CN110305350A - 一种符合食品安全的智能控湿薄膜及其制备方法和应用 - Google Patents
一种符合食品安全的智能控湿薄膜及其制备方法和应用 Download PDFInfo
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- CN110305350A CN110305350A CN201810230528.6A CN201810230528A CN110305350A CN 110305350 A CN110305350 A CN 110305350A CN 201810230528 A CN201810230528 A CN 201810230528A CN 110305350 A CN110305350 A CN 110305350A
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- humidity control
- food safety
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Abstract
本发明属于功能薄膜领域，涉及一种符合食品安全的智能控湿薄膜及其制备方法和应用。所述符合食品安全的智能控湿薄膜包括基层和附加层，所述附加层位于基层一侧或两侧；其中，所述基层为多孔薄膜，选自聚芳香醚多孔薄膜、聚乙烯多孔薄膜和聚丙烯多孔薄膜中的至少一种；所述附加层为致密薄膜，其材质含有聚乙烯醇和辅助组分，以及任选的交联剂和/或抗菌剂；所述辅助组分为符合食品安全的水溶性金属盐、酸溶性金属氧化物、纤维素及纤维素衍生物和多元醇中的至少一种。本发明的智能控湿薄膜具有智能控湿能力，具有氧气阻隔性能并符合食品安全，可用于具有保鲜功能的果蔬盒及具有保鲜果蔬盒的冰箱。
Description
技术领域
本发明属于功能薄膜领域，更具体地，涉及一种符合食品安全的智能控湿薄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，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，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
本发明的目的是为了克服现有技术存在的上述缺陷，提供一种智能控湿薄膜，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，具有阻气性能，并且，该薄膜的原料均符合食品安全。本发明进一步提供所述该薄膜的制备方法，该方法工艺简单、成本低。因此，本发明提供的薄膜特别适合应用于蔬菜水果的保鲜包装。
本发明的第一方面提供一种符合食品安全的智能控湿薄膜，包括基层和附加层，所述附加层位于基层一侧或两侧；其中，
所述基层为多孔薄膜，选自聚芳香醚多孔薄膜、聚乙烯多孔薄膜和聚丙烯多孔薄膜中的至少一种；
所述附加层为致密薄膜，其材质含有聚乙烯醇和辅助组分，以及任选的交联剂和/或抗菌剂；所述辅助组分为符合食品安全的水溶性金属盐、酸溶性金属氧化物、纤维素及纤维素衍生物和多元醇中的至少一种。
本发明中，为实现智能控湿，所述基层需为多孔薄膜，所述附加层需为致密薄膜。所述多孔薄膜和致密薄膜的概念和术语范畴为本领域技术人员公知。作为附加层的致密薄膜可通过将含有附加层组分的溶液涂布至基层表面并干燥的方式制得。
根据本发明，所述智能控湿薄膜为多层，当智能控湿薄膜为两层时，所述附加层位于基层一侧，当智能控湿薄膜为三层时，所述附加层位于基层两侧，在需要的情况下，所述智能控湿薄膜也可以为超过三层的更多层，附加层和基层可以间隔布置。其中，所述基层优选为单层结构。
本发明中，所述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。
根据本发明，优选地，所述聚芳香醚多孔薄膜的材质包括但不限于聚砜、酚酞型聚砜、聚醚砜、磺化聚醚砜、聚醚酮和磺化聚醚酮中的至少一种；优选为聚砜、酚酞型聚砜和聚醚砜中的至少一种。所述聚芳香醚多孔薄膜可商购获得或通过本领域常规方法制备获得，例如将聚砜溶液涂覆在无纺布上，通过相转化可制得聚砜多孔薄膜。
根据本发明，所述聚乙烯多孔薄膜的材质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。
根据本发明，所述聚丙烯多孔薄膜的材质优选为均聚聚丙烯、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。
根据本发明，所述聚乙烯醇和辅助组分的相对含量以形成致密薄膜为限，优选地，以附加层总重量为基准，所述聚乙烯醇的含量为50-99wt％，优选为66-98wt％，进一步优选为70-95wt％；所述辅助组分的含量为1-50wt％，优选为2-34wt％，进一步优选为5-30wt％。
根据本发明，较高分子量和醇解度的聚乙烯醇更有利于形成致密薄膜，优选地，所述聚乙烯醇的重均分子量为10000-500000，进一步优选为20000-200000；醇解度优选为70％-100％，进一步优选为88％-99％。
本领域技术人员知晓符合食品安全的判定标准，可根据需要在上述组分范围内选择合适的物质。根据本发明，所述辅助组分优选为氯化锂、氯化钠、硫酸钙晶须、氧化铝、、氧化钙、氧化镁、纳米纤维素、羟乙基纤维素、丙二醇、甘油、山梨醇和蔗糖中的至少一种。
根据本发明，交联剂和抗菌剂为可选含有的组分，交联剂的加入可使智能控湿薄膜具有更好的氧气阻隔性能，抗菌剂的加入可使智能控湿薄膜具有抗菌性能。
以所述附加层的总重量为基准，所述交联剂的含量为0-10wt％，优选为0.1-7wt％，进一步优选为2-6wt％。所述交联剂为甲醛、戊二醛、马来酸和马来酸酐中的至少一种，优选为马来酸和/或马来酸酐。
以所述附加层的总重量为基准，所述抗菌剂的含量为0-20wt％，优选为0.1-10wt％；所述抗菌剂为纳米氧化锌、纳米氧化钛、纳米银、纳米铜、壳聚糖、山梨酸钾、丝胶、羟苯甲酯和西吡氯铵中的至少一种，优选为纳米氧化钛、壳聚糖、山梨酸钾和丝胶中的至少一种。
上述优选的组分可获得更优透湿度和阻气性的薄膜。
根据本发明，所述基层和附加层的厚度可根据需要确定，一般地，所述基层的厚度可以为5-1000微米，优选为10-100微米，进一步优选为60-95微米；所述附加层的厚度可以为0.5-100微米，优选为2-20微米。
本发明的第二方面提供一种符合食品安全的智能控湿薄膜的制备方法，包括以下步骤：
(1)将上述智能控湿薄膜的附加层的各组分充分溶解或者分散于水中，配制成溶液或者分散液；
(2)将步骤(1)中得到的溶液或者分散液涂布于上述智能控湿薄膜的基层的一面或两面；烘干后得到所述智能控湿薄膜。
可以采用任何常规的涂布方法将步骤(1)中得到的溶液或者分散液涂布于基层，包括但不限于：刷涂、淋涂、喷涂。
根据本发明，步骤(1)中的溶液或者分散液的质量浓度可以为0.5％-30％，优选为1％-10％，进一步优选为5％-10％。
根据本发明，步骤(2)中烘干的温度可以为50℃-100℃，优选为60℃-90℃。可在常规的各种加热装置中完成烘干步骤，如烘箱。烘干的时间可根据需要确定，例如为5-30min。
根据本发明，交联剂可以在配制附加层的溶液或分散液时加入，也可以在烘干后单独涂布，或分两步在上述两个时机加入。在烘干后单独涂布的步骤包括：将交联剂单独配制成溶液或分散液，将含有交联剂的溶液或分散液涂布于步骤(2)的烘干后的薄膜的一面或两面，再次烘干后得到所述智能控湿薄膜；所述含有交联剂的溶液或分散液的质量浓度优选为0.5％-10％，进一步优选为1％-5％。再次烘干的条件可与第一次烘干条件相同。
本发明的第三方面提供上述智能控湿薄膜和/或由上述制备方法制得的智能控湿薄膜在蔬菜水果保鲜包装中的应用。
本发明的智能控湿薄膜具有智能控湿能力，在相对湿度较低时保持果蔬湿度，在相对湿度较高时增大透湿从而防止水果蔬菜结露溃烂，此外，该智能控湿薄膜具有氧气阻隔性能并符合食品安全，可用于具有保鲜功能的果蔬盒及具有保鲜果蔬盒的冰箱。
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。
具体实施方式
下面将更详细地描述本发明的优选实施方式。
智能控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。
聚砜，百灵威，数均分子量为8000。
聚醚砜，BASF，Ultrason E6020 P，数均分子量为12000。
聚酯无纺布，燕山石油化工公司，数均分子量为20000。
聚丙烯，F1002B，中石化扬子石化。
聚乙烯，L501(5000S)，中石化扬子石化。
致密的聚丙烯双向拉伸薄膜，中石化镇海炼化，F280Z。
聚乙烯醇A，西陇化工，牌号为PVA124，重均分子量为105000，醇解度为99％。
聚乙烯醇B，西陇化工，牌号为PVA1788，重均分子量为74800，醇解度为88％。
氯化锂，百灵威，99％。
氧化铝，百灵威，纯度90％。
甘油，百灵威，纯度98％。
羟乙基纤维素，Sigma-Aldrich，﹥95％。
纳米氧化钛，百灵威，99.5％，粒径10-30nm。
纳米银，百灵威，99.5％，粒径10-30nm。
山梨酸钾，伊诺凯，99％。
马来酸，伊诺凯，99％。
马来酸酐，伊诺凯，99％。
薄膜单向拉伸机，广州普同，MESI-LL。
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7g聚乙烯醇A加入100mL蒸馏水中，充分溶解。然后加入2.1g氯化锂、0.2g山梨酸钾、0.35g马来酸酐，搅拌30min至混合均匀，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，得到智能控湿薄膜A1，其基层厚度为70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；附加层厚度为9微米。
对比例1
根据与实施例1相同的方法制备薄膜，不同的是，不加入氯化锂。得到薄膜D1。
对比例2
根据与实施例1相同的方法制备薄膜，不同的是，不使用多孔聚丙烯薄膜，而使用致密的聚丙烯双向拉伸薄膜。得到薄膜D2。
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6g聚乙烯醇A和2g羟乙基纤维素加入100mL蒸馏水中，充分溶解，再加入0.2g山梨酸钾，0.35g马来酸酐，搅拌30min至混合均匀，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60℃下烘干12min，得到智能控湿薄膜A2，其基层厚度为70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；附加层厚度为12微米。
实施例3
将聚砜溶于N,N-二甲基甲酰胺中，制得浓度为18％的聚砜溶液。将该溶液于25℃下静置脱泡120min后均匀涂覆在聚酯无纺布上，然后在25℃的水中浸泡60min，经三次水洗后得到聚砜多孔薄膜。
将6g聚乙烯醇A与0.32g甘油加入到100mL蒸馏水中，充分搅拌直至完全溶解。然后加入0.2g纳米氧化钛，充分搅拌至混合均匀，得到涂覆液。将此涂覆液均匀地刷涂在聚砜多孔薄膜两面，然后将其置于烘箱中，在80℃下烘干8min，得到烘干后的薄膜，将含有0.2g马来酸的10mL水溶液均匀地刷涂在烘干后的薄膜两面，在80℃下烘干8min，得到智能控湿薄膜A3，其基层厚度为90微米，孔径为0.85微米，孔隙率为45％，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；附加层厚度为10微米。
实施例4
根据与实施例1相同的方法制备薄膜，不同的是，溶液中不加入马来酸酐，得到智能控湿薄膜A4。
实施例5
将聚醚砜溶于N,N-二甲基甲酰胺中，制得浓度为18％的聚醚砜溶液。将该溶液于25℃下静置脱泡120min后均匀涂覆在聚酯无纺布上，然后在25℃的水中浸泡60min，经三次水洗后得到聚醚砜多孔薄膜。
将7g聚乙烯醇B加入100mL蒸馏水中，充分溶解。然后加入2.1g氯化锂、0.2g纳米银、0.35g马来酸酐，搅拌30min至混合均匀，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，得到智能控湿薄膜A5，其基层厚度为85微米，孔径为0.91微米，孔隙率为38％，孔径在平均孔径正负一个数量级范围内的孔占全部孔的70％以上；附加层厚度为9微米。
实施例6
根据与实施例2相同的方法制备薄膜，不同的是，用等重量的氧化铝代替羟乙基纤维素，得到智能控湿薄膜A6。
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)，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：薄膜的透湿性和气体阻隔性能测试结果
| 序号 | 透湿度(50％RH) | 透湿度(90％RH) | 阻气性(O<sub>2</sub>) |
| A1 | 188 | 1583 | 5.3×10<sup>-5</sup> |
| D1 | 32 | 337 | 1.7×10<sup>-5</sup> |
| D2 | 9 | 15 | 3.2×10<sup>-6</sup> |
| A2 | 122 | 1384 | 7.2×10<sup>-5</sup> |
| A3 | 98 | 1256 | 6.6×10<sup>-5</sup> |
| A4 | 210 | 1637 | 2.0×10<sup>-4</sup> |
| A5 | 160 | 1458 | 5.5×10<sup>-5</sup> |
| A6 | 83 | 1042 | 5.7×10<sup>-5</sup> |
由表1可见，本发明的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。
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 (16)
1.一种符合食品安全的智能控湿薄膜，包括基层和附加层，所述附加层位于基层一侧或两侧；其中，
所述基层为多孔薄膜，选自聚芳香醚多孔薄膜、聚乙烯多孔薄膜和聚丙烯多孔薄膜中的至少一种；
所述附加层为致密薄膜，其材质含有聚乙烯醇和辅助组分，以及任选的交联剂和/或抗菌剂；所述辅助组分为符合食品安全的水溶性金属盐、酸溶性金属氧化物、纤维素及纤维素衍生物和多元醇中的至少一种。
2.根据权利要求1所述的智能控湿薄膜，其中，所述多孔薄膜的孔径为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。
3.根据权利要求1所述的智能控湿薄膜，其中，所述聚芳香醚多孔薄膜的材质为聚砜、酚酞型聚砜、聚醚砜、磺化聚醚砜、聚醚酮和磺化聚醚酮中的至少一种，优选为聚砜、酚酞型聚砜和聚醚砜中的至少一种；
所述聚乙烯多孔薄膜的材质为高密度聚乙烯、线性低密度聚乙烯和低密度聚乙烯中的至少一种；
所述聚丙烯多孔薄膜的材质为均聚聚丙烯、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。
4.根据权利要求1所述的智能控湿薄膜，其中，以附加层总重量为基准，所述聚乙烯醇的含量为50-99wt％，优选为66-98wt％，所述辅助组分的含量为1-50wt％，优选为2-34wt％。
5.根据权利要求1所述的智能控湿薄膜，其中，所述聚乙烯醇的重均分子量为10000-500000，优选为20000-200000；醇解度为70％-100％，优选为88％-99％。
6.根据权利要求1所述的智能控湿薄膜，其中，所述辅助组分为氯化锂、氯化钠、硫酸钙晶须、氧化铝、氧化钙、氧化镁、纳米纤维素、羟乙基纤维素、丙二醇、甘油、山梨醇和蔗糖中的至少一种。
7.根据权利要求1-6中任意一项所述的智能控湿薄膜，其中，以所述附加层的总重量为基准，所述交联剂的含量为0-10wt％，优选为0.1-7wt％。
8.根据权利要求1-6中任意一项所述的智能控湿薄膜，其中，所述交联剂为甲醛、戊二醛、马来酸和马来酸酐中的至少一种，优选为马来酸和/或马来酸酐。
9.根据权利要求1-6中任意一项所述的智能控湿薄膜，其中，以所述附加层的总重量为基准，所述抗菌剂的含量为0-20wt％，优选为0.1-10wt％。
10.根据权利要求1-6中任意一项所述的智能控湿薄膜，其中，所述抗菌剂为纳米氧化锌、纳米氧化钛、纳米银、纳米铜、壳聚糖、山梨酸钾、丝胶、羟苯甲酯和西吡氯铵中的至少一种，优选为纳米氧化钛、壳聚糖、山梨酸钾和丝胶中的至少一种。
11.根据权利要求1-6中任意一项所述的智能控湿薄膜，其中，所述基层的厚度为5-1000微米，优选为10-100微米；所述附加层的厚度为0.5-100微米，优选为2-20微米。
12.一种符合食品安全的智能控湿薄膜的制备方法，包括以下步骤：
(1)将如权利要求1-11中任意一项所述的智能控湿薄膜的附加层的各组分充分溶解或者分散于水中，配制成溶液或者分散液；
(2)将步骤(1)中得到的溶液或者分散液涂布于如权利要求1-11中任意一项所述的智能控湿薄膜的基层的一面或两面；烘干后得到所述智能控湿薄膜。
13.根据权利要求12所述的制备方法，其中，步骤(1)中的溶液或者分散液的质量浓度为0.5％-30％，优选为1％-10％。
14.根据权利要求12所述的制备方法，其中，步骤(2)中烘干的温度为50℃-100℃，优选为60℃-90℃。
15.根据权利要求12-14中任意一项所述的制备方法，其中，将交联剂单独配制成溶液或分散液，将含有交联剂的溶液或分散液涂布于步骤(2)的烘干后的薄膜的一面或两面，再次烘干后得到所述智能控湿薄膜；所述含有交联剂的溶液或分散液的质量浓度优选为0.5％-10％，进一步优选为1％-5％。
16.权利要求1-11中任意一项所述的智能控湿薄膜和/或由权利要求12-15中任意一项所述的制备方法制得的智能控湿薄膜在蔬菜水果保鲜包装中的应用。
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