CN106163799B - 吸氧性多层容器及其制造方法 - Google Patents
吸氧性多层容器及其制造方法 Download PDFInfo
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- CN106163799B CN106163799B CN201580016033.8A CN201580016033A CN106163799B CN 106163799 B CN106163799 B CN 106163799B CN 201580016033 A CN201580016033 A CN 201580016033A CN 106163799 B CN106163799 B CN 106163799B
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- oxygen
- oxygen uptake
- laminated vessel
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Abstract
一种吸氧性多层容器,其依次具有至少如下的3层:第一树脂层:其含有热塑性树脂;吸氧层:其含有包含聚酯化合物(a)和过渡金属催化剂的吸氧性树脂组合物,所述聚酯化合物(a)含有具有萘满环的结构单元;和第二树脂层:其含有与前述第一树脂层中含有的前述热塑性树脂同种的热塑性树脂,所述吸氧性多层容器包含玻璃化转变温度为50~110℃的环烯烃聚合物作为前述热塑性树脂。
Description
技术领域
本发明涉及吸氧性多层容器及其制造方法。
背景技术
作为受到氧气的影响而容易发生变质或劣化的各种物品,例如可以举出食品、饮料、药品、化妆品等。出于防止这样的各种物品的氧气氧化、长期保存的目的,使用对容纳有这些各种物品的包装体内的氧气进行去除的吸氧剂。
另外,还提出了许多对于容纳这些各种物品的容器自身赋予吸氧性的吸氧性容器。其中,作为在从低湿度至高湿度的宽泛的湿度条件下氧气阻隔性能和吸氧性能优异的吸氧性容器,开发了含有具有规定的萘满环的聚合物和过渡金属催化剂的吸氧性多层容器(参照专利文献1)。
现有技术文献
专利文献
专利文献1:国际公开第2013/077436号
发明内容
发明要解决的问题
然而,专利文献1等中记载的现有的吸氧性多层容器等中存在以各层中使用的树脂的组合等难以以高水平兼顾耐冲击性、成型加工性、透明性全部的问题。
本发明是鉴于上述事实作出的,其目的在于,提供耐冲击性、成型加工性、以及透明性优异的吸氧性多层容器。
用于解决问题的方案
本发明人等对吸氧性多层容器进行了深入研究,结果发现,如下的吸氧性多层容器能够解决上述课题,至此完成了本发明,所述吸氧性多层容器依次具有至少如下的3层:第一树脂层:其含有热塑性树脂(b);吸氧层:其含有包含聚酯化合物(a)和过渡金属催化剂的吸氧性树脂组合物,所述聚酯化合物(a)含有具有萘满环的结构单元;和第二树脂层:其含有热塑性树脂(b),所述吸氧性多层容器使用玻璃化转变温度为50~110℃的环烯烃聚合物作为热塑性树脂(b)。
即,本发明如下。
<1>一种吸氧性多层容器,其依次具有至少如下的3层:
第一树脂层:其含有热塑性树脂;
吸氧层:其含有包含聚酯化合物(a)和过渡金属催化剂的吸氧性树脂组合物,所述聚酯化合物(a)含有具有萘满环的结构单元;和
第二树脂层:其含有与前述第一树脂层中含有的前述热塑性树脂同种的热塑性树脂,
所述吸氧性多层容器包含玻璃化转变温度为50~110℃的环烯烃聚合物作为前述热塑性树脂。
<2>根据上述<1>所述的吸氧性多层容器,其中,前述热塑性树脂在剪切速率为1216sec-1且温度为260℃时的熔融粘度为100~300Pa·sec。
<3>根据上述<1>或<2>所述的吸氧性多层容器,其中,前述热塑性树脂在剪切速率为1216sec-1且温度为260℃时的熔融粘度与前述聚酯化合物(a)在剪切速率为1216sec-1且温度为260℃时的熔融粘度之差的绝对值为0~150Pa·sec。
<4>根据上述<1>~<3>中任一项所述的吸氧性多层容器,其中,前述聚酯化合物(a)包含下述式(1)所示的结构单元。
<5>根据上述<4>所述的吸氧性多层容器,其中,前述式(1)所示的结构单元相对于前述聚酯化合物(a)含有的全部结构单元的比率为50~100摩尔%。
<6>根据上述<1>~<5>中任一项所述的吸氧性多层容器,其中,前述过渡金属催化剂包含选自由锰、铁、钴、镍和铜组成的组中的至少1种过渡金属。
<7>根据上述<1>~<6>中任一项所述的吸氧性多层容器,其中,相对于前述聚酯化合物100质量份,以过渡金属量计包含0.001~10质量份前述过渡金属催化剂。
<8>一种吸氧性多层容器的制造方法,其是上述<1>~<7>中任一项所述的吸氧性多层容器的制造方法,其包括如下的工序:
从注射料筒注射出前述第一层、前述吸氧层、以及前述第二层至少这3层,从而制成多层容器,
前述工序中,前述第一层的注射料筒温度与前述吸氧层的注射料筒温度之差的绝对值为0~30℃。
发明的效果
根据本发明能够提供耐冲击性、成型加工性、以及透明性优异的吸氧性多层容器。另外,吸氧性多层容器的成型加工性得到改善,因此能够提供外观更加优异的吸氧性多层容器。
具体实施方式
以下,对用于实施本发明的方式(以下,简称为“本实施方式”)进行说明。需要说明的是,下面的本实施方式是用于说明本发明的例示,本发明不限于以下内容。本发明可在其主旨的范围内适宜地变形而实施。
本实施方式的吸氧性多层容器依次具有至少如下的3层:第一树脂层(层B1),其含有热塑性树脂(b);吸氧层(层A),其含有包含聚酯化合物(a)和过渡金属催化剂的吸氧性树脂组合物,所述聚酯化合物(a)含有具有萘满环的结构单元;和第二树脂层(层B2),其含有与第一树脂层中含有的热塑性树脂同种的热塑性树脂(b),所述吸氧性多层容器包含玻璃化转变温度为50~110℃的环烯烃聚合物作为热塑性树脂(b)。以下,有时将第一树脂层(层B1)和第二树脂层(层B2)概括为“层B”。
本实施方式的吸氧性多层容器使用玻璃化转变温度为50~110℃的环烯烃聚合物(COP)作为热塑性树脂(b)来吸收容器内的氧气,因此即使在自容器外透过或侵入容器壁面的氧气为少量的情况下,也能够吸收该透过或侵入的氧气,从而防止要保存的内容物品(被保存物)因氧气导致的变质等。
对于本实施方式的吸氧性多层容器的层构成,只要这些层以B1/A/B2的顺序排列,就对吸氧层(层A)和树脂层(层B(层B1、B2))的个数、种类没有特别限制。例如,进而也可以是具有2个层B的B/B/A/B/B这3种5层的构成。另外,本实施方式的吸氧性多层容器根据需要也可以包含粘接层(层AD)等任意层,例如也可以是B/AD/B/A/B/AD/B这4种7层的构成。
[吸氧层(层A)]
本实施方式的吸氧层(层A)含有包含聚酯化合物(a)和过渡金属催化剂的吸氧性树脂组合物,所述聚酯化合物(a)具有萘满环作为结构单元。
<聚酯化合物(a)>
聚酯化合物(a)只要是具有萘满环作为结构单元的聚酯化合物就没有特别限制,例如可以使用专利文献1等中记载的聚酯化合物。从成型加工性和吸氧性能的观点出发,优选含有选自由下述通式(i)~(iv)组成的组中的至少1个具有萘满环的结构单元的聚酯化合物(a)。尤其,通式(i)所示的结构单元更优选选自由下述式(1)~(3)组成的组中的至少1个。进而,其中,进一步优选具有下述式(1)的结构单元的聚酯化合物。此处,“具有…作为结构单元”表示化合物中具有1个以上该结构单元。这样的结构单元优选作为重复单元包含于聚酯化合物(a)中。如此,聚酯化合物为聚合物时,也可以是上述结构单元的均聚物、上述结构单元与其它结构单元的无规共聚物、上述结构单元与其它结构单元的嵌段共聚物中的任一者。
(式中,R各自独立地表示氢原子或一价的取代基,一价的取代基为选自由卤原子、烷基、烯基、炔基、芳基、杂环基、氰基、羟基、羧基、酯基、酰胺基、硝基、烷氧基、芳氧基、酰基、氨基、硫代基、烷基硫代基、芳基硫代基、杂环硫代基、以及酰亚胺基组成的组中的至少1种,它们也可以进一步具有取代基。m表示0~3的整数,n表示0~7的整数,萘满环的苄基位的至少一者键合有氢原子。X表示含有选自由芳香烃基、饱和或不饱和的脂环式烃基、直链状或支链状的饱和或不饱和的脂肪族烃基、以及杂环基组成的组中的至少1个基团的2价基团。)
进而,从成型加工性和吸氧性能的观点出发,上述式(1)所示的结构单元相对于聚酯化合物(a)含有的全部结构单元的比率优选为50~100摩尔%,更优选为70~100摩尔%,进一步优选为90~100摩尔%。将式(1)所示的结构单元的比率设为上述范围,从而进一步提高本实施方式的效果,能够以更高的水平维持吸氧性多层容器的耐冲击性、成型加工性、透明性、以及吸氧性能等物性的平衡。
进而,聚酯化合物(a)可以还含有来自3元以上的多元醇、3元以上的多元羧酸及其衍生物、3元以上的羟基羧酸及其衍生物中的至少1种多官能化合物的结构单元。这些多官能化合物可以单独使用1种,也可以组合使用2种以上。含有来自这些多官能化合物的结构单元时,可向聚酯化合物(a)中导入支链结构,能够得到分子量比通常高且粘度提高了的聚酯化合物(a)。作为多官能化合物,可以举出甘油、三羟甲基丙烷、季戊四醇等多元醇;偏苯三酸、偏苯三酸酐、均苯四甲酸、均苯四甲酸酐等多元羧酸及其衍生物;等,但不限于此。其中,优选甘油。
聚酯化合物(a)含有来自多官能化合物的结构单元时,来自多官能化合物的结构单元相对于聚酯化合物(a)含有的全部结构单元的比率优选为0.01~5摩尔%,更优选为0.1~3摩尔%,进一步优选为0.2~1摩尔%。
聚酯化合物(a)可由专利文献1等中记载的公知的方法来进行制造。例如,可以将作为单体具有萘满环的单体或其衍生物与二元醇等多官能化合物或其衍生物进行缩聚来得到。进而,也可以以不影响性能的程度在聚酯化合物(a)中引入不具有萘满环的结构单元作为共聚成分。具体而言,也可以将专利文献1中记载的公知的化合物用作共聚成分。
聚酯化合物(a)优选在萘满环的苄基位中的至少1者具有氢原子。可以认为,通过组合使用萘满环的苄基位具有氢原子的聚酯化合物与过渡金属催化剂,苄基位的氢被夺走,从而体现出优异的吸氧性能(但本实施方式的作用不限于此)。
另外,本实施方式的吸氧性树脂组合物在其优选的方案中能够抑制吸氧后的低分子量化合物的生成。其理由虽不明确,但例如可推测是基于以下氧化反应的机理。即,可以认为,聚酯化合物(a)中,首先,位于萘满环的苄基位的氢被夺走而生成自由基,其后,通过自由基与氧气的反应,苄基位的碳被氧化,生成羟基或酮基。因此可以推测,吸氧性树脂组合物中不存在氧化反应导致的分子链的切断,能够维持聚酯化合物(a)的结构,因此在吸氧后不易生成成为气味的原因的低分子量的有机化合物,其结果,能够抑制吸氧后的气味强度的增大并且能够防止低分子量化合物向内容物中的混入(但本实施方式的作用不限于此)。
对聚酯化合物(a)的玻璃化转变温度(Tg)没有特别限制,从吸氧性多层容器的成型加工性等观点出发,优选为50~110℃,更优选为60~80℃,进一步优选为60~75℃,更进一步优选为65~75℃。通过将玻璃化转变温度设为上述范围,从而进一步提高吸氧性多层容器的成型加工性和吸氧速度。需要说明的是,此处所谓的玻璃化转变温度表示通过差示扫描量热测定测得的值,可由后述实施例中记载的方法来测定。
对聚酯化合物(a)的特性粘度(使用了苯酚与1,1,2,2-四氯乙烷的质量比6:4的混合溶剂的、25℃下的测定值)没有特别限制,从吸氧性多层容器的成型加工性的观点出发,优选为0.1~2.0dL/g,更优选为0.5~1.5dL/g,进一步优选为0.8~1.0dL/g。
对聚酯化合物(a)的熔融粘度没有特别限制,从吸氧性多层容器的成型加工性的观点出发,温度为260℃且剪切速率为1216sec-1时的熔融粘度优选为100~300Pa·sec,更优选为150~250Pa·sec。将熔融粘度设为上述范围,从而进一步提高吸氧性多层容器的成型加工性。
<过渡金属催化剂>
作为吸氧性树脂组合物中使用的过渡金属催化剂,只要是可作为聚酯化合物(a)的氧化反应的催化剂起作用的物质,就可以从公知的物质中适宜地选择使用,没有特别限制。
作为过渡金属催化剂的具体例子,例如可以举出过渡金属的有机酸盐、卤化物、磷酸盐、亚磷酸盐、次磷酸盐、硝酸盐、硫酸盐、氧化物、氢氧化物等。此处,作为过渡金属催化剂中包含的过渡金属,例如可以举出钛、钒、铬、锰、铁、钴、镍、铜、锌、钌、铑等,不限于此。其中,优选锰、铁、钴、镍、铜。另外,作为有机酸,例如可以举出乙酸、丙酸、辛酸、月桂酸、硬脂酸、乙酰丙酮、二甲基二硫代氨基甲酸、棕榈酸、2-乙基己酸、新癸酸、亚油酸、妥尔油酸(tolic acid)、油酸、癸酸、环烷酸等,不限于此。过渡金属催化剂优选将这些中的一种过渡金属与有机酸组合而成的催化剂,更优选的组合是:过渡金属为锰、铁、钴、镍或铜;有机酸为乙酸、硬脂酸、2-乙基己酸、油酸或环烷酸。需要说明的是,过渡金属催化剂可以单独使用1种,也可以组合使用2种以上。
过渡金属催化剂的含量可根据使用的聚酯化合物(a)、过渡金属催化剂的种类、以及所期望的性能来适宜地设定,没有特别限制。从吸氧性树脂组合物的吸氧性能的观点出发,过渡金属催化剂的含量相对于聚酯化合物(a)100质量份,以过渡金属量计优选为0.001~10质量份,更优选为0.002~2质量份,进一步优选为0.005~1质量份。
聚酯化合物(a)和过渡金属催化剂可用公知的方法进行混合,但优选利用挤出机进行混炼。通过使用挤出机,能够得到分散性更加良好的吸氧性树脂组合物。另外,在不过度有损本实施方式的效果的范围内,也可以在吸氧性树脂组合物中添加干燥剂、颜料、染料、抗氧剂、增滑剂、抗静电剂、稳定剂等添加剂;碳酸钙、粘土、云母、二氧化硅等填充剂;除臭剂等,但不限于以上所示的物质,可以混合各种材料。
需要说明的是,为了促进吸氧反应,本实施方式的吸氧性树脂组合物根据需要可以还含有自由基引发剂、光引发剂。另外,在不阻碍本实施方式的目的的范围内,本实施方式的吸氧性树脂组合物可与其它的热塑性树脂用挤出机进行混炼。这些自由基引发剂、光引发剂、其它的热塑性树脂可以使用专利文献1中记载的公知的物质。
层A中的热塑性树脂(a)的含量优选为50质量%以上,更优选为70质量%以上,进一步优选为90质量%以上。热塑性树脂(a)的含量为上述范围时,与小于50质量%的情况相比,能够进一步提高吸氧性能。
对吸氧层(层A)的厚度没有特别限制,优选为1~1000μm,更优选为20~800μm,进一步优选为50~700μm。将层A的厚度设为上述范围,从而能够不有损经济性、进一步提高吸氧性能。
[含有热塑性树脂(b)的树脂层(层B(层B1、B2))]
本实施方式的层B为含有热塑性树脂(b)的树脂层。对层B的热塑性树脂(b)的含有率没有特别限制,优选为70~100质量%,更优选为80~100质量%,进一步优选为90~100质量%。
本实施方式的吸氧性多层容器至少具有2层的层B,也可以具有3层以上,多个层B的构成可以相同或不同。从制造上的便利性、吸氧性多层容器的性能的观点出发,层B1和层B2优选为相同的成分组成。层B的厚度可根据用途来适宜地决定,从确保多层容器所需的掉落耐性等强度、柔软性等各种物性的观点出发,优选为5~1000μm,更优选为50~800μm,进一步优选为100~500μm。从制造上的便利性、吸氧性多层容器的性能的观点出发,优选层B1与层B2的厚度相同。
<热塑性树脂(b)>
热塑性树脂(b)包含玻璃化转变温度为50~110℃的环烯烃聚合物(COP)。COP是指,至少作为单体使用降冰片烯系单体进行开环聚合并对其氢化而成的聚合物。COP在分子结构中具有脂环结构、为非晶性。作为降冰片烯系单体,可以举出2-降冰片烯和/或具有取代基的2-降冰片烯化合物。作为具有取代基的2-降冰片烯化合物,可以举出:具有烷基、烷叉基、芳香基作为取代基的2-降冰片烯;以及这些取代基中具有卤素、羟基、酯基、烷氧基、氰基、酰胺基、酰亚胺基、甲硅烷基等的2-降冰片烯等。作为具体例子,可以举出2-降冰片烯、5-甲基-2-降冰片烯、5,5-二甲基-2-降冰片烯、5-乙基-2-降冰片烯、5-丁基-2-降冰片烯、5-乙叉基-2-降冰片烯、5-甲氧羰基-2-降冰片烯、5-氰基-2-降冰片烯、5-甲基-5-甲氧羰基-2-降冰片烯、5-苯基-2-降冰片烯、5-苯基-5-甲基-2-降冰片烯、5-己基-2-降冰片烯、5-辛基-2-降冰片烯、5-十八烷基-2-降冰片烯等。
COP也可以是在使降冰片烯系单体聚合时组合使用能够与降冰片烯系单体共聚的其它单体而使其共聚而成的聚合物。例如,也可以使用降冰片烯系单体和其它环烯烃类至少作为单体进行开环聚合。作为其它环烯烃类,例如可以举出环戊烯、环辛烯、双环戊二烯、甲基双环戊二烯、二甲基双环戊二烯、5,6-二氢双环戊二烯等。
聚合时,作为聚合催化剂将TiCl4、WCl6、MoCl5、VCl5、NiCl2、PdCl2等过渡金属化合物以及Al、Li、Na、Mg等典型金属的烷基化合物等组合而进行聚合。另外,也可以根据需要用公知方法、例如将Ni、Pd等作为催化剂进行氢化。
作为COP,可以使用公知的聚合物,例如可以举出日本特开平5-317411号公报等中记载的聚合物等。另外,COP可以使用市售品。作为这样的市售品,例如可以从Nippon ZeonCo.,Ltd.制造的“ZEONEX”(商标)、“ZEONOR”(商标)、大协精工公司制造的“Daikyo ResinCZ”(商标)等之类的等级中适宜地选择合适的市售品。COP还具有如下的优点:耐热性、耐光性等化学性质、耐化学试剂性等显示出如聚烯烃树脂那样的特征,另一方面机械特性、熔融、流动特性、尺寸精度等物理性质显示出作为非晶性树脂的特征。作为玻璃化转变温度为50~110℃的COP,例如可以举出Nippon Zeon Co.,Ltd.制造的商品名“ZEONEX 5000”(玻璃化转变温度68℃,在剪切速率为1216sec-1且温度为260℃时的熔融粘度194Pa·sec)等。
热塑性树脂(b)的玻璃化转变温度(Tg)为0~110℃,更优选为60~80℃,进一步优选为60~75℃。将玻璃化转变温度设为上述范围,从而进一步提高吸氧性多层容器的成型加工性。需要说明的是,此处所谓的玻璃化转变温度表示通过差示扫描量热测定测得的值,能够通过后述实施例中记载的方法进行测定。需要说明的是,对于COP的玻璃化转变温度(Tg),降冰片烯系单体的含量越多,Tg越趋于变低。另外,双环戊二烯等环烯烃类、3环以上的多环式降冰片烯系单体的含量越多,Tg越趋于变高。而且,越多地包含环状结构,Tg越趋于变高。基于这样的事实,若适宜地控制COP的结构,则能够有效地控制Tg。
进而,热塑性树脂(b)的玻璃化转变温度(Tg)与聚酯化合物(a)的玻璃化转变温度(Tg)之差的绝对值优选为0~40℃,更优选为0~20℃。玻璃化转变温度(Tg)的差的绝对值越小,吸氧性多层容器的成型加工性越进一步提高。
对热塑性树脂(b)的熔融粘度没有特别限制,从吸氧性多层容器的成型加工性的观点出发,在温度为260℃且剪切速率为1216sec-1时的熔融粘度优选为100~300Pa·sec,更优选为150~250Pa·sec。将熔融粘度设为上述范围,从而进一步提高吸氧性多层容器的成型加工性。
进而,热塑性树脂(b)在温度为260℃且剪切速率为1216sec-1时的熔融粘度与聚酯化合物(a)在温度为260℃且剪切速率为1216sec-1时的熔融粘度之差的绝对值优选为0~150Pa·sec,更优选为0~100Pa·sec。在温度为260℃且剪切速率为1216sec-1时的熔融粘度的差的绝对值越小,吸氧性多层容器的成型加工性越进一步提高。
在不过度有损本实施方式的效果的范围内,层B也可以还含有除COP以外的热塑性树脂、公知的添加剂。COP相对于构成层B的热塑性树脂组合物的总量的含量没有特别限制,优选为50~100质量%,从透明性的观点出发,更优选为70~100质量%,进一步优选为90~100质量%。
本实施方式的吸氧性多层容器在吸氧层(层A)、含有热塑性树脂(b)的层(层B(层B1,层B2))的基础上根据期望的性能等也可以还包含任意的层。作为这样的任意的层,例如可以举出粘接层等。
关于本实施方式的吸氧性多层容器,在相邻的2个层之间无法得到实用的层间粘接强度时,优选在该2个层之间设置粘接层(层AD)。粘接层优选包含具有粘接性的热塑性树脂。作为具有粘接性的热塑性树脂,例如可以举出将聚烯烃系树脂(聚乙烯或聚丙烯等)用不饱和羧酸(丙烯酸、甲基丙烯酸、马来酸、马来酸酐、富马酸、衣康酸等)改性而成的酸改性聚烯烃树脂、以聚酯系嵌段共聚物为主要成分的聚酯系热塑性弹性体等。作为粘接层,从粘接性的观点出发,优选使用与用作层B的热塑性树脂同种的树脂改性的物质。从发挥实用的粘接强度并且维持优异的成型加工性的观点出发,粘接层的厚度优选为2~100μm,更优选为5~90μm,进一步优选为10~80μm。
<吸氧性多层容器的制造方法>
对本实施方式的吸氧性多层容器的制造方法没有特别限制,优选通过注射成型法进行制造。进而,包括将第一层(层B1)、吸氧层(层A)、和第二层(层B2)至少这3层从注射料筒注射出来而制成多层容器的工序,该工序中,第一层(层B1)的注射料筒温度与吸氧层(层A)的注射料筒温度之差的绝对值更优选为0~30℃。例如,作为3层结构B/A/B的多层容器的制造方法,使用2台以上具备注射机的成型机、注射用模具,将构成层A的材料以及构成层B的材料从各自的注射料筒经由模具热流道注射到空腔内,从而能够制造与注射用模具的形状相对应的多层容器。该方法在各层B(层B1、层B2等)的成分组成相同时是特别适宜的。
另外,作为5层结构B/A/B/A/B的多层容器的制造方法,首先将构成层B的材料从注射料筒注射出来,接着将构成层A的材料单独从注射料筒注射出来,最后将其它的构成层B的材料从其它的注射料筒注射出来。由此充满空腔,从而能够制造5层结构B/A/B/A/B的多层容器。该方法在各层B(层B1、层B2等)的成分组成相同时是特别适宜的。
或者另外,作为5层结构B/A/B/A/B的多层容器的其它的制造方法,首先将构成层B的材料从注射料筒注射出来。接着,将构成层A的材料从其它的注射料筒注射出来的同时与其它的构成层B的树脂一起从其它的注射料筒同时注射出来。由此充满空腔,从而能够制造5层结构B/A/B/A/B的多层容器。该方法在各层B(层B1、层B2等)的成分组成相同时是特别适宜的。
从成型加工性的观点出发,构成层B的材料的注射温度与构成层A的材料的注射温度之差的绝对值优选为0~30℃,更优选为0~20℃,进一步优选为0~10℃。此处所谓的注射温度是指经过注射料筒的材料的温度。另外,从成型加工性的观点出发,各层的注射温度下的熔融粘度的差的绝对值优选为0~150Pa·sec,更优选为0~100Pa·sec。此处所谓的各层的熔融粘度是指,以注射温度经过注射料筒的材料的熔融粘度。
本实施方式的吸氧性多层容器的制造方法通常优选为注射成型法,但也可以利用压缩成型法等来得到多层成型体。例如,在热塑性树脂熔融物中设置吸氧性树脂剂,将该熔融块供给于阳模,并且利用阴模进行压缩,对压缩成型物进行冷却固化,从而得到成型体。另外,也可以利用挤出成型、压缩成型(片材成型、吹塑成型)等成型方法成型加工成所期望的容器形状。
[吸氧性多层容器]
对本实施方式的吸氧性多层容器的形状、大小等没有特别限制,可根据要容纳、保存的物品来适宜地设定。作为这样的容器形态的优选例,可以举出袋、杯子、盘、瓶、小瓶、安瓿、预填充注射器、真空采血管等。
进而,例如将片状(有时称为“薄膜状”)的吸氧性多层体进行制袋,能够制成三向密封的平袋、自立袋、角撑板包装袋、枕形包装袋、包括主室和副室且在主室和副室之间设置有易剥离壁的多室袋、收缩薄膜包装等。另外,通过实施热成型能够制成任意形状的容器。
更具体而言,将上述片材状的吸氧性多层体用真空成型、压空成型、模塞助压成型等方法进行成型,从而能够制作盘、杯子、瓶、管、PTP(压入包装)等规定形状的吸氧性多层容器。另外,使用注射机将熔融的树脂通过多层多重模具共注射或逐次注射到注射模具中,从而能够一次性地成型为规定形状的多层容器。
需要说明的是,在制作具有凸缘部的吸氧性多层容器时,也可以对该凸缘部实施赋予易剥离功能的特殊加工。另外,将上述吸氧性多层体用作容器的盖材、顶部密封等构件,从而能够赋予这些容器吸氧功能。
在使用本实施方式的吸氧性多层容器时,可照射能量射线从而促进吸氧反应的引发或者提高吸氧速度。作为能量射线,例如可以利用可见光、紫外线、X射线、电子射线、γ射线等。照射能量的量可根据所使用的能量射线的种类来适宜地选择。
本实施方式的吸氧性多层容器在吸氧时水分不是必须的,因此还具有在从低湿度至高湿度的宽泛的湿度条件(相对湿度0%~100%)下能够发挥优异的吸氧性能而且内容物的品质保持性也优异的优点。因此,适合各种特殊物品的保存、容纳。例如,还适合药品等的保存、容纳。例如,可填充维生素A、维生素B2、维生素B12、维生素C、维生素D、维生素E、维生素K等维生素剂;阿托品等生物碱;肾上腺素、胰岛素等激素剂;葡萄糖、麦芽糖等糖类;头孢曲松、头孢菌素、环孢菌素等抗生素;奥沙唑仑、氟硝西泮、氯噻西泮、氯巴占等苯并二氮系化学试剂;等,任意的天然物、化合物。本实施方式的吸氧性多层容器在填充这些天然物、化合物时,这些天然物、化合物的吸附量少,而且能够抑制由它们的氧化导致的变质,还能够抑制溶剂(例如水分)的蒸腾(transpiration)。另外,作为除药品以外的被保存物的具体例子,可以举出牛奶、果汁、咖啡、茶类、酒精饮料等饮料;酱、酱油、色拉调料等液体调味料;汤、炖菜、咖喱饭等烹饪食品;果酱、蛋黄酱等糊剂状食品;金枪鱼、鱼贝等水产制品;奶酪、黄油等乳加工品;肉、蒜肠、红肠、火腿等畜肉加工品;胡萝卜、马铃薯等蔬菜类;鸡蛋;面类;烹调前的米类、烹调过的米饭、米粥等加工米制品;粉末调味料、粉末咖啡、婴幼儿用奶粉、婴幼儿用烹饪食品、粉末节食食品、护理调理食品、干燥蔬菜、煎饼等干燥食品;农药、杀虫剂等化学品;化妆品;宠物食品;洗剂等各种物品,但不特别限于此。
[杀菌处理]
需要说明的是,在这些被保存物的填充(包装)前后,能够以适合被保存物的形式实施容器、被保存物的杀菌处理。作为杀菌方法,例如可以举出100℃以下的热水处理、100℃以上的加压热水处理、130℃以上的超高温加热处理等加热杀菌;紫外线、微波、γ射线等电磁波杀菌;环氧乙烷等气体处理;过氧化氢、次氯酸等化学试剂杀菌;等。
实施例
下面使用实施例和比较例对本发明进一步详细地说明,但本发明不因此而受限定。需要说明的是,除非另有说明,NMR测定是使用BRUKER公司制造的“AVANCE III-500”在室温下进行的。需要说明的是,下面的实施例中将小瓶作为例子举出,但对于安瓿、预填充注射器的所需特性与对于小瓶的所需特性为相同程度,因此关于这一点,本发明也不因这些实施例而使其范围受限。
后述制造例中得到的化合物等的各种物性值是根据以下测定方法和测定装置测定的。
(玻璃化转变温度的测定方法)
玻璃化转变温度是根据JIS K7122测定的。测定装置使用了差示扫描量热仪(DSC;岛津制作所社制,“DSC-60”)。需要说明的是,DSC的测定条件如下。
测定装置:岛津制作所社制,“DSC-60”
测定起始温度:25℃
升温速度:10℃/分钟
到达温度:220℃
降温速度:5℃/分钟
(熔融粘度的测定方法)
熔融粘度是使用东洋精机制作所社制造的毛细管流变仪“capillography 1D”在温度为260℃且剪切速率为1216sec-1的条件下测定的。
[单体合成例]
在内部容积18L的高压釜中投入2,6-萘二羧酸二甲酯2.20kg、2-丙醇11.0kg、活性炭上负载有5%钯的催化剂350g(50wt%含水制品)。接着,将高压釜内的空气用氮气进行置换,进而将氮气置换成氢气之后,供给氢气至高压釜内的压力成为0.8MPa。接着,启动搅拌机,将转速调节为500rpm,用30分钟将内温升高至100℃之后,进而供给氢气使压力成为1MPa。其后,为了应对反应的进行所带来的压力降低,持续供给氢气以维持1MPa。7小时后,压力降低消失,因此冷却高压釜,释放未反应的残留氢气,然后从高压釜取出反应液。过滤反应液,去除催化剂,然后用旋转蒸发器从分离滤液将2-丙醇蒸发掉。在得到的粗产物中加入2-丙醇4.40kg,通过重结晶进行纯化,以80%的收率(相对于2,6-萘二羧酸二甲酯的收率)得到2,6-萘满二羧酸二甲酯。需要说明的是,NMR的分析结果如下。1H‐NMR(400MHzCDCl3)δ7.76-7.96(2H m),7.15(1H d),3.89(3H s),3.70(3H s),2.70-3.09(5H m),1.80-1.95(1H m)。
<聚合物制造例>
(制造例1)
在具备填充塔式精馏塔、分凝器、全凝器、冷阱、搅拌机、加热装置、以及氮气导入管的聚酯树脂制造装置中投入单体合成例中得到的2,6-萘满二羧酸二甲酯543g、乙二醇217g、作为多官能化合物的甘油1.0g、钛酸四丁酯0.038g、乙酸锌0.15g,在氮气气氛下升温至230℃,进行酯交换反应。使二羧酸成分的反应转化率成为90%以上以后,用90分钟逐渐地进行升温和减压,在260℃、133Pa以下进行1小时缩聚,得到具有下述式(1)所示的重复结构的聚酯化合物(1)。
使用差示扫描量热仪(DSC)测定得到的聚酯化合物(1)的玻璃化转变温度和熔点。其结果,聚酯化合物(1)的玻璃化转变温度为69℃,由于是非晶性,因此无法确认熔点。另外,使用毛细管流变仪(东洋精机制作所社制,“capillography 1D”)测定聚酯化合物(1)的熔融粘度。将聚酯化合物(1)的物性示于表1。
[表1]
1)在剪切速率为1216sec-1且温度为260℃时的熔融粘度
<小瓶的制造>
根据下述条件从注射料筒注射构成层B的材料,接着从其它的注射料筒同时注射构成层A的材料与构成层B的树脂,接着以所需量注射构成层B的树脂,以充满注射模具内的空腔,得到B/A/B这3层结构的注射成型体。将得到的注射成型体冷却至规定的温度,转移至吹塑模具之后,进行吹塑成型,从而制造小瓶(瓶部)。以15秒循环1次的方式实施该工序,连续反复3小时(3小时的连续成型)。
·小瓶的总质量:5g
·层A的质量:小瓶的总质量的30质量%
<小瓶的形状>
将总高设为45mm、外径设为24mmφ、壁厚设为1mm。需要说明的是,小瓶的制造中使用了注射吹塑一体型成型机(日精ASB机械公司制,型号“ASB12N―10T”,取4个)。
<小瓶的评价>
对于实施例和比较例中得到的小瓶的成型加工性、掉落试验、透氧率、透明性,用以下方法测定并进行评价。
·成型加工性
根据小瓶(瓶部)的3层结构的外观等评价上述“<小瓶的制造>”中的小瓶(瓶部)的成型加工性。具体而言,根据以下基准来评价成型加工性。
(a)用目视判断层A与层B(层B1、层B2)的界面为不平滑、不整齐导致的外观的参差不齐的有无(“不整齐”的有无)。然后,求出判断为没有不整齐的小瓶的个数相对于通过3小时的连续成型而得到的小瓶的总数的比率。将该比率作为“获得率”(没有不整齐的小瓶的个数/小瓶的总数)。
(b)对树脂成分等附着在得到的小瓶的底部(与从模具注射出来时的浇口部相当)导致的凹凸的有无进行判断(“凹凸”的有无)。
A:获得率90%以上,无凹凸
B:获得率90%以上,有凹凸
C:获得率50%以上且小于90%,无凹凸
D:获得率50%以上且小于90%,有凹凸
E:获得率小于50%,无凹凸
F:获得率小于50%,有凹凸
·耐冲击性试验(掉落试验)
在小瓶中填充纯水10mL,用橡胶栓和铝盖进行密封。使该容器从1.5m的高度掉落,调查是否存在小瓶的破损。然后,破损时,将填充在内部的水由破裂处飞溅的情况判断为不良。对20个样品进行调查。需要说明的是,着地面为不锈钢制的平滑面,以使小瓶的底部接触着地面的方式使所述容器掉落。
·透氧率(OTR)
在23℃、小瓶外部的相对湿度50%、小瓶内部的相对湿度100%的气氛下,测定从测定开始起第30天的透氧率。测定使用了透氧率测定装置(MOCON公司制,商品名“OX-TRAN2-21 ML”)。测定值越低,表示氧气阻隔性越良好。需要说明的是,测定的检测阈值为透氧率5×10-5mL/(0.21atm·天·包装)。
·透明性
使用雾度仪(日本电色工业社制,“色差·浊度测定仪COH-400”)并根据JIS K7136测定小瓶的透明性(雾度值)。需要说明的是,将距小瓶底部15mm的小瓶侧面部作为测定位置。
(实施例1)
相对于聚酯化合物(1)100质量份,以钴量为0.02质量份的方式将硬脂酸钴(II)进行干混合,得到吸氧性树脂组合物。使用该吸氧性树脂组合物作为构成层A的树脂,另外,层B使用环烯烃聚合物1(Nippon Zeon Co.,Ltd.制,商品名“ZEONEX 5000”,玻璃化转变温度68℃,剪切速率为1216sec-1且温度为260℃时的熔融粘度194Pa·sec)。然后,在以下所示成型条件下制造小瓶,进行评价。需要说明的是,小瓶的注射时,不存在树脂对模具的附着,上述“成型加工性”的评价结果为“A”。将实施例1的制造条件和物性示于表2。
(小瓶的成型条件)
层A用注射料筒温度:260℃
层B用注射料筒温度:260℃
注射模具内树脂流道温度:260℃
注射模具温度:50℃
吹塑成型冷却水温度:30℃
循环时间:15秒
(比较例1)
层B使用环烯烃聚合物2(Nippon Zeon Co.,Ltd.制,商品名“ZEONEX 690R”,玻璃化转变温度136℃,剪切速率为1216sec-1且温度为260℃的熔融粘度362Pa·sec)以及设为以下所示的成型条件,除此以外,与实施例1同样地制造小瓶,进行评价。需要说明的是,小瓶的注射时,在连续成型开始后30分钟以内可确认树脂对模具的附着,连续成型时,树脂一旦附着于模具上,其后在制造的小瓶的底部连续地产生了凹凸。并且,上述“·成型加工性”的评价结果为“F”。将比较例1的制造条件和物性结果示于表2。
(小瓶的成型条件)
层A用注射料筒温度:260℃
层B用注射料筒温度:300℃
注射模具内树脂流道温度:300℃
注射模具温度:90℃
吹塑成型冷却水温度:30℃
循环时间:15秒
[表2]
1)剪切速率为1216sec-1且温度为260℃时的熔融粘度
2)单位:mL/(0.21atm·天·包装),检测阈值:5×10-5mL/(0.21atm·天·包装)
如由表2明确的那样,还至少确认到,实施例1具有良好的氧气阻隔性,成型加工性、耐冲击性、透明性优异。
本申请基于2014年3月26日向日本专利特许厅申请的日本专利申请(日本特愿2014-062918),将其内容作为参照并援引入本文。
产业上的可利用性
本发明的吸氧性多层容器可用于保存以食品、饮料、药品、化妆品为代表的各种对象物的容器等广泛的用途。
Claims (6)
1.一种吸氧性多层容器,其依次具有至少如下的3层:
第一树脂层:其含有热塑性树脂;
吸氧层:其含有包含聚酯化合物(a)和过渡金属催化剂的吸氧性树脂组合物,所述聚酯化合物(a)含有具有萘满环的结构单元;和
第二树脂层:其含有与所述第一树脂层中含有的所述热塑性树脂同种的热塑性树脂,
所述吸氧性多层容器包含玻璃化转变温度为50~110℃的环烯烃聚合物作为所述热塑性树脂,
所述热塑性树脂与所述聚酯化合物(a)的玻璃化转变温度之差的绝对值为0~40℃,
其中,所述聚酯化合物(a)包含下述式(1)所示的结构单元,所述式(1)所示的结构单元相对于所述聚酯化合物(a)含有的全部结构单元的比率为50~90摩尔%,
。
2.根据权利要求1所述的吸氧性多层容器,其中,所述热塑性树脂在剪切速率为1216sec-1且温度为260℃时的熔融粘度为100~300Pa・sec。
3.根据权利要求1或2所述的吸氧性多层容器,其中,所述热塑性树脂在剪切速率为1216sec-1且温度为260℃时的熔融粘度与所述聚酯化合物(a)在剪切速率为1216sec-1且温度为260℃时的熔融粘度之差的绝对值为0~150Pa・sec。
4.根据权利要求1或2所述的吸氧性多层容器,其中,所述过渡金属催化剂包含选自由锰、铁、钴、镍和铜组成的组中的至少1种过渡金属。
5.根据权利要求1或2所述的吸氧性多层容器,其中,相对于所述聚酯化合物100质量份,以过渡金属量计包含0.001~10质量份所述过渡金属催化剂。
6.一种吸氧性多层容器的制造方法,其是权利要求1~5中任一项所述的吸氧性多层容器的制造方法,其包括如下的工序:从注射料筒注射出所述第一层、所述吸氧层、以及所述第二层至少这3层,从而制成多层容器,
所述工序中,所述第一层的注射料筒温度与所述吸氧层的注射料筒温度之差的绝对值为0~30℃。
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