CN106414572B - 用于制造不含pvc和增塑剂的泡沫装饰片的复合片材及方法 - Google Patents

用于制造不含pvc和增塑剂的泡沫装饰片的复合片材及方法 Download PDF

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CN106414572B
CN106414572B CN201580012220.9A CN201580012220A CN106414572B CN 106414572 B CN106414572 B CN 106414572B CN 201580012220 A CN201580012220 A CN 201580012220A CN 106414572 B CN106414572 B CN 106414572B
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composite sheet
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polyolefin
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CN106414572A (zh
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阿列克谢·艾汀博士
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DG Demans AG
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Abstract

本发明涉及一种包括或由以下部分组成的复合片材：(i)基层；以及(ii)结合至该基层的可发泡层。该可发泡层包含或由以下组分组成：100重量份的具有小于0.1GPa的弹性模量的聚烯烃材料，0.1‑10重量份的发泡剂；以及0‑200重量份的添加剂。该可发泡层具有0.05mm至0.3mm的厚度。本发明还涉及一种使用该复合片材的装饰片的制造工艺。

Description

用于制造不含PVC和增塑剂的泡沫装饰片的复合片材及方法
技术领域
本发明涉及一种用于制造装饰片的复合片材以及该装饰片的相应制造方法。
背景技术
现今广泛使用的装饰片，其由一侧上的具有泡沫增塑聚氯乙烯(PVC)的复合片材和另一侧的纸或非织造材料构成。这些装饰片的应用之一是墙面覆盖材料。由于与基于天然纸张的墙纸相比它们具有耐磨性、可洗性、耐久性以及低成本而非常受欢迎。现有的主流乙烯基墙面覆盖材料生产技术包括三个主要步骤：
1.在纸或非织造片材上涂布一或多层可发泡物
2.在可发泡片材上印刷
3.使片材发泡和进一步处理例如压花、切割、包装等。
发泡非常重要并且是墙面覆盖材料生产的必要组成部分，因为它可以低成本产生较厚的层。该墙面覆盖材料通常通过机械压花或化学压花，以形成花纹和使图案更逼真和更有吸引力。
选择PVC作为材料的主要缺点是PVC的制造会对环境产生负面影响。此外，为达到需要的性能例如强度和韧性，PVC必须与疑似对健康有害且可迁移至室内环境的稳定剂、塑化剂和溶剂混合。此外，PVC回收和燃烧由于盐酸的形成和能量回收低而成问题。
聚烯烃(PO)材料是可行的并且环境友好的PVC替代方案并且能够不含塑化剂和溶剂而使用。聚烯烃材料广泛地用于例如食品包装并且被允许与食品直接接触。此外，它们能够被回收或能够通过燃烧来回收能量。它们能够潜在地提供乙烯基墙面覆盖材料的一些优点而没有乙烯基的生态缺点。
JP 2002096433 A公开了一种具有优秀的耐叠压的阻燃墙纸。该墙纸包括基层、泡沫树脂层和装饰层，其中所述的泡沫树脂层由包含发泡剂的乙烯-醋酸乙烯酯共聚物树脂、无机组分和阻燃剂制成，并且其中乙烯-醋酸乙烯酯共聚物树脂含有20％至22％的醋酸乙烯酯并具有45g/10min至85g/10min的熔体流动速率。
US 5,407,617 A公开了一种制造地板和墙面覆盖材料的工艺，该覆盖材料包括泡沫层。该方法包括以下步骤：在背层上撒粉末混合物，然后使其熔化和变光滑以在该背层上形成平滑层。该粉末混合物包括100份热塑聚合物、0-100份填料以及0.5-7份发泡剂。
关于泡沫装饰片的制造工艺，已知的一个缺点是复合片材出现显著卷曲使得更大规模的生产成为不可能。卷曲是由于不同材料的热膨胀不同而产生并且取决于每层的机械膨胀性能和热膨胀性能以及单层厚度。如，由具有高热膨胀性能的塑料制成的顶层和具有低热膨胀性能的纸或起绒布(fleece)制成的底层这两层组成的复合片材在墙面覆盖材料生产过程中的热-冷循环期间容易卷曲。
并且如本领域中已知的，泡沫墙面覆盖材料的生产中，通常在膨胀之前在可发泡的层压板上进行印刷。这样做是因为在分开的层上进行印刷随后层压将会非常的昂贵，并且以现有的印刷技术在泡沫层上进行印刷是不可行的，这是因为泡沫层不平坦并且基底太厚。
发明内容
本发明的复合片材可克服或至少减少现有技术的前述局限性中的一种或多种。该复合片材包括或由以下部分组成：(i)基层(base layer)和(ii)(直接地)结合至基层的可发泡层(foamable layer)。该可发泡层包括或由以下组分组成：
·100重量份的弹性模量小于0.1GPa的聚烯烃材料；
·0.1-10重量份的发泡剂；以及
·0-200重量份的添加剂。
该可发泡层具有0.05mm至0.3mm的厚度，其大概相当于50g/m2至300g/m2。
不同的多层结构能够潜在地用于该可发泡塑料层。例如在层压情况下，在基底(substrate)和可发泡薄膜之间的层能够不含发泡剂，并且利用回收材料。并且，可发泡层能够由两层——包含回收材料的底层和包含白色染料并适合于印刷的顶部面层组成。
出人意料地，已经发现通过使用一组特定的塑料，能够使卷曲效应最小化并且大规模和连续地生产出不卷曲的用于制造泡沫装饰片的复合片材。
该基层应当具有与可发泡层比更高的尺寸稳定性。该基层具有大于1GPa的弹性模量，在0℃至200℃的温度范围下显示出小于2％的收缩/膨胀，并且具有0.05mm至0.15mm的厚度，其大概相当于50g/m2至150g/m2。由于基层的稳定性，该复合片材在泡沫墙面覆盖材料的制造过程期间的尺寸稳定性被改善。这对于任何印刷工艺都是必要的，因为如果不稳定，泡沫将会在发泡期间在所有三个维度上膨胀，导致印刷对花准确不受控或受控不良。至于具有高弹性模量的尺寸稳定且坚硬的基层以及尺寸不稳定但柔软的可发泡聚烯烃层，能够获得在发泡期间只在Z维度上膨胀的复合片材。
适合用于基层的材料可以是纸或类纸材料、非织造材料即起绒布、织造织物、非织造织物和塑料薄片。优选地，使用纸或起绒布。
该可发泡层具有0.05mm至0.3mm的厚度。它包括或由以下组分组成：聚烯烃材料、发泡剂，以及可选地，添加剂。
聚烯烃是由烯烃或不同烯烃例如乙烯、丙烯、丁烯、戊烯、己烯和辛烯的组合生产的一类聚合物中的任何一种。在此，术语烯烃还包括烯烃与其他不饱和单体例如醋酸乙烯酯的共聚物。聚烯烃由于它们优秀的化学和物理性能以及它们的高性价比最近已被广泛地使用。本发明的聚烯烃优选地具有10000至30000的平均分子量，并且它们的熔化温度应当低于发泡剂的分解温度，优选地在50℃至110℃范围内。
此外，聚烯烃应当具有小于0.1GPa的弹性模量，并且优选地选自热塑性弹性体聚烯烃(又称为热塑性弹性体聚烯烃共混物，TPE-o)、乙烯醋酸乙烯酯共聚物(ethylenevinyl acetate coploymers)、无规立构聚丙烯(atactic polypropylene ploymers)或它们的混合物构成的组。该热塑性弹性体聚烯烃通过本领域已知的方法，例如使用茂金属或其它催化剂将乙烯与丁烯、己烯、辛烯或丙烯的共聚来生产。以此方式，产生了低密度和低结晶度、柔软的聚烯烃。低密度聚烯烃(或极低密度聚烯烃)和热塑性聚烯烃弹性体之间的界限未有明确定义，因为两者都是乙烯的共聚物。然而，只要其弹性模量低于0.1GPa，任何聚烯烃共聚物都能够在本发明中使用。在下面内容中，热塑性聚烯烃弹性体用于表示任何具有0.1GPa以下弹性模量的聚烯烃共聚物。
根据另一个实施例，包括弹性模量大于0.1GPa聚烯烃的聚烯烃共混物可以用作所述聚烯烃材料，例如只要聚烯烃共混物的总弹性模量小于0.1GPa，如LDPE(低密度聚烯烃)、HDPE(高密度聚烯烃)和PP(聚丙烯)，可以被使用。因此，所述聚烯烃材料可以是包括弹性模量大于0.1GPa的聚烯烃和弹性模量小于0.1GPa聚烯烃的聚烯烃共混物，致使聚烯烃共混物的总弹性模量小于0.1GPa。
弹性模量是对物体或物质在被作用一个力时弹性(即，非永久地)变形的趋势的数学描述。物体的弹性模量被定义为其弹性变形范围中的应力应变曲线的斜率[阿斯克兰德，唐纳德·R.，符勒，普拉迪普·P.(2006)，材料自然科学与工程学(第五版)，圣智学习(Thescience and engineering of materials(5th ed.),Cengage Learning)，第198页]。
热塑性弹性体(TPE)是具有热塑性能和弹性性能(也被定义为包括热可逆网状物(thermo-reversible network)的弹性体)的共聚物或聚合物的混合物，通常地是塑料和橡胶。具体地，所述聚烯烃材料可以是聚烯烃共混物(TPE-o)。可混合的橡胶是天然橡胶、乙烯-丙烯橡胶、丁基橡胶、聚异丁烯、聚丁二烯、苯乙烯/丁二烯橡胶等。
优选地，聚烯烃是密度小于0.96g/cm3的低密度聚烯烃，更优选地密度小于0.90g/cm3。此外，聚烯烃可以具有小于40％的结晶度，更优选地具有小于25％的结晶度。
如本文所用，术语“发泡剂”指的是室温下是液体或固体，具有比聚烯烃(或聚烯烃共混物中的至少一种化合物)的熔化温度更高的分解温度，并且在被加热至高于该分解温度的温度时分解同时释放出气体例如氮气、二氧化碳、氨气的可热分解剂(heat-decomposable agent)。该发泡剂可以选自偶氮二酰胺(azodicarbonamide)和/或其金属盐、联二脲(hydrazodicarbonamide)、碳酸氢钠、三肼基均三嗪(trihydrazino-sym-triazine)、pp'-氧代双苯磺酰肼(pp'-oxybis-benzenesulfonylhydrazide)、二亚硝基五次甲基四胺(dinitroso-pentamethylene-tetramine)、偶氮二异丁腈(azobisisbutyl-ordinitrile)、对甲苯磺酰肼(p-toluenesulfonylhydrazide)和二苯磺酰肼醚(bisbenzenesulfonyl hydrazide)构成的组。优选地，使用偶氮二酰胺或碳酸氢钠。
发泡剂的量能够根据所需的膨胀系数来确定。在形成可发泡层的组合物中发泡剂的优选量是在1至5重量份范围内。
发泡剂的分解温度优选地在120℃至200℃范围内。
除所述聚烯烃材料和发泡剂外，可发泡层还可以包括添加剂。如本文中所用，术语“添加剂”指的是为了实现可发泡层的某些性能而被加入到可发泡层中的物质。这些添加剂可以具有迥然不同的性质。适用的添加剂是催化剂、染料、填料(filler)、消光剂(mattingagent)、微生物菌剂(microbial agent)、紫外稳定剂、阻燃剂和释放化合物。
例如，为了降低发泡剂的分解温度，如本领域已知的可添加催化剂。这种催化剂可以选自氧化锌、蓖麻酸钡(barium ricinoleate)、甲氧基马来酸锡(tin methoxymaleate)、水合硅酸钙、硬脂酸钙、硬脂酸锌、乙酸铅、月桂酸锌、辛酸锌和戊基亚磷酸镉构成的组。
为了降低聚烯烃材料尤其是热塑性弹性体聚烯烃的热膨胀系数，可添加热膨胀远远低于聚合物的添加剂如填料，例如矿物填料(比如，交谈或白垩)。
添加剂的总量应当是0至200重量份，优选地是50至80重量份。
本发明还指向一种泡沫装饰片，尤其是泡沫墙面覆盖材料的制造方法。该方法包括以下步骤：
(a)提供如上所述的复合片材；
(b)可选地，在该复合片材上进行印刷；以及
(c)该复合片材的发泡。
根据步骤(a)，提供本发明的包括基层和可发泡层的复合片材。该可发泡层可以通过本领域中不同的已知方法来制造。一种可能性是其单一化合物混合并且通过砑辊机、压片机等形成片材。然后，该薄膜可以通过熔化或化学层压被直接地连接至基层。
在可发泡层连接到基层上后，可视需要进行本领域中已知的附加处理，例如交联、着色、表面处理等。为了改善薄膜发泡，如本领域中已知的需要足够的熔体强度。交联能够被用来提高熔体强度。交联能够通过使用例如电离辐射或通过使用交联剂来实现。优选地，使用电离辐射的交联通过具有100-300kV电压和10-200kGy剂量，优选地10-100kGy剂量的电子束来进行。应用本领域中已知的在低电压和高电压运行的两种不同电子束来改善泡沫表面结构。
可替换地，交联能够采用在高温时分解成自由基的交联剂来完成。交联剂的具体示例是包含各种种类例如过氧化二异丙苯、烷基过氧化物、过氧化二叔丁基和芳烷基过氧化物的有机过氧化物。
复合片材的着色能够通过印刷方法例如凹版印刷、柔性版印刷、丝网印刷或喷墨印刷来实现(步骤(b))。
其他的表面处理能够通过例如冠状处理方法(coronary treatment)来实现。
在步骤(c)中，该复合片材发泡来形成泡沫装饰片，分别地形成泡沫墙面覆盖材料。步骤(c)中的温度优选地根据使用的发泡剂和催化剂在120℃至210℃范围内。
在发泡后，泡沫片能够如本领域已知的通过结构化的冷轧辊进行机械压花或使用抑制剂系统来进行化学压花。
该复合片材能够以0.5m至3.0m的宽度进行连续生产。
附图说明
现根据实施例和附图对本发明进行描述：
图1是层压板的卷曲示意图；
图2是示出三种复合片材的卷曲照片，其中一种复合片材(左)具有由弹性模量小于0.1GPa的聚烯烃材料制成的可发泡层，另外两种复合片材具有由弹性模量大于0.1GPa的聚烯烃材料制成的可发泡层；
图3是泡沫横截面的显微镜视图，A：具有小于0.1GPa的弹性模量的可发泡层，B：增塑的PVC复合片材；
图4是压花泡沫的照片，A：具有小于0.1GPa的弹性模量的可发泡层，B：增塑的PVC复合片材。
具体实施方式
将根据示例性实施例对本发明进行描述。
使用包括基层和直接地结合至该基层的可发泡层的复合片材来生产墙面覆盖材料的主要问题是卷曲。具体地，当出现显著卷曲时，生产具有0.5m至3.0m宽度的墙面覆盖材料几乎不可能。原理上，该效应是基于基层和可发泡层的不同膨胀性能。众所周知，塑料具有高热膨胀率，此外，一旦冷却就会发生的结晶化进一步增加收缩。然而，加热是墙面覆盖材料生产中不可避免的过程，例如在基层上涂覆可发泡层期间、在顶部墨层印刷后或在加热通道中发泡时。在后续冷却阶段中，顶部聚烯烃层相比基层可能收缩更多。在那种情况中，出现如图1中所示的卷曲。
参考图1，附图标记10表示具有高热膨胀/收缩性能的可发泡层，附图标记12表示具有低热膨胀/收缩性能的基层。X表示在冷却阶段期间出现的卷曲。
根据层压体热应力的公知理论，该卷曲取决于每层的机械性能和热性能以及厚度。在知名的由两层(图1具有顶层10和底层12)构成的层合梁的铁木辛柯(Timoshenko)分析解中，该梁在温度T0时没有卷曲，当温度变为T时，该梁曲率为kb：
其中m＝t1/t2，弹性模量比n＝E1/E2，总厚度h＝t1+t2，温度变化ΔT＝T-T0，以及热系数失配Δα＝α2-α1。
方程能够用于研究曲率半径以及基于此的卷曲与薄膜厚度、每层的弹性模量、热膨胀系数等的关系。当弹性模量比E1/E2小于0.05时，曲率半径和卷曲随着E1/E2比的降低而急剧减小，因此需要具有小于0.1GPa的弹性模量的柔软顶层。标准聚烯烃例如LDPE和HDPE(高密度聚烯烃)或PP(聚丙烯)甚至具有更高的模量(>1GPa)，因而卷曲更厉害。因此，用标准聚烯烃，几乎不可能得到需要的涂覆厚度而不卷曲。
然而，通过使用特定组的软塑料，能够使卷曲效应最小化和生产不卷曲的层压板。该组软塑料包括热塑性弹性体聚烯烃、乙烯醋酸乙烯共聚物、无规立构聚丙烯或它们的模量小于0.1GPa的混合物。
不同的复合片材已通过在如下的基层上(直接地)熔化处理可发泡层来制造：
该基层片材由纸或非织造材料制成，具有0.1mm的厚度、大于1GPa的弹性模量以及在高达220℃时小于2％的收缩/膨胀。
实施例1
所述可发泡层由具有小于0.1GPa的弹性模量的聚烯烃材料制成。该可发泡层的组分在140℃、60RPM下混合。然后，该可发泡层在140℃下被层压在纸上。
更具体地，该可发泡层由以下组分组成：
乙烯-辛烯共聚物，熔体流动指数5，模量0.011GPa 100重量份
偶氮二甲酰胺 5重量份
ZnO 1重量份
该层具有0.15mm的厚度并且良好地附着至基底。在冷却至室温后未出现卷曲。
对比例1
可发泡层由以下组分组成：
LDPE，熔体流动指数10，模数0.32GPa 100重量份
偶氮二甲酰胺 5重量份
ZnO 1重量份
该层具有0.15mm的厚度并且良好地附着至基底。在冷却至室温后出现一些卷曲。
对比例2
可发泡层由以下组分组成：
HDPE，熔体流动指数3，模数1.5GPa 100重量份
偶氮二甲酰胺 5重量份
ZnO 1重量份
该层具有0.15mm的厚度并且良好地附着至基底。
在冷却至室温后出现显著卷曲。
图2示出了根据如上描述制造的三种不同复合片材。实施例1的具有由弹性模量小于0.1GPa的聚烯烃材料制成的可发泡层的复合片材未表现卷曲(左)。为了对比，制造了两种具有由弹性模量大于0.1GPa的聚烯烃材料制成的可发泡层的复合片材(对比例1和对比例2)。与左侧无卷曲的复合片材形成对比的是，这两种对比片材都显示出典型的卷曲(在图2中部的对比例1的中度卷曲以及图2右侧的对比例2的极度卷曲)。
实施例1及对比例1、2表明，为了获得不卷曲的复合片材，顶层必须由具有小于0.1GPa的弹性模量并且热膨胀系数尽可能低的软塑料制成。
上述的样品通过160kV、10mA和20-100kGy的变化剂量的电子束辐射进行交联，并且在225℃进行发泡。所有样品表现发泡。
实施例2
所述可发泡层由以下组分组成：
乙烯-辛烯共聚物，熔体流动指数5，模数0.011GPa 100重量份
碳酸钙 60重量份
活化的偶氮二甲酰胺 5重量份
二氧化钛 10重量份
过氧化二异丙苯 1重量份
层厚约0.15mm。在下一步骤中，该层被层压到基层上并且在170℃交联1分钟。该层在实验室凹版印刷机上以适用于聚烯烃表面的水基墨进行印刷并且在对流炉中在205℃发泡1分钟。图3示出了与用于墙面覆盖材料的基于PVC的泡沫(B)相比，展现了良好发泡的包括小于0.1GPa的可发泡层的复合片材(A)。
实施例3
所述可发泡层由以下组分组成：
乙烯-辛烯共聚物，熔体流动指数17，模数0.06GPa 100重量份
LDPE，熔体流动指数10，模数0.32GPa 10重量份
碳酸钙 60重量份
偶氮二甲酰胺 5重量份
氧化锌 1重量份
该层具有0.2mm厚度被层压到0.1mm的非织造材料上，并且在对流炉中在215℃发泡1分钟。之后在约140℃进行热压花。图4示出了与PVC复合片材(B)相比，包括小于0.1GPa的可发泡层的复合片材(A)的压花结构。

Claims (8)

1.一种用于装饰墙面覆盖材料的复合片材，其包括或由以下部分组成：
(i) 基层，所述基层选自纸、类纸材料、非织造材料、织造织物、非织造织物和塑料薄片构成的组；以及
(ii)可发泡层，其结合至所述基层并且包含或由以下组分组成：
100重量份的具有小于0.1GPa的室温下的弹性模量的聚烯烃材料；
0.1-10重量份的发泡剂；以及
0-200重量份的添加剂；
其中所述可发泡层具有0.05mm至0.3mm的厚度；
所述可发泡层与所述基层在室温下的弹性模量之比小于0.05。
2.根据权利要求1所述的复合片材，其特征在于，所述聚烯烃材料选自包括以下项的组：热塑性弹性体聚烯烃、乙烯醋酸乙烯酯共聚物、无规立构聚丙烯或它们的混合物构成的组。
3.根据权利要求1或2所述的复合片材，其特征在于，所述发泡剂选自偶氮二酰胺和/或其金属盐、联二脲、碳酸氢钠、三肼基均三嗪、pp'-氧代双苯磺酰肼、二亚硝基五次甲基四胺、偶氮二异丁腈、对甲苯磺酰肼和二苯磺酰肼醚构成的组。
4.根据权利要求1或2所述的复合片材，其特征在于，所述添加剂选自催化剂、染料、填料、消光剂、微生物菌剂、紫外稳定剂和阻燃剂构成的组。
5.根据权利要求4所述的复合片材，其特征在于，所述添加剂包括催化剂，并且所述催化剂选自氧化锌、蓖麻酸钡、甲氧基马来酸锡、水合硅酸钙、硬脂酸钙、硬脂酸锌、乙酸铅、月桂酸锌、辛酸锌和戊基亚磷酸镉构成的组。
6.根据权利要求1所述的复合片材，其特征在于，所述聚烯烃材料是聚烯烃共混物，所述聚烯烃共混物包括室温下的弹性模数弹性模量大于0.1GPa的聚烯烃和室温下的弹性模数弹性模量小于0.1GPa的聚烯烃，使所述聚烯烃共混物的室温下的总弹性模数弹性模量小于0.1GPa。
7.一种用于生产泡沫装饰片的方法，包括以下步骤：
(a)提供如前述权利要求中任一项所述的复合片材；
(b)可选地，在所述复合片材上进行印刷；以及
(c)所述复合片材的发泡。
8.一种装饰片，其由权利要求7的所述方法生产。
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