CN107099047A - 一种pe保鲜涂布膜的制备方法与用途 - Google Patents

一种pe保鲜涂布膜的制备方法与用途 Download PDF

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CN107099047A
CN107099047A CN201710418012.XA CN201710418012A CN107099047A CN 107099047 A CN107099047 A CN 107099047A CN 201710418012 A CN201710418012 A CN 201710418012A CN 107099047 A CN107099047 A CN 107099047A
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余赞
田璐
钟文
罗臻
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Changde Deyuan Investment Promotion Co ltd
Changde Jinde New Material Technology Co Ltd
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Abstract

本发明属于包装材料技术领域，具体涉及一种PE保鲜涂布膜的制备方法与用途。本发明以桑树纤维为生物质原料制备的棒状纳米生物颗粒，以羧甲基壳聚糖为抗菌剂制备出改性聚乙烯醇涂布液，然后对PE基材进行涂布得保鲜防腐性能的涂布膜。较传统的TiO2、SiO2等无机纳米粒子改性，本发明以棒状纳米生物颗粒与聚乙烯醇具有较好的生物相容性，制备出的保鲜涂布膜阻隔性能优异。

Description

一种PE保鲜涂布膜的制备方法与用途
技术领域
本发明属于包装材料技术领域，具体涉及一种PE保鲜涂布膜的制备方法与用途。
背景技术
保鲜膜是一种塑料包装制品，通常以乙烯为母料通过聚合反应制成，主要用于微波炉食品加热、冰箱食物保存、生鲜及熟食包装等场合，在家庭生活、超市卖场、宾馆饭店及工业生产的食品包装领域都有广泛应用。根据所用材料及添加塑化剂不同，保鲜膜分为多种类型，可适用于不同的场合。保鲜膜以其方便、经济、美观的特点受到了人们的青睐。然而，由于在生产过程中普遍添加了塑化剂，保鲜膜对人体健康的影响也受到了人们的关注。
聚乙烯醇（Polyvinyl alcohol，PVA）是一种多羟基聚合物，具有良好的成膜性能，在低湿环境中，PVA膜具有良好的气体阻隔性能，所以常常作为涂布液涂布于聚乙烯（polyethylene ，简称PE）基材的表面。但是聚乙烯醇涂布液由于耐水性能和耐候性能差，所以通常需要改性，PVA的耐水性主要通过缩醛化、氨基树脂、尿素、硼酸、硅烷偶联剂于PVA发生化学反应进行改性，但是需要加入一些化学试剂，不利于环保，尤其是作为一些食品、果蔬的包装材料；PVA进行耐水性改性的同时，通过加入纳米粒子（SiO2、TiO2、黏土）使PVA涂布液的力学性能，如附着力、抗冲击性能、柔韧性、阻隔性能等有不同程度的改进。
生物质资源的利用主要体现在以下几个方面，生物质材料、生物质能源和纸浆，其中生物质材料是以生物质资源为原材料，通过物理、化学和生物的手段，加工出的性能优良、无污染可降解、可再生的新型材料。其中用来制作包装制品或者包装用途，能够起到保护产品、方便储运、促进销售作用的生物质材料，称为生物质包装材料。
将生物质材料作为改性剂用来改性聚乙烯醇涂布液，采用改性的聚乙烯醇涂布液来制备PE涂布膜的技术方案未见文献报道。
发明内容
本发明的目的是克服现有技术中聚乙烯醇涂布液需要采用化工试剂进行耐水性改性的缺点，本发明提供一种采取生物质材料对聚乙烯醇改性来制备涂布液，并涂布于PE基材上形成PE保鲜涂布膜，本发明制备的涂布膜不仅具有良好的阻隔性能，能够实现良好的保鲜效果，而且具有一定的防腐杀菌性能。
本发明是通过以下技术方案实现上述目的的，一种PE保鲜涂布膜的制备方法，包括以下步骤：
1) 棒状纳米生物质颗粒的制备：
将桑树皮粉碎成粒径为100mm以下的颗粒物，然后将颗粒物置于10%Wt的氢氧化钠水溶液中于70℃下机械搅拌6h，然后过滤洗涤至中性并烘干；将烘干后的颗粒物采取10%wt的磷酸水溶液于80℃下搅拌3h，然后过滤水洗至中性并烘干得一次酸化颗粒物；将一次酸化颗粒物置于5%wt的盐酸水溶液中于90℃下搅拌2h，然后以2000rpm的转速下离心，离心物采用水洗至中性后真空干燥并粉碎得二次酸化后的颗粒物；将二次酸化后的颗粒物置于30%wt的硫酸水溶液中于70℃搅拌1h，然后在12000rpm的转速下离心，取清液室温透析14天，然后进行冻干得棒状纳米生物质颗粒；本发明采用硫酸对桑树皮进行纤维素的水解，其机理是当硫酸水解纤维素时，首先质子会进入非结晶区，利于糖苷键的断裂，从而形成了具有一定尺寸的纳米纤维结构；
2) 改性聚乙烯醇涂布液的制备：
将10g聚乙烯醇加入到200ml 10%V乙醇的水溶液中，然后加入0.3-0.5g棒状纳米生物质颗粒、升温至86℃以上搅拌分散0.5h得分散液，然后向分散液中加入羧甲基壳聚糖的醋酸水溶液和增塑剂超声分散2h得改性聚乙烯醇涂布液；
3) 将改性聚乙烯醇涂布液采用钢丝刮刀涂布法在PE基材表面进行涂布，然后干燥得PE保鲜涂布膜。
优选的，步骤2）所述聚乙烯醇的分子量为12-15万，醇解度为85%以上，20℃下4%wt聚乙烯醇水溶液的粘度为3.6-4.0MPa.S。
优选的，步骤2）所述羧甲基壳聚糖的醋酸水溶液由以下制备方法制备：将羧甲基壳聚糖分散在1%V的醋酸水溶液中，制备成4%wt的羧甲基壳聚糖水溶液，然后加入吐温80于50℃下搅拌2h得羧甲基壳聚糖的醋酸水溶液；优选的，步骤2）所述羧甲基壳聚糖的醋酸水溶液的加入量为3-4ml。
优选的，步骤2）所述增塑剂为邻苯二甲酸酯或甘油，优选为甘油；所述增塑剂的用量为0.2-0.4g。
优选的，所述PE基材厚度为60μm；改性聚乙烯醇涂布液在PE基材上涂布的量为1.4-1.6g/m2，涂布厚度为4-8μm；优选的改性聚乙烯醇涂布液在PE基材上涂布的量为1.5g/m2，涂布厚度为6μm；薄膜的透氧率小于0.6cm3/(m-2.24h-1.0.1MPa-1)，水蒸气透过量为2.3g.m-2.24h-1。
本发明制备出的PE保鲜涂布膜可用于果蔬的保鲜，如樱桃、西红柿、猕猴桃，尤其是樱桃可保鲜长达20天，硬度、水分和腐败率均较单独PE薄膜效果好。
与现有技术相比，本发明具有如下优点：
1）本发明提供了一种以桑树纤维为原料制备的棒状纳米生物颗粒来改性聚乙烯醇涂布液，使制备出的聚乙烯醇涂布液的稳定性得到大大改善，有利于涂布液的涂覆；较传统的TiO2、SiO2等无机纳米粒子改性，本发明以棒状纳米生物颗粒与聚乙烯醇具有较好的生物相容性；
2）发明制备的改性聚乙烯醇涂布液与PE基材形成的涂布膜阻隔性能大大优于纯PE薄膜，本发明制备出的薄膜的透氧率小于0.6cm3/(m-2.24h-1.0.1MPa-1)，水蒸气透过量为2.3g.m-2.24h-1；
3）本发明制备出的PE保鲜涂布膜可广泛用于樱桃、西红柿、猕猴桃的保鲜，保鲜涂布膜具有一定的抗菌性，对大肠杆菌的杀菌率达到97%以上。
附图说明
图1为本发明制备的棒状纳米生物质颗粒扫描电镜图（SEM）。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明了，下面结合具体实施方式，对本发明进一步详细说明。应该理解，这些描述只是示例性的，而并非要限制本发明的范围。
本发明使用的聚乙烯醇来源于上海美梦佳化工科技有限公司，分子量为12-15万，醇解度为85%以上，20℃下4%wt聚乙烯醇水溶液的粘度为3.6-4.0MPa.S。
实施例1
1） 棒状纳米生物质颗粒的制备：
将10kg桑树皮粉碎成粒径为80mm以下的颗粒物，然后将颗粒物置于100L 10%Wt的氢氧化钠水溶液中于70℃下机械搅拌6h，然后过滤水洗至中性并50℃下烘干；将烘干后的颗粒物采取100L 10%wt的磷酸水溶液于80℃下搅拌3h，然后过滤水洗至中性并烘干得一次酸化颗粒物；将一次酸化颗粒物置于5%wt的盐酸水溶液中于90℃下搅拌2h，然后以2000rpm的转速下离心，离心物采用水洗至中性后真空干燥并粉碎得二次酸化后的颗粒物；将二次酸化后的颗粒物置于30%wt的硫酸水溶液中于70℃搅拌1h，然后在12000rpm的转速下离心，取清液室温透析14天，然后进行冻干得棒状纳米生物质颗粒；
棒状纳米生物质颗粒的扫描电镜如图1所示，从图中可以看出本发明制备出的棒状纳米生物质颗粒粒径均小于200nm以下，具有很好的纳米效应，而且无颗粒聚集的现象，可均匀分散在在聚乙烯醇涂布液中。
2） 改性聚乙烯醇涂布液的制备：
将10g聚乙烯醇加入到200ml 10%V乙醇的水溶液中，然后加入0.5g棒状纳米生物质颗粒、升温至86℃以上搅拌分散0.5h得分散液，然后向分散液中加入羧甲基壳聚糖的醋酸水溶液3ml和增塑剂邻苯二甲酸二(2-乙基己)酯0.2g超声分散2h得改性聚乙烯醇涂布液；羧甲基壳聚糖的醋酸水溶液由以下制备方法制备：将羧甲基壳聚糖分散在1%V的醋酸水溶液中，制备成4%wt的羧甲基壳聚糖水溶液，然后加入0.4g吐温80于50℃下、1200rpm的转速下搅拌2h得羧甲基壳聚糖的醋酸水溶液。
3） 将改性聚乙烯醇涂布液采用钢丝刮刀涂布法在厚度为60μm的PE基材表面进行涂布，然后60℃下干燥8h得PE保鲜涂布膜；改性聚乙烯醇涂布液在PE基材上涂布的量为1.4g/m2，涂布厚度为4μm。
实施例2
1） 棒状纳米生物质颗粒的制备：
将10kg桑树皮粉碎成粒径为60mm以下的颗粒物，然后将颗粒物置于100L 10%Wt的氢氧化钠水溶液中于70℃下机械搅拌6h，然后过滤水洗至中性并50℃下烘干；将烘干后的颗粒物采取100L 10%wt的磷酸水溶液于80℃下搅拌3h，然后过滤水洗至中性并烘干得一次酸化颗粒物；将一次酸化颗粒物置于5%wt的盐酸水溶液中于90℃下搅拌2h，然后以2000rpm的转速下离心，离心物采用水洗至中性后真空干燥并粉碎得二次酸化后的颗粒物；将二次酸化后的颗粒物置于30%wt的硫酸水溶液中于70℃搅拌1h，然后在12000rpm的转速下离心，取清液室温透析14天，然后进行冻干得棒状纳米生物质颗粒。
2） 改性聚乙烯醇涂布液的制备：
将10g聚乙烯醇加入到200ml 10%V乙醇的水溶液中，然后加入0.3g棒状纳米生物质颗粒、升温至86℃以上搅拌分散0.5h得分散液，然后向分散液中加入羧甲基壳聚糖的醋酸水溶液3ml和增塑剂邻苯二甲酸二(2-乙基己)酯0.2g超声分散2h得改性聚乙烯醇涂布液；羧甲基壳聚糖的醋酸水溶液由以下制备方法制备：将羧甲基壳聚糖分散在1%V的醋酸水溶液中，制备成4%wt的羧甲基壳聚糖水溶液，然后加入0.4g吐温80于50℃下1200rpm的转速下搅拌2h得羧甲基壳聚糖的醋酸水溶液。
3） 将改性聚乙烯醇涂布液采用钢丝刮刀涂布法在厚度为60μm的PE基材表面进行涂布，然后60℃下干燥8h得PE保鲜涂布膜；改性聚乙烯醇涂布液在PE基材（为克服表面能低的缺点，表面经电晕处理过）上涂布的量为1.4g/m2，涂布厚度为4μm。
对实施例2制备的改性聚乙烯醇涂布液进行粘度测试，试验采用Zahn杯（3号杯，上海普申化工机械有限公司，测试时间S），测量三次取其平均值，试验结果表明：
10℃下本发明制备的改性聚乙烯醇涂布液放置1天的粘度为40.2S，放置4天的粘度为46.4S，无明显增长；作为对比，与实施例2中改性聚乙烯醇涂布液相比制备过程中不添加棒状纳米生物质颗粒，其余原料与制备方法与实施例2中完全相同，制备出的聚乙烯醇涂布液10℃放置1天的粘度为56.1S，10℃放置4天的粘度为67.2S；所以本发明的棒状纳米生物质颗粒大大提高了聚乙烯涂布液的稳定性。
研发过程中，在确定改性聚乙烯醇涂布液在PE基材上的涂布量时，以透过率（氧气和水蒸气）为衡量指标确定了最终涂布的量为1.4-1.6g/m2，优选为1.5g/m2，表1为涂布量与透过率的关系：
表1涂膜量与透过率的关系
随着改性聚乙烯醇涂布液涂布量的增加，制备出PE保鲜涂布膜的阻隔性能不断提高，涂布量为1.5g/m2时达到最优。
采用本发明实施例2制备的涂布膜对樱桃、西红柿、猕猴桃进行保鲜测试，以失水率为衡量指标测试其保鲜程度，以普通PE保鲜膜为对比；结果如表2所示：
表2保鲜涂布膜的保鲜性能（失水率和腐败率为衡量指标）
以上结果表明，本发明制备的保鲜涂布膜对果蔬具有良好的防霉保鲜作用，尤其是对樱桃，失水率和腐败率远远小于普通PE膜。
尽管已经详细描述了本发明的实施方式，但是应该理解的是，在不偏离本发明的精神和范围的情况下，可以对本发明的实施方式做出各种改变、替换和变更。

Claims (9)

1.一种PE保鲜涂布膜的制备方法，包括以下步骤：
1) 棒状纳米生物质颗粒的制备：
将桑树皮粉碎成粒径为100mm以下的颗粒物，然后将颗粒物置于10%Wt的氢氧化钠水溶液中于70℃下机械搅拌6h，然后过滤洗涤至中性并烘干；将烘干后的颗粒物采取10%wt的磷酸水溶液于80℃下搅拌3h，然后过滤水洗至中性并烘干得一次酸化颗粒物；将一次酸化颗粒物置于5%wt的盐酸水溶液中于90℃下搅拌2h，然后以2000rpm的转速下离心，离心物采用水洗至中性后真空干燥并粉碎得二次酸化后的颗粒物；将二次酸化后的颗粒物置于30%wt的硫酸水溶液中于70℃搅拌1h，然后在12000rpm的转速下离心，取清液室温透析14天，然后进行冻干得棒状纳米生物质颗粒；
2) 改性聚乙烯醇涂布液的制备：
将10g聚乙烯醇加入到200ml 10%V乙醇的水溶液中，然后加入0.3-0.5g棒状纳米生物质颗粒、升温至86℃以上搅拌分散0.5h得分散液，然后向分散液中加入羧甲基壳聚糖的醋酸水溶液和增塑剂超声分散2h得改性聚乙烯醇涂布液；
3) 将改性聚乙烯醇涂布液采用钢丝刮刀涂布法在PE基材表面进行涂布，然后干燥得PE保鲜涂布膜。
2.根据权利要求1所述的制备方法，其特征在于：步骤2）所述聚乙烯醇的分子量为12-15万，醇解度为85%以上，20℃下4%wt聚乙烯醇水溶液的粘度为3.6-4.0MPa.S。
3.根据权利要求1所述的制备方法，其特征在于：步骤2）所述羧甲基壳聚糖的醋酸水溶液由以下制备方法制备：将羧甲基壳聚糖分散在1%V的醋酸水溶液中，制备成4%wt的羧甲基壳聚糖水溶液，然后加入吐温80于50℃下搅拌2h得羧甲基壳聚糖的醋酸水溶液；步骤2）所述羧甲基壳聚糖的醋酸水溶液的加入量为3-4ml。
4.根据权利要求1所述的制备方法，其特征在于：步骤2）所述增塑剂为邻苯二甲酸酯或甘油，所述增塑剂的用量为0.2-0.4g。
5.根据权利要求4所述的制备方法，其特征在于：步骤2）所述增塑剂为甘油，所述增塑剂的用量为0.3g。
6.根据权利要求1所述的制备方法，其特征在于：所述PE基材厚度为60μm；改性聚乙烯醇涂布液在PE基材上涂布的量为1.4-1.6g/m2，涂布厚度为4-8μm。
7.根据权利要求6所述的制备方法，其特征在于：改性聚乙烯醇涂布液在PE基材上涂布的量为1.5g/m2，涂布厚度为6μm。
8.一种PE保鲜涂布膜的用途，所述PE保鲜涂布膜由权利要求1所述制备方法制备，其特征在于：用于樱桃、西红柿、猕猴桃的保鲜。
9.根据权利要求8所述的用途，其特征在于：用于樱桃的保鲜。
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