CN111716846A - 一种包含磺化聚芳香醚类聚合物的阻气透湿薄膜及其制备方法和应用 - Google Patents
一种包含磺化聚芳香醚类聚合物的阻气透湿薄膜及其制备方法和应用 Download PDFInfo
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- CN111716846A CN111716846A CN201910200974.7A CN201910200974A CN111716846A CN 111716846 A CN111716846 A CN 111716846A CN 201910200974 A CN201910200974 A CN 201910200974A CN 111716846 A CN111716846 A CN 111716846A
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- moisture
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- permeable film
- ether polymer
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 64
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- 238000000034 method Methods 0.000 claims description 16
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Abstract
本发明公开了一种包含磺化聚芳香醚类聚合物的阻气透湿薄膜。所述薄膜包括支撑层和功能层，其中，所述支撑层为单层结构，所述功能层存在于支撑层的一侧，或者同时存在于支撑层的两侧；所述支撑层为多孔薄膜，支撑层的材料为聚乙烯、聚丙烯或它们的组合物；所述功能层为致密薄膜，所述功能层包含磺化聚芳香醚类聚合物和无机吸湿剂。本发明还公开了该透湿薄膜的制备方法。该透湿薄膜用于具有保鲜功能的果蔬盒及具有保鲜果蔬盒的冰箱。该膜具有阻气透湿能力，在相对湿度较高时优异的透湿性可以防止水果蔬菜结露溃烂。另一方面，该膜阻气性好，防止果蔬在氧气下快速腐烂。
Description
技术领域
本发明涉及薄膜领域，具体地说，是涉及一种包含磺化聚芳香醚类聚合物的阻气透湿薄膜及其制备方法和应用，该复合薄膜运用在冰箱冷藏室的保鲜收纳盒上可以有效的延长蔬菜水果保鲜时间。
背景技术
水果和蔬菜是人类重要的食品，它是人们取得基本营养物(维生素、扩物质、复合碳水化合物等)的主要来源。随着人们生活水平的日益提高，对新鲜水果和蔬菜的保鲜度要求越来越高。果蔬在收获之后仍能继续进行呼吸和蒸腾等生命活动，在存储过程中会发生水分散失和营养物质的消耗。温度每升高10℃，果蔬呼吸强度就增加一倍。家庭果蔬保鲜方法是将果蔬放置在冰箱中冷藏，减缓果蔬呼吸。在果蔬中，水分是重要成分，影响着水果和蔬菜嫩度、鲜度和味道。周围湿度过低会导致果蔬水分丧失和失重，但湿度过高会使得果蔬表面水分凝结，使真菌生长，加速水果和蔬菜腐烂和变质。因此控制新鲜果蔬储存湿度是非常重要的，将有利于延长果蔬的保鲜时间。使用阻隔性薄膜，可防止由于氧气等气体的渗透，抑制新鲜果蔬呼吸作用，有利于延长果蔬的保鲜时间。
市场上用于减少水分散失的果蔬盒上的几种功能性薄膜“感温透湿膜”、“硅滤膜”、“感湿透湿膜”的效果并不令人满意。感温透湿膜在高湿低温下膜表面容易结露；硅滤膜具有保湿功能，但透湿性无法随湿度而改变；感湿透湿膜是在纸基基材上施涂黏胶溶液，性能符合要求但是制备过程不环保，工艺复杂，且在加工工艺中有可能存在氯含量超标的问题。
CN105986511A专利公开了在干湿强度较高的原纸上施涂亲水保水及成膜性好的天然高分子聚合物的技术，但成本比较高。CN104029449B专利公开了一种大透湿量涂层膜，基础层为膨体聚四氟乙烯膜层，涂层为含有汉麻杆芯超细微粉的聚氨基甲酸酯乳液共聚涂层，该膜用于汽车车灯壳体，但不具有智能控湿性能。CN103507339A专利公开了一种感湿透湿膜，该膜是再生纤维素保持在无纺布的基材中，但不具备阻隔气体性能。CN103107301A公开了一种无机涂层锂离子电池隔膜，包含多层结构，分别为多孔柔性底膜和涂覆于底膜两侧的涂层，涂层包含聚乙烯醇和沸石粒子，该专利涂层的辅助成分并没有金属盐成分，且复合膜不具备智能控湿的功能。CN1864829A公开了一种亲水-憎水双极复合膜及其制备方法，该膜具有双层结构，底层为多孔支撑层，上层为含氯化锂的亲水膜，该膜具有高透湿和对其它气体分子强阻挡作用，但是并不具备智能控湿性。WO2013066012A1专利公开了一种含有无机粒子的多孔膜和包含亲水和疏水物质聚合物粘结层，该膜是用于提高锂电池隔膜的热稳定性，并不具备智能控湿性能。WO2012133805A1公开了一种透湿膜，其多孔基材优选聚四氟乙烯，价格贵，且该膜的高透湿性能不佳。US20030054155A1公开了一种防水透湿复合膜，疏水层为聚四氟乙烯，亲水层为聚氨酯，该膜具有高透湿性，但并不具备智能控湿性能。
发明内容
为了克服现有技术存在的上述缺陷，本发明提供一种阻气透湿复合薄膜，在低湿度的情况下保湿，在高湿度的情况下具有强排湿能力，并且具有阻气性能的薄膜。本发明进一步提供所述该复合膜的制备方法，该方法工艺简单、成本低。因此，本发明提供的透湿薄膜特别适合应用于蔬菜水果的保鲜包装。
本发明的目的之一为提供一种包含磺化聚芳香醚类聚合物的阻气透湿薄膜，所述薄膜为多层结构，包括支撑层和功能层；其中，所述支撑层为单层结构，所述功能层存在于支撑层的一侧，或者同时存在于支撑层的两侧；
所述支撑层为多孔薄膜，支撑层的材料为聚乙烯、聚丙烯或它们的组合物。
所述功能层为致密薄膜，所述功能层包含磺化聚芳香醚类聚合物和无机吸湿剂。以磺化聚芳香醚类聚合物和无机吸湿剂的总重量为基准，所述磺化聚芳香醚类聚合物的含量为50～99wt％，优选为66～98wt％，所述无机吸湿剂的含量为1～50wt％，优选为2～34wt％。所述功能层含有抗菌剂，以所述功能层的总重量为基准，所述抗菌剂的含量为0～20wt％，优选为0.1～10wt％。
优选地，所述磺化聚芳香醚类聚合物为现有技术中具有下式结构至少之一的聚合物：
其中，R为O＝S＝O或C＝O，m和n均为1～100的整数。
所述磺化聚芳香醚类聚合物的分子量为10000～100000，优选为50000～90000。
所述磺化聚芳香醚类聚合物的离子交换容量为0.5～2.5mmol/g，优选为1.0～2.0mmol/g。
所述无机吸湿剂可选自现有技术中已有的无机吸湿剂，优选为金属盐吸湿剂或纳米粒子吸湿剂，其中金属盐吸湿剂优选为硫酸钠、氯化钙、氯化锂、氟化铯、溴化锂、氟化锂中的一种或多种，优选为硫酸钠、氯化钙、氯化锂、氟化锂中的一种或多种；纳米粒子吸湿剂优选为凹凸棒土、硅藻土、石墨烯、氧化石墨烯、碳纳米管、分子筛中的一种或多种混合，优选为凹凸棒土、氧化石墨烯中的一种或多种。
优选地，所述支撑层多孔薄膜的孔径为0.02～10微米，更优选为0.05～5微米。
优选地，所述支撑层的厚度为5～1000微米，更优选为10～100微米。
优选地，所述功能层的厚度为0.05～100微米，更优选为0.1～20微米。
其中，支撑层的材料中，所述的聚乙烯包括高密度聚乙烯、线性低密度聚乙烯、低密度聚乙烯中的一种或多种构成的组合物；所述的聚丙烯包括均聚聚丙烯、无规共聚聚丙烯、嵌段共聚聚丙烯、抗冲共聚聚丙烯中的一种或多种构成的组合物。所述的聚丙烯、聚乙烯的组合物为聚丙烯聚乙烯熔融共混后得到的组合物。
所述的支撑层多孔薄膜可市售而得，也可以采用现有技术中的常用制膜方法制得。比如，采用现有技术中的薄膜拉伸机将聚乙烯、聚丙烯或它们的组合物采用通常的薄膜拉伸工艺进行拉伸而制得所述支撑层的薄膜。薄膜拉伸机可以是单向或双向拉伸机。
其中，所述功能层还可含有抗菌剂。以所述功能层的总重量为基准，所述抗菌剂的含量为0～20wt％，优选为0.1～10wt％。所述抗菌剂可采用现有技术中已有的能用于塑料领域的抗菌剂，优选为纳米氧化锌、纳米银、纳米铜、丝胶、季铵盐、羟苯甲酯、西吡氯铵中的一种或多种，更优选为纳米氧化锌、纳米银、季铵盐中的一种或者多种。
本发明目的之二为提供一种所述的包含磺化聚芳香醚类聚合物的阻气透湿薄膜的制备方法，包括以下步骤：
(1)将包括磺化聚芳香醚类聚合物和无机吸湿剂在内的功能层各组分充分溶解或者分散到溶剂中，配制成溶液或者分散液；
(2)将步骤(1)得到的溶液或者分散液附着于所述支撑层的一面或两面；
(3)将步骤(2)得到的薄膜烘干，得到所述阻气透湿薄膜。
其中，步骤(1)中，所述溶剂为甲酸、乙二醇单甲醚、N，N-二甲基甲酰胺、N，N-二甲基乙酰胺、N-甲基吡咯烷酮、二甲基亚砜、乙二醇、乙酸、乙二醇二甲醚中的一种或几种，优选为甲酸、N，N-二甲基甲酰胺。
步骤(1)中，溶液或分散液中磺化聚芳香醚类聚合物的质量浓度为0.5％～30％，优选为1％～20％；溶液或分散液中无机吸湿剂的质量浓度为0.05％～5％，优选为0.1％～2.5％；溶液或分散液中抗菌剂的质量浓度为0.05％～5％，优选为0.1％～2％。
步骤(2)中，附着方式可采用现有的各种液体附着方式，通常采用刷涂、淋涂或喷涂中的一种或多种组合。
步骤(3)中，实现烘干即可，烘干温度以不使得各层树脂熔融、降解为上限，烘干至薄膜干燥为止。优选烘干温度为50～100℃，更优选为60～90℃；烘干时间优选为1～20min，更优选为3～10min。所采用的烘干设备采用现有技术中通常的烘干设备。
本发明的目的之三为提供所述的包含磺化聚芳香醚类聚合物的阻气透湿薄膜在蔬菜水果保鲜包装上的应用。
磺化聚芳香醚类主链含有磺酸盐，其吸湿性较强，为膜具有良好的透湿性打下基础，同时分子结构排列较为紧密，具有优异的阻气性。本发明的阻气透湿薄膜采用磺化聚芳香醚类聚合物和无机吸湿剂，不仅具有良好的氧气阻隔性，并且在低湿度的情况下保湿，在高湿度的情况下具有强排湿能力。
该透湿薄膜用于具有保鲜功能的果蔬盒及具有保鲜果蔬盒的冰箱。该膜具有阻气透湿能力，在相对湿度较高时优异的透湿性可以防止水果蔬菜结露溃烂。另一方面，该膜阻气性好，防止果蔬在氧气下快速腐烂。
具体实施方式
在以下实施例和对比例中：
(1)透湿性测试：将智能控湿薄膜固定在装有一定质量硅胶干燥剂的透湿杯封口处后，将透湿杯放入恒温恒湿箱中，在50％或者90％湿度下放置24h后取出，称量干燥剂的质量，其增重就为该膜面积下的透湿量。
(2)阻氧性：利用阻氧性测试仪测得(济南蓝光机电科技有限公司，型号OX2/231)。
(3)磺化聚芳香醚类聚合物的离子交换容量采用酸碱滴定方法进行测定。
另外，在以下实施例和对比例中：
磺化聚芳香醚均购自天津砚津科技有限公司，凹凸棒土、氧化石墨烯均购自百灵威科技有限公司，乙二醇单甲醚、甲酸、N，N-二甲基甲酰胺、硫酸钠、氯化锂以及氟化锂均购自国药集团化学试剂有限公司。
实施例1：
将2kg聚丙烯(F1002B，中石化扬子石化)在薄膜单向拉伸机(广州普同，MESI-LL)上拉伸成多孔薄膜(多孔薄膜的平均孔径为2微米)。将5g具有式(Ⅰ)结构的磺化聚醚砜(数均分子量为65000，离子交换容量为1.86)加入95g甲酸中，充分溶解。将2.1g氯化锂、0.2g纳米氧化锌加至所得溶液中，充分搅拌至混合均匀。将此溶液均匀地刷涂在聚丙烯多孔薄膜的一个表面上，然后将其置于烘箱中，在70℃下烘干10min，得到阻气透湿薄膜(A1)。其中，聚丙烯支撑层的厚度为25微米，功能层的厚度为10微米。
实施例2：
将2kg聚丙烯(F1002B，中石化扬子石化)在薄膜单向拉伸机(广州普同，MESI-LL)上拉伸成多孔薄膜(多孔薄膜的平均孔径为2微米)。将7g具有式(II)结构的磺化聚醚砜(数均分子量为58000，离子交换容量为2.10)加入93g乙二醇单甲醚中，充分溶解。将1.4g氟化锂、0.2g纳米氧化锌(百灵威，99.5％，粒径10-30nm)加至所得溶液中，充分搅拌至混合均匀。将此溶液均匀地刷涂在聚丙烯多孔薄膜的一个表面上，然后将其置于烘箱中，在70℃下烘干10min得到阻气透湿薄膜(A2)。其中，聚丙烯支撑层的厚度为25微米，功能层的厚度为12微米。
实施例3：
将2kg聚丙烯(F1002B，中石化扬子石化)在薄膜单向拉伸机(广州普同，MESI-LL)上拉伸成多孔薄膜(多孔薄膜的平均孔径为2微米)。将9g具有式(Ⅲ)结构的磺化聚醚砜(数均分子量为80000，离子交换容量为1.67)加入91g的N，N-二甲基甲酰胺中，充分溶解。将2.7g凹凸棒土(百灵威，直径为10纳米，长度为1微米)、0.2g纳米氧化锌(百灵威，99.5％，粒径10-30nm)加至所得溶液中，充分搅拌至混合均匀。将此溶液均匀地刷涂在聚丙烯多孔薄膜的一个表面上，然后将其置于烘箱中，在70℃下烘干10min得到阻气透湿薄膜(A3)。其中，聚丙烯支撑层的厚度为25微米，功能层的厚度为13微米。
实施例4：
将2kg聚丙烯(F1002B，中石化扬子石化)在薄膜单向拉伸机(广州普同，MESI-LL)上拉伸成多孔薄膜(多孔薄膜的平均孔径为2微米)。将2.5g具有式(Ⅰ)结构的磺化聚醚砜(数均分子量为65000，离子交换容量为1.86)加入95g甲酸中，充分溶解。将2.2g氯化锂、0.3g纳米氧化锌加至所得溶液中，充分搅拌至混合均匀。将此溶液均匀地刷涂在聚丙烯多孔薄膜上，然后将其置于烘箱中，在70℃下烘干10min，得到阻气透湿薄膜(A4)。其中，聚丙烯支撑层的厚度为25微米，功能层的厚度为8微米。
实施例5：
和实施例1步骤相同，不同的是，用具有式(Ⅳ)结构的磺化聚醚砜(数均分子量为58000，离子交换容量为1.59)取代具有式(Ⅰ)结构的磺化聚醚砜。其中，聚丙烯支撑层的厚度为25微米，功能层的厚度为9微米。
实施例6：
和实施例1步骤相同，不同的是，用氧化石墨烯(百灵威，直径:0.5-3μm，厚度:0.55-3.74nm，层数:≤10)取代氯化锂。其中，聚丙烯支撑层的厚度为25微米，功能层的厚度为11微米。
实施例7：
和实施例1步骤相同，不同的是，用硫酸钠取代氯化锂。其中，聚丙烯支撑层的厚度为25微米，功能层的厚度为10微米。
对比例1：
和实施例1同样的操作，不同的是涂覆溶液中不含有吸湿剂。
测试例：
对上述复合膜进行水蒸气透过率测试，数据结果见表1。在测试温度为25℃，透过面湿度为分别为50％和90％的测试条件下，得到每天每平方米薄膜的水蒸气透过量(g/m2/day)。
对上述复合膜进行气体阻隔性能检测，得到氧气透过率[cm3·cm/(cm2·s·Pa)]，数据结果见表1。
表1：复合膜的透湿性和气体阻隔性能测试结果
由表1可见，上述智能控湿薄膜具有良好的氧气阻隔性，且具有智能控湿能力，即在湿度较低时，该智能控湿薄膜的透湿度降低，具有保湿的能力，可保持果蔬湿度；反之，在湿度较高时，该智能控湿薄膜的透湿度提高，具有强排湿能力，从而可防止水果蔬菜结露溃烂，具有很好的应用前景。
Claims (13)
1.一种包含磺化聚芳香醚类聚合物的阻气透湿薄膜，其特征在于所述薄膜包括支撑层和功能层，其中，所述支撑层为单层结构，所述功能层存在于支撑层的一侧，或者同时存在于支撑层的两侧；
所述支撑层为多孔薄膜，支撑层的材料为聚乙烯、聚丙烯或它们的组合物；
所述功能层为致密薄膜，所述功能层包含磺化聚芳香醚类聚合物和无机吸湿剂，以磺化聚芳香醚类聚合物和无机吸湿剂的总重量为基准，所述磺化聚芳香醚类聚合物的含量为50～99wt％，所述无机吸湿剂的含量为1～50wt％；所述功能层含有抗菌剂，以所述功能层的总重量为基准，所述抗菌剂的含量为0～20wt％。
2.根据权利要求1所述的阻气透湿薄膜，其特征在于：
以磺化聚芳香醚类聚合物和无机吸湿剂的总重量为基准，所述磺化聚芳香醚类聚合物的含量为66～98wt％，所述无机吸湿剂的含量为2～34wt％。
3.根据权利要求1所述的阻气透湿薄膜，其特征在于：
所述磺化聚芳香醚类聚合物具有如下式结构中的至少一种结构：
其中，R为O＝S＝O或C＝O，m和n均为1～100的整数。
4.根据权利要求1所述的阻气透湿薄膜，其特征在于：
所述无机吸湿剂为金属盐吸湿剂或纳米粒子吸湿剂，其中金属盐吸湿剂优选为硫酸钠、氯化钙、氯化锂、氟化铯、溴化锂、氟化锂中的一种或多种，纳米粒子吸湿剂优选为凹凸棒土、硅藻土、石墨烯、氧化石墨烯、碳纳米管、分子筛中的一种或多种。
5.根据权利要求1所述的阻气透湿薄膜，其特征在于：
所述磺化聚芳香醚类聚合物的分子量为10000～100000，优选为50000～90000；磺化聚芳香醚类聚合物的离子交换容量为0.5～2.5mmol/g，优选为1.0～2.0mmol/g。
6.根据权利要求1所述的阻气透湿薄膜，其特征在于：
所述支撑层多孔薄膜的孔径为0.02～10微米，优选为0.05～5微米。
7.根据权利要求1所述的阻气透湿薄膜，其特征在于：
所述支撑层的厚度为5～1000微米，优选为10～100微米；所述功能层的厚度为0.05～100微米，优选为0.1～20微米。
8.根据权利要求1所述的阻气透湿薄膜，其特征在于：
以所述功能层的总重量为基准，所述抗菌剂的含量为0.1～10wt％。
9.根据权利要求1所述的阻气透湿薄膜，其特征在于：
所述抗菌剂为纳米氧化锌、纳米银、纳米铜、丝胶、季铵盐、羟苯甲酯、西吡氯铵中的一种或多种。
10.一种根据权利要求1～9之任一项所述的包含磺化聚芳香醚类聚合物的阻气透湿薄膜的制备方法，其特征在于包括以下步骤：
(1)将功能层各组分充分溶解或者分散到溶剂中，配制成溶液或者分散液；
(2)将步骤(1)得到的溶液或者分散液附着于所述支撑层的一面或两面；
(3)将步骤(2)得到的薄膜烘干，得到所述阻气透湿薄膜。
11.根据权利要求10所述的阻气透湿薄膜的制备方法，其特征在于：
步骤(1)中，所述溶剂为甲酸、乙二醇单甲醚、N，N-二甲基甲酰胺、N，N-二甲基乙酰胺、N-甲基吡咯烷酮、二甲基亚砜、乙二醇、乙酸、乙二醇二甲醚中的一种或几种；
步骤(1)中，溶液或分散液中磺化聚芳香醚类聚合物的质量浓度为0.5％～30％，优选为1％～20％；溶液或分散液中无机吸湿剂的质量浓度为0.05％～5％，优选为0.1％～2.5％；溶液或分散液中抗菌剂的质量浓度为0.05％～5％，优选为0.1％～2％。
12.根据权利要求10所述的阻气透湿薄膜的制备方法，其特征在于：
步骤(3)中，烘干温度为50～100℃，烘干时间为1～20min。
13.根据权利要求1～9之任一项所述的包含磺化聚芳香醚类聚合物的阻气透湿薄膜在蔬菜水果保鲜包装上的应用。
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