CN108778726A - 氧气阻隔膜和层压材料及其制造方法 - Google Patents

氧气阻隔膜和层压材料及其制造方法 Download PDF

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Publication number
CN108778726A
CN108778726A CN201780016974.0A CN201780016974A CN108778726A CN 108778726 A CN108778726 A CN 108778726A CN 201780016974 A CN201780016974 A CN 201780016974A CN 108778726 A CN108778726 A CN 108778726A
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film
layer
mfc
laminated material
oxygen barrier
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CN201780016974.0A
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CN108778726B (zh
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I.海斯卡宁
E.索克科宁
V.里布
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Stora Enso Oyj
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Stora Enso Oyj
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Abstract

本发明涉及基于纤维的氧气阻隔膜，其包含(i)微原纤化纤维素(MFC)膜、(ii)氧气阻隔聚合物层、(iii)任选的连接层以及(iv)最外侧的聚烯烃层。本发明甚至涉及层压材料，其中所述多层膜借助中间聚乙烯层与纤维质的纸或板基材结合。氧气阻隔聚合物层(其优选为EVOH)和聚烯烃层通过共挤出置于MFC膜上。根据本发明的膜和层压材料的目标在于在高湿度条件下的改进的氧气阻隔以及在对氧敏感的食物包装中具有应用。

Description

氧气阻隔膜和层压材料及其制造方法
本发明涉及基于纤维的氧气阻隔膜和包含该膜的层压材料(层合物)。本发明甚至涵盖制造该膜和层压材料的方法，以及膜或层压材料的用途。
背景技术
存在着特定的聚合物，其已经常规地用于提供氧气阻隔层，其是一层对氧气是高度不渗透的材料。乙基乙烯醇共聚物(EVOH)、聚酰胺(PA)、聚乙烯醇共聚物(PVOH)和聚氯乙烯(PVC)是这样的聚合物的实例。
在包装行业需要有效的氧气阻隔层用于屏蔽对氧敏感的产品，由此延长它们的保质期。这些特别地包括许多食物产品。已知的具有氧气阻隔性质的包装材料可包括聚合物膜或涂覆有氧气阻隔聚合物的层(通常作为多层涂层结构的一部分)的纤维质的纸或板。
最近，微原纤化纤维素(MFC)膜(其中原纤维通过氢键相互键合)已经被提出用作气体阻隔层。出版物EP 2 554 589 A1描述了该膜的制备，其中在纸或聚合物基底上涂覆水性纤维素纳米纤维分散体，干燥且最终作为纳米纤维膜片被剥离。教导用于改进气体阻隔膜的实施方式包括加入无机化合物用于改进在潮湿条件下的水蒸气不可渗透性，以及加入热塑性聚合物(例如LDPE)层以赋予可热封性。
WO 2015/034426 A1描述了MFC膜作为用于食物或液体包装目的的氧气阻隔聚合物膜。MFC膜通过对原纤化纤维素悬浮体进行真空过滤，随后干燥来制造。该出版物教导了纤维的交联，以便降低膜对水和湿气的亲和性。包装材料可包含与基材材料结合的MFC膜，所述基材材料可以是纸或纸板。EVOH、PA、PET、LDPE或HDPE层可作为水蒸气阻隔膜加入，或者作为最外侧的层或者夹在基材材料和MFC膜层之间。
WO 2011/078770 A1描述了包含纸或纸板基底、MFC层和最外侧的聚合物层(优选PE或PET)的基于纤维的包装材料。MFC层优选通过湿涂添加至基底，且聚合物层通过层压或挤出涂覆置于MFC层之上。任选地，EVOH层可以夹在MFC和最外侧的聚合物层之间的方式包括进来。MFC和聚合物的结合据称赋予材料阻隔性质，比如对氧气和蒸气的抗性。
SE 1351552 A1描述了特别地用于高压灭菌包装的多层包装材料，其包含纤维质的纸或板基材、涂覆至纤维质基材上的MFC层分散体和一个或多个朝向包装内部的内部聚合物层。在纤维质基材的背侧上提供另一个聚合物涂层。聚合物层的目的在于提供高压灭菌所需的液体阻隔，且MFC层的目的在于替代之前使用的铝作为氧气阻隔层。PA或EVOH层可作为另一个氧气阻隔层加入。
由MFC膜赋予的气体阻隔性是基于膜的无孔塑化特性。然而，该气体阻隔性在高湿度条件下被破坏。即便作为氧气阻隔材料的EVOH对湿度也是敏感的，且倾向于失去阻隔性质。加入屏蔽MFC或EVOH氧气阻隔层的外侧蒸气阻隔PE层也不能提供完全的补偿。
MFC膜的另一方面在于为了实现优异的氧气阻隔，其中氧气透过率(OTR)低于50ml/m2，或优选低于15ml/m2，在24h内在50％的相对湿度(RH)下(ASTM标准D3985-05)，膜必须以低生产速度制造，这是高成本的。在高速度下生产的低成本膜的OTR在100-8000ml/m2的范围内或甚至更高。现有技术已经认为这样的膜作为氧气阻隔层是无用的。
发明内容
因此存在新的基于MFC膜的技术方案的空间，该方案改进了氧气阻隔，特别是在高湿度条件下，比如炎热的热带气候。根据本发明，新颖的基于纤维的氧气阻隔膜包含(i)微原纤化纤维素(MFC)膜、(ii)氧气阻隔聚合物层、(iii)任选的连接层以及(iv)最外侧的聚烯烃层，氧气阻隔聚合物和聚烯烃层(ii，iv)通过共挤出置于MFC膜(i)上。
层(ii)的氧气阻隔聚合物可选自乙基乙烯醇共聚物(EVOH)、聚酰胺(PA)、聚乙烯醇共聚物(PVOH)和聚氯乙烯(PVC)。在这些聚合物中，EVOH是特别优选的。
发明人已经令人惊奇地发现，当通过挤出使EVOH与预制的MFC膜直接接触时，氧气阻隔性得以改进，并且与预期相反甚至承受得起湿度而无显著的劣化。此外，这与现有技术中使用的外部PE蒸气阻隔层无关。不受理论的束缚，现假设该改进是因为沿着MFC膜和EVOH之间的边界表面的结晶的缘故，其中挤出的熔融EVOH紧密地跟随着MFC膜的最细小的不平整性(不均匀性)。此外，形成了结晶的氧气阻隔层，无论MFC膜的OTR值如何，这都使得在不透氧气、对水分不敏感的包装中使用低质量的膜成为可能。还有，已经发现，根据本发明的膜降低了卷曲的倾向。
本发明中需要的最外侧的聚烯烃层对于在共挤出中支撑EVOH层是必要的。优选地，聚烯烃为聚乙烯(PE)，比如低密度聚乙烯(LDPE)，这使得多层膜具有优越的可热封性。如已知的那样，PE也是水蒸气阻隔物，即便本发明没有特别地依赖此性质。
用于将聚烯烃层粘附至氧气阻隔聚合物(例如EVOH)层的任选的连接层可以是乙烯共聚物。该连接聚合物在本领域中是已知的。
优选地，MFC膜是预制的MFC膜，重量为20-40g/m2。可用于本发明的这类膜的制造在本领域中是已知的。
出于本发明的目的，MFC膜层本身在24h内在23℃和50％RH下的OTR为100-8000ml/m2、优选500-2000ml/m2通常是足够的。通过本发明，最终的多层膜的OTR会显著地低于那些相当适度(modest)的数值。
在MFC膜的背侧上还可存在挤出的聚烯烃层。出于此目的，可热封的聚乙烯比如LDPE是优选的。
目前描述的根据本发明的产物是柔性膜，其特别地可用作用于对氧敏感的产品的包装膜。本发明的另一实施方式为层压材料，其包括作为其多层结构的一部分的该膜。一般地，根据本发明的层压材料包含(i)纤维质的纸或板基材、(ii)聚乙烯(PE)层、(iii)微原纤化纤维素(MFC)膜、(iv)氧气阻隔聚合物层、(v)任选的连接层以及(vi)最外侧的聚烯烃层。
上述膜产品的描述适用于根据本发明的层压材料的层(ii)至(vi)。因此，氧气阻隔聚合物层(iv)优选为EVOH层且最外侧的聚烯烃层(vi)优选为PE层，特别是LDPE层。在MFC膜(iii)的背侧上的PE层(ii)形成了在MFC膜层(iii)和纸或板基材(i)之间的密封层(seal)。
对于层压材料的可热封性，可向纤维质的纸或板基材的背侧提供可热封的聚烯烃层。
如果最外侧的聚烯烃层是聚丙烯(PP)而不是PE，则根据本发明的膜和层压材料甚至会承受在最高达约130℃的高温和高蒸气压下的高压灭菌。
纤维质基材可包含130-250g/m2、优选200-250g/m2重量的纸板，或替代地，纤维质基材可包含40-130g/m2重量的纸。
本发明甚至涵盖制造上述膜产品的方法，该方法特征在于将氧气阻隔聚合物层、可能的连接层和聚烯烃层共挤出至MFC膜上。用于制造上述层压材料的根据本发明的方法的特征在于将膜产品干层压至涂覆有PE层的纸或板基材。该PE涂层是为了与MFC膜层形成粘合。
最后，本发明涵盖上述膜或上述层压材料用于经受高湿度条件的密封食物包装的用途。特别地，这样的用途涉及干食物包装，其中食物受到保护以免受氧气以及湿度的影响。
具体实施方式
在本专利申请的上下文中，微原纤化纤维素(MFC)应意指至少一个维度小于100nm的纳米尺度纤维素颗粒纤维或原纤维。MFC包含部分或完全原纤化的纤维素或木质纤维素纤维。释放的原纤维的直径小于100nm，而实际的原纤维直径或粒度分布和/或纵横比(长度/宽度)取决于来源和制造方法。最小的原纤维被称为初级原纤维(基础原纤维，elementary fibril)，并且直径为约2-4nm(参见例如Chinga-Carrasco，G.，Cellulosefibres，nanofibrils and microfibrils,:The morphological sequence of MFCcomponents from a plant physiology and fibre technology point of view，Nanoscale research letters 2011，6:417)，而通常聚集形式的初级原纤维(也定义为微原纤维(Fengel,D.,Ultrastructural behavior of cell wall polysaccharides,TappiJ.,1970年3月,第53卷,No.3.))是当例如通过使用延长的磨浆方法或压降解离(压降分解，pressure-drop disintegration)方法制造MFC时获得的主要产物。取决于来源和制造方法，原纤维的长度可在约1至大于10微米范围内变化。粗MFC等级可能含有相当大部分的原纤化纤维，即来自管胞的突出的原纤维(纤维素纤维)，且具有一定量的从管胞释放的原纤维(纤维素纤维)。
MFC存在不同的缩写，比如纤维素微原纤维、原纤化纤维素、纳米原纤化纤维素、原纤维聚集物、纳米尺度纤维素原纤维、纤维素纳米纤维、纤维素纳米原纤维、纤维素微纤维、纤维素原纤维、微原纤纤维素、微原纤维聚集物和纤维素微原纤维聚集物。MFC的特征还可在于各种物理或物理-化学性质，如大的表面积或其在分散在水中时在低固体(1-5重量％)下形成凝胶状材料的能力。纤维素纤维优选被原纤化至这样的程度，即使得形成的MFC的最终比表面积为约1至约200m2/g，或优选50-200m2/g，用BET方法对冷冻干燥的材料进行测定。
存在多种方法制造MFC，比如单次磨浆或多次磨浆(multiple pass refining)、预水解随后通过磨浆或高剪切解离或释放原纤维。通常需要一个或若干个预处理步骤以便使得MFC制造既节能又可持续。待供给的纸浆的纤维素纤维因此可以酶的方式或化学方式预处理，例如以减少半纤维素或木质素的量。在原纤化之前纤维素纤维可以化学方式改性，其中纤维素分子含有除在原始纤维素中发现的官能团以外(或更多)的官能团。这些基团尤其包括羧甲基(CMC)、醛和/或羧基(通过N-氧基介导的氧化获得的纤维素，例如"TEMPO")，或季铵(阳离子纤维素)。在以上述方法之一改性或氧化之后，更容易将纤维解离成MFC或纳米原纤维尺寸或NFC。
纳米原纤(nanofibrillar)纤维素可能含有一些半纤维素；量取决于植物来源。经预处理的纤维的机械解离，例如水解的、预溶胀的、或氧化的纤维素原材料用合适的设备进行，比如磨浆机、研磨机、均质器、胶体排除装置(colloider)、摩擦研磨机、超声超声波仪、流化器比如微流化器、宏观流化器或流化器型均化器。取决于MFC制造方法，产物还可含有细料、或纳米结晶纤维素或例如存在于木材纤维中或造纸方法中的其他化学品。产物还可含有多种量的未被有效地原纤化的微米尺寸的纤维颗粒。
从木材纤维素纤维生产MFC，包括从阔叶木或针叶木纤维这两者。其还可从微生物来源、农作物纤维(比如麦草浆，竹子，甘蔗渣)或其他非木材纤维来源制造。其优选从纸浆制得，其包括来自原生纤维的纸浆，例如机械、化学和/或热机械纸浆。其还可从损纸或再生纸制得。
MFC的上述定义包括但不限于对纤维素纳米原纤维(CMF)新提出的TAPPI标准W13021，其定义了含有多根初级原纤维的纤维素纳米纤维材料，其具有结晶和无定形区域这两者，具有高纵横比，其中宽度为5-30nm且纵横比通常大于50。
为实施本发明，MFC膜(纳米纸)优选在造纸机上制备，所述造纸机适用于由0.1-1.0重量％稠度的MFC悬浮体生产膜(对于MFC，不包括可能的固体添加剂比如填料)，且微纤维的纤维长度为100nm-200μm，优选100nm-10μm(如至少70SR、优选至少90SR的肖伯尔-瑞格勒(Schopper-Riegler)滤水数(drainability number)所表明的)。机器速度可以是100m/min，优选300m/min或甚至更高。在这样的速度下，幅材快速地被脱水和干燥，且大规模生产可以经济的方式实现。MFC膜的重量可为约20-40g/m2。膜在24h内在23℃和50％RH下的OTR在100-8000ml/m2、优选500-2000ml/m2的范围内。对于氧气阻隔，这些透过率本身并不显著，但生产这些“二等(second rate)”MFC膜的成本很低。
替代地，可通过将5-25重量％的稠度的水性MFC悬浮体浇注(cast)至聚合物基底上形成涂层膜，随后通过干燥并且最终通过将其从基底剥离从而将膜分离来制备MFC膜。
下一步是将氧气阻隔聚合物层和聚烯烃层共挤出至干燥的MFC膜上。优选地，氧气阻隔聚合物为EVOH且聚烯烃是可热封的LDPE。LDPE的作用是在共挤出中支撑EVOH层。为了更好地将LDPE粘附至EVOH连接层，可将乙烯共聚物作为共挤出中的中间层而包括进来。合适的挤出聚合物层重量为3-30g/m2的EVOH，0.5-15g/m2的连接聚合物，和10-50g/m2的LDPE。可将10-40g/m2的LDPE的可热封的层挤出至MFC膜层的背侧上。
在共挤出过程中，EVOH层使其自身适应于MFC膜表面的最细小的不规则性，实现紧密贴合，据信这产生了单一的结晶层，形成了大大优于单独通过MFC膜和EVOH层所获得的氧气阻隔层，并且远高于两者简单的加和。
上述多层膜本身可用于包装对氧敏感的食物，所述食物在高湿度条件下储存和销售。
本发明的替代实施方式，即包含MFC膜层的层压材料，可基于由化学或木材纸浆制得的纤维质的纸、纸板或卡纸板。优选地，纤维质基材为130-250g/m2、优选200-250g/m2重量的纸板，或40-130g/m2重量的纸。在第一步，用10-20g/m2聚乙烯(优选LDPE)的层来挤出涂覆纤维质基材。随后的第二步是干燥或将如上所述的基于MFC膜的多层膜挤出层压至经PE涂覆的纤维质基材，其包括将未涂覆的或经LDPE涂覆的MFC膜的背侧粘附至纤维质基材的PE涂层。可通过挤出至纤维质基材的背侧上而加入可热封的LDPE层。该层压材料可用于例如必须与氧气和高湿度相屏蔽的干燥食物比如咖啡、茶、巧克力、饼干等的可热封的纸板箱或盒包装。
实施例
制备具有以下结构的第一多层层压材料：(i)15g/m2的LDPE层，(ii)70g/m2的纸层(“Lumiflex 70”)，(iii)12g/m2的LDPE层，(iv)30g/m2的MFC膜层，(v)6g/m2的EVOH层，(vi)5g/m2的乙烯共聚物连接层，和(vii)45g/m2的LDPE层。
制备第二多层层压材料，其对应于如上所述的第一多层层压材料，不同之处在于(ii)200g/m2的纸板层替代了“Lumiflex 70”纸层。
在不同温度和相对湿度下测量氧气和水蒸气透过率的结果示于表1。由于23℃的温度和50％的RH表示正常室内环境，38℃的温度和85％的RH对于热带高湿度环境是典型的，其对于包装业具有挑战性，且这是本发明特别针对处理的。
因此，所测量的低OTR源自根据本发明的基于纸和板的层压材料。然而，结果并没有显著地劣于缺乏纤维质的纸或板基材的膜所预期的结果，因为包含在层压材料中的多余的PE和基材层对氧气阻隔性基本上没有贡献，其主要取决于MFC/EVOH界面结构。

Claims (16)

1.基于纤维的氧气阻隔膜，其包含：
(i)微原纤化纤维素(MFC)膜，
(ii)氧气阻隔聚合物层，
(iii)任选的连接层，和
(iv)最外侧的聚烯烃层。
其中所述氧气阻隔聚合物和聚烯烃层通过共挤出置于MFC膜上。
2.权利要求1的膜，其特征在于所述氧气阻隔聚合物选自乙基乙烯醇共聚物(EVOH)、聚酰胺(PA)、聚乙烯醇共聚物(PVOH)和聚氯乙烯(PVC)。
3.权利要求2的膜，其特征在于所述氧气阻隔聚合物为EVOH。
4.前述权利要求中任一项的膜，其特征在于所述聚烯烃为聚乙烯(PE)。
5.前述权利要求中任一项的膜，其特征在于MFC膜为20-40g/m2重量的预制的MFC膜。
6.前述权利要求中任一项的膜，其特征在于MFC膜的氧气透过率(OTR)高于50ml/m2，优选在100-8000ml/m2的范围内(ASTMD3985-05)，在50％的相对湿度下。
7.前述权利要求中任一项的膜，其特征在于在MFC膜的背侧上具有挤出的聚烯烃层。
8.包含前述权利要求中任一项的膜的层压材料，所述层压材料包含：
(i)纤维质的纸或板基材，
(ii)聚乙烯(PE)层，
(iii)微原纤化纤维素(MFC)膜，
(iv)氧气阻隔聚合物层，
(v)任选的连接层，和
(vi)最外侧的聚烯烃层
其中所述氧气阻隔聚合物和聚烯烃层通过共挤出置于MFC膜上。
9.权利要求8的层压材料，其特征在于纤维质的纸或板基材的背侧提供有可热封的聚烯烃层。
10.权利要求8或9的层压材料，其特征在于纤维质基材(i)包含130-250g/m2、优选200-250g/m2重量的纸板。
11.权利要求8或9的层压材料，其特征在于纤维质基材(i)包含40-130g/m2重量的纸。
12.制造权利要求1-7中任一项的膜的方法，其特征在于将氧气阻隔聚合物层、可能的连接层和聚烯烃层共挤出至MFC膜上。
13.权利要求12的方法，其特征在于将EVOH、连接层和聚乙烯或聚丙烯层共挤出至MFC膜上。
14.制造权利要8-11中任一项的层压材料的方法，其特征在于将根据权利要求1-7中任一项获得的膜干层压至涂覆有PE层的纸或板基材。
15.权利要求1-7中任一项的膜或权利要求8-11中任一项的层压材料用于经受高湿度条件的密封食物包装的用途。
16.根据权利要求15所述的用途，其用于干食物包装。
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