CN102869489A - 多层容器、多层容器用模具以及多层容器的制造方法 - Google Patents
多层容器、多层容器用模具以及多层容器的制造方法 Download PDFInfo
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- CN102869489A CN102869489A CN201180020373XA CN201180020373A CN102869489A CN 102869489 A CN102869489 A CN 102869489A CN 201180020373X A CN201180020373X A CN 201180020373XA CN 201180020373 A CN201180020373 A CN 201180020373A CN 102869489 A CN102869489 A CN 102869489A
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- resin
- laminated vessel
- gas
- barrier layer
- mould
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Abstract
本发明提供一种多层容器，其即使不采用会提高制造成本之类的特殊装置、工艺烦杂的成型方法也能够制造，其耐层间剥离性及气体阻隔性优异，具体来说，提供一种多层容器，其具有在最内层与最外层之间至少具有气体阻隔层的3层以上的层叠结构，在由前述层叠结构形成的部位中，前述气体阻隔层具有厚度达到该气体阻隔层最大厚度的0.01~0.9倍的部分。本发明还提供适合于制造该多层容器的模具，以及使用了该模具的多层容器的制造方法。
Description
技术领域
本发明涉及层间剥离受到抑制、气体阻隔性优异的多层容器，适合于制造该多层容器的模具，以及使用了该模具的多层容器的制造方法。
背景技术
现今，以聚对苯二甲酸乙二醇酯（PET）等聚酯为主体的塑料容器等多层容器广泛用于茶、果汁饮料、碳酸饮料等中，在塑料容器当中，小型塑料容器所占的比例逐年提高。将容器小型化时，由于每单位体积的表面积的比例增加，所以存在随着塑料容器的小型化、内容物的保质期变短的倾向。另外，近年来，也将塑料容器用作易于受氧、光影响的啤酒的容器，此外还将塑料容器用作温茶的容器，塑料容器的利用范围逐渐拓宽，因而要求进一步提高塑料容器的气体阻隔性。
针对上述要求，作为赋予多层容器气体阻隔性的方法，开发了使用热塑性聚酯树脂和气体阻隔性树脂的多层容器或掺混容器；对热塑性聚酯树脂单层瓶施以碳涂覆、蒸镀、涂布阻隔树脂等而成的阻隔涂层容器等。
作为多层容器的一个例子，将以下容器实用化：以PET等热塑性聚酯树脂作为形成最内层和最外层的树脂，以聚己二酰间苯二甲胺（称为聚酰胺MXD6）等具有气体阻隔性的热塑性树脂作为形成内层的树脂，并将上述树脂同时或依次注射而充满模具的模腔，从而成型为具有3层或5层结构的预成型坯（型坯），并对所得到的预成型坯进行双轴拉伸吹塑成型而成的容器。
此外，开发了能阻断来自容器外的氧并且具有捕捉容器内的氧的氧捕捉功能的树脂，并将其应用于多层容器。作为氧捕捉性容器，从氧吸收速度、透明性、强度、成型性等方面考虑，开发了将混合有过渡金属系催化剂的“聚酰胺MXD6树脂”（三菱瓦斯化学株式会社制造）组合物作为气体阻隔层的多层容器。
上述多层容器由于其良好的气体阻隔性而被用作啤酒、茶、碳酸饮料等的容器。通过在这些用途中使用多层容器，能够维持内容物的品质、改善保质期（可保存时间），另一方面，存在不同树脂间、例如最内层和最外层与气体阻隔层之间出现层间剥离，导致商品价值受损的问题。
作为改善此种问题的方法，专利文献1中记载了：在将构成最内层和最外层的树脂最后注射入模具腔内时，使用能够以规定量逆流到气体阻隔层侧的逆流调节装置，制作层间夹杂有粗混合树脂的预成型坯，从而改善层间剥离。另外，专利文献2中记载了以下方法：在将预成型坯二次成型时，使预成型坯加热收缩，之后再用高压进行吹塑的方法。
现有技术文献
专利文献
专利文献1：日本特开2000-254963号公报
专利文献2：日本特开2001-206336号公报
发明内容
发明要解决的问题
然而，专利文献1中记载的方法由于使用特殊的逆流调节装置，因而存在制造成本升高的问题。另一方面，如专利文献2中记载的方法那样，使预成型坯加热收缩之后再用高压进行吹塑的成型方法存在赋形性差、出现成型品的形状不良且工艺烦杂的问题。
本发明的课题在于提供一种多层容器、适合于制造该多层容器的模具，以及使用该模具的多层容器的制造方法，所述多层容器即使不采用会提高制造成本之类的特殊装置、工艺烦杂的成型方法也能够制造，其耐层间剥离性及气体阻隔性优异。
用于解决问题的方案
本发明涉及下述[1]～[13]。
[1]一种多层容器，其特征在于，该多层容器具有在最内层与最外层之间至少具有气体阻隔层的3层以上的层叠结构，
在由前述层叠结构形成的部位中，前述气体阻隔层具有厚度达到该气体阻隔层最大厚度的0.01~0.9倍的部分。
[2]根据上述[1]所述的多层容器，其中，由前述层叠结构形成的部位的质量是整个多层容器的30质量%以上。
[3]根据上述[1]或[2]所述的多层容器，其中，前述层叠结构为3层或5层的层叠结构。
[4]根据上述[1]～[3]中任一项所述的多层容器，其中，构成前述气体阻隔层的成分为选自聚酰胺树脂、含有间苯二甲基的聚酰胺树脂、乙烯-醋酸乙烯共聚物树脂、聚丙烯腈树脂、聚偏二氯乙烯树脂和聚乙醇酸中的至少1种。
[5]根据上述[4]所述的多层容器，其中，前述聚酰胺树脂为含有间苯二甲基的聚酰胺树脂。
[6]根据上述[1]～[5]中任一项所述的多层容器，其中，构成前述层叠结构的最内层、最外层的成分分别为选自热塑性聚酯树脂、热塑性共聚聚酯树脂、聚烯烃系树脂、脂肪族聚酰胺树脂、聚碳酸酯树脂、聚丙烯腈树脂、聚氯乙烯树脂和聚苯乙烯树脂中的至少1种。
[7]根据上述[1]～[6]中任一项所述的多层容器，其为瓶体。
[8]一种多层容器用模具，其特征在于，其具备：
（I）设置有模腔的冷半部、以及
（II）设置有连接第一压射缸的内部和模腔的第一树脂流路、连接第二压射缸的内部和模腔的第二树脂流路、以及第一树脂流路和第二树脂流路的合流部的热半部，
该热半部（II）所具有的前述合流部位于向前述冷半部（I）所具有的模腔开口的浇口部的上游，且在第二树脂流路内具有部分地阻碍树脂流动的装置。
[9]根据上述[8]所述的多层容器用模具，其中，部分地阻碍树脂流动的装置是在第二树脂流路内的至少一部分设置凸部的装置，
在与第二树脂流路的流动方向垂直的方向的截面上，将直径方向的最长部的长度设为amm、并将圆周的切线方向的最长部的长度设为bmm时，a和b满足以下关系：
0.01r≤a≤1r （式1）
0.01r≤b≤1r （式2）
（上述式中，r表示第二树脂流路的半径（mm）。）
[10]根据上述[8]或[9]所述的多层容器用模具，其中，部分地阻碍树脂流动的装置是在第二树脂流路内的至少两处设置凸部的装置。
[11]根据上述[8]～[10]中任一项所述的多层容器用模具，其中，前述凸部设置在第一树脂流路和第二树脂流路的合流部的上游侧0cm~5cm之间。
[12]一种多层容器的制造方法，其特征在于，其使用上述[8]～[11]中任一项所述的模具进行成型，前述多层容器具有在最内层和最外层之间至少具有气体阻隔层的3层以上的层叠结构，且在由前述层叠结构形成的部位中，前述气体阻隔层具有厚度达到该气体阻隔层最大厚度的0.01~0.9倍的部分。
[13]一种多层容器的制造方法，其特征在于，其使用上述[8]～[11]中任一项所述的模具形成多层预成型坯，接着对该多层预成型坯进行吹塑成型，所述多层容器具有在最内层和最外层之间至少具有气体阻隔层的3层以上的层叠结构，且在由前述层叠结构形成的部位中，前述气体阻隔层具有厚度达到该气体阻隔层最大厚度的0.01~0.9倍的部分。
发明的效果
本发明的多层容器的耐层间剥离性以及气体阻隔性优异。此外，即使不将多层容器制成凹凸部、弯曲部少的形状，也能够避免层间剥离，因而可以提高容器形状的自由度。
另外，通过使用本申请发明的多层容器用模具，即使不采用会提高制造成本之类的特殊装置、工艺烦杂的成型方法，也能够制造前述多层容器。
附图说明
图1为实施例1中使用的模具的示意图，为显示完全未进行注射成型状态的模具的图。
图2为实施例1中使用的模具的示意图，为显示多层容器即将成型之前的模具的状态的图。
图3为模腔附近的示意图，其用于说明实施例1中使用的模具的部分地阻碍树脂流动的装置的配置位置。
图4为第一树脂流路和第二树脂流路的合流部附近的示意图，其用于说明本发明的模具的部分地阻碍树脂流动的装置的配置位置。
图5的（a）为将本发明的模具的部分地阻碍树脂流动的装置沿图4的箭头A-A方向切割而成的截面的示意图。（b）为将本发明的模具的部分地阻碍树脂流动的装置沿图4的箭头B-B方向切割而成的截面的示意图。
图6为将本发明的模具的部分地阻碍树脂流动的装置的一个实施方式沿图4的箭头A-A方向切割而成的截面的示意图。此外，（d）为在树脂流路23B的中心部也设置树脂流路23A、在中心部的该树脂流路23A的外周部也设置部分地阻碍树脂流动的装置的模具的示意图。
图7为将实施例1中的模具的部分地阻碍树脂流动的装置的形状沿图4的箭头A-A方向及箭头B-B方向切割而成的截面的示意图。
图8为使用本发明的模具而成型的多层容器截面的第二树脂层（气体阻隔层）的示意图。
具体实施方式
[多层容器]
本发明的多层容器为具有以下特征的多层容器，该多层容器具有在最内层与最外层之间至少具有气体阻隔层的3层以上的层叠结构，在由前述层叠结构形成的部位中，前述气体阻隔层具有厚度（t1）达到该气体阻隔层最大厚度（t0）的0.01~0.9倍的部位（以下有时称为气体阻隔层的凹部）。
前述气体阻隔层通过具有厚度达到该气体阻隔层最大厚度（t0）的0.9倍以下（气体阻隔层只要是连续的，即为0.01~0.9倍）的凹部，从而使多层容器的层间剥离得到有效地抑制。从该观点考虑，前述气体阻隔层优选具有厚度达到该气体阻隔层最大厚度的0.01~0.8倍、更优选达到0.02~0.7倍、进一步优选达到0.03~0.6倍、特别优选达到0.05~0.5倍的凹部。对气体阻隔层的凹部的位置没有特别制限，在将多层容器水平地环切（roundslices）时的截面中，可以存在至少一个凹部，从进一步提高耐层间剥离性的观点考虑，优选存在2个以上（2~15个左右）、更优选存在3个以上（3~10个左右）、进一步优选存在4个以上（4~8个左右）的凹部。在将多层容器水平地环切时的截面中存在多个凹部的情况下，各个凹部的t1/t0比可以相同，也可以不同。
本发明的多层容器的具有前述气体阻隔层的层叠结构优选为3层或5层。从使多层容器的气体阻隔性良好的观点考虑，由前述层叠结构形成的部位的质量优选为整个多层容器的30质量%以上，更优选为40质量%以上，更优选为50质量%以上，更优选为60%以上，进一步优选为70%以上，特别优选为80以上。
多层容器的最外层和最内层的厚度以及除气体阻隔层以外的各层的厚度分别优选为0.01~2mm，更优选为0.05~1.5mm；气体阻隔层的厚度优选为0.005~0.2mm（5~200μm），更优选为0.01~0.15mm（10~150μm）。另外，多层容器的厚度在整个瓶中并不需要是固定的，通常优选为0.2~4mm左右。
在本发明的多层容器中，相对于由具有气体阻隔层的层叠结构形成的部位的总质量，气体阻隔层的质量优选为1~20质量%。如果在该范围内，则气体阻隔性变得良好，而且由作为前体的多层预成型坯成型为多层容器变得容易。以该观点考虑，相对于由具有气体阻隔层的层叠结构形成的部位的总质量，气体阻隔层的质量更优选为2~15质量%，进一步优选为3~10质量%。
本发明的多层容器由于耐层间剥离性和气体阻隔性优异，因而适合用作液体饮料、液体食品等的容器，对其形状没有特别限制，优选为瓶体。
（除气体阻隔层以外的层的成分）
对构成本发明的多层容器中含有的、除气体阻隔层以外的层（包括最外层和最内层。）的成分没有特别限制，可以使用饮料容器等多层容器中所使用的成分。作为构成气体阻隔层以外的层的成分，例如可列举出聚对苯二甲酸乙二醇酯（PET）、聚乳酸（PLA）、聚2,6-萘二甲酸乙二醇酯（PEN）等热塑性聚酯树脂；热塑性共聚聚酯树脂；聚烯烃系树脂；脂肪族聚酰胺树脂；聚碳酸酯树脂；聚丙烯腈树脂；聚氯乙烯树脂；聚苯乙烯树脂等。它们可以单独使用1种，也可以组合使用2种以上。作为组合使用2种以上的成分，可列举出将PET和PEN掺混而成的成分等。其中，优选为聚酯树脂（以下称为聚酯（A））。此外，并不排除最外层和最内层以及其它的任一层也具有气体阻隔性，也可以所有的层均具有气体阻隔性，但从制造成本的观点等考虑，通常采用利用上述成分夹持气体阻隔层的方式。
作为聚酯（A），适宜使用聚对苯二甲酸乙二醇酯（PET）或聚乳酸（PLA）。其中，聚对苯二甲酸乙二醇酯由于其在透明性、机械强度、注射成型性、拉伸吹塑成型性方面均体现优异的特性，因而更为优选。
在此，聚对苯二甲酸乙二醇酯是指通常二元羧酸成分的80摩尔%以上、优选90摩尔%以上为对苯二甲酸，且二元醇成分的80摩尔%以上、优选90摩尔%以上为乙二醇的聚酯。作为剩余部分的除对苯二甲酸以外的酸成分，可以使用间苯二甲酸、4,4-二苯醚二甲酸、1,4-萘二甲酸、2,6-萘二甲酸、己二酸、癸二酸、1,10-癸二羧酸、六氢对苯二甲酸。另外，作为剩余部分的除乙二醇以外的二元醇成分，可列举出丙二醇、1,4-丁二醇、新戊二醇、二乙二醇、环己烷二甲醇、2,2’-双(4-羟基乙氧基苯基)丙烷、2,2-双(4-羟基乙氧基苯基)丙烷等。此外，作为热塑性聚酯树脂的原料单体，还可以使用对羟基苯甲酸等羟基酸。
聚酯（A）的特性粘度优选为0.55~1.3，更优选为0.65~1.2，进一步优选为0.70~0.9。特性粘度为0.55以上时，能够得到透明的非晶状态的多层预成型坯，此外，所得多层容器的机械强度也变得充分。如果特性粘度为1.3以下，则在成型时容易进行瓶成型而不会使流动性受损。此外，特性粘度（η）使用苯酚/四氯乙烷=6/4（质量比）的混合溶剂。另外，特性粘度的测定根据ASTM D4603-03、ASTM D1601等而求出。
本发明的多层容器的最外层或最内层优选主要由聚酯（A）构成，在不损害本发明的特征的范围内，可以在聚酯（A）中配合使用其它的热塑性树脂、各种添加剂。此时，优选最外层或最内层的90质量%以上为聚酯（A）。
作为其它的热塑性树脂，可列举出聚2,6-萘二甲酸乙二醇酯等热塑性聚酯树脂、聚烯烃系树脂、聚碳酸酯、聚丙烯腈、聚氯乙烯、聚苯乙烯等。
另外，作为添加剂，可列举出紫外线吸收剂，氧吸收剂，着色剂，用于促进预成型坯的加热、在成型时缩短循环时间的红外吸收剂（再热添加剂，reheat additive）等。
（气体阻隔层的成分）
对构成本发明的多层容器中含有的气体阻隔层的成分没有特别限制，可以使用公知的具有气体阻隔性的树脂。作为构成气体阻隔层的成分，优选满足下述透氧系数的成分，例如可列举出含有间苯二甲基的聚酰胺树脂（MX尼龙树脂）等聚酰胺树脂；乙烯-醋酸乙烯酯共聚物树脂；聚丙烯腈树脂；聚偏二氯乙烯树脂；聚乙醇酸（PGA）等。这些成分可以单独使用1种，也可以组合使用2种以上。其中，从气体阻隔性及再循环性的观点考虑，优选为聚酰胺树脂，更优选为含有间苯二甲基的聚酰胺树脂。
本说明书中，“具有气体阻隔性”是指，在成型为多层容器时，在温度23℃、相对湿度80%RH的条件下，构成气体阻隔层的层自身的透氧系数为1.0cc·mm/(m2·day·atm)以下。该透氧系数优选为0.8cc·mm/(m2·day·atm)以下，更优选为0.20cc·mm/(m2·day·atm)以下，进一步优选为0.15cc·mm/(m2·day·atm)以下，特别优选为0.09cc·mm/(m2·day·atm)以下。通过将具有前述气体阻隔性的树脂用作气体阻隔层，能够使所得多层容器的气体阻隔性能变得良好、延长要保存的内容物的保质期。
作为优选用作气体阻隔层的成分的、含有间苯二甲基的聚酰胺树脂（MX尼龙树脂），优选的是，将含有70摩尔%以上间苯二甲胺的二胺成分与含有50摩尔%以上碳原子数4~20的α,ω-直链脂肪族二元羧酸的二元羧酸成分缩聚而得到的聚酰胺（以下称为聚酰胺（B））。该聚酰胺（B）的阻隔性能好，此外，在与前述聚酯（A）的共注射成型性、共拉伸吹塑成型性方面体现优异的特性，成型性良好。
聚酰胺（B）中的二胺成分优选含有70摩尔%以上、更优选含有75摩尔%以上、进一步优选含有80摩尔%以上的间苯二甲胺。如果二胺成分中的间苯二甲胺量为70摩尔%以上，则聚酰胺（B）的气体阻隔性变得良好。
在聚酰胺（B）中，作为除间苯二甲胺以外的能够使用的二胺成分，可列举出：四亚甲基二胺、五亚甲基二胺、2-甲基戊二胺、六亚甲基二胺、七亚甲基二胺、八亚甲基二胺、九亚甲基二胺、十亚甲基二胺、十二亚甲基二胺、2,2,4-三甲基六亚甲基二胺、2,4,4-三甲基六亚甲基二胺等脂肪族二胺；1,3-双(氨甲基)环己烷、1,4-双(氨甲基)环己烷、1,3-环己烷二胺、1,4-环己烷二胺、双(4-氨基环己基)甲烷、2,2-双(4-氨基环己基)丙烷、双(氨甲基)萘烷、双(氨甲基)三环癸烷等脂环式二胺；双(4-氨基苯基)醚、对苯二胺、对苯二甲胺、二(氨甲基)萘等具有芳香环的二胺类等，但并不限于这些二胺成分。
聚酰胺（B）中的二元羧酸成分优选含有50摩尔%以上、更优选含有70摩尔%以上、进一步优选含有80摩尔%以上的碳原子数4~20的α,ω-直链脂肪族二元羧酸。α,ω-直链脂肪族二元羧酸为上述范围时，聚酰胺具有优异的气体阻隔性和成型性。作为碳原子数4~20的α,ω-直链脂肪族二元羧酸，例如可列举出琥珀酸、戊二酸、庚二酸、辛二酸、壬二酸、己二酸、癸二酸、十一烷二酸、十二烷二酸等脂肪族二元羧酸。其中，优选为己二酸、癸二酸。
另外，在聚酰胺（B）中，作为除α,ω-直链脂肪族二元羧酸以外的二元羧酸，可列举出对苯二甲酸、间苯二甲酸、2,6-萘二甲酸等芳香族二元羧酸类。
作为聚酰胺（B）的二元羧酸成分，优选的是，使用包含100~50摩尔%的碳原子数4~20的α,ω-直链脂肪族二元羧酸、0~50摩尔%的芳香族二元羧酸的二元羧酸成分。
聚酰胺（B）可以通过熔融缩聚法来制造。例如，通过以下方法制造：将由间苯二甲胺和己二酸形成的尼龙盐在水的存在下、在加压状态下升温，边除去所加入的水和缩合水边使尼龙盐以熔融状态进行聚合的方法。另外，也可以通过将间苯二甲胺直接加入到熔融状态的己二酸中，并在常压下缩聚的方法进行制造。此时，为了使反应体系维持均匀的液态，将间苯二甲胺连续地加入到己二酸中，其间以反应温度不低于生成的低聚酰胺和聚酰胺的熔点的方式边对反应体系升温边进行缩聚。此外，在缩聚反应时，还可以添加少量的一元胺、一元羧酸作为分子量调节剂。
另外，聚酰胺（B）也可以在采用熔融聚合法制造后，通过进行固相聚合来进行缩聚。对聚酰胺的制造方法没有特别限制，采用以往公知的方法、聚合条件进行制造。
这些MX尼龙树脂的相对粘度通常为1.5以上就是适合的，优选为2~4，更优选为2.1~3.5。此外，相对粘度为将1g树脂溶解在100ml 96%硫酸中、使用凯能-芬斯克型粘度计在25℃下测定时的粘度。
聚酰胺（B）的数均分子量优选为18000~43500，更优选为20000~30000。为该范围时，多层成型品的成型良好，所得多层容器的耐层间剥离性优异。此外，聚酰胺（B）的数均分子量为18000~43500时，聚酰胺（B）的相对粘度约为2.3~4.2，聚酰胺（B）的数均分子量为20000~30000时，聚酰胺（B）的相对粘度约为2.4~3.2。
为了提高熔融成型时的加工稳定性，或者为了防止聚酰胺（B）的着色，可以在聚酰胺（B）中添加磷化合物。作为该磷化合物，优选使用包含碱金属或碱土金属的磷化合物。例如可列举出磷酸、次磷酸、亚磷酸的钠、镁、钙等碱金属盐或碱土金属盐，尤其是使用了次磷酸的碱金属盐或碱土金属盐的聚酰胺（B）的防止聚酰胺着色的效果特别优异，因而优选使用。聚酰胺（B）中的磷化合物的浓度以磷原子计优选为1~500ppm，更优选为350ppm以下，进一步优选为200ppm以下。即使磷原子浓度超过500ppm，也无法再提高防止着色的效果。另外，磷原子浓度如果为500ppm以下，利用添加有该磷化合物的聚酰胺（B）而得到的薄膜的雾度值不会过度上升。
以提高耐层间剥离性为目的，可以在聚酰胺（B）中添加其它的聚酰胺。例如可列举出：公知作为聚(己内酰胺)的聚(6-氨基己酸)（PA-6）、聚(己二酰己二胺)（PA-6,6）、聚(7-氨基庚酸)（PA-7）、聚(10-氨基癸酸)（PA-10）、聚(11-氨基十一烷酸)（PA-11）、聚(12-氨基十二烷酸)（PA-12）、聚(癸二酰己二胺)（PA-6,10）、聚(壬二酰己二胺)（PA-6,9）、聚(己二酰丁二胺)（PA-4,6）的均聚物，己内酰胺/己二酰己二胺共聚物（PA-6,6/6）、己二酰己二胺/己内酰胺共聚物（PA-6/6,6）等脂肪族聚酰胺；聚(间苯二甲酰己二胺)（PA-6I）、间苯二甲酰己二胺/对苯二甲酰己二胺共聚物（PA-6I/6T）、聚(间苯二甲酰间苯二甲胺)（PA-MXDI）、己内酰胺/间苯二甲酰间苯二甲胺共聚物（PA-6/MXDI）、己内酰胺/间苯二酰己二胺共聚物（PA-6/6I）等无定形半芳香族聚酰胺等，并且不限于这些聚酰胺。
前述气体阻隔层优选主要由聚酰胺（B）构成，从气体阻隔性能的观点考虑，更优选包含70质量%以上、进一步优选包含80质量%以上、特别优选包含90质量%以上的聚酰胺（B）。
在不明显损害本发明的效果的前提下，可以在前述气体阻隔层中掺混聚酯、烯烃、苯氧基树脂等其它树脂中的1种或多种。
另外，可以添加玻璃纤维、碳纤维等无机填充剂；玻璃鳞片、滑石、高岭土、云母、蒙脱石、有机粘土等板状无机填充剂；各种弹性体类等耐冲击性改性材料；结晶成核剂；脂肪酸酰胺系、脂肪酸金属盐系、脂肪酸酰胺系化合物等润滑剂；铜化合物、有机或无机卤素系化合物、受阻酚系、受阻胺系、肼系、硫系化合物、磷系化合物等抗氧化剂；热稳定剂；防着色剂；苯并三唑系等紫外线吸收剂；脱模剂；增塑剂；着色剂；阻燃剂；作为赋予氧捕捉能力的化合物的、包含钴金属的化合物，以防止聚酰胺凝胶化为目的的碱化合物等添加剂。
（多层容器用模具）
关于本发明的多层容器，通过使用以下的模具，即使不采用会提高制造成本之类的特殊装置、工艺烦杂的成型方法，也能够制造。下面对该模具进行详细地说明。
本发明的多层容器用模具（以下有时简称为模具）具有以下特征，其具备：（I）设置有模腔的冷半部；以及（II）设置有连接第一压射缸的内部和模腔的第一树脂流路、连接第二压射缸的内部和模腔的第二树脂流路、以及第一树脂流路和第二树脂流路的合流部的热半部，该热半部（II）所具有的前述合流部位于向前述冷半部（I）所具有的模腔开口的浇口部的上游，且在第二树脂流路内具有部分地阻碍树脂流动的装置。
另外，在本说明书中，“上游”是指压射缸侧，“下游”是指模腔侧。
本发明的模具是用于成型多层容器的装置中所使用的模具，例如图1所示那样地、由热半部（22）和冷半部（21）构成。热半部（22）具有使通过注射成型装置的螺杆而熔融塑化的树脂维持熔融状态地流动的配管。热半部（22）具有连接第一压射缸（10A）的内部和模腔（25）的第一树脂流路（23A）、连接第二压射缸（10B）的内部和模腔（25）的第二树脂流路（23B）、以及第一树脂流路（23A）和第二树脂流路（23B）进行合流的合流部。第二树脂流路（23B）中流动有作为构成多层容器的气体阻隔层的成分的第二树脂（例如聚酰胺（B）等）。第一树脂流路（23A）中流动有作为构成最外层和最内层的成分的第一树脂（前述“除构成气体阻隔层的成分以外的树脂”、例如聚酯（A）等）。此外，第一树脂也可以具有气体阻隔性。
冷半部（21）为将熔融塑化的树脂注射、冷却并成型为多层容器的部分。冷半部（21)的内部具有至少1个以上的模腔。
作为一般的多层成型装置用模具的结构，可以参考日本特开平11-165330、日本特开昭63-99918、日本特表2001-504763等。本发明的模具的特征在于模具的热半部（22）的第二树脂流路（23B）中具有部分地阻碍树脂流动的装置（28）（参照图1~3）。
将第一树脂流路（23A）、第二树脂流路（23B）沿与树脂的流动方向垂直的面进行切割时，本发明的模具的截面的流路的配管的形状优选为圆形，但并不限定于前述形状，也可以制成矩形等任意形状。
在本发明的模具中，通过在第二树脂流路（23B）内设置部分地阻碍树脂流动的装置，可以使所得多层容器的第二树脂层（气体阻隔层）的一部分中产生由于树脂流动受到阻碍而导致层的厚度变薄的部位，具体来说，产生厚度达到第二树脂层最大厚度的如上所述的0.01~0.9倍的部位（凹部）。另外，图8表示使用本发明的模具而成型的多层容器中的第二树脂层（气体阻隔层）的截面形状的一个实施方式。
如此，通过改变多层容器的第二树脂层圆周方向的厚度，来抑制多层容器的层间剥离。通常认为改变厚度会造成表面积增加，因而会促进层间剥离，但是第一树脂层呈楔入第二树脂层的形状，结果却带来了与预测相反的效果。推测这是因为形成了前述形状，对多层容器施加冲击等应力时，第二树脂层相对于第一树脂层的冲击随动性增强，因而提高了多层容器的耐层间剥离性。
在本发明的模具中，第二树脂流路（23B）内配置的部分地阻碍树脂流动的装置配置于第二树脂流路（23B）的侧壁，从增强第二树脂层相对于第一树脂层的冲击随动性而提高耐层间剥离性的观点考虑，该装置的配置数量优选为2个以上，更优选为3个以上，进一步优选为4个以上。对于配置数量的上限值没有特别限制，从增强第二树脂层相对于第一树脂层的冲击随动性而提高耐层间剥离性的观点考虑，优选为15个以下，更优选为12个以下，进一步优选为10个以下，特别优选为8个以下。因而，从相同的观点考虑，部分地阻碍树脂流动的装置的配置数量优选为2~15，更优选为2~12，更优选为3~12，更优选为3~10，进一步优选为4~10，特别优选为4~8。
在本发明的模具中，部分地阻碍树脂流动的装置优选设置于第一树脂流路（23A）和第二树脂流路（23B）的合流部与第二压射缸（10B）之间的第二树脂流路（23B）内。该情况下，部分地阻碍树脂流动的装置配置在上述合流部附近，优选配置在该合流部的上游侧0cm~5cm之间，更优选配置在该合流部的上游侧0cm~3cm、进一步优选0cm~1cm、特别优选0cm~0.5cm之间。部分地阻碍树脂流动的装置按上述范围配置时，易于改变所得多层容器的第二树脂层圆周方向的厚度。
另外，在配置2个以上的部分地阻碍树脂流动的装置的情况下，关于相互的配置位置，可以以与第二树脂流路（23B）和第一树脂流路（23A）进行合流的合流部的距离相同的方式进行配置，也可以以距离不同的方式进行配置。
图4表示本发明的模具的一个实施方式。对部分地阻碍树脂流动的装置的形状进行说明。图5的（a）表示将部分地阻碍树脂流动的装置沿与树脂流路的树脂流动方向垂直的方向切割时的、截面（沿图4的A-A方向的切割面）的形状的示意图（其中，仅图示了一个部分地阻碍树脂流动的装置。）。
将部分地阻碍树脂流动的装置的截面（垂直方向）的直径方向的最长部的长度设为amm、并将圆周的切线方向的最长部的长度设为bmm时，从耐层间剥离性的观点考虑，该部分地阻碍树脂流动的装置a和b优选分别满足以下的式子。此外，直径方向的最长部的长度a与圆周的切线方向的最长部的长度b呈垂直关系。另外，r表示第二树脂流路的半径，优选为0.5~5mm，更优选为0.5~4mm，进一步优选为1~3mm。
0.01r≤a≤1r
0.01r≤b≤1r
a的下限值优选为0.03r，更优选为0.05r，进一步优选为0.1r。a的上限值优选为0.9r，更优选为0.8r，进一步优选为0.7r。
另外，b的下限值优选为0.03r，更优选为0.05r，进一步优选为0.1r。b的上限值优选为0.9r，更优选为0.8r，进一步优选为0.7r。
此外，对将部分地阻碍树脂流动的装置沿与树脂流路的树脂流动方向垂直的方向切割时的、截面的形状没有特别限制，例如可列举出：除与流路接触的面以外的部分的形状为圆形、半圆形、三角形、四边形、梯形等多边形，矩形（参照图6）。
下面，图5的（b）表示将部分地阻碍树脂流动的装置沿与树脂流路的树脂流动方向平行的方向切割时的、截面（沿图4的B-B方向的切割面）的形状的示意图（其中，仅图示了一个部分地阻碍树脂流动的装置。）。
将部分地阻碍树脂流动的装置的截面（平行方向）的直径方向的最长部的长度设为amm、并将与树脂流动平行方向的最长部的长度设为ymm时，从耐层间剥离性的观点考虑，该部分地阻碍树脂流动的装置的a和y优选分别满足以下的式子。此外，直径方向的最长部的长度a和与树脂流动平行的方向的最长部的长度y呈垂直关系。另外，r如上述定义，优选范围也相同。
0.01r≤a≤1r
0.01r≤y≤2r
a的下限值优选为0.03r，更优选为0.05r，进一步优选为0.1r。a的上限值优选为0.9r，更优选为0.8r，进一步优选为0.7r。各个下限值及上限值可以选择任意的组合。
另外，y的下限值优选为0.03r，更优选为0.05r，进一步优选为0.1r。y的上限值优选为1.8r，更优选为1.5r。各个下限值及上限值可以选择任意的组合。
此外，对将部分地阻碍树脂流动的装置沿与树脂流路的树脂流动方向平行的方向切割时的、截面的形状没有特别限制，例如可列举出：除与流路接触的面之外的部分的形状为圆形、半圆形、三角形、四边形、梯形等多边形，矩形。
作为部分地阻碍树脂流动的装置，前述a、b和y为以上范围时，存在第二树脂层相对于第一树脂层的冲击随动性增强而进一步提高耐层间剥离性的倾向。
作为本发明的模具的部分地阻碍树脂流动的装置的整体形状，例如，可以为线状、针状、棒状、板状、圆柱状、半圆柱状、球状，也可以为三角锥状、长方体状、正方体状、圆锥状、梯形状，且并不限于这些形状。
另外，对构成部分地阻碍树脂流动的装置的材料没有特别限制，例如可以是与模具相同的金属材料，也可以是铁、铝、铜、锌等金属，还可以是具有与该金属的附着性的热固性树脂。
[多层容器的制造方法]
本发明还提供以下的多层容器的制造方法。
一种多层容器的制造方法，其特征在于，其使用前述多层容器用模具进行成型，前述多层容器具有在最内层和最外层之间至少具有气体阻隔层的3层以上的层叠结构，且在由前述层叠结构形成的部位中，前述气体阻隔层具有厚度（t1）达到该气体阻隔层最大厚度（t0）的0.01~0.9倍的部位；以及
一种多层容器的制造方法，其特征在于，其使用前述多层容器用模具形成多层预成型坯，接着对该多层预成型坯进行吹塑成型，前述多层容器具有在最内层和最外层之间至少具有气体阻隔层的3层以上的层叠结构，且在由前述层叠结构形成的部位中，前述气体阻隔层具有厚度（t1）达到该气体阻隔层最大厚度（t0）的0.01~0.9倍的部位。
本发明的多层容器可以使用如上前述的本发明的多层容器用模具进行制造，具体来说，可以使用具有两个压射缸的注射成型机，将聚酯（A）由第一树脂流路（23A）侧的压射缸、将具有气体阻隔性的树脂（气体阻隔性树脂）由第二树脂流路（23B）侧的压射缸经由热半部（22）注射入冷半部（21）的模腔（25）内来进行制造。
本发明的多层容器可以直接使用用本发明的模具成型的多层容器，也可以使用用本发明的模具成型为多层预成型坯（例如部分具有3层或5层的层叠结构的预成型坯）、接着通过加热处理并进行吹塑成型而成的多层容器（例如部分具有3层或5层的层叠结构的多层容器）。优选为将多层预成型坯吹塑成型而得到的多层容器。作为多层容器，可列举出多层瓶和多层杯等。
对具有3层或5层的层叠结构的多层预成型坯的制造方法没有特别限制，可以利用公知的方法。例如，可以如下制造3层结构（第一树脂层/第二树脂层/第一树脂层）的多层预成型坯：通过由第一树脂流路（23A）侧的压射缸注射构成最内层和最外层的树脂、由第二树脂流路（23B）侧的压射缸注射构成气体阻隔层的树脂的工序，持续注射第一树脂，同时注射需要量的第二树脂，之后停止注射第一树脂而制造。另外，可以使用第一树脂层流动于第二树脂层的中心的模具（参照图6的（d）），持续注射第一树脂，同时注射需要量的第二树脂，之后停止注射第一树脂来制造3层结构（第一树脂层/第二树脂层/第一树脂层）的多层预成型坯。
另外，可以如下制造5层结构（第一树脂层/第二树脂层/第一树脂层/第二树脂层/第一树脂层）的多层预成型坯：通过使用由第一树脂流路（23A）侧的压射缸注射构成最内层和最外层的第一树脂、由第二树脂流路（23B）侧的压射缸注射第二树脂的工序，首先注射第一树脂，接着单独注射第二树脂，最后注射第一树脂来充满模腔（25）而制造。
另外，制造多层预成型坯的方法不仅限于上述方法。
使用本发明的模具成型得到的多层预成型坯可以通过进一步双轴拉伸吹塑成型而成型为多层容器。例如，双轴拉伸吹塑时，优选将多层预成型坯的表面加热至90~110℃而进行吹塑成型，该加热温度更优选为95~108℃。为该加热温度范围内时，吹塑成型性良好，且构成最外层、最内层的第一树脂层（聚酯（A）层）未因冷拉伸而白化，第二树脂层（气体阻隔层）未因结晶化而白化，耐层间剥离性变得更好。另外，可以使用红外辐射温度计测定表面温度。通常可以将辐射率设定为0.95来进行测定。此外，加热多层预成型坯的表面时，通常优选用多台以上的加热器进行加热，并且加热器的输出平衡也重要。优选的是，根据外界气温、多层预成型坯的表面的加热温度，适当调整加热器的输出平衡、加热时间。
使用本发明的模具成型的多层容器的成型性良好，难以因掉落、冲击而引发层间剥离。另外，即使是含有凹凸部、弯曲部的形状也难以引发层间剥离，因而多层容器的形状不限于凹凸部、弯曲部少的形状，设计自由度变大。本发明的多层容器适合于容纳、保存例如碳酸饮料、果汁、水、牛奶、啤酒、葡萄酒、日本酒、威士忌、烧酒、咖啡、茶、果冻饮料、健康饮料等液体饮料，调味液、沙司（sauce）、酱油、沙拉酱（dressing）、液体高汤等调味料，液体汤等液体系食品，液态药品，化妆水，化妆乳液，美发剂，染发剂，洗发水等各种物品。
实施例
以下，参照附图并根据实施例对本发明进一步进行详细地说明，但本发明并不限定于这些实施例。另外，各个实施例或比较例中制造的多层容器的各种评价按照以下的方法进行。
（1）耐层间剥离性的评价方法
根据ASTM D2463-95方法（Procedure）B，通过容器的下落试验求出层间剥离高度，作为耐层间剥离性的指标。首先在多层容器内注满水并封盖，然后从任意的高度使多层容器下落，通过目视判定有无层间剥离。此时，以多层容器的底部与地面接触的方式使多层容器垂直下落。下落高度的间隔设为15cm，所有测试容器数设为30个。
其中，层间剥离高度越高，表示耐层间剥离性越好。
（2）透氧率（OTR）的测定方法
根据ASTM D3985测定多层容器的透氧率（OTR），作为气体阻隔性的指标。具体来说，使用透氧率测定装置（MODERNCONTROLS,INC制造类型：OX-TRAN 2/61）测定23℃、瓶内部100%RH、瓶外部50%RH下的透氧率[cc/(bottle·day·0.21atm)]。
其中，数值越低，表示氧的透过量越少、气体阻隔性越高。
（3）多层容器的气体阻隔层的最大厚度（t0）以及凹部的厚度（t1）的测定方法
将多层容器从底面接地部位以1cm的间隔进行环切，截面涂布碘酒。可见到气体阻隔层被碘酒染色成红褐色~黑色。使用KEYENCE CORPORATION制造的数码显微镜观察该截面，测定厚度并求出t0和t1。
＜实施例1＞
使用前述的如图1所示的模具（20）。在距该模具（20）的第一树脂流路（23A）和第二树脂流路（23B）的合流部0.1cm上游侧的、第二树脂流路（23B）的侧壁上，如图7的（a）所示地在树脂流路的侧壁等间距地配置4个形状相同的圆柱状（直径0.2mmφ、长度3mm）的部分地阻碍树脂流动的装置（成分：与模具相同的金属）。
部分地阻碍树脂流动的装置的形状：圆柱状、r=1.5mm
向与树脂流路垂直的方向切出的截面：a=0.2mm、b=0.2mm
向与树脂流路平行的方向切出的截面：a=0.2mm、y=3.0mm
使用聚对苯二甲酸乙二醇酯（Japan Unipet Co.Ltd.,制造“RT543C”，特性粘度：0.75dl/g）作为最外层及最内层用的第一树脂。另外，使用聚酰胺MXD6（N-MXD6、三菱瓦斯化学株式会社制造“MX nylon S6007”、相对粘度：2.70、透氧率：0.1cc·mm/m2·day·atm）作为气体阻隔层用的第二树脂。
使用上述模具（20）和名机制作所制造的注射成型机（类型：M200，四射成型（four-shot molding）），按照下述条件持续注射第一树脂，同时注射第二树脂，之后停止注射第一树脂，从而注射成型为由“第一树脂层/第二树脂层/第一树脂层”构成的全长95mm、外径22mm、壁厚4.2mm、重量27g的3层预成型坯，并使其冷却。
接着，按照下述条件对所得3层预成型坯进行双轴拉伸吹塑成型，得到全长223mm、外径65mm、内部容积500ml、底部形状为花瓣（pataloid）型的多层容器。以下记载了吹塑条件。
所得多层容器的评价结果示于表1。
（3层预成型坯的注射成型条件）
第一树脂流路侧的压射缸温度 ：270℃
第二树脂流路侧的压射缸温度 ：260℃
模具内的树脂流路温度 ：270
模具冷却水温度 ：15℃
多层预成型坯中的第二树脂的比例：5质量%
（双轴拉伸吹塑成型条件）
吹塑成型机：类型“EFB 1000ET”（Frontier公司制造）
预成型坯加热温度 ：101℃
拉伸杆用压力 ：0.5MPa
一次吹塑压力 ：07MPa
二次吹塑压力 ：2.5MPa
一次吹塑延迟时间 ：0.34sec
一次吹塑时间 ：0.30sec
二次吹塑时间 ：2.0sec
吹塑排气时间 ：0.6sec
模具温度 ：30℃
＜实施例2＞
在实施例1中，除了将部分地阻碍模具内的树脂流动的装置变更为表1前述的形状以外，同样地得到多层容器。所得多层容器的评价结果示于表1。
＜制造例1＞
（聚癸二酰间苯二甲胺（N-MXD10）的合成）
将反应釜内的癸二酸（伊藤制油株式会社制造，TA级）以170℃加热熔融后，边搅拌内容物，边以与癸二酸的摩尔比达到1:1的方式缓慢滴加间苯二甲胺（三菱瓦斯化学株式会社制造），并加热升温至240℃。滴加结束后，进一步加热升温至260℃。
反应结束后，以股线状取出内容物，并用造粒机颗粒化，将所得颗粒投入桶混机中，在减压下进行固相聚合，得到调节分子量后的聚癸二酰间苯二甲胺（以下称为N-MXD10）。N-MXD10的熔点为191℃、玻璃化转变温度为60℃、数均分子量为23000、透氧系数为0.8cc·mm/m2·day·atm。
＜比较例1＞
在实施例1中，除了不在第二树脂流路内设置部分地阻碍模具内的树脂流动的装置以外，同样地得到多层容器。所得多层容器的评价结果示于表1。
＜实施例3＞
在实施例1中，将部分地阻碍模具内的树脂流动的装置变更为表1所述的形状，使用聚乳酸（PLA、Unitika Limited制造，TERRAMAC等级TP-4000）作为第一树脂，使用制造例1中得到的聚癸二酰间苯二甲胺（N-MXD10）作为第二树脂，除此以外，同样地得到多层容器。所得多层容器的评价结果示于表1。
＜比较例2＞
在实施例3中，除了不在第二树脂流路内设置部分地阻碍模具内的树脂流动的装置以外，同样地得到多层容器。所得多层容器的评价结果示于表1。
＜实施例4＞
在实施例1中，除了将部分地阻碍模具内的树脂流动的装置变更为表1所述的形状（变更为a=0.63mm）以外，同样地得到多层容器。所得多层容器的评价结果示于表1。
[表1]
1)距第一树脂流路和第二树脂流路的合流部的距离
2)沿与树脂流路的树脂的流动方向垂直的方向切割时的截面
3)沿与树脂流路的树脂的流动方向平行的方向切割时的截面
由表1可知，使用本发明的设置有部分地阻碍树脂流动的装置的模具成型的多层容器显示非常优异的耐层间剥离性，与此相对，而使用未设置有部分地阻碍树脂流动的装置的模具成型的多层容器的耐层间剥离性差。
产业上的可利用性
本发明的多层容器的成型性良好，不难以因掉落、冲击而引发层间剥离。另外，即使是含有凹凸部、弯曲部的形状也难以引发层间剥离，因而多层容器的形状不限于凹凸部、弯曲部少的形状，设计自由度变大。本发明的多层容器适合于容纳、保存例如碳酸饮料、果汁、水、牛奶、啤酒、葡萄酒、日本酒、威士忌、烧酒、咖啡、茶、果冻饮料、健康饮料等液体饮料，调味液、沙司、酱油、沙拉酱、液体高汤等调味料，液体汤等液体系食品，液态药品，化妆水，化妆乳液，美发剂，染发剂，洗发水等各种物品。
附图标记说明
20…模具
21…冷半部
22…热半部
23A、23B…树脂流路
24…浇口部
25…模腔
26…浇口裁切销（gate cut pin）
27…气压缸
28…部分地阻碍树脂流动的装置
40A、40B…树脂或熔融树脂
a…部分地阻碍树脂流动的装置沿A-A方向的截面的直径方向的最长部的长度
b…部分地阻碍树脂流动的装置沿A-A方向的截面的圆周的切线方向的最长部的长度
y…相对于树脂流动方向的水平方向的最长部的长度
Claims (13)
1.一种多层容器，其特征在于，该多层容器具有在最内层与最外层之间至少具有气体阻隔层的3层以上的层叠结构，
在由所述层叠结构形成的部位中，所述气体阻隔层具有厚度达到该气体阻隔层最大厚度的0.01~0.9倍的部分。
2.根据权利要求1所述的多层容器，其中，由所述层叠结构形成的部位的质量是整个多层容器的30质量%以上。
3.根据权利要求1或2所述的多层容器，其中，所述层叠结构为3层或5层的层叠结构。
4.根据权利要求1~3中任一项所述的多层容器，其中，构成所述气体阻隔层的成分为选自聚酰胺树脂、乙烯-醋酸乙烯酯共聚物树脂、聚丙烯腈树脂、聚偏二氯乙烯树脂以及聚乙醇酸中的至少1种。
5.根据权利要求4所述的多层容器，其中，所述聚酰胺树脂为含有间苯二甲基的聚酰胺树脂。
6.根据权利要求1~5中任一项所述的多层容器，其中，构成所述层叠结构的最内层、最外层的成分分别为选自热塑性聚酯树脂、热塑性共聚聚酯树脂、聚烯烃类树脂、脂肪族聚酰胺树脂、聚碳酸酯树脂、聚丙烯腈树脂、聚氯乙烯树脂以及聚苯乙烯树脂中的至少1种。
7.根据权利要求1~6中任一项所述的多层容器，其为瓶体。
8.一种多层容器用模具，其特征在于，其具备：
（I）设置有模腔的冷半部、以及
（II）设置有连接第一压射缸的内部和模腔的第一树脂流路、连接第二压射缸的内部和模腔的第二树脂流路、以及第一树脂流路和第二树脂流路的合流部的热半部，
该热半部（II）所具有的所述合流部位于向所述冷半部（I）所具有的模腔开口的浇口部的上游，且在第二树脂流路内具有部分地阻碍树脂流动的装置。
9.根据权利要求8所述的多层容器用模具，其中，部分地阻碍树脂流动的装置是在第二树脂流路内的至少一部分设置凸部的装置，
在与第二树脂流路的流动方向垂直的方向的截面上，将直径方向的最长部的长度设为amm、并将圆周的切线方向的最长部的长度设为bmm时，a和b满足以下关系：
0.01r≤a≤1r （式1)
0.01r≤b≤1r （式2）
上述式中，r表示第二树脂流路的半径（mm）。
10.根据权利要求8或9所述的多层容器用模具，其中，部分地阻碍树脂流动的装置是在第二树脂流路内的至少两处设置凸部的装置。
11.根据权利要求8~10中任一项所述的多层容器用模具，其中，所述凸部设置在第一树脂流路和第二树脂流路的合流部的上游侧0cm~5cm之间。
12.一种多层容器的制造方法，其特征在于，其使用权利要求8~11中任一项所述的模具进行成型，所述多层容器具有在最内层和最外层之间至少具有气体阻隔层的3层以上的层叠结构，且在由所述层叠结构形成的部位中，所述气体阻隔层具有厚度达到该气体阻隔层最大厚度的0.01~0.9倍的部分。
13.一种多层容器的制造方法，其特征在于，其使用权利要求8~11中任一项所述的模具形成多层预成型坯，接着对该多层预成型坯进行吹塑成型，所述多层容器具有在最内层和最外层之间至少具有气体阻隔层的3层以上的层叠结构，且在由所述层叠结构形成的部位中，所述气体阻隔层具有厚度达到该气体阻隔层最大厚度的0.01~0.9倍的部分。
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| EP2618982B1 (en) * | 2010-09-21 | 2018-10-31 | Mold-Masters (2007) Limited | Coinjection hot runner injection molding system |
-
2011
- 2011-04-15 MX MX2012012151A patent/MX2012012151A/es active IP Right Grant
- 2011-04-15 CN CN201180020373.XA patent/CN102869489B/zh active Active
- 2011-04-15 WO PCT/JP2011/059443 patent/WO2011132622A1/ja active Application Filing
- 2011-04-15 RU RU2012149956/05A patent/RU2570053C2/ru not_active IP Right Cessation
- 2011-04-15 US US13/642,367 patent/US8815359B2/en active Active
- 2011-04-15 JP JP2012511645A patent/JP5783169B2/ja active Active
- 2011-04-15 EP EP11771957.5A patent/EP2561970B1/en active Active
- 2011-04-15 BR BR112012027108A patent/BR112012027108A2/pt not_active Application Discontinuation
- 2011-04-15 KR KR1020127027628A patent/KR101863897B1/ko active IP Right Grant
- 2011-04-18 TW TW100113387A patent/TWI545007B/zh not_active IP Right Cessation
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2014
- 2014-04-10 US US14/250,011 patent/US9701076B2/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3825036A (en) * | 1971-05-19 | 1974-07-23 | Creators Ltd | Reinforced plastics tubes |
| US6344249B1 (en) * | 1999-03-11 | 2002-02-05 | Mitsubishi Gas Chemical Company, Inc. | Multi-layered article |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103978635A (zh) * | 2014-04-21 | 2014-08-13 | 上海翔洲电气科技有限公司 | 一种矿用挂接式电缆挂钩的注塑工艺 |
| CN104097298A (zh) * | 2014-07-21 | 2014-10-15 | 常熟市金马模具有限公司 | 一种注塑模具潜浇口 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2561970B1 (en) | 2021-07-21 |
| TWI545007B (zh) | 2016-08-11 |
| CN102869489B (zh) | 2016-05-25 |
| EP2561970A1 (en) | 2013-02-27 |
| KR101863897B1 (ko) | 2018-05-31 |
| KR20130077817A (ko) | 2013-07-09 |
| RU2012149956A (ru) | 2014-05-27 |
| US20140220167A1 (en) | 2014-08-07 |
| JP5783169B2 (ja) | 2015-09-24 |
| US8815359B2 (en) | 2014-08-26 |
| EP2561970A4 (en) | 2014-08-13 |
| BR112012027108A2 (pt) | 2016-07-26 |
| TW201202021A (en) | 2012-01-16 |
| US9701076B2 (en) | 2017-07-11 |
| US20130095265A1 (en) | 2013-04-18 |
| WO2011132622A1 (ja) | 2011-10-27 |
| JPWO2011132622A1 (ja) | 2013-07-18 |
| RU2570053C2 (ru) | 2015-12-10 |
| MX2012012151A (es) | 2012-11-21 |
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