CN108202517A - 多层膜 - Google Patents

多层膜 Download PDF

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Publication number
CN108202517A
CN108202517A CN201611176087.3A CN201611176087A CN108202517A CN 108202517 A CN108202517 A CN 108202517A CN 201611176087 A CN201611176087 A CN 201611176087A CN 108202517 A CN108202517 A CN 108202517A
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China
Prior art keywords
eva
sealant
total weight
10min
multilayer films
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CN201611176087.3A
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Inventor
樊玲
J·西拉乔瓦
B·埃施彻特范登
周军
宫峰
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SABIC Global Technologies BV
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SABIC Global Technologies BV
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Priority to CN201611176087.3A priority Critical patent/CN108202517A/zh
Priority to US16/462,723 priority patent/US20200079060A1/en
Priority to CN201780072713.0A priority patent/CN110023075A/zh
Priority to PCT/CN2017/111119 priority patent/WO2018113455A1/en
Priority to EP17884477.5A priority patent/EP3554824A4/en
Publication of CN108202517A publication Critical patent/CN108202517A/zh
Pending legal-status Critical Current

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    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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Abstract

本发明涉及用于密封剥离应用的多层膜、包括所述膜的制品和所述膜的用途。

Description

多层膜
本发明涉及用于密封剥离应用的多层膜、包括所述膜的制品和所述膜的用途。
用于密封剥离应用的膜为可热密封膜，所述膜可热密封至自身或者至基材，所述膜具有有限的剥离强度，从而易于沿着密封处打开。
用于包装领域、尤其是食品包装领域的可热密封膜通常可容易地沿着密封处剥离，以便被除去或允许打开包装。在这种情况下，剥离强度应该对应于对消费者友好的打开力。
为了实现这一点，已经提出了聚烯烃材料的可热密封膜，其通常包含支撑层和密封层。这样的膜通常称为密封剥离膜或用于密封剥离和/或易开应用的膜。例如由US20020013415已知这样的膜。
但尽管本领域中有在先研究，仍一直需要具有改进特性的膜，尤其是在不同基材、特别是极性基材如聚对苯二甲酸乙二醇酯(PET)基材上的改进的粘附和/或宽的密封温度范围和/或低的密封温度。
因此，本发明的目的是提供用于密封剥离应用的多层膜，所述膜在热密封时，尤其是在极性基材如PET基材上具有良好的粘附性和/或宽的密封温度范围和/或低的密封温度。
该目的通过多层膜来实现，所述膜包括至少两个层，即覆盖层和密封层，其中密封层基于其总重量包含25-80wt.％的EVA和20-75wt.％的LLDPE或由它们组成，其中EVA包括第一EVA和第二EVA。含有两种不同的EVA由此可有助于具有较宽的密封温度范围和/或允许关于所述密封温度范围更大的灵活性和/或低的密封温度，所述密封温度优选80-150℃，进一步优选80-120℃，进一步优选80-100℃或90-110℃。
由此，密封温度范围为可实现在PET基材上热密封以获得密封强度的温度范围，尤其是例如采用15mm的带材宽度和200mm/min的分离速率，所述密封强度为例如通过ASTMF88方法C测定的2.2-9N/15mm，优选2.5-8.5N/15mm，进一步优选2.7-8N/15mm。标准测试条件ASTM F88方法C如下：停留时间为1.5秒，压力为4bar，密封条尺寸的宽度和长度为10mm*150mm，分离速率为200mm/min，密封温度可为例如80-150℃，优选在80℃和/或90℃和/或110℃和/或130℃和/或150℃。
由此，本发明可特别允许使用相对低的密封温度、尤其是例如80-90℃、优选80℃/或90℃的密封温度来实现较高的剥离强度(优选如上文所述进行测定)，优选例如>2N/15mm。
由此，第一EVA和第二EVA可通过它们的至少一种特性、尤其是例如它们的乙酸乙烯酯含量和/或它们的熔体流动速率(MFR)来区别。MFR的差异可为例如最高值的至少25％，进一步优选至少30％。乙酸乙烯酯含量的差异可为例如至少10wt.％，优选至少20wt.％，进一步优选至少25wt.％，进一步优选至少30wt.％，进一步优选至少35wt.％，进一步优选至少40wt.％。这可进一步有助于加宽密封温度范围。
第一或第二EVA中一个的乙酸乙烯酯含量可低于20wt.％，优选低于15wt.％，进一步优选低于10wt.％，而第一或第二EVA中另一个的乙酸乙烯酯含量可高于20wt.％，优选高于25wt.％，进一步优选高于30wt.％，进一步优选高于40wt.％，基于各EVA的总重量。这可进一步有助于加宽密封温度范围。
此外，具有最高乙酸乙烯酯含量和/或第一和第二EVA的最高熔体流动速率的EVA在密封层中的存在量可为30-58wt.％，优选37-50wt.％，基于密封层的总重量和/或基于密封层中EVA的总重量。这可进一步有助于加宽密封温度范围和/或增加剥离强度，尤其是在较低温度下，例如在80-90℃的温度下。
此外，具有最低乙酸乙烯酯含量和/或第一和第二EVA的最低熔体流动速率的EVA在密封层中的存在量可为2-15wt.％，优选3-10wt.％，基于密封层的总重量和/或基于密封层中EVA的总重量。这可进一步有助于加宽密封温度范围和/或增加剥离强度，尤其是在较低温度下，例如在80-90℃的温度下。
线型低密度聚乙烯(LLDPE)可为乙烯和至少一种α-烯烃的共聚物，所述α-烯烃例如1-丁烯、1-戊烯、1-己烯、1-辛烯或4-甲基戊烯-1，最优选1-丁烯、1-己烯或1-辛烯。乙烯共聚物可尤其为聚烯烃塑性体或聚烯烃弹性体。优选地，LLDPE的α-烯烃共聚单体的存在量例如可为乙烯-α烯烃共聚物的约1-约25，优选5-约20wt.％，更优选为约7-约15wt.％。如本文所用的LLDPE可例如使用金属茂和/或Ziegler-Natta催化剂来生产。
优选地，本发明的LLDPE的密度在0.850和<0.945g/cm3之间，更优选0.900-0.935g/cm3，进一步优选0.915-0.927g/cm3。出于本发明的目的，使用ISO1872-2来确定LLDPE的密度。
优选地，LLDPE的熔体流动指数为0.3-15g/10min，1-10g/10min，例如2-6g/10min，例如2.5-3.7g/10min。出于本发明的目的，这里使用ISO1133:2011(190℃/2.16kg)确定熔体流动指数。
线型低密度聚乙烯在密封层中的量基于所述层总重量可优选为20-75wt.％、25-70wt.％或45-60wt.％。
乙烯乙酸乙烯酯(EVA)为乙烯和乙酸乙烯酯的共聚物。
优选地，EVA的熔体流动指数为1-35g/10min，例如2-30g/10min，例如1.5-20g/10min，例如1.5-4g/10min或10-20g/10min。出于本发明的目的，这里使用ASTM-D1238(190℃/2.16kg)确定EVA的熔体流动指数。
优选地，本发明的EVA的密度为0.900-0.999g/cm3，更优选0.910-0.965g/cm3，进一步优选0.920-0.960g/cm3。出于本发明的目的，使用ISO1183确定EVA的密度。
EVA的乙酸乙烯酯含量可为例如4-50wt.％，优选8-45wt.％，进一步优选10-40wt.％，进一步优选15-35wt.％。这可有助于在极性基材如PET基材上的良好粘附性。
EVA在密封层中的量基于所述层总重量可优选为25-80wt.％、30-75wt.％或30-49wt.％。这可有助于在极性基材如PET基材上的良好粘附性。
本发明的多层膜可包括至少一个、优选只有一个密封层。
本发明的多层膜可包括至少一个、优选至少两个、进一步优选至少三个，进一步优选至少四个、进一步优选至少五个覆盖层。
密封层可优选由基于所述层总重量25-80wt.％的EVA和20-75wt.％的LLDPE组成可能意味着密封层可优选不包括任何另外的聚合物和/或可不包括任何另外的聚烯烃和/或可不包括任何LDPE。
优选地，当密封层的EVA含量为<50wt.％时，EVA的乙酸乙烯酯含量可为>20wt.％。替代地，当密封层的EVA含量为>50wt.％时，EVA的乙酸乙烯酯含量可为<20wt.％。这可有助于在极性基材如PET基材上的良好粘附性。
本发明多层膜的密封层可优选例如包含仅一种LLDPE和/或不包含两种或更多种例如密度和/或MFR不同的不同LLDPE。
本发明多层膜的密封层可优选例如包含仅一种EVA和/或不包含两种或更多种例如乙酸乙烯酯含量和/或MFR不同的不同EVA。
本发明的多层膜可包括设置在密封层上且与密封层接触的第一LDPE覆盖层和设置在所述LDPE覆盖层上且与其接触的LLDPE和LDPE的共混物的第二覆盖层。
本发明的多层膜可包括设置在密封层上且与密封层接触的第一LDPE覆盖层，设置在所述LDPE覆盖层上且与其接触的LLDPE和LDPE的共混物的第二覆盖层，设置在所述LLDPE/LDPE共混物覆盖层上且与其接触的第三粘合剂覆盖层和设置在所述粘合剂覆盖层上且与其接触的第四尼龙覆盖层。由此，密封层和尼龙覆盖层代表最外层。
LDPE、HDPE和LLDPE的生产方法汇总于Handbook of Polyethylene by AndrewPeacock(2000；Dekker；ISBN 0824795466)第43-66页。催化剂可以分为三个不同的子类，包括Ziegler Natta催化剂、Phillips催化剂和单位点催化剂。后一类是不同类化合物的家族，金属茂催化剂为其中之一。如在所述Handbook的第53-54页所阐述的，Ziegler-Natta催化的聚合物经由第l-lll族金属的有机金属化合物或氢化物与第IV-VIII族过渡金属的衍生物相互作用而获得。(改性)Ziegler-Natta催化剂的例子为基于四氯化钛和有机金属化合物三乙基铝的催化剂。金属茂催化剂和Ziegler Natta催化剂之间的差别在于活性位点的分布。Ziegler Natta催化剂为多相的和具有多个活性位点。因此使用这些不同催化剂生产的聚合物在例如分子量分布和共聚单体分布方面是不同的。
适合于LLDPE生产的技术包括但不限于气相流化床聚合、溶液聚合和浆液聚合。
优选地，低密度聚乙烯(LDPE)的密度为0.915-0.932g/cm3，进一步优选例如0.917-0.926g/cm3。优选地，使用ISO1133:2011(190℃/2.16kg)确定的熔体流动指数为0.01-4g/10min，例如0.09-3g/10min，例如0.1-1g/10min，例如0.2-0.6g/10min。
本发明膜中应用的LDPE可使用釜式高压技术和管状反应器技术来生产。
优选地，HDPE的密度为0.940-0.965g/cm3。优选地，使用ISO1133:2011(190℃/2.16kg)确定的熔体流动指数为0.1-4g/10min，例如0.3-3g/10min，例如0.2-2g/10min，例如0.5-1.5g/10min。
本发明密封层的组分可优选合计达密封层的100wt.％。
本发明多层膜的厚度可为例如15-200μm，例如50-150μm，尤其是例如60-125μm。本发明多层膜的所有层不需要具有相同的厚度。例如，多层膜中的一个或多个层可比其它层更厚，尤其是例如为增加生产方法的稳定性。每个层或所有层可具有例如10-23μm、优选15-25μm的厚度。
例如，本发明多层膜的每个层可包含的添加剂量基于所述层总重量为0-10wt.％，尤其是例如0-8wt.％，其中聚合物和添加剂的总和为100wt.％，基于所述层总重量。
由此，添加剂可尤其例如为UV稳定剂、抗静电剂、滑动剂/抗粘连剂、用作聚合物处理助剂的氟弹性体和/或它们中两种或更多种的混合物。尤其是例如芥酸酰胺和/或油酸酰胺和/或二氧化硅和/或滑石。
每个层可还包含适合量的其它添加剂，例如填料、抗氧化剂、颜料和聚合物，这取决于多层膜的具体用途。通常，添加剂在层中的存在量基于所述层可为10-10000ppm，例如100-5000ppm。因此，本发明还涉及多层膜，其中一个或多个层还包含一种或多种添加剂或其它添加剂。
本发明的多层膜对PET的剥离强度可为例如1-20N/15mm，优选1.5-15N/15mm，进一步优选1.5-8.5N/15mm，进一步优选3-8N/15mm或3-6N/15mm，尤其优选2.2-9N/15mm，进一步优选2.5-8.5N/15mm，进一步优选2.7-8N/15mm，尤其是例如密封温度为80-150℃，优选在80℃/或90℃/或100℃/或110℃/或130℃/或150℃下。这可有助于实现充分易开。
剥离强度可根据ASTM F88方法C对作为基材的PET进行测量，其中使用15mm的带材宽度、200mm/min的分离速率和80-150℃、优选90-150℃的密封温度，其中使样品在测量之前冷却至少72h。标准测试条件如下：停留时间为1.5秒，压力为4bar，密封条尺寸的宽度和长度为10mm*150mm，分离速率为200mm/min，密封温度为80-150℃，优选80℃和/或90℃和/或110℃和/或130℃和/或150℃。
密封层可优选通过例如在120-200℃、优选155-180℃、进一步优选155-165℃或170-180℃的温度下熔融共混LLDPE和EVA获得。由此在较低温度下熔融共混密封层的LLDPE和EVA可有助于改进剥离强度。
本发明还涉及包括本发明的多层膜的制品和/或包装。
此外，本发明还涉及本发明的多层膜用于食品包装应用的用途。
另外注意的是，本发明涉及本文所描述的特征的所有可能组合，特别优选权利要求中存在的那些特征组合。
另外注意的是，术语“包含”或“包括”不排除其它要素的存在。但还要理解的是，对包含某些组分的产品的描述还公开了由这些组分组成的产品。
现在，本发明通过以下的实施例进行进一步解释。
实施例
如下表1所示，密封层在来自W&P的ZSK-26MC双螺杆挤出机中配混。对于NT和LT条件，最大挤出温度分别为170和160℃。类似地，同样对于NT和LT条件，熔体温度分别为175℃和162℃，螺杆速度分别为300rpm和250rpm。在NT和LT条件中，输出均为15kg/小时。
表1
参数 UOM *NT *LT
进料(区域0)温度 ℃ 50 50
区域1温度 ℃ 100 100
区域2温度 ℃ 130 130
区域3温度 ℃ 140 130
区域4温度 ℃ 150 130
区域5温度 ℃ 160 125
区域6温度 ℃ 160 125
区域7温度 ℃ 160 125
区域8温度 ℃ 160 115
区域9温度 ℃ 160 110
区域10温度 ℃ 160 100
模头温度 ℃ 170 160
螺杆速度 rpm 300 250
通量 kg/hr 15 15
熔体温度 ％ 175 162
用于配混的正常温度条件(NT)和较低温度条件(LT)记录在上表1中。
五个不同的密封层1、2、3a、3b和4使用下表2中所列组合物获得。1、2、3a和3b作为对比，而4为本发明。
表2
作为EVA，使用三种Dupont等级ELVAX460、LEVAMELT450和EVAFLEX EV250(Dupont-Mitsui)。此外，来自Lanxess的LEVAMELT 450也可以用作EVA。所使用的EVA列在下表5中。作为LLDPE，使用SABIC等级6318BE。使用记录在上表1中的较低温度(LT)配混条件生产密封层3b。
化合物的熔体流动指数可使用ASTM-D1238(190℃/2.16KG)确定。
3层膜在Labtech，LF400COEX多层吹膜挤出机上生产，如下表3所示，BUR为2，模隙为2.0，总厚度为50微米。
将包含30wt.％的SABIC等级2201H0W的低密度聚乙烯和70wt.％的SABIC等级6118NSF的线型低密度聚乙烯的第二覆盖层设置为与第一覆盖层接触。SABIC等级2201H0W的低密度聚乙烯的第一覆盖层设置为与密封层接触。
第二覆盖层、第一覆盖层和密封层的厚度分别为17.5微米、17.5微米和15微米。第二覆盖层、第一覆盖层和密封层的挤出温度分别为210℃、210℃和175℃。
表3
在使用在3层膜上提供的CTP-2000K等离子体发生器进行电晕处理后，使用来自Simeile的FM380层压机，使用粘合剂物质即Liofol LA2788将上述3层膜层压为15微米双轴取向尼龙膜。涂层重量为2.85g/m2。
表4给出了对于不同密封温度使用具有不同密封层1、2、3a和3b(参见表2)的上述3层膜(参见表3)获得的剥离强度，以N/15mm计。
表4：剥离强度(N/15mm)
密封温度 80℃ 90℃ 110℃ 130℃ 150℃
密封层No.1 1.99 1.76 6.43 8.11 10.86
密封层No.2 0.79 3.68 4.50 3.50 4.92
密封层No.3a 0.91 1.93 3.52 3.00 4.10
密封层No.3b 0.43 0.72 5.60 4.60 6.14
密封层No.4 2.81 4.01 5.72 5.00 7.07
剥离强度根据ASTM F88方法C进行测量，在室温下保持72小时后，所述膜利用来自Brugger的HSG-C密封机密封至带材宽度为15mm的250微米PET膜上。标准测试条件如下：停留时间为1.5秒，压力为4bar，密封条尺寸的宽度和长度为10mm*150mm，密封温度为80-150℃，分离速率为200mm/min。由上可见，可达到在PET基材上热密封的密封温度范围，以达到采用15mm的带材宽度和200mm/min的分离速率的密封强度为2.5-8N/15mm，优选2.7-8N/15mm，所述密封强度通过ASTM F88方法C测定。与作为对比例的密封层1、2、3a和3b相比，本发明的密封层4使所述密封温度范围变宽。特别地，使用80-90℃的密封温度，优选使用80℃/或90℃的密封温度，可实现较高的剥离强度。
表5：所使用的EVA
等级 供应商 MI VA含量(wt.％) 密度
ELVAX460 Dupont 2.5 18 0.941
EVAFLEX EV250 Dupont-Mitsui 15 28 0.950
LEVAMELT 450 Lanxess 3 45 0.99
ELVAX 760A Dupont 2 9.3 0.93

Claims (15)

1.用于密封剥离应用的多层膜，其包括至少两个层，即覆盖层和密封层，其中密封层基于其总重量包括25-80wt.％的EVA和20-75wt.％的LLDPE，其中EVA包括第一EVA和第二EVA。
2.权利要求1所述的多层膜，其中LLDPE的密度在0.850和<0.945g/cm3之间，更优选0.900-0.935g/cm3，进一步优选0.915-0.927g/cm3。
3.权利要求1或2所述的多层膜，其中LLDPE的熔体流动指数为0.3-15g/10min，1-10g/10min，优选2-6g/10min，进一步优选2.5-3.5g/10min。
4.权利要求1-3任一项所述的多层膜，其中LLDPE在密封层中的量基于所述层总重量为20-75wt.％，优选基于所述层总重量为25-70wt.％或基于所述层总重量为51-70wt.％。
5.权利要求1-4任一项所述的多层膜，其中EVA在密封层中的量基于所述层总重量为25-80wt.％，优选基于所述层总重量为30-75wt.％或基于所述层总重量为30-49wt.％。
6.权利要求1-5任一项所述的多层膜，其中EVA的熔体流动指数为1-35g/10min，例如2-30g/10min，例如2-20g/10min，例如2-3g/10min或10-20g/10min。
7.权利要求1-6任一项所述的多层膜，其中EVA的乙酸乙烯酯含量可以为例如4-50wt.％，优选8-45wt.％，进一步优选10-40wt.％，进一步优选15-35wt.％。
8.权利要求1-7任一项所述的多层膜，其中第一或第二EVA中一个的乙酸乙烯酯含量低于20wt.％，优选低于15wt.％，进一步优选低于10wt.％，而第一或第二EVA中另一个的乙酸乙烯酯含量可高于20wt.％，优选高于25wt.％，进一步优选高于30wt.％，进一步优选高于40wt.％，基于各EVA的总重量。
9.权利要求1-8任一项所述的多层膜，其中密封层由25-80wt.％的EVA和20-75wt.％的LLDPE组成，基于所述层的总重量。
10.权利要求1-9任一项所述的多层膜，其中当密封层的EVA含量为<50wt.％时，EVA的乙酸乙烯酯含量可为>20wt.％，或当密封层的EVA含量为>50wt.％时，EVA的乙酸乙烯酯含量可为<20wt.％。
11.权利要求1-10任一项所述的多层膜，其中具有最高乙酸乙烯酯含量和/或第一和第二EVA的最高熔体流动速率的EVA在密封层中的存在量为30-58wt.％，优选37-50wt.％，基于密封层的总重量和/或基于密封层中EVA的总重量。
12.权利要求1-11任一项所述的多层膜，其中具有最低乙酸乙烯酯含量和/或第一和第二EVA的最低熔体流动速率的EVA在密封层中的存在量为2-15wt.％，优选3-10wt.％，基于密封层的总重量和/或基于密封层中EVA的总重量。
13.权利要求1-12任一项所述的多层膜，其中所述膜对PET的剥离强度为1-20N/15mm，优选1.5-15N/15mm，进一步优选1.6-12N/15mm，进一步优选1.5-8.5N/15mm，进一步优选2-8N/15mm或3-6N/15mm，特别优选2.2-9N/15mm，进一步优选2.5-8.5N/15mm，进一步优选2.7-8N/15mm。
14.包括权利要求1-13任一项所述的多层膜的制品和/或包装。
15.权利要求1-13任一项所述的多层膜用于食品包装应用的用途。
CN201611176087.3A 2016-12-19 2016-12-19 多层膜 Pending CN108202517A (zh)

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CN201780072713.0A CN110023075A (zh) 2016-12-19 2017-11-15 多层膜
PCT/CN2017/111119 WO2018113455A1 (en) 2016-12-19 2017-11-15 Multi-layer film
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JP7547730B2 (ja) * 2019-01-23 2024-09-10 東ソー株式会社 樹脂組成物およびその樹脂組成物を用いた成形品
JP7563039B2 (ja) 2020-08-17 2024-10-08 東ソー株式会社 樹脂組成物、改質剤およびその改質剤を含む組成物

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