CN109415152A - 适合用于包装的乙烯清除材料及其制造方法 - Google Patents

适合用于包装的乙烯清除材料及其制造方法 Download PDF

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CN109415152A
CN109415152A CN201780041563.7A CN201780041563A CN109415152A CN 109415152 A CN109415152 A CN 109415152A CN 201780041563 A CN201780041563 A CN 201780041563A CN 109415152 A CN109415152 A CN 109415152A
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ethylene
cellulose
scavenger
absorbent
dispersion
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CN109415152B (zh
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K.巴克福尔克
I.海斯卡宁
E.索科宁
S.兰派宁
S.西托宁
M.安德森
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Stora Enso Oyj
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Abstract

本发明涉及包含纳米尺寸的纤维素和乙烯清除剂或乙烯吸收剂的适合用于包装的材料。本发明还涉及制造这种材料的方法，该材料可以是纸、标签、纸板、塑料或膜产品。

Description

适合用于包装的乙烯清除材料及其制造方法
技术领域
本发明涉及包含纳米尺寸的纤维素和乙烯清除剂或乙烯吸收剂的适合用于包装的材料。本发明还涉及制造这种材料的方法，该材料可以是纸、标签、纸板、塑料或膜产品。
背景技术
食品和食品产品，包括包装的食品和食品产品，通常会遇到两个主要问题：微生物污染和品质劣化。
当一些产品如水果和蔬菜成熟时，其释放乙烯，一种加速成熟的气体，导致水果和蔬菜变得有斑点、柔软和腐烂。除了质地变化外，产品的味道、气味或营养成分也可能发生变化。与乙烯有关的问题在发展中国家造成了很大一部分的收获后损失。
本领域有各种方法和产品，用于保护食品材料免受乙烯气体的负面影响。经常使用改变(改性)的气氛或在较低温度下储存，尽管这些可能对产品的至少一些感官性质具有负面影响。引入乙烯清除性质的方法包括使用高锰酸钾作为乙烯氧化剂，如WO 2005/000369 A1和EP 0 515 764 A2中所公开。将高锰酸钾掺入到具有高表面积的吸收材料中，例如氧化铝、二氧化硅、粘土和活性炭。然而，由于高锰酸钾的毒性，在欧洲禁止使用高锰酸钾，并且在美国存在程度受到限制，吸收材料只能储存在囊中。另一方面，将不同的功能性矿物质掺入到聚合物膜中也是公知的，并且这类产品已经是在市场上可获得的。
JP2242767公开了一种由塑料膜制成的袋，其具有确定的透气性和至少30mm的防水性并且含有新鲜蔬菜，以及另一种膜袋，其含有一起放置在波纹纤维板箱中的气体吸附剂，优选地放置在在其波纹表面的中央凹槽中设置有阻隔层的箱中。塑料膜可以具有分散在其中的由开孔或细纤维素纤维组成的多孔物质的粉末。
本领域已知的许多方法是基于包括乙烯气体分解剂或催化剂在内的吸收剂。现有的解决方案已经对各种膜、纸和纸板包装解决方案等进行测试。
现有解决方案的一个问题是有限的可用表面积。纳米材料的使用通常需要大量的粘合剂或保留化学品，或者必须通过涂料(涂覆)添加。另一个问题是通常所添加的材料的最大量受到限制，因为其会影响例如所涉及材料的强度或阻隔性质。例如，在聚乙烯塑料中，较高量的吸收剂或载体颗粒会影响强度性质并因此影响材料的可转化性。因此，在维持材料的机械性质的同时可以添加的乙烯清除剂的量通常不足以获得对包装的水果或蔬菜的期望的抗成熟效果。
因此需要改进的包装产品，特别是可以帮助解决与包装的食品的品质劣化有关的问题的产品。
发明内容
出人意料地发现，通过将纳米尺寸的纤维素掺入适合用于包装的材料中，其中所述材料包含乙烯清除剂或乙烯吸收剂，可以克服一些上述问题。
如本文所使用的术语纳米尺寸的纤维素包括微原纤化纤维素(MFC)和纳米晶纤维素。
适合用于包装的材料可以是纸、标签、纸板、塑料或膜或涂料(涂层)。
在本发明的一个实施方案中，将乙烯清除剂或乙烯吸收剂掺入到材料中，即在制造或制备纳米尺寸的纤维素时存在乙烯清除剂或乙烯吸收剂或在形成膜或幅材之前将其与纳米尺寸的纤维素混合。
包含乙烯清除剂和/或乙烯吸收剂和纳米尺寸的纤维素的材料还可以通过涂覆或印刷方法施加，或者每种组分单独或一起施加。
在本发明的另一个实施方案中，通过涂覆或浸渍将乙烯清除剂或乙烯吸收剂掺入到适合用于包装的材料中。
本发明的一个实施方案是在适合用于包装的材料中或材料上使用的涂料，其包含纳米尺寸的纤维素和乙烯清除和/或乙烯吸收剂。涂料通常包含至少1g/m2、优选至少5g/m2、更优选至少10g/m2的乙烯清除剂和/或乙烯吸收剂。
根据本发明的材料通常包含至少1％的纳米尺寸的纤维素，优选至少5％的纳米尺寸的纤维素，更优选至少10％的纳米尺寸的纤维素。
在本发明的一个实施方案中，根据本发明的材料包含0.05至50重量％的乙烯清除剂和/或乙烯吸收剂，优选0.1至20重量％。
还可以用例如无机催化剂通过化学气相沉积或原子层沉积方法来改性纳米尺寸的纤维素。在这种情况下，优选纳米尺寸的纤维素材料具有相对较高的表面积，其可以暴露于无机化学品的沉积。
本发明的一个方面是纸、标签、纸板、塑料或膜产品，其包含、涂覆有或浸渍有纳米尺寸的纤维素和乙烯清除剂或乙烯吸收剂。膜可以由塑料材料、生物聚合物或纤维素或纤维素原纤维、再生纤维素、生物塑料等制成。产品可以是刚性包装产品或柔性包装如袋。
使用根据本发明的材料制备的最终包装可以具有多层根据本发明的所述纸、纸板或膜。这些层可以层压在一起。在本发明的一个实施方案中，乙烯清除剂或乙烯吸收剂以标签的形式存在于最终包装中，其上任选地布置顶部涂层。顶部涂层可以在一侧包含胶粘剂，使得顶部涂层可以被移除，例如被剥离，从而使乙烯清除剂或乙烯吸收剂暴露和活化。所述顶部涂层可能对湿度和/或水分敏感，使得顶部涂层可能在增加的湿度或水分下失去(loose，释放)其气体阻隔性质，从而使乙烯清除剂或乙烯吸收剂暴露和活化。在本发明的一个实施方案中，这可以通过使用包含纳米尺寸的纤维素(如微原纤化纤维素)的顶部涂层来实现。因此，可以首先将乙烯清除剂或乙烯吸收剂包封，但在移除包封物之后，乙烯清除剂或乙烯吸收剂变得暴露和活化。
在本发明的一个实施方案中，适合用于包装的材料具有高表面积以及优选地高乙烯、CO2和O2渗透性，这可以通过使用吸收剂来实现，但也可以通过使用例如醇或脱粘剂或通过使纳米尺寸的纤维素微絮凝来实现。
在本发明的一个实施方案中，适合用于包装的材料是薄的，优选<50gsm(g/m2)，更优选<30gsm。在另一个实施方案中，材料较厚，例如大于50gsm或大于100gsm。
在本发明的一个实施方案中，适合用于包装的材料的气体渗透性>50cm3/m2/天，对于厚度为30μm的膜在50％相对湿度下和在23℃下测定。在一个实施方案中，由OTR值确定的气体渗透性>500，优选>1000。
在本发明的一个实施方案中，适合用于包装的材料具有高含量的乙烯吸收剂，优选>10重量％，更优选>30重量％。
在本发明的一个实施方案中，可以将乙烯清除剂或乙烯吸收剂添加到制造纸、标签或纸板产品的工艺的湿部，或者可以通过表面施胶、浸渍、涂覆或通过印刷添加。或者，可以通过使用原子层沉积(ALD)或化学气相沉积或类似方法来使微原纤化纤维素膜官能化。
在本发明的一个实施方案中，适合用于包装的材料中的纳米尺寸的纤维素，如微原纤化纤维素，应具有SR>70，更优选>80。SR表示Schopper Riegler值，其可以使用本领域已知的方法来实现和测定。
在本发明的一个实施方案中，用于制备适合用于包装的材料的幅材还可以含有长纤维，例如<30％牛皮纸纤维(kraft fiber)或更优选<20％牛皮纸纤维。
在本发明的一个实施方案中，适合用于包装的材料具有高表面积，优选BET>100m2/g，最优选>200m2/g。
具体实施方式
在本发明中使用的乙烯清除剂可以例如选自：高锰酸钾、在木炭上的碘酸或溴酸钾、溴酸钾和硫酸、溴液体、氧化银、稀土氧化物、磷酸盐化合物、氯酸盐化合物、亚铁氰(ferrocyanin)化合物、次氯酸盐(hypochlorite)、次氯酸盐(hypochlorite salt)和溴化物或碘化物盐、氯酸盐、亚氯酸盐、某种金属和金属氧化物、K高锰酸盐、抗坏血酸、柠檬酸钠和水、过氧化物、高锰酸钠(其可能需要载体如沸石)、高碘酸、高锰酸钙或碘酸钾、过氧化锰酸钾、雪硅钙石和银、硬硅钙石和银、硫酸亚铁七水合物和氢氧化钙、溴化碳质分子筛、溴化氢和乙烯基吡啶树脂的溴加合物、溴加成的乙烯基喹啉型树脂、次氯酸钙、次氯酸钠、次氯酸钾和次氯酸镁。起乙烯清除剂作用的催化化学品包括含有硫酸钯催化剂(用于检测)的钼酸铵，掺入乙烯可渗透基底中的缺电子二烯或三烯(具有吸电子取代基的苯、吡啶、二嗪、三嗪或四嗪，优选氟代烷基、砜基和/或酯基，其中酯基是二羧基化或二羧基甲基化的)，疏水性(氢硅烷化)催化剂，具有例如Pt，由CuCl和AlCl3的配位制成的高分子络合物，Ti-、Al-、Ni或Fe-氧化物，钯cpd.，其吸附在炭黑上，金属氧化物例如氧化铝和金属例如铂，环糊精和PEI，用氯化钯处理的活性炭，钯掺杂的Zeolite Socony Mobil(ZSM)-5，或在暴露于光(如UV光或阳光)后获得其乙烯清除性质的光敏剂。
在本发明的一个实施方案中，乙烯清除剂是催化剂或催化化学品，例如含铂或含钯催化剂。
催化剂可以使用本领域已知的方法制备。催化剂可以是催化剂掺杂的沸石的形式或使用除沸石之外的其他吸收剂。催化剂，例如含铂或含钯催化剂还可以在不存在沸石的情况下存在于适合用于包装的材料中。
在本发明的一个实施方案中，乙烯清除剂是含铂或含钯催化剂或由CuCl和/或AlCl3的配位制成的高分子络合物。
在本发明的一个实施方案中，纳米尺寸的纤维素是MFC。
适合用于包装的材料还可以用所谓的流延(cast)方法制造。在有或没有乙烯清除剂或乙烯吸收剂(例如催化剂或其前体)的情况下，将MFC或细纤维素的悬浮液沉积在载体基底上，其为半透性或不可渗透的。然后干燥以制备自立式膜或其中间产品。一种选择是在第二步中通过任何所提及的表面处理步骤添加乙烯清除剂或乙烯吸收剂。流延涂覆还更适合于基于溶剂的方法。
该材料可以进一步用添加剂改性，例如低分子碳水化合物，例如半纤维素山梨糖醇等，其对水和水分敏感，即允许结构溶胀。
本发明的一个方面是微原纤化纤维素膜，其中吸收了催化剂形式的乙烯清除剂，例如含铂或含钯催化剂。
在本发明中使用的乙烯吸收剂可以例如选自木炭、沸石、二氧化硅、改性二氧化硅、氧化铝、硅酸盐、海泡石(sepolite)、蒙脱石、膨润土、travertite或者人造沸石(permutite)、方石英、粘矿(viscid ore)、粘土、珊瑚、菜籽油、碳纤维、长石斑状安山岩、碳纳米颗粒、蛭石、锗、绿坡缕石、石墨、腐殖质、珠光体、砖块、雪硅钙石和有机树脂。
在本发明的一个实施方案中，将乙烯清除剂或乙烯吸收剂掺入到适合用于包装的材料中。在该实施方案中，在制备微原纤化纤维素时存在乙烯清除剂或乙烯吸收剂，或在形成幅材之前将其与微原纤化纤维素混合。该实施方案包括制备包含微原纤化纤维素和乙烯清除剂或乙烯吸收剂的分散体的方法，其中该方法包括以下步骤：提供包含任选地经预处理的纤维素纤维的浆料，向浆料添加乙烯清除剂或乙烯吸收剂，并且通过机械分解处理浆料，从而形成包含微原纤化纤维素的分散体，其中乙烯清除剂或乙烯吸收剂被吸收到微原纤化纤维素的表面。通过机械分解处理包含任选地经预处理的纤维素纤维和乙烯清除剂或乙烯吸收剂的浆料，可以制备稳定的分散体。
机械分解优选在压力均化器中进行。已经表明，通过使用压力均化器，可以制备具有更多敞开区域的微原纤化纤维素，同时以非常有效的方式使分散体的乙烯清除剂或乙烯吸收剂分散。
压力均化器中使用的压力优选在500-4000Bar之间，更优选在1000-2000Bar之间。纤维或中间产品可以在有或没有加工添加剂如稳定剂或乙烯清除剂或其前体的情况下原纤化一次或若干次。
微原纤化纤维素与分散体的乙烯清除剂或乙烯吸收剂之间的重量比优选为10:90至90:10。该比例可以变化，这取决于分散体包含何种微原纤化纤维素和乙烯清除剂或乙烯吸收剂。
优选一定比例的分散体的乙烯清除剂或乙烯吸收剂被吸收在微原纤化纤维素的表面上或其中。
待通过机械分解处理的浆料的干含量优选为纤维的0.05-30重量％。浆料的干含量取决于所使用的乙烯清除剂或乙烯吸收剂，使用何种MFC以及使用何种设备进行机械分解。
通过机械分解处理后的分散体的干含量优选高于纤维的50重量％。优选在机械分解后将分散体脱水以增加干含量。通过增加干含量，可以以更有效的方式将分散体运输到其他位置。此外，已经表明，通过增加分散体的干含量，甚至进一步增加了稳定性。
在一个实施方案中。该方法还可以包括在机械分解之后洗涤分散体。以这种方式，可以从分散体中除去任何游离的乙烯清除剂或乙烯吸收剂。
机械分解可以在许多不同种类的机械处理设备中进行，例如精磨机或研磨机，例如Masuko研磨机或现有技术中公开的用于制造MFC的精磨机或研磨机。然而，优选使用压力均化器，其以非常有效的方式由经预处理的纤维制备微原纤化纤维素纤维，以及潜在地使乙烯清除剂或乙烯吸收剂均化。在机械分解期间使用高压，并且压力优选在500-4000Bar之间，优选在1000-2000Bar之间。最佳压力通常为约1500Bar。所需的压力取决于所处理的材料。然而，太高的压力通常不利于使用，因为设备的磨损太高。具体的压力均化器的一个实例是所谓的微流化器。
在本发明的一个实施方案中，在造纸机中或根据湿法成网制备方法形成基膜，通过将如上所述的悬浮液或分散体提供到丝网上并且将幅材脱水形成中间薄基底或所述基膜。提供包含如上所述的微原纤化纤维素的悬浮液或分散体以形成所述基膜。悬浮液或分散体可以是完全水性的，或者还含有除水之外的其他溶剂，例如醇，例如水和乙醇的共溶剂混合物。
在本发明的一个实施方案中，在根据本发明的材料的制造中使用泡沫形成或泡沫涂覆。
根据一个实施方案，悬浮液或分散体的微原纤化纤维素含量可以为60至99.9重量％，基于悬浮液或分散体的固体重量计。在一个实施方案中，悬浮液或分散体的微原纤化纤维素含量可以为70至99重量％，70至95重量％，或75至90重量％。
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的纳米尺度的纤维素颗粒纤维或原纤维。MFC包括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基础原纤维(初级原纤维)并且直径约为2-4nm(参见例如Chinga-Carrasco,G.,Cellulose fibres,nanofibrils and microfibrils,:Themorphological sequence of MFC components from a plant physiology and fibretechnology point of view,Nanoscale research letters 2011,6:417)，而常见的是聚集形式的基础原纤维(其也被定义为微原纤维)(Fengel,D.,Ultrastructural behaviorof cell wall polysaccharides,Tappi J.,March 1970,Vol 53,No.3.)是在制造MFC时获得的主要产品，例如通过使用延长的精磨过程或压降分解过程制造。取决于来源和制造过程，原纤维的长度可以在约1至大于10微米的范围内变化。粗MFC级可能含有相当大部分的原纤化纤维，即来自管胞(纤维素纤维)的突出原纤维，以及一定量的从管胞(纤维素纤维)释放的原纤维。
MFC有不同的首字母缩略词，例如纤维素微原纤维、原纤化纤维素、纳米原纤化纤维素、原纤维聚集体、纳米级纤维素原纤维、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、微原纤状纤维素、微原纤维聚集体和纤维素微原纤维聚集体。MFC的特征还在于各种物理或物理化学性质，例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。纤维素纤维优选原纤化至这样的程度，即，使得所形成的MFC的最终比表面积为约1至约300m2/g，例如1至200m2/g或更优选50-200m2/g，用BET方法对冷冻干燥的材料进行测定。
存在制造MFC的各种方法，例如单次或多次精磨，预水解然后是精磨或高剪切分解或原纤维的释放。通常需要一个或若干个预处理步骤，以使MFC制造既节能又可持续。因此，待供应的纸浆的纤维素纤维可以进行酶法或化学预处理，例如以降低半纤维素或木质素的量。纤维素纤维可以在原纤化之前进行化学改性，其中纤维素分子含有除了在原始纤维素中所发现的之外的其他(或更多)官能团。这些基团尤其包括羧甲基(CM)、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)。在以上述方法之一进行改性或氧化后，更容易将纤维分解成MFC或纳米原纤状尺寸原纤维。
纳米原纤状纤维素可以含有一些半纤维素；其量取决于植物来源。经预处理的纤维例如水解的、预溶胀的或氧化的纤维素原料的机械分解用合适的设备进行，例如精磨机，研磨机，均化器，胶体排出装置(colloider)，摩擦研磨机，超声波超声仪，流化器如微流化器、宏观流化器或流化剂型均化器。取决于MFC制造方法，产品还可能含有细粒或纳米结晶纤维素或例如在木质纤维或造纸过程中存在的其他化学品。该产品还可能含有各种量的未被有效地原纤化的微米尺寸的纤维颗粒。
MFC由木质纤维素纤维制备，包括硬木或软木纤维两者。其还可以由微生物来源、农业纤维如麦草浆、竹子、甘蔗渣或其他非木质纤维来源制成。其优选由纸浆制成，包括来自原始纤维的纸浆，例如，机械、化学和/或热机械纸浆。其还可以由损纸或再生纸制成。
上述MFC的定义包括但不限于在纤维素纳米原纤维(CMF)上新提出的TAPPI标准W13021，其定义了含有多个基础原纤维的纤维素纳米纤维材料，其具有结晶和无定形区域两者。
根据另一个实施方案，悬浮液或分散体可以包含不同类型的纤维例如微原纤化纤维素和一定量的其他类型的纤维例如牛皮纸纤维、细粒、增强纤维、合成纤维、溶解浆、TMP或CTMP、PGW等的混合物。
悬浮液或分散体还可以包含其他工艺或功能添加剂，例如填料、颜料、湿强度化学品、干强度化学品、助留化学品、交联剂、软化剂或增塑剂、粘合底漆、润湿剂、杀生物剂、光学染料、荧光增白剂、消泡化学品、疏水化学品如AKD、ASA、蜡、树脂等。还可以使用施胶压榨机或印刷机来添加添加剂。
可以用于制造根据本发明的材料的造纸机可以是用于生产纸、纸板、薄纸或类似产品的技术人员已知的任何常规类型的机器。
在将湿幅材放置在丝网上之后，将其脱水。根据一个实施方案，在丝网上的脱水可以通过使用已知技术用单丝网或双丝网系统、无摩擦脱水、膜辅助脱水、真空或超声辅助脱水等来进行。在丝网部分之后，将湿幅材通过机械压榨进一步脱水和干燥，包括靴式压榨、热空气、辐射干燥、对流干燥等。膜还可以通过软或硬辊隙(或各种组合)压延机等干燥或平滑。
根据一个实施方案，湿幅材通过真空脱水，即在将配料放置在丝网上时将水和其他液体从配料中吸出。
鉴于以上对本发明的详细描述，其他修改和变化对于本领域技术人员而言将变得明显。然而，应该清楚的是，可以在不脱离本发明的精神和范围的情况下进行这样的其他修改和变化。

Claims (13)

1.适合用于包装的材料，其包含纳米尺寸的纤维素和乙烯清除和/或乙烯吸收剂。
2.根据权利要求1所述的适合用于包装的材料，其中所述材料是或包括纸、标签、膜或纸板或塑料产品。
3.根据权利要求1或2所述的适合用于包装的材料，其中乙烯清除剂是催化剂，例如含铂或含钯催化剂。
4.根据权利要求1-3中任一项所述的材料，其中所述材料是涂料或印刷在表面上。
5.根据权利要求1-4中任一项所述的材料，其中乙烯清除剂和/或乙烯吸收剂可为经活化的。
6.根据权利要求1-5中任一项所述的材料，其中乙烯清除剂和/或乙烯吸收剂可通过使保护性涂层溶解的水分或湿度的增加而暴露，或通过移除覆盖乙烯清除剂和/或乙烯吸收剂的顶部涂层而暴露。
7.根据权利要求1-6中任一项所述的材料，其中纳米尺寸的纤维素是微原纤化纤维素。
8.制备包含微原纤化纤维素和乙烯清除剂或乙烯吸收剂的分散体的方法，其中该方法包括以下步骤：
a)提供包含纤维素纤维的浆料，其中纤维素纤维已经任选地通过机械处理、酶处理、羧甲基化、TEMPO氧化、CMC接枝、化学溶胀或酸水解进行预处理，
b)向浆料添加乙烯清除剂或乙烯吸收剂，并且通过机械分解处理浆料，从而形成包含微原纤化纤维素的分散体，其中乙烯清除剂或乙烯吸收剂被吸收到微原纤化纤维素的表面。
9.根据权利要求8所述的方法，其中机械分解在均化器中进行。
10.根据权利要求9所述的方法，其中均化器中的压力为500至2000bar。
11.制备适合用于包装的材料的方法，包括使用在权利要求8的步骤b)中获得的分散体形成幅材和将所述幅材脱水和/或干燥的步骤。
12.分散体，其包含微原纤化纤维素和乙烯清除剂或乙烯吸收剂，其中乙烯清除剂或乙烯吸收剂被吸收到微原纤化纤维素的表面。
13.根据权利要求12所述的分散体用于涂覆或浸渍纸、标签、纸板、塑料或膜产品的用途。
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