CN101522388B - 阻隔性良好的注塑成型体 - Google Patents
阻隔性良好的注塑成型体 Download PDFInfo
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- CN101522388B CN101522388B CN2007800383420A CN200780038342A CN101522388B CN 101522388 B CN101522388 B CN 101522388B CN 2007800383420 A CN2007800383420 A CN 2007800383420A CN 200780038342 A CN200780038342 A CN 200780038342A CN 101522388 B CN101522388 B CN 101522388B
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- polyamide
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Abstract
本发明提供了一种多层注塑成型体，该多层注塑成型体包括阻隔性树脂组合物层，该阻隔性树脂组合物层含有10-70质量％的聚酰胺树脂A、90-30质量％的改性聚烯烃B等，其中，所述聚酰胺树脂A中，二胺结构单元的70摩尔％以上来自于间苯二甲胺，二羧酸结构单元的70摩尔％以上来自于α，ω-直链脂肪族二羧酸和间苯二甲酸的摩尔比例为30∶70至100∶0的二羧酸，所述α，ω-直链脂肪族二羧酸的碳原子数为4-20；本发明还提供了一种多层注塑成型体，该多层注塑成型体包括阻隔性树脂组合物层，该阻隔性树脂组合物层含有50-90质量％的所述聚酰胺树脂A、2-45质量％的改性聚烯烃B以及2-45质量％的不含间苯二甲基的聚酰胺D；本发明还提供了一种注塑成型体，该注塑成型体含有10-60质量％的所述聚酰胺树脂A、40-90质量％的聚烯烃E，且聚酰胺树脂A的至少一部分分散为层状。这些成形体具有良好的阻隔性。
Description
技术领域
本发明涉及阻隔性和外观等良好的注塑成型体，详细地说，涉及阻隔性、外观、耐剥离性、耐热性等良好的多层注塑成型体及阻隔性和外观等良好的单层注塑成型体。
背景技术
注塑成型可以制备具有复杂的形状的成型体，生产率高，因此，在机械零件、汽车零件、电气·电子零件、食品·医药等容器等中广泛普及。尤其是关于饮料等的容器，为了能够拧紧盖子，多使用口栓的螺纹形状良好的注塑成型体。
作为用于注塑成型的材料，可以使用含有聚乙烯、聚丙烯等的聚烯烃、聚酯、聚苯乙烯等通用性树脂等，其中，从成型时的流动性、耐热性优良、轻量性、低吸湿性、且廉价的方面考虑，聚丙烯等的聚烯烃广泛用于容器等的各种用途中。
但是，聚烯烃对氧气等的气体阻隔性差，因此，不适合用于对易受氧气等的影响的内容物的保存、高温等的环境下的保存性有要求的食品·医药等的容器。因此，公开了在聚烯烃中混合聚酰胺等的阻隔性材料，提高阻隔性的方法(参照专利文献1、2)。
通过这些方法，可以改善阻隔性，但是由于阻隔性材料的特殊的分散状态也是必要的，因此，阻隔性的改善不充分，另外，由于在表面附近聚酰胺分布不均，因此，存在产生外观不良等的问题。即，在专利文献1中，在双轴延伸中，吹塑成型的成型方法是必须的，在不进行双轴延伸吹塑的情况下，阻隔性差。另外，虽然在专利文献2中记载了在聚烯烃中存在多个无定形聚酰胺的复合成型品，但是关于具有结晶性的聚酰胺和具有间苯二甲基骨架的聚酰胺并没有记载。
另一方面，在注塑成型方法中，对于形成具有阻隔层的多层结构，由于聚烯烃和阻隔材料之间没有粘接性，因此，聚烯烃层/粘接层/阻隔层/粘接层/聚烯烃层这样的具有粘接层的至少5层结构是必须的，在这种情况下，在结构上或成型性方面存在困难，因此，几乎不能在工业上实施。因此，公开了通过在聚烯烃中掺合具有粘接性的改性聚烯烃以提高聚烯烃层与阻隔层之间的粘接性而不要粘接层的方法(参照专利文献3)。虽然通过该方法可以改善粘接性，但是存在为了提高粘接性而需要大量添加价格高的改性聚烯烃、或由添加改性聚烯烃而引起耐热性降低的问题。
本发明人以前提出了将含有70摩尔％以上的间苯二甲胺的二胺成分与α，ω-直链脂肪族二羧酸和间苯二甲酸的混合二羧酸缩聚而得到的聚酰胺树脂作为燃料阻隔用树脂(参照专利文献4)。该聚酰胺树脂具有良好的阻隔性，但是关于使用了该聚酰胺树脂的多层注塑成型体，要求耐剥离性的改善。
专利文献1：特开2004-292037号公报
专利文献2：特开2005-8664号公报
专利文献3：特开2006-131275号公报
专利文献4：特开2004-352985号公报
发明内容
本发明为了解决由注塑成型得到的容器的上述的问题而提供了阻隔性、外观、耐剥离性及耐热性等良好的多层注塑成型体及阻隔性和外观等良好的、可以在经济上有利制备的单层注塑成型体。
本发明人为了达到上述目的而进行了深入研究，结果发现，将使用了含有特定结构的聚酰胺树脂和改性聚烯烃、或所述聚酰胺树脂和改性聚烯烃及其它的聚酰胺树脂的树脂层的多层注塑成型体，或使所述聚酰胺树脂层状分散在混合聚烯烃中而成的注塑成型体作为阻隔层，可以达到上述目的，从而完成本发明。
即，本发明提供了以下的注塑成型体。
1、一种多层注塑成型体，其特征在于，该多层注塑成型体包括至少一层阻隔性树脂组合物层，该阻隔性树脂组合物层含有10-70质量％的聚酰胺树脂A、90-30质量％的改性聚烯烃B以及0-50质量％的聚烯烃C，其中，所述聚酰胺树脂A为含有二胺结构单元和二羧酸结构单元的聚酰胺树脂，所述二胺结构单元的70摩尔％以上来自于间苯二甲胺，所述二羧酸结构单元的70摩尔％以上来自于α，ω-直链脂肪族二羧酸和间苯二甲酸的摩尔比例为30∶70至100∶0的二羧酸，所述α，ω-直链脂肪族二羧酸的碳原子数为4-20。
2、一种多层注塑成型体，其特征在于，该多层注塑成型体包括至少一层阻隔性树脂组合物层，该阻隔性树脂组合物层含有50-90质量％的聚酰胺树脂A、2-45质量％的改性聚烯烃B以及2-45质量％的不含间苯二甲基的聚酰胺D，其中，所述聚酰胺树脂A为含有二胺结构单元和二羧酸结构单元的聚酰胺树脂，所述二胺结构单元的70摩尔％以上来自于间苯二甲胺，所述二羧酸结构单元的70摩尔％以上来自于α，ω-直链脂肪族二羧酸和间苯二甲酸的摩尔比例为30∶70至100∶0的二羧酸，所述α，ω-直链脂肪族二羧酸的碳原子数为4-20。
3、一种注塑成型体，其特征在于，该成型体含有10-60质量％的聚酰胺树脂A和40-90质量％的混合聚烯烃E，所述聚酰胺树脂A的至少一部分分散为层状，其中，所述聚酰胺树脂A为含有二胺结构单元和二羧酸结构单元的聚酰胺树脂，所述二胺结构单元的70摩尔％以上来自于间苯二甲胺，所述二羧酸结构单元的70摩尔％以上来自于α，ω-直链脂肪族二羧酸和间苯二甲酸的摩尔比例为30∶70至100∶0的二羧酸，所述α，ω-直链脂肪族二羧酸的碳原子数为4-20；所述混合聚烯烃E含有40-100质量％的聚烯烃C和0-60质量％的改性聚烯烃B。
4、根据上述1或2所述的注塑成型体，其中，所述聚酰胺树脂A在温度为25℃、浓度为1g/100ml的条件下、以96质量％的浓硫酸为溶剂进行测定时的相对粘度为2.5以上。
5、根据上述1-3中任意一项所述的注塑成型体，其中，所述改性聚烯烃B为用不饱和羧酸或其酸酐对聚烯烃C进行接枝改性后的物质。
6、根据上述2所述的注塑成型体，其中，所述不含间苯二甲基的聚酰胺D为选自尼龙-6、尼龙-66及尼龙-666的脂肪族聚酰胺。
7、根据上述2所述的注塑成型体，其中，所述不含间苯二甲基的聚酰胺D在温度为25℃、浓度为1g/100ml的条件下、以96质量％的浓硫酸为溶剂进行测定时的相对粘度小于5的脂肪族聚酰胺。
8、根据上述1或2所述的注塑成型体，其中，所述多层注塑成型体为所述阻隔性树脂组合物层被夹在含有聚烯烃的热塑性树脂层F中的多层注塑成型体。
9、根据权利要求1或2所述的注塑成型体，其中，所述多层注塑成型体通过双轴延伸吹塑成型而形成为多层延伸注塑成型体。
本发明的上述1的多层注塑成型体(也称为多层注塑成型体I)及上述2的多层注塑成型体(也称为多层注塑成型体II)，阻隔性、耐剥离性、耐热性和外观良好，尤其是能防止成型体的运输时或下落时受到冲击时阻隔性树脂层与其相邻层之间的剥离，而且即使凹凸部、弯曲部较多也能避免剥离，设计自由度大。
另外，本发明的上述3的注塑成型体(也称为单层注塑成型体)的阻隔性和外观良好，能在经济上有利地制备。
因此，多层注塑成型体I、II及单层注塑成型体适合用于饮料、汤等的液态食品及可进行蒸煮等的处理的食品·医药用容器。
具体实施方式
本发明的多层注塑成型体I、II及单层注塑成型体中使用的聚酰胺树脂A为含有二胺结构单元和二羧酸结构单元的聚酰胺树脂，所述二胺结构单元的70摩尔％以上来自于间苯二甲胺，所述二羧酸结构单元的70摩尔％以上来自于α，ω-直链脂肪族二羧酸和间苯二甲酸的摩尔比例为30∶70至100∶0的二羧酸，其中，所述α，ω-直链脂肪族二羧酸的碳原子数为4-20。
本发明的多层注塑成型体I、II包括至少一层以该聚酰胺树脂A为主要成分的阻隔性树脂组合物层，优选该阻隔性树脂组合物层被夹在含有聚烯烃的热塑性树脂层E中。
另外，本发明的单层注塑成型体中，聚酰胺树脂A的至少一部分层状分散在含有聚烯烃C的成型体中。
用作制备聚酰胺树脂A时的原料的除间苯二甲胺以外的二胺，可以例示出：脂肪族二胺，如丁二胺、戊二胺、2-甲基戊二胺、己二胺、庚二胺、辛二胺、壬二胺、癸二胺、1，12-二氨基十二烷、2，2，4-三甲基己二胺、2，4，4-三甲基己二胺等；脂环族二胺，如1，3-双(氨甲基)环己烷、1，4-双(氨甲基)环己烷、1，3-二氨基环己烷、1，4-二氨基环己烷、双(4-氨基环己基)甲烷、2，2-双(4-氨基环己基)丙烷、双(氨甲基)十氢化萘(包括结构异构体)、双(氨甲基)三环庚烷(包括结构异构体)等；具有芳香环的二胺类，如双(4-氨苯基)醚、对苯二胺、对苯二甲胺、双(氨甲基)萘(包括结构异构体)等。这些可以以在全部的二胺成分中为30摩尔％以下的范围使用。
所述碳原子数为4-20的α，ω-直链脂肪族二羧酸，可以例示出例如琥珀酸、戊二酸、庚二酸、辛二酸、壬二酸、己二酸、癸二酸、十一碳烷二酸、十二碳烷二酸等的脂肪族二羧酸，其中，优选为己二酸。
含有碳原子数为4-20的α，ω-直链脂肪族二羧酸和间苯二甲酸的混合二羧酸中的碳原子数为4-20的α，ω-直链脂肪族二羧酸和间苯二甲酸的摩尔比为30∶70至100∶0，优选为30∶70至95∶5，更优选为40∶60至95∶5，进一步优选为60∶40至90∶10。含有该范围的间苯二甲酸时，可以提高阻隔性。另外，与只有碳原子数为4-20的α，ω-直链脂肪族二羧酸的情况相比，不仅得到的聚酰胺树脂的熔点降低、可以以更低温度成型、能够降低制备能量、缩短成型循环，而且熔融粘度增高、对该树脂的收缩(ドロ一ダゥンdrawdown)等的成型加工性得以提高。
在本发明中，上述含有碳原子数为4-20的α，ω-直链脂肪族二羧酸和间苯二甲酸的二羧酸以外的二羧酸，可以列举出：苯二甲酸化合物，如对苯二甲酸、邻苯二甲酸等；萘二甲酸，如1，2-萘二甲酸、1，3-萘二甲酸、1，4-萘二甲酸、1，5-萘二甲酸、1，6-萘二甲酸、1，7-萘二甲酸、1，8-萘二甲酸、2，3-萘二甲酸、2，6-萘二甲酸、2，7-萘二甲酸等；单羧酸，如苯甲酸、丙酸、乙酸等；多元羧酸，如偏苯三酸、均苯四甲酸等；羧酸酐，如偏苯三酸酐、均苯四甲酸酐等。
本发明中使用的聚酰胺树脂A中，这些二羧酸以外的二羧酸结构单元为全部的二羧酸结构单元的30摩尔％以下的范围。
聚酰胺树脂A通过将含有70摩尔％以上的间苯二甲胺的二胺成分与含有70摩尔％以上的摩尔比例为30∶70至100∶0的碳原子数为4-20的α，ω-直链脂肪族二羧酸和间苯二甲酸的二羧酸成分缩聚来制备，其制备方法没有特别的限定，可以通过常压熔融聚合法、加压熔融聚合法等的以往公知的方法来制备。
例如，通过一边将含有间苯二甲胺和己二酸，或者间苯二甲胺、己二酸及间苯二甲酸的尼龙盐在水的存在下在加压下升温，取出加入的水及缩合水，一边在熔融状态下聚合的方法来制备。另外，也可以通过在熔融状态的己二酸、或者己二酸和间苯二甲酸的混合物中直接加入间苯二甲胺，在常压下进行缩聚的方法来制备。在该情况下，为了不使反应体系固化，连续加入间苯二甲胺，使反应体系升温至该连续加入间苯二甲胺期间的反应温度为生成的酰胺低聚物和聚酰胺的熔点以上，同时进行缩聚。
通过缩聚得到聚酰胺树脂A时，在不损害性能的范围内，也可以在缩聚反应体系中加入内酰胺类(如ε-己内酰胺、ω-十二内酰胺、ω-庚内酰胺等)、氨基酸等(如6-氨基己酸、7-氨基己酸、11-氨基十一烷酸、12-氨基十二烷酸、9-氨基壬酸、对氨甲基苯甲酸等)。
聚酰胺树脂A优选为进行上述缩合后，进一步进行加热处理以增大了熔融粘度的聚酰胺树脂。加热处理的方法可举出例如：使用旋转辊等的间歇式加热装置，在惰性气体氛围中或减压下，在水的存在下缓慢加热，避免熔融粘着且结晶化后，再进行加热处理的方法；使用沟型搅拌加热装置，在惰性气体氛围中加热、结晶化后，使用漏斗形状的加热装置，在惰性气体氛围下进行加热处理的方法；使用沟型搅拌加热装置结晶化后，使用旋转辊等的间歇式加热装置来进行加热处理的方法等。其中，优选使用间歇式加热装置来进行结晶化和加热处理的方法。作为处理条件，优选为通过在相对于熔融聚合得到的聚酰胺树脂A为1-30质量％的水的存在下、且花费0.5-4小时从70℃升温至120℃进行结晶化，然后，在惰性气体氛围中或减压下，在“聚酰胺树脂A的熔点-50℃”至“聚酰胺树脂A的熔点-10℃”的温度下进行加热处理1-12小时的条件。
在多层注塑成型体I、II的情况下，聚酰胺树脂A优选使用在温度为25℃、浓度为1g/100ml的条件下、以96质量％的浓硫酸为溶剂测定的相对粘度为2.5以上的聚酰胺树脂，更优选使用所述相对粘度为3以上的聚酰胺树脂。相对粘度不足2.5时，粘接性不够好，有时会发生剥离。
单层注塑成型体的情况下，聚酰胺树脂A优选使用所述相对粘度为2.5以下的聚酰胺树脂，更优选使用所述相对粘度为2.3以下的聚酰胺树脂。在单层注塑成型体中，相对粘度超过2.5时，有时阻隔性不够好。
在本发明的多层注塑成型体I、II及单层注塑成型体中，优选控制聚酰胺树脂A的熔点为160-240℃的范围，更优选为170-230℃，进一步优选为180-230℃。
另外，在多层注塑成型体I的情况下，通过使聚酰胺树脂A的熔点接近改性聚烯烃B和聚烯烃C的熔点，能够抑制由多层成型体制作时的树脂间的成型温度差引起的厚度不均匀等的不良情况的发生、及由树脂劣化引起的臭气和着色。
另外，在多层注塑成型体II的情况下，通过使聚酰胺树脂A的熔点接近夹有阻隔性树脂组合物层的热塑性树脂F的熔点，能够抑制由多层成型体制作时的树脂间的成型温度差引起的厚度不均匀等的不良情况的发生、及由树脂劣化引起的臭气和着色。
聚酰胺树脂A的玻璃化点优选为80-130℃的范围。通过使聚酰胺的玻璃化点为80℃以上，能得到高温下的阻隔性良好的聚酰胺树脂。
另外，聚酰胺树脂A适合使用末端氨基浓度不足40μ当量/g，优选为10-30μ当量/g，更优选羧基浓度为40-100μ当量/g以上的聚酰胺树脂。通过使末端氨基浓度在上述范围，能抑制得到的阻隔层着色成黄色。
为了提高熔融成型时的加工稳定性、或者为了防止该聚酰胺的着色，优选聚酰胺树脂A中含有磷化合物。磷化合物适合使用含有碱金属或碱土类金属的磷化合物，可举出例如钠、镁、钙等的磷酸盐、次磷酸盐、亚磷酸盐，使用了碱金属或碱土类金属的次磷酸盐的聚酰胺树脂A，聚酰胺的防止着色效果特别好，因此优选使用。聚酰胺树脂A中的磷化合物的浓度，以磷原子计为200ppm以下，优选为160ppm以下，更优选为100ppm以下。
另外，除上述磷化合物以外，在不损害本发明的效果的范围内，也可以在聚酰胺树脂A中加入润滑剂、消光剂、热稳定剂、耐候稳定剂、紫外线吸收剂、晶核剂、增塑剂、阻燃剂、防静电剂、防止着色剂、防凝胶剂等的添加剂等，但是并不限定于上述物质，也可以混合各种材料。
聚酰胺树脂A，优选在使用前干燥至水分率为0.10质量％以下，优选为0.08质量％以下，更优选为0.05质量％以下。通过使水分率为0.10质量％以下，熔融混合时，不会因由聚酰胺树脂A产生的水分而产生气泡。干燥聚酰胺树脂A的情况，可以通过公知的方法来进行。可举出例如在带有真空泵的可加热的滚筒(旋转式真空槽)中或减压干燥机中加入聚酰胺树脂A，在减压下在聚合物的熔点以下、优选在160℃以下的温度下加热干燥的方法等。
作为本发明中的改性聚烯烃B，适合使用用不饱和羧酸或其酸酐对聚烯烃C进行接枝改性后的物质。
本发明中使用的聚烯烃C可举出多种，优选为低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、线性低密度聚乙烯、聚丙烯、聚1-丁烯、聚4-甲基-1-戊烯(1-ポリメチルペンテン)等的碳原子数为2以上、优选为2-8的乙烯系烃的单独聚合物；碳原子数为3-20的α-烯烃的单独聚合物；碳原子数为3-20的α-烯烃的共聚物(乙烯-丙烯共聚物、乙烯-丙烯-二烯三元共聚物、乙烯·1-丁烯共聚物、乙烯·4-甲基-1-戊烯共聚物、乙烯·1-己烯共聚物、乙烯·1-辛烯共聚物、乙烯·1-庚烯共聚物、丙烯·1-丁烯共聚物、丙烯·4-甲基-1-戊烯共聚物、丙烯·1-己烯共聚物、丙烯·1-辛烯共聚物、丙烯·1-庚烯共聚物等)；碳原子数为3-20的α-烯烃和环状烯烃的共聚物(与降冰片烯的共聚物等)。这些聚烯烃可以单独使用，也可以以两种类以上的混合物使用。
这些聚烯烃中，优选聚乙烯、聚丙烯、聚1-丁烯、或α-烯烃与环状烯烃的共聚物等的玻璃化点高的树脂，其中，优选使用耐热性良好的聚丙烯。
本发明中使用的聚烯烃C在190℃、2.16kgf的负载下的熔体流动速率(MFR)优选为1-100克/10分钟的范围。通过使MFR为1克/10分钟以上，不会产生厚度不均匀等的成型性不良的情况。
如上所述，本发明中使用的改性聚烯烃B为用不饱和羧酸或其酸酐对上述聚烯烃C进行接枝改性后的物质，适合的为作为相溶化剂或粘合剂广泛使用的物质。
不饱和羧酸或其酸酐的具体例子，可举出丙烯酸、甲基丙烯酸、α-乙基丙烯酸、马来酸、富马酸、衣康酸、柠康酸、四氢苯二甲酸、氯代马来酸、丁烯基琥珀酸等及它们的酸酐。其中，优选使用马来酸及马来酸酐。
将上述不饱和羧酸或其酸酐接枝共聚于聚烯烃上而得到改性聚烯烃B的方法，可以使用以往公知的各种方法。例如，可举出使用挤出机等使聚烯烃熔融，添加接枝单体进行共聚的方法；或者使聚烯烃溶解于溶剂中并添加接枝单体进行共聚的方法，使聚烯烃成为水悬浊液以后添加接枝单体进行共聚的方法等。
这样进行接枝改性后的改性聚烯烃B，可举出モディックAP-P502、モディックAP-P565、モディックAP-P502(以上为三菱化学(株)制)、ァドマ一GT6(三井化学(株)制)、ァドテックスDU0500(日本ポリェチレン(株)制)等。
本发明中使用的改性聚烯烃B在190℃、2.16kgf的负载下的熔体流动速率(MFR)优选为0.5-50克/10分钟的范围。通过使MFR为该范围，能得到良好的粘接性和成型性。
在多层注塑成型体I的情况下，阻隔性树脂组合物层通过混合上述聚酰胺树脂A、改性聚烯烃B和聚烯烃C而得到，在该阻隔性树脂组合物中含有10-70质量％的聚酰胺树脂A、90-30质量％的改性聚烯烃B及0-50质量％的聚烯烃C，优选含有15-65质量％的A成分、85-35质量％的B成分及0-40质量％的C成分，更优选含有20-60质量％的A成分、80-40质量％的B成分及0-30质量％的C成分。通过使A成分为10质量％以上，能得到充分的阻隔性；通过使A成分的含量为70质量％以下，能得到与相邻的层充分的粘接性。另外，通过使B成分的含量为30质量％以上，能得到充分的粘接性；通过使B成分的含量为90质量％以下，能得到充分的阻隔性。通过使C成分的含量为50质量％以下，能得到充分的粘接性。
在多层注塑成型体II的情况下，阻隔性树脂组合物层通过混合上述聚酰胺树脂A、改性聚烯烃B及不含间苯二甲基的聚酰胺D而得到，在该阻隔性树脂组合物中含有50-90质量％的聚酰胺树脂A、2-45质量％的改性聚烯烃B及2-45质量％的不含间苯二甲基的聚烯烃D，优选含有55-85质量％的A成分、5-40质量％的B成分及5-40质量％的D成分。
在上述不含间苯二甲基的聚酰胺D中，优选比聚酰胺树脂A更柔软的聚酰胺，可举出尼龙-4、尼龙-6、尼龙-12、尼龙-66、尼龙-46、尼龙-610、尼龙-612、尼龙666(尼龙6和尼龙66的共聚物)等的脂肪族聚酰胺，其中优选使用尼龙-6、尼龙-66及尼龙-666。
在使用这样的不含间苯二甲基的聚酰胺D的情况下，通过使A成分的含量为50质量％以上，能得到充分的阻隔性；通过使A成分的含量为90质量％以下，能得到与相邻的层的充分的粘接性。另外，通过使B成分的含量为20质量％以上，能得到充分的粘接性；通过使B成分的含量为45质量％以下，能得到充分的阻隔性。
不含间苯二甲基的聚酰胺D在温度为25℃、浓度为1g/100ml的条件下、以96质量％的浓硫酸为溶剂进行测定时的相对粘度优选为不足5，更优选不足4。通过使相对粘度不足5，用挤出机进行预混合时，不会产生挤出变动或丝束中断等的不好情况。
另外，该不含间苯二甲基的聚酰胺D的相对粘度，可以通过精确称取1g的不含间苯二甲基的聚酰胺D，在100ml的96质量％的硫酸中在20-30℃下搅拌溶解；完全溶解后，快速用卡农芬斯克型粘度计取5cc溶液，在25℃的恒温槽中放置10分钟后，测定下落速度(t)；另外，同样测定96质量％的硫酸的下落速度(to)，用相对粘度＝t/to计算出。
如上所述，本发明的多层注塑成型体I、II包括至少一层所述阻隔性树脂组合物层，该阻隔性树脂组合物层优选被夹在热塑性树脂层F中。
该热塑性树脂层F可以使用各种热塑性树脂，但是优选聚烯烃。作为夹有阻隔性树脂组合物层的热塑性树脂层F中使用的聚烯烃，可例示出选自直链状低密度聚乙烯，低密度聚乙烯，中密度聚乙烯，高密度聚乙烯，超高分子量高密度聚乙烯，聚丙烯，或乙烯、丙烯和丁烯等中的两种以上的烯烃的共聚物，及它们的混合物。其中，聚丙烯由于耐热性良好而优选。另外，上述热塑性树脂层F中使用的聚烯烃，可以与弹性体等的其它的树脂混合、或例如与碳黑或阻燃剂等的其它的添加剂混合使用。
作为制备本发明的多层注塑成型体I、II的一个例子，可举出使用具有两个注塑气缸的注塑成型机，将热塑性树脂和阻隔性树脂组合物分别从外壳侧、中心侧各自的注塑气缸通过热浇道模，在模具腔内注塑得到多层注塑成型体的方法，进一步还可以通过将该多层注塑成型体进行双轴延伸吹塑成型得到多层延伸注塑成型体。多层注塑成型体的吹塑成型使用以往公知的方法即可，例如，可以采用将多层注塑成型体的表面加热到120-170℃后进行吹塑成型的方法。吹塑压力通常为1-4MPa。
在上述方法中，在从外壳侧注塑气缸注塑构成最内层及最外层的聚烯烃等的热塑性树脂，从中心侧注塑气缸注塑构成阻隔性树脂组合物层的阻隔性树脂组合物的工序中，通过首先注塑热塑性树脂，然后注塑阻隔性树脂组合物，再注塑必要量的热塑性树脂填满模具腔来制备三层结构(热塑性树脂/阻隔性树脂组合物/热塑性树脂)的多层注塑成型体。另外，制备多层型坯(パリソン)的方法，并不仅限定于这些方法。
多层注塑成型体I、II中的热塑性树脂层F的厚度优选平均为0.01-3.0mm，阻隔性树脂组合物层的厚度优选平均为0.005-2mm。另外，含有多层注塑成型体I、II的多层容器的厚度没必要容器整体一致，通常平均为0.01-5.0mm的范围。
通过对本发明中得到的多层注塑成型体I、II进行双轴延伸，能得到多层延伸注塑成型体。双轴延伸的方法可以通过一般的吹塑成型机来进行成型。
例如，使用双轴延伸吹塑成型机，用远红外加热器等，对注塑成型体加热15秒至5分钟，用伸长杆(ストレッチロッド)和0.5-3.5MPa的压力通过吹塑成型而得到。
本发明中的多层注塑成型体I、II，可以将溢料或成型时的次品再次熔融、再利用。此时，从强度方面考虑，优选将再利用品配置在阻隔性树脂组合物层外侧的层中。
另外，在不损害本发明的目的的范围内，可以在各个树脂层添加润滑剂，脱模剂，抗氧剂，加工稳定剂，热稳定剂，紫外线吸收剂，层状硅酸盐，晶核剂，Co、Mn、Zn等的无机或有机金属盐，配位化合物等。
如上所述，本发明的单层注塑成型体为含有聚烯烃C的成型体，聚酰胺树脂A的至少一部分分散为层状。
上述含有聚烯烃C的成型体可使用含有40-100质量％的聚烯烃C和60-0质量％的改性聚烯烃B、优选含有50-90质量％的聚烯烃C和10-50质量％的改性聚烯烃B的混合聚烯烃E。
在本发明的单层注塑成型体中使用的聚酰胺树脂A中，根据需要，也可以添加尼龙6、尼龙66、尼龙666等其它的聚酰胺，乙烯-乙烯醇共聚树脂，乙烯醇系共聚树脂，丙烯腈树脂等。
即，本发明的单层注塑成型体中的注塑成型体为将上述混合聚烯烃E和聚酰胺树脂A熔融混合、通过注塑成型得到的单层成型体，在该成型体中，相对于混合聚烯烃E和聚酰胺A的合计，以E成分为40-90质量％、A成分为60-10质量％，优选E成分为50-85质量％、A成分为50-15质量％，更优选E成分为55-80质量％、A成分为45-20质量％，特别优选E成分为55-75质量％、A成分为45-25质量％的比例含有所述混合聚烯烃E和聚酰胺树脂A。通过使E成分为40质量％以上，能得到强度良好的成型体；或者通过使E成分为90质量％以下，不会使阻隔性不充分。
在本发明的单层注塑成型体中使用的树脂，也可以使用预先用挤出机进行熔融混炼后的树脂，在注塑成型前，也可以使用干式混合后的树脂。
另外，本发明的单层注塑成型体，可以使用以往公知的注塑成型机来制备。单层注塑成型体的层的厚度优选平均为0.1-5.0mm，更优选为0.2-4mm。
本发明的单层注塑成型体为聚酰胺树脂A的至少一部分分散为层状而成的，特别优选聚酰胺树脂A在成型体的表层部分定向分散为层状。
本发明的单层注塑成型体，也可以再次熔融溢料或成型时的次品，作为循环层而导入。此时，优选从强度方面调节各树脂的添加量。
另外，本发明的单层注塑成型体，在不损害发明目的的限度内，可以在所述混合聚烯烃E或聚酰胺树脂A中添加润滑剂，脱模剂，抗氧剂，加工稳定剂，热稳定剂，紫外线吸收剂，层状硅酸盐，晶核剂，Co、Mn、Zn等的无机或有机金属盐，配位化合物等。
这样得到的本发明的多层注塑成型体I、II及单层注塑成型体具有良好的气体阻隔性，可用作储存各种产品的容器，例如：液体系食品，液体系食品的代表包括碳酸饮料、果汁、水、牛奶、日本酒、威士忌、烧酒、咖啡、茶、果冻饮料、健康饮料等的液体饮料，调味液、酱、酱油、调味品、液体汤料、蛋黄酱、豆酱、磨碎的香辣调味料等的调味料，果子酱、奶油、巧克力浆等的糊状食品，液体汤、煮菜、泡菜、炖菜等的液体加工食品；高水分食品，高水分食品的代表包括荞麦面条、面条、拉面等的生面条及煮熟的面条、精白米、调湿米、无洗米等的烹饪前的米类或烹饪后的做饭米、什锦饭、红小豆糯米饭、米粥等的加工米产品类，粉末汤、粉状高汤(だしの素)等的粉末调味料等；低水分食品，低水分食品的代表包括干燥蔬菜、咖啡豆、咖啡粉、茶、以谷物为原料的点心等；农药或杀虫剂等的固体状或溶液状的化学药品、液体及糊状的医药品、化妆水、化妆油、化妆乳液、定发剂、染发剂、洗发液、肥皂、洗涤剂等。
实施例
下面通过实施例等详细说明本发明，另外，在实施例等中，聚酰胺树脂A及注塑成型体的评价方法按如下方法进行。
(1)聚酰胺树脂A的相对粘度
精确称取1g的聚酰胺树脂A，在20-30℃下搅拌溶解于100ml的96质量％的硫酸中。完全溶解后，快速取5cc溶液加到卡农芬斯克型粘度计中，在25℃的恒温槽中放置10分钟后，测定下落速度(t)。另外，同样测定96质量％的硫酸的下落速度(to)，用相对粘度＝t/to计算出。
(2)阻隔性树脂组合物的挤出性
将阻隔性树脂组合物的各树脂粉末干式混合后，用气缸直径为37mm、安装有具有反向捏合元件(逆メェレメント)的逗留部的强炼型的螺旋的双螺杆挤出机，在260℃、10kg/小时、100RPM的条件下，如下所述评价进行挤出混炼时的挤出稳定性。
a：挤出稳定、b：有点不稳定、c：不稳定
(3)多层注塑成型体的成型性
切开多层注塑成型体容器的本体部，如下所述评价阻隔性树脂组合物层的厚度的均匀性。
a：厚度均匀、b：厚度有点不均匀、c：厚度不均匀
(4)耐剥离性
<多层注塑成型体>
关于切割多层注塑成型体容器的本体部而得到的环状的切片，如下所示评价用手剥离阻隔性树脂组合物层和外侧层时的剥离状态。
a：剥离时有阻力感、b：剥离时有一点阻力感、c：剥离时没有阻力感。
<多层延伸注塑成型体>
目视观察3次压坏多层延伸注塑成型体容器的本体部时的阻隔性树脂组合物层和外侧层的剥离状态，如下所示进行评价。
a：没有剥离、b：有一点剥离、c：有明确的剥离。
(5)氧气阻隔性(氧气透过率)
在23℃、注塑成型体容器内部的相对湿度60％、外部的相对湿度50％的氛围下，根据ASTM D3985测定注塑成型体的氧气透过率。使用モダンコントロ一ルズ社制OX-TRAN 10/50A进行测定。
(6)多层注塑成型体的耐热性
在多层注塑成型体容器中注入20ml的水、或者在多层延伸注塑成型体容器中注入500ml的水，盖上盖子，在高压釜[トミ一工业(株)制]中在90℃下进行30分钟蒸馏处理，目视确认容器的变形，如下所述进行评价。
a：未变形、b：有一点变形、c：变形。
(7)单层注塑成型体的分散状态
切制得到的单层注塑成型体容器的截面，涂布稀碘酒[月岛药品(株)制]，使聚酰胺染色后，用显微镜观察分散状态。观察到聚酰胺在成型体的表层部分上分散为层状，则记为“层状”；整体分散为粒状，则记为“粒化”。
制备方法A(多层注塑成型体的制备)
使用名机制作所(株)制的注塑成型机(型号：M200、4个)，制备全长为95mm、外径为22mm、厚度为4.0mm的三层注塑成型体型坯。
(三层注塑成型体的成型条件)
外壳侧注塑气缸温度：240℃
中心侧注塑气缸温度：260℃
模具内树脂流路温度：260℃
模具冷却水温度：15℃
多层成型体容器中的阻隔性树脂组合物的比例：20重量％
制备方法B(多层延伸注塑成型体容器的制备)
由上述制备例A得到的三层注塑成型体型坯，使用预塑成型机(クルップコ一ポプラスト(KRUPP CORPOPLAST)社制、型号：LB-01)进行双轴延伸预塑成型，制备下述形状的三层延伸注塑成型体容器(瓶子)。
形状：全长为223mm、外径为65mm、内容积为500ml、聚丙烯/阻隔性树脂层/聚丙烯＝0.12mm/0.06mm/0.12mm、底部形状为香槟瓶型。
(双轴延伸预塑成型的成型条件)
型坯加热温度：160℃
预塑压力：1.5MPa
制备方法C(多层注塑成型体容器的制备)
使用名机制作所(株)制的注塑成型机(型号：M200、4个)，制备全长为95mm、外径为25mm、厚度为3.0mm的三层注塑成型体型坯。
(三层注塑成型体的成型条件)
外壳侧注塑气缸温度：240℃
中心侧注塑气缸温度：260℃
模具内树脂流路温度：260℃
模具冷却水温度：15℃
多层成型体中的阻隔性树脂组合物的比例：10重量％
制备方法D(单层注塑成型体容器的制备)
使用名机制作所(株)制的注塑成型机(型号：M200、4个)，制备全长为95mm、外径为22mm、厚度为4.0mm的单层注塑成型体型坯。
(注塑成型体的成型条件)
外壳侧注塑气缸温度：240℃
中心侧注塑气缸温度：260℃
模具内树脂流路温度：260℃
模具冷却水温度：15℃
制备例1(聚酰胺树脂：A4的制备)
称取14.2kg(97.1mol)的己二酸和1.0kg(6.2mol)的间苯二甲酸，加入具备搅拌机、分凝器、冷凝器、滴加槽、及氮气导入管的带有套管的50L的反应罐中，充分置换氮气，再在少量的氮气气流下，在160℃下制成含有熔融己二酸和间苯二甲酸的均匀的浆料。在搅拌下利用1小时来滴加14.0kg(102.6mol)的间苯二甲胺。在此期间，使内温连续上升至247℃。滴加间苯二甲胺的同时馏出的水，通过分凝器和冷凝器排出到体系外。间苯二甲胺滴加结束后，将内温升温至260℃，继续反应1小时。得到的聚合物从反应罐下部的喷嘴作为线束取出，用水冷却后剪切成颗粒状。
然后，将该颗粒加入到不锈钢制的旋转辊式的加热装置中，以10rpm进行旋转。充分置换氮气，再在少量的氮气气流下，将反应体系内从室温升温至150℃。在反应体系内的温度达到150℃的时间点进行减压至1torr以下，再花110分钟将体系内的温度升温至210℃。从体系内的温度达到210℃的时间点开始，在相同的温度下继续反应180分钟。反应结束后，结束减压，在氮气气流下降低体系内的温度，在达到60℃的时间点取出颗粒，得到聚酰胺树脂A4。得到的聚酰胺树脂A4的相对粘度为2.7，熔点为232℃。
实施例1-3、比较例1-3
通过上述制备方法A使用第1表所述的材料，制备三层结构的多层成型体容器(型坯)，评价耐剥离性、氧气阻隔性及耐热性。结果如第1表所示。另外，比较例2及3中得到的多层成型体容器由于阻隔性树脂组合物层和相邻层容易剥离，因此，未进行氧气阻隔性和耐热性的评价。
实施例4-7、比较例4-5
通过上述制备方法B使用第2表所述的材料，制备三层结构的多层成型体容器(瓶子)，评价耐剥离性、氧气阻隔性及耐热性。结果如第2表所示。
实施例8-12、比较例6-9
通过上述制备方法C使用第3表所述的材料，制备三层结构的多层成型体容器(型坯)，评价挤出性、成型性、耐剥离性、氧气阻隔性及耐热性。结果如第3表所示。比较例7中得到的多层成型体容器由于阻隔性树脂组合物层(中间层)和相邻层容易剥离，因此，未进行氧气阻隔性和耐热性的评价。
实施例13-19、比较例10-11
通过上述制备方法D使用第4表所述的材料，制备单层注塑成型体容器(型坯)，评价分散性及氧气阻隔性。结果如第4表所示。
另外，第1表-第4表中的记号如下所述。
(聚酰胺树脂)
A1：相对粘度为3.8的聚酰胺MXD6(三菱瓦斯化学(株)制的MX尼龙S6121、含有间苯二甲胺和己二酸的聚酰胺树脂)
A2：相对粘度为2.6的聚酰胺MXD6(三菱瓦斯化学(株)制的MX尼龙S6007、含有间苯二甲胺和己二酸的聚酰胺树脂)
A3：相对粘度为2.1的聚酰胺MXD6(三菱瓦斯化学(株)制的MX尼龙S6001、含有间苯二甲胺和己二酸的聚酰胺树脂)
A4：制备例1中得到的聚酰胺树脂。
(改性聚烯烃)
B1：モディックAP-P502(三菱化学(株)制、MFR＝1.3、密度＝0.89)。
B2：モディックAP-P565(三菱化学(株)制、MFR＝5.7、密度＝0.89)。
B3：ァドマ一GT6(三井化学(株)制、MFR＝0.9)
B4：モディックAP-P502(三菱化学(株)制、MFR＝1.3)
(聚烯烃)
C1：ノバテックMG03E(日本ポリプロ(株)制的聚丙烯、无规聚合物、MFR＝30)。
C2：ノバテックPP-M06A(日本ポリプロ(株)制的均聚聚丙烯、MFR＝60)
C3：ノバテックHD-HB431(日本聚乙烯(株)制的聚乙烯、MFR＝0.35、密度＝0.96)
C4：ノバテックHD-HY540(日本聚乙烯(株)制的聚乙烯、MFR＝1.0、密度＝0.96)
C5：ノバテックHD-HJ580(日本聚乙烯(株)制的聚乙烯、MFR＝12、密度＝0.96)
C6：ノバテックPP-FY6(日本ポリプロ(株)制的聚丙烯、MFR＝2.5、密度＝0.90)
(不含间苯二甲基的聚酰胺)
D1：UBE尼龙-1030B(宇部兴产(株)制的尼龙-6、相对粘度＝4.1)。
D2：UBE尼龙-1024B(宇部兴产(株)制的尼龙-6、相对粘度＝3.5)。
工业实用性
本发明的多层注塑成型体I、II，阻隔性、耐剥离性、耐热性和外观良好，尤其是能防止成型体的运输时或下落时受到冲击时阻隔性树脂层与其相邻层之间的剥离，而且即使凹凸部、弯曲部较多也能避免剥离，设计自由度大，另外，本发明的单层注塑成型体，阻隔层和外观良好，可以经济地有利地制备。
因此，这些多层注塑成型体I、II及单层注塑成型体适合用作饮料、汤等的液状食品及可进行蒸煮等的处理的食品·医药用容器。
Claims (7)
1.一种多层注塑成型体，其特征在于，该多层注塑成型体包括至少一层阻隔性树脂组合物层，该阻隔性树脂组合物层含有50-90质量％的聚酰胺树脂A、2-45质量％的改性聚烯烃B以及2-45质量％的不含间苯二甲基的聚酰胺D，其中，所述聚酰胺树脂A为含有二胺结构单元和二羧酸结构单元的聚酰胺树脂，所述二胺结构单元的70摩尔％以上来自于间苯二甲胺，所述二羧酸结构单元的70摩尔％以上来自于α，ω-直链脂肪族二羧酸和间苯二甲酸的摩尔比例为30∶70至100∶0的二羧酸，所述α，ω-直链脂肪族二羧酸的碳原子数为4-20。
2.根据权利要求1所述的注塑成型体，其中，所述聚酰胺树脂A在温度为25℃、浓度为1g/100ml的条件下、以96质量％的浓硫酸为溶剂进行测定时的相对粘度为2.5以上。
3.根据权利要求1或2所述的注塑成型体，其中，所述改性聚烯烃B为用不饱和羧酸或其酸酐对聚烯烃C进行接枝改性后的物质。
4.根据权利要求1所述的注塑成型体，其中，所述不含间苯二甲基的聚酰胺D为选自尼龙-6、尼龙-66及尼龙-666的脂肪族聚酰胺。
5.根据权利要求1所述的注塑成型体，其中，所述不含间苯二甲基的聚酰胺D为在温度为25℃、浓度为1g/100ml的条件下、以96质量％的浓硫酸为溶剂进行测定时的相对粘度小于5的脂肪族聚酰胺。
6.根据权利要求1所述的注塑成型体，其中，所述多层注塑成型体为所述阻隔性树脂组合物层被夹在含有聚烯烃的热塑性树脂层F中的多层注塑成型体。
7.根据权利要求1所述的注塑成型体，其中，所述多层注塑成型体通过双轴延伸吹塑成型而形成为多层延伸注塑成型体。
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| US9114895B2 (en) | 2015-08-25 |
| RU2011136806A (ru) | 2013-03-10 |
| KR101409069B1 (ko) | 2014-06-18 |
| ES2389192T3 (es) | 2012-10-24 |
| EP2082861A1 (en) | 2009-07-29 |
| ES2404886T3 (es) | 2013-05-29 |
| EP2397300A2 (en) | 2011-12-21 |
| RU2583264C2 (ru) | 2016-05-10 |
| EP2311622A1 (en) | 2011-04-20 |
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| EP2397300A3 (en) | 2013-07-03 |
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| KR20090079200A (ko) | 2009-07-21 |
| PL2082861T3 (pl) | 2012-10-31 |
| PT2082861E (pt) | 2012-06-28 |
| US20130219836A1 (en) | 2013-08-29 |
| US20120082861A1 (en) | 2012-04-05 |
| WO2008047902A1 (fr) | 2008-04-24 |
| US20100304164A1 (en) | 2010-12-02 |
| EP2082861A4 (en) | 2010-06-02 |
| EP2311622B1 (en) | 2013-03-13 |
| DK2311622T3 (da) | 2013-06-10 |
| CN101522388A (zh) | 2009-09-02 |
| US20120263962A1 (en) | 2012-10-18 |
| CN102336959A (zh) | 2012-02-01 |
| PT2311622E (pt) | 2013-04-18 |
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