共混(Si-TiO2/PVA=2.00wt%),在超声功率为600W的条件下超声30分钟,经真空度为-0.1MPa的真空脱气装置中脱气30分钟,采用流延法在尺寸为25cm×25cm的玻璃模具中成膜,成膜环境温度为25℃,相对湿度为50%,并平衡7天,即制备一种可降解的PVA/纳米Si-TiO2抑菌包装材料。本实施例的可降解的PVA/纳米Si-TiO2抑菌包装材料的抑菌性结果见表1,机械性能和渗透性能结果见表2。
实施例2
本实施例涉及一种可降解的纳米抑菌薄膜的制备方法,其包括如下步骤:
硅烷偶联剂改性纳米TiO2:0.1g纳米TiO2(粒径为100nm)与0.02g硅烷偶联剂(氨丙基三乙氧基硅烷,APS)加入至10mL丙酮溶液中,在超声功率为500W的条件下超声偶联30分钟,纯水洗涤2次,过滤,真空干燥4h,干燥物研磨后即成改性纳米TiO2(Si-TiO2)。聚乙烯醇/纳米Si-TiO2包装材料的制备:3g聚乙烯醇(1797型)粉末加入97mL纯水中,于95℃下加热搅拌2小时,冷却得到3%聚乙烯醇水溶液。将0.04g纳米Si-TiO2和0.08g分散剂聚乙二醇400(PEG400)加入上述聚乙烯醇(PVA)水溶液中共混(Si-TiO2/PVA=2.67wt%),在超声功率为600W的条件下超声30分钟,经真空度为-0.1MPa的真空脱气装置中脱气30分钟,采用流延法在尺寸为25cm×25cm的玻璃模具中成膜,成膜环境温度为25℃,相对湿度为50%,并平衡7天,即制备一种可降解的PVA/纳米Si-TiO2抑菌包装材料。本实施例的可降解的PVA/纳米Si-TiO2抑菌包装材料的抑菌性结果见表1,机械性能和渗透性能结果见表2。
实施例3
本实施例涉及一种可降解的纳米抑菌薄膜的制备方法,其包括如下步骤:
硅烷偶联剂改性纳米TiO2:0.1g纳米TiO2(粒径为100nm)与0.01g硅烷偶联剂(氨丙基三乙氧基硅烷,APS)加入至10mL丙酮溶液中,在超声功率为600W的条件下超声偶联30分钟,纯水洗涤2次,过滤,真空干燥4h,干燥物研磨后即成改性纳米TiO2(Si-TiO2)。聚乙烯醇/纳米Si-TiO2包装材料的制备:3g聚乙烯醇(1797型)粉末加入97mL纯水中,于95℃下加热搅拌2小时,冷却得到3%聚乙烯醇水溶液。将0.04g纳米Si-TiO2和0.04g分散剂聚乙二醇400(PEG400)加入上述聚乙烯醇(PVA)水溶液中共混(Si-TiO2/PVA=1.33wt%),在超声功率为600W的条件下超声30分钟,经真空度为-0.1MPa的真空脱气装置中脱气30分钟,采用流延法在尺寸为25cm×25cm的玻璃模具中成膜,成膜环境温度为25℃,相对湿度为50%,并平衡7天,即制备一种可降解的PVA/纳米Si-TiO2抑菌包装材料。本实施例的可降解的PVA/纳米Si-TiO2抑菌包装材料的抑菌性结果见表1,机械性能和渗透性能结果见表2。
表1
表1为可降解的PVA/纳米Si-TiO2抑菌包装材料的对大肠杆菌和金黄色葡萄球菌的抑制率。空白是纯PVA材料,PVA/纳米Si-TiO2材料分别添加不同量的纳米Si-TiO2,即Si-TiO2与PVA的质量比为1.33%,2.00%和2.67%。由表1可以看出,与空白相比,PVA/纳米Si-TiO2材料对大肠杆菌和金黄色葡萄球菌的抑制效果均明显,特别是Si-TiO2与PVA的质量比为2.00%时抑制率最高。
表2
表2为可降解的PVA/纳米Si-TiO2抑菌包装材料的机械性能和渗透性能结果。空白是纯PVA材料,PVA/纳米Si-TiO2材料分别添加不同量的纳米Si-TiO2,即Si-TiO2与PVA的质量比为1.33%,2.00%和2.67%。由表2可以看出,与空白相比,PVA/纳米Si-TiO2材料的拉伸强度、断裂伸长率增强,透湿性降低,特别是Si-TiO2与PVA的质量比2.67%时拉伸强度、断裂伸长率最强,透湿性最低。
以上对本发明的具体实施例进行了描述。需要理解的是,本发明并不局限于上述特定实施方式,本领域技术人员可以在权利要求的范围内做出各种变形或修改,这并不影响本发明的实质内容。
Claims (9)
1.一种可降解的纳米抑菌薄膜的制备方法,其特征在于,包括如下步骤:
制备纳米Si-TiO2;
将纳米Si-TiO2、分散剂加入可降解聚合物水溶液中,混合均匀,脱气后得到制膜液;
将所述制膜液进行流延成膜,得到所述可降解的纳米抑菌薄膜;
其中,所述纳米Si-TiO2的制备方法为:将纳米TiO2与硅烷偶联剂分散在丙酮中,在超声的条件下进行偶联,经过滤、水洗、真空干燥、研磨后制备成纳米Si-TiO2。
2.如权利要求1所述的可降解的纳米抑菌薄膜的制备方法,其特征在于,所述纳米Si-TiO2的粒径为60~100nm。
3.如权利要求1所述的可降解的纳米抑菌薄膜的制备方法,其特征在于,所述超声的功率为500~700W。
4.如权利要求1所述的可降解的纳米抑菌薄膜的制备方法,其特征在于,所述纳米Si-TiO2和分散剂的总质量与可降解聚合物的质量比为(1~5):100。
5.如权利要求1或4所述的可降解的纳米抑菌薄膜的制备方法,其特征在于,所述硅烷偶联剂为氨丙基三乙氧基硅烷,所述分散剂为聚乙二醇;所述可降解聚合物选自聚乙烯醇、聚维酮、淀粉、聚乳酸中的至少一种。
6.如权利要求5所述的可降解的纳米抑菌薄膜的制备方法,其特征在于,所述聚乙二醇的平均分子量为400,聚乙烯醇为1797型,指的是聚合度为1700,醇解度为97%的聚乙烯醇。
7.如权利要求1所述的可降解的纳米抑菌薄膜的制备方法,其特征在于,所述纳米TiO2与硅烷偶联剂的质量比为100:(5~20),纳米TiO2与丙酮的质量体积比为1g:100mL。
8.如权利要求1所述的可降解的纳米抑菌薄膜的制备方法,其特征在于,所述可降解聚合物水溶液的制备方法为:
将3g可降解聚合物粉末加入97mL水中,在95℃下进行搅拌,得到质量分数为3%的可降解聚合物水溶液。
9.如权利要求1所述的可降解的纳米抑菌薄膜的制备方法,其特征在于,所述流延成膜的温度为25℃,相对湿度为50%。
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