CN114426699A - 一种三明治型阻气透湿复合膜及其制备方法和应用 - Google Patents
一种三明治型阻气透湿复合膜及其制备方法和应用 Download PDFInfo
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- CN114426699A CN114426699A CN202011014823.1A CN202011014823A CN114426699A CN 114426699 A CN114426699 A CN 114426699A CN 202011014823 A CN202011014823 A CN 202011014823A CN 114426699 A CN114426699 A CN 114426699A
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Abstract
本发明一种三明治型阻气透湿复合膜及其制备方法和应用。该三明治型阻气透湿复合薄膜包括排湿层、阻气层和吸湿层,所述阻气层位于排湿层与吸湿层之间;所述排湿层为多孔薄膜,所述吸湿层具有贯通的双连续网络孔结构,所述网络孔结构由三维无规网络骨架构成,骨架上分布着纳米级的凸起,所述吸湿层包括至少两种聚合物。所述复合薄膜中具有高孔隙率微孔结构的吸湿层有助于提高膜的吸湿性,而疏水的多孔排湿层又有助于提高膜的排湿性,交联的阻气层对氧气具有很好的阻隔性,将三者复合在一起即可制得具有三明治结构的高透湿性、高阻氧性的用于果蔬保鲜的薄膜。
Description
技术领域
本发明涉及功能薄膜领域,具体地说,是涉及一种三明治型阻气透湿复合膜及其制备方法和应用。
背景技术
水果和蔬菜是人类重要的食品,是人们取得基本营养物(维生素、矿物质、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。使用高透湿性保鲜隔膜,有利于延长果蔬的保鲜时间。
CN105986511A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。
CN104029449A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。
CN103507339A公开了一种感湿透湿膜,该膜将再生纤维素保持在无纺布的基材中。
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,该涂层的辅助成分并没有金属盐成分。
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。
WO2013066012A1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,该膜用于提高锂电池隔膜的热稳定性。
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。
以上发明专利均是利用在基材上构建亲水吸湿层来提高复合膜的透湿性。本发明提出了一种三明治结构的阻气透湿膜:以疏水的多孔膜作为排湿层,致密的高分子交联薄膜作为阻气层,具有高孔隙率和微孔道结构的薄膜作为吸湿层。
发明内容
本发明的目的是为了克服现有技术存在的上述缺陷,提供一种高透湿、高阻气的三明治型复合膜。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,本发明提供的复合膜具有高透湿性、高阻氧性,特别适合应用于蔬菜水果的保鲜包装。
本发明目的之一为提供一种三明治型阻气透湿复合膜,包括三层结构:排湿层、阻气层和吸湿层,所述阻气层位于排湿层与吸湿层之间;其中,
所述排湿层为多孔薄膜;
所述阻气层与排湿层的表面贴合;
所述吸湿层为多孔结构,与阻气层的表面贴合;所述吸湿层具有贯通的双连续网络孔结构,所述网络孔结构由三维无规网络骨架构成,骨架上分布着纳米级的凸起,所述吸湿层的材料包括至少两种聚合物。
以上所述三明治型阻气透湿复合膜中,所述排湿层的多孔薄膜可以为单层或两层复合结构,优选单层结构。所述排湿层多孔薄膜的材料为聚乙烯、聚丙烯、聚苯乙烯、聚对苯二甲酸二醇酯、聚己内酰胺中的至少一种。
根据本发明,所述聚乙烯优选为高密度聚乙烯(HDPE)、线性低密度聚乙烯(LLDPE)和低密度聚乙烯(LDPE)中的至少一种;所述聚丙烯优选为均聚聚丙烯、无规共聚聚丙烯、嵌段共聚聚丙烯和抗冲共聚聚丙烯中的至少一种。
本发明中,所述排湿层多孔薄膜的孔径优选为0.02~10微米,进一步优选为0.05~5微米,更优选为0.1~2微米;孔隙率为30%~80%,优选为40%~70%;孔径在平均孔径正负一个数量级范围内的孔占全部孔的50%以上,优选占全部孔的80%以上。
以上所述三明治型阻气透湿复合膜中,所述阻气层的材料为聚乙烯醇、壳聚糖、海藻酸钠、羟丙基甲基纤维素、羟乙基甲基纤维素中的至少一种,优选为聚乙烯醇、壳聚糖、海藻酸钠中的至少一种。
以上所述三明治型阻气透湿复合膜中,所述吸湿层的孔隙率优选为50~90%,更优选为60~80%;
优选地,所述吸湿层的平均孔径为0.1~5μm,骨架上分布的凸起尺寸为20~400nm。
所述吸湿层由包括至少两种聚合物的聚合物混合物得到,其中聚合物至少包括聚合物1和聚合物2。优选地,所述吸湿层通过将所述聚合物的混合物进行雾化预处理结合非溶剂致相分离法而得到。
所述吸湿层的材料包括聚合物1和聚合物2,其中,所述聚合物1选自聚氯乙烯、聚砜、聚醚砜、磺化聚醚砜、聚醚醚酮、聚醚酮、聚丙烯腈、聚芳香醚、醋酸纤维素、聚偏氟乙烯、聚酰亚胺、丙烯腈-苯乙烯共聚物、以及它们改性后的聚合物中的至少一种,优选为聚丙烯腈、聚醚砜和聚砜中的至少一种;所述聚合物2选自聚乙烯吡咯烷酮、聚乙二醇、聚氧乙烯聚氧丙烯醚嵌段共聚物中的至少一种,优选为聚乙二醇和聚乙烯吡咯烷酮中的至少一种。
所述吸湿层中聚合物1和聚合物2的重量比为1:(0.05~5),优选为1:(0.3~2)。
根据本发明,所述排湿层、阻气层和吸湿层的厚度可根据需要确定,进一步地,所述排湿层的厚度为5~1000微米,优选为20~100微米;所述阻气层的厚度为0.1~50微米,优选为0.5~10微米;所述吸湿层的厚度为5~30微米,优选为10~20微米。
本发明目的之二为提供一种三明治型阻气透湿复合膜的制备方法,包括以下步骤:
(1)将阻气层材料溶于水中,加入交联剂,调节溶液pH为1~2,制得涂覆液A;
(2)将所得涂覆液A涂覆在排湿层的表面,烘干得到含阻气层的双层复合膜;
(3)将至少两种聚合物溶解于溶剂中配制聚合物溶液,制得涂覆液B,其中聚合物包括聚合物1和聚合物2;
(4)将步骤(3)得到的涂覆液B附着于所述双层复合膜的阻气层表面,进行雾化预处理,其中雾化预处理为在雾化的液滴浴中停留一段时间;然后浸入凝固浴,得到所述透湿复合膜。
根据本发明三明治型阻气透湿复合膜的制备方法,步骤(1)中所述阻气层的高分子材料为聚乙烯醇、壳聚糖、海藻酸钠、羟丙基甲基纤维素以及羟乙基甲基纤维素中的一种或几种混合;
所述交联剂为甲醛、乙二醛、丙二醛、丁二醛、戊二醛中的一种或几种混合,优选为甲醛、戊二醛中的至少一种。
根据本发明三明治型阻气透湿复合膜的制备方法,对步骤(1)中所述涂覆液中高分子材料以及交联剂的含量没有特殊限定,进一步地,所述涂覆液A中,阻气层材料的浓度为0.5~10wt%,优选为1~5wt%;交联剂的浓度为0.05~1wt%,优选为0.1~0.5wt%。
根据本发明三明治型阻气透湿复合膜的制备方法,所述排湿层多孔薄膜为单层时可市售而得,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、聚苯乙烯、聚对苯二甲酸二醇酯和聚己内酰胺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。
当所述排湿层为两层时,两层的材质可以不同,如聚乙烯与聚丙烯复合而成的多孔薄膜。所述排湿层可市售而得,也可以采用现有技术中的复合薄膜的常用制膜方法制得。
可以采用任何常规的涂布方法将步骤(1)得到的涂覆液A涂布于所述排湿层表面,包括但不限于:刷涂、淋涂、喷涂。
根据本发明三明治型阻气透湿复合膜的制备方法,步骤(2)中烘干的温度为50℃~100℃,优选为60℃~90℃;烘干时间为1~60min,优选为3~30min。
根据本发明三明治型阻气透湿复合膜的制备方法,步骤(3)中,使用的聚合物1材料可以包括但不限于:聚氯乙烯、聚砜、聚醚砜、磺化聚醚砜、聚醚醚酮、聚醚酮、聚丙烯腈、聚芳香醚、醋酸纤维素、聚偏氟乙烯、聚酰亚胺、丙烯腈-苯乙烯共聚物、以及它们改性后的聚合物中的至少一种;
所述聚合物2为可以与聚合物1在聚合物1的良溶剂中互溶且具有亲水性的高分子材料,可以包括但不限于:聚乙烯吡咯烷酮、聚乙二醇、聚氧乙烯聚氧丙烯醚嵌段共聚物等中的至少一种。
其中聚合物1和聚合物2的重量比为1:(0.05~5),优选为1:(0.3~2)。
所述涂覆液B中,聚合物1的浓度为5~20wt%,优选为10~15wt%;聚合物2的浓度为1~20wt%,优选为10~15wt%。
根据本发明三明治型阻气透湿复合膜的制备方法,步骤(3)中所述的溶剂为聚合物1和聚合物2的良溶剂,其包括但不限于N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、丙酮、N-甲基-2-吡咯烷酮、二甲基亚砜、四甲基亚砜、四氢呋喃、二氧六环、乙腈、氯仿、四甲基亚砜等中的至少一种,优选为N,N-二甲基甲酰胺。
根据本发明,所述涂覆液B中还可加入氯化锂、溴化锂、碘化锂以及氯化钙等无机盐类助剂,其用量为本领域的常规用量。
本发明三明治型阻气透湿复合膜的制备方法中所述吸湿层成膜通过诱导相分离成膜,所述的诱导相分离分为两步,即雾化预处理工艺结合非溶剂致相分离,首先在雾化液滴浴中停留进行部分诱导相分离,接着进入非溶剂凝固浴进行完全相分离。
本发明的雾化预处理方法与通常意义上的蒸汽诱导相分离(VIPS)有很大的区别,后者是指在一定的高湿度(或者饱和湿度)条件下发生相分离,不会涉及雾化的液滴浴。
根据本发明三明治型阻气透湿复合膜的制备方法,可以采用任何常规的涂布方法将步骤(3)得到的涂覆液B涂布于阻气层表面,包括但不限于:刷涂、淋涂、喷涂。
以上涂覆中,可采用刮刀制膜,也可采用四面制备器或涂布丝棒刮膜。
步骤(4)中,所述雾化预处理,即是将聚合物溶液涂覆后,将其在雾化的液滴浴中停留接触一定时间。其中获得雾化的液滴浴的方法没有特别限定,可采用常规的各种液体雾化的方法,例如压力雾化、转盘雾化、高压气流雾化、声波雾化等方法。
根据本发明,步骤(4)中雾化时间为1~60s,优选为10~30s;
复合膜表面与雾化喷头之间的距离为1~20cm,优选为5~10cm。
所述液滴浴中液滴的尺寸为1~50μm,优选为5~18μm;
雾化预处理中液滴为聚合物1的不良溶剂,可以为水、乙醇、乙二醇等单一组份的,也可以是水与极性非质子溶剂或其它溶剂组成的,还也可是盐、酸、碱的溶液。
所述凝固浴为聚合物1的不良溶剂,可以为水、乙醇、乙二醇等单一组份的,也可以是水与极性非质子溶剂或其它溶剂组成的,如氢氧化钠水溶液。
本发明中,因为两种聚合物1和聚合物2的溶解性和浸润性差异,在非溶剂致相分离的过程中相分离速度存在差异,即形成骨架和纳米凸起结构。
根据本发明一个优选的实施方式,所述制备方法可包括以下步骤:
(1)将一定量的用于制备阻气层的高分子材料溶于水中,加入交联剂,充分搅拌至完全溶解后,调节溶液pH为1~2,真空脱泡,制得涂覆液A;
(2)将排湿层多孔薄膜固定在玻璃板上,采用喷涂或刷涂的方式,在其表面均匀地涂上一层步骤(1)所述的涂覆液A,加热烘干,得到双层复合膜;
(3)将一定量的用于制备吸湿层的聚合物材料溶于有机溶剂中,充分搅拌至完全溶解后,真空脱泡,制得涂覆液B;
(4)利用四面制备器,将步骤(3)得到的涂覆液B均匀刮制在步骤(2)得到的双层复合膜的阻气层表面,然后用空气加湿器进行雾化处理,最后,将得到的复合膜浸入到去离子水中,完成相转化,得到所述三明治型阻气透湿复合膜。
本发明的目的之三为提供所述三明治型阻气透湿复合膜和/或由所述制备方法制得的三明治型阻气透湿复合膜在蔬菜水果保鲜包装中的应用。
经发明人的深入研究发现,具有高孔隙率微孔结构的吸湿层有助于提高膜的吸湿性,而疏水的多孔排湿层又有助于提高膜的排湿性,交联的高分子薄膜阻气层对氧气具有很好的阻隔性,将三者复合在一起即可制得具有三明治结构的高透湿性、高阻氧性的用于果蔬保鲜的薄膜。
本发明的其它特征和优点将在随后具体实施方式部分予以详细说明。
附图说明
图1为实施例1透湿复合薄膜的吸湿层的表面形貌图。
图2为实施例1透湿复合薄膜的吸湿层的断面形貌图。
图3为对比例1透湿复合薄膜的表面形貌图。
图4为对比例1透湿复合薄膜的断面形貌图。
具体实施方式
下面结合具体实施例对本发明进行具体的描述,有必要在此指出的是以下实施例只用于对本发明的进一步说明,不能理解为对本发明保护范围的限制,本领域技术人员根据本发明内容对本发明做出的一些非本质的改进和调整仍属本发明的保护范围。
本发明具体实施方式中所用原料为市售所得。
透湿薄膜的基层和附加层的厚度通过上海六菱测厚仪测定;孔结构包括孔径和孔隙率通过压汞法测量,采用仪器AutoporeIII-9420型压汞仪。
聚丙烯,F1002B,中石化扬子石化。
聚乙烯,L501(5000S),中石化扬子石化。
聚乙烯吡咯烷酮,百灵威,重均分子量为58000。
聚乙二醇,百灵威,重均分子量为20000。
聚砜,苏威,牌号为P3500。
聚醚砜,巴斯夫,牌号为E6020P。
聚丙烯腈,百灵威。
N,N-二甲基甲酰胺,国药集团化学试剂有限公司,分析纯。
聚乙烯醇(PVA)(醇解度为99%,日本可乐丽,牌号为124)。
壳聚糖(百灵威)。
羟丙基甲基纤维素(百灵威)。
羟乙基甲基纤维素(百灵威)。
海藻酸钠(百灵威)。
加湿器,荣事达牌,功率为25W,型号为RS-V40K。
薄膜单向拉伸机,广州普同,MESI-LL。
扫描电镜,日本日立公司,型号S-4800。
实施例1
将2kg聚丙烯在薄膜单向拉伸机上拉伸成聚丙烯多孔薄膜。
将1g聚乙烯醇加入98.9g蒸馏水中,充分溶解。将0.1g戊二醛加至所得溶液中,充分搅拌至混合均匀,并用硫酸调节溶液的pH为2,得到涂覆液。将此涂覆液均匀地刷涂在聚丙烯多孔薄膜一面,然后将其置于烘箱中,在70℃下烘干10min,得到双层复合膜。
将15g聚丙烯腈,15g聚乙烯吡咯烷酮溶于70gN,N-二甲基甲酰胺溶剂中,充分溶解后,真空脱泡,得到涂覆液;将聚丙烯多孔薄膜固定在玻璃板上,利用四面制备器(狭缝为100μm)将涂覆液均匀地刮制在上述得到的复合膜聚乙烯醇表面上;通过加湿器对膜表面上的涂覆液进行雾化处理10s,雾化喷头距离膜表面5cm;再将复合膜浸入去离子水中,以使相转化完全,最终得到阻气透湿复合膜A1。
其聚丙烯排湿层厚度为25微米,孔径为0.25微米,孔隙率为50%,孔径在平均孔径正负一个数量级范围内的孔占全部孔的85%以上;聚乙烯醇阻气层厚度为1.8微米;聚丙烯腈吸湿层的厚度为15微米,孔隙率为80%,平均孔径为2.2μm,骨架上分布的凸起尺寸为100~200nm。
图1给出了复合膜吸湿层的表面形貌,由图可以看出,膜表面有大量微米级的孔以及纳米级的突起结构,纳米级的突起结构增加了膜表面和湿气的接触面积,有助于提高膜表面的吸湿能力。
实施例2
将2kg聚丙烯在薄膜单向拉伸机上拉伸成聚丙烯多孔薄膜。
将2.5g壳聚糖加入97.25g蒸馏水中,充分溶解。将0.25g甲醛加至所得溶液中,充分搅拌至混合均匀,并用硫酸调节溶液的pH为2,得到涂覆液。将此涂覆液均匀地刷涂在聚丙烯多孔薄膜一面,然后将其置于烘箱中,在70℃下烘干10min,得到双层复合膜。
将10g聚醚砜,10g聚乙二醇溶于80gN,N-二甲基甲酰胺溶剂中,充分溶解后,真空脱泡,得到涂覆液;将聚丙烯多孔薄膜固定在玻璃板上,利用四面制备器(狭缝为100μm)将涂覆液均匀地刮制在上述得到的复合膜壳聚糖表面上;通过加湿器对膜表面上的涂覆液进行雾化处理10s,雾化喷头距离膜表面5cm;再将复合膜浸入去离子水中,以使相转化完全,最终得到阻气透湿复合膜A2。
其聚丙烯排湿层厚度为25微米,孔径为0.25微米,孔隙率为50%,孔径在平均孔径正负一个数量级范围内的孔占全部孔的85%以上;壳聚糖阻气层厚度为4.5微米;聚醚砜吸湿层的厚度为12微米,孔隙率为60%,平均孔径为0.5μm,骨架上分布的凸起尺寸为20~60nm。
实施例3
将2kg聚乙烯在薄膜单向拉伸机上拉伸成聚乙烯多孔薄膜。
将5g海藻酸钠加入94.5g蒸馏水中,充分溶解。将0.5g戊二醛加至所得溶液中,充分搅拌至混合均匀,并用硫酸调节溶液的pH为2,得到涂覆液。将此涂覆液均匀地刷涂在聚丙烯多孔薄膜一面,然后将其置于烘箱中,在70℃下烘干10min,得到双层复合膜。
将15g聚砜,15g聚乙烯吡咯烷酮溶于70gN,N-二甲基甲酰胺溶剂中,充分溶解后,真空脱泡,得到涂覆液;将聚乙烯多孔薄膜固定在玻璃板上,利用四面制备器(狭缝为100μm)将涂覆液均匀地刮制在上述得到的复合膜聚乙烯醇表面上;通过加湿器对膜表面上的涂覆液进行雾化处理10s,雾化喷头距离膜表面5cm;再将复合膜浸入去离子水中,以使相转化完全,最终得到阻气透湿复合膜A3。
其聚乙烯排湿层厚度为25微米,孔径为0.25微米,孔隙率为50%,孔径在平均孔径正负一个数量级范围内的孔占全部孔的85%以上;海藻酸钠阻气层厚度为7.6微米;聚砜吸湿层的厚度为18微米,孔隙率为72%,平均孔径为1.5μm,骨架上分布的凸起尺寸为50~80nm。
实施例4
根据与实施例1相同的方法制备薄膜,不同的是,将聚乙烯醇替换成羟乙基甲基纤维素,得到透湿合薄膜A4。
实施例5
根据与实施例1相同的方法制备薄膜,不同的是,将聚乙烯醇替换成羟丙基甲基纤维素,得到透湿复合薄膜A5。
实施例6
根据与实施例1相同的方法制备薄膜,不同的是,聚丙烯腈与聚乙烯吡咯烷酮的用量分别为15g和5g,得到透湿复合薄膜A6。
实施例7
根据与实施例1相同的方法制备薄膜,不同的是,聚丙烯腈与聚乙烯吡咯烷酮的用量分别为10g和20g,得到透湿复合薄膜A7。
实施例8
根据与实施例1相同的方法制备薄膜,不同的是,雾化过程中,雾化时间为30s,雾化喷头与膜表面之间的距离为10cm,得到透湿复合薄膜A8。
对比例1
将2kg聚丙烯在薄膜单向拉伸机上拉伸成聚丙烯多孔薄膜。
将1g聚乙烯醇加入98.9g蒸馏水中,充分溶解。将0.1g戊二醛加至所得溶液中,充分搅拌至混合均匀,并用硫酸调节溶液的pH为2,得到涂覆液。将此涂覆液均匀地刷涂在聚丙烯多孔薄膜一面,然后将其置于烘箱中,在70℃下烘干10min,得到复合膜D1。
图3为复合膜D1的扫描电镜表面形貌照片,由图可以看出,表面是一层致密、无缺陷的交联聚乙烯醇薄膜。
图4为复合膜D1的扫描电镜断面形貌照片,由图可以看出,最上层为交联的聚乙烯醇,厚度为5微米。
对比例2
将2kg聚丙烯在薄膜单向拉伸机上拉伸成聚丙烯多孔薄膜。
将15g聚丙烯腈,15g聚乙烯吡咯烷酮溶于70gN,N-二甲基甲酰胺溶剂中,充分溶解后,真空脱泡,得到涂覆液;将聚丙烯多孔薄膜固定在玻璃板上,利用四面制备器(狭缝为100μm)将涂覆液均匀地刮制在聚丙烯多孔薄膜上;通过加湿器对膜表面上的涂覆液进行雾化处理10s,雾化喷头距离膜表面5cm;再将复合膜浸入去离子水中,以使相转化完全,最终得到复合膜D2。
对比例3
将2kg聚丙烯在薄膜单向拉伸机上拉伸成聚丙烯多孔薄膜。
将1g聚乙烯醇加入98.9g蒸馏水中,充分溶解。将0.1g戊二醛加至所得溶液中,充分搅拌至混合均匀,并用硫酸调节溶液的pH为2,得到涂覆液。将此涂覆液均匀地刷涂在聚丙烯多孔薄膜一面,然后将其置于烘箱中,在70℃下烘干10min,得到双层复合膜。
将15g聚丙烯腈,15g聚乙烯吡咯烷酮溶于70gN,N-二甲基甲酰胺溶剂中,充分溶解后,真空脱泡,得到涂覆液;将聚丙烯多孔薄膜固定在玻璃板上,利用四面制备器(狭缝为100μm)将涂覆液均匀地刮制在上述得到的复合膜聚乙烯醇表面上;再将复合膜浸入去离子水中,使相转化完全,最终得到阻气透湿复合膜D3。
测试例
根据GB/T 1037-1988,对上述薄膜进行水蒸气透过率测试,在测试温度为25℃,透过面湿度为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),数据结果见表1。
根据GB/T 19789-2005对上述薄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:复合膜的透湿性和阻气性能测试结果
序号 | 透湿度(90%RH) | 阻气性(O<sub>2</sub>) |
A1 | 1480 | 4.5×10<sup>-6</sup> |
A2 | 1378 | 8.7×10<sup>-6</sup> |
A3 | 1320 | 9.0×10<sup>-6</sup> |
A4 | 1556 | 5.4×10<sup>-5</sup> |
A5 | 1542 | 6.7×10<sup>-5</sup> |
A6 | 1305 | 4.8×10<sup>-6</sup> |
A7 | 1593 | 6.2×10<sup>-5</sup> |
A8 | 1417 | 6.3×10<sup>-6</sup> |
D1 | 895 | 4.9×10<sup>-6</sup> |
D2 | 1567 | 不具有阻气性 |
D3 | 326 | 3.1×10<sup>-6</sup> |
由表1可见,通过雾化的方法,得到高孔隙率的多孔吸湿层,通过多孔微孔道的吸湿效应,提高了膜的透湿能力;同时,阻气层的交联结构对氧气起到了有效的阻隔作用,这样有助于果蔬长期处在90%RH以及低氧气含量的环境中,有利于果蔬长期保鲜。
以上已经描述了本发明的各实施例,上述说明是示例性的,并非穷尽性的,并且也不限于所披露的各实施例。在不偏离所说明的各实施例的范围和精神的情况下,对于本技术领域的普通技术人员来说许多修改和变更都是显而易见的。
Claims (14)
1.一种三明治型阻气透湿复合膜,所述复合膜包括三层结构:排湿层、阻气层和吸湿层,所述阻气层位于排湿层与吸湿层之间;所述排湿层为多孔薄膜,所述吸湿层具有贯通的双连续网络孔结构,所述网络孔结构由三维无规网络骨架构成,骨架上分布着纳米级的凸起,所述吸湿层的材料包括至少两种聚合物。
2.根据权利要求1所述的三明治型阻气透湿复合膜,其特征在于:
所述吸湿层的孔隙率为50~90%,优选为60~80%;
所述吸湿层的平均孔径为0.1~5μm,骨架上分布的凸起尺寸为20~400nm。
3.根据权利要求1所述的三明治型阻气透湿复合膜,其特征在于:
所述排湿层的材料为聚乙烯、聚丙烯、聚苯乙烯、聚对苯二甲酸二醇酯、聚己内酰胺中的至少一种;和/或,
所述阻气层的材料为聚乙烯醇、壳聚糖、海藻酸钠、羟丙基甲基纤维素、羟乙基甲基纤维素中的至少一种;和/或,
所述吸湿层的材料包括聚合物1和聚合物2,其中所述聚合物1选自聚氯乙烯、聚砜、聚醚砜、磺化聚醚砜、聚醚醚酮、聚醚酮、聚丙烯腈、聚芳香醚、醋酸纤维素、聚偏氟乙烯、聚酰亚胺、丙烯腈-苯乙烯共聚物、以及它们改性后的聚合物中的至少一种;所述聚合物2选自聚乙烯吡咯烷酮、聚乙二醇、聚氧乙烯聚氧丙烯醚嵌段共聚物中的至少一种。
4.根据权利要求3所述的三明治型阻气透湿复合膜,其特征在于:
所述吸湿层中聚合物1和聚合物2的重量比为1:(0.05~5),优选为1:(0.3~2)。
5.根据权利要求1所述的三明治型阻气透湿复合膜,其特征在于:
所述排湿层的孔径为0.02~10微米,优选为0.05~5微米;孔隙率为30~80%,优选为40~70%;孔径在平均孔径正负一个数量级范围内的孔占全部孔的50%以上,优选占全部孔的80%以上。
6.根据权利要求1所述的三明治型阻气透湿复合膜,其特征在于:
所述排湿层的厚度为5~1000微米,优选为20~100微米;所述阻气层的厚度为0.1~50微米,优选为0.5~10微米;所述吸湿层的厚度为5~30微米,优选为10~20微米。
7.根据权利要求1~6之任一项所述的三明治型阻气透湿复合膜,其特征在于:
所述吸湿层通过将所述聚合物的混合物进行雾化预处理结合非溶剂致相分离法而得到。
8.一种根据权利要求1~7之任一项所述的三明治型阻气透湿复合膜的制备方法,包括以下步骤:
(1)将阻气层材料溶于水中,加入交联剂,调节溶液pH为1~2,制得涂覆液A;
(2)将所得涂覆液A涂覆在排湿层的表面,烘干得到含阻气层的双层复合膜;
(3)将至少两种聚合物溶解于溶剂中配制聚合物溶液,制得涂覆液B,其中聚合物包括聚合物1和聚合物2;
(4)将步骤(3)得到的涂覆液B附着于所述双层复合膜的阻气层表面,进行雾化预处理,其中雾化预处理为在雾化的液滴浴中停留一段时间;然后浸入凝固浴,得到所述透湿复合膜。
9.根据权利要求8所述的复合膜的制备方法,其特征在于:
步骤(1)中,所述交联剂为甲醛、乙二醛、丙二醛、丁二醛、戊二醛中的至少一种;和/或,
涂覆液A中,阻气层材料的浓度为0.5~10wt%,优选为1~5wt%;交联剂的浓度为0.05~1wt%,优选为0.1~0.5wt%。
10.根据权利要求8所述的复合膜的制备方法,其特征在于:
步骤(2)中,烘干的温度为50~100℃,优选为60~90℃;烘干时间为1~60min,优选为3~30min。
11.根据权利要求8所述的复合膜的制备方法,其特征在于:
步骤(3)中,涂覆液B中聚合物1的浓度为5~20wt%,优选为10~15wt%;聚合物2的浓度为1~20wt%,优选为10~15wt%;和/或,
所述溶剂为聚合物1和聚合物2的良溶剂。
12.根据权利要求8所述的复合膜的制备方法,其特征在于:
步骤(4)中,雾化时间为1~60s,优选为10~30s;和/或,
复合膜表面与雾化喷头之间的距离为1~20cm,优选为5~10cm;和/或,
所述液滴浴中液滴的尺寸为1~50μm,优选为5~18μm;和/或,
所述液滴为聚合物1的不良溶剂;和/或,
所述凝固浴为聚合物1的不良溶剂。
13.根据权利要求11或12所述的复合膜的制备方法,其特征在于:
所述良溶剂选自N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、丙酮、N-甲基-2-吡咯烷酮、二甲基亚砜、四氢呋喃、二氧六环、乙腈、氯仿、四甲基亚砜中的至少一种;和/或,
所述不良溶剂选自水、乙醇、乙二醇中的至少一种。
14.权利要求1~7之任一项所述的三明治型阻气透湿复合膜和/或由权利要求8~13之任一项所述的制备方法制得的复合膜在蔬菜水果保鲜包装中的应用。
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