CN111630112B - 吸氧性树脂组合物及容器 - Google Patents
吸氧性树脂组合物及容器 Download PDFInfo
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- CN111630112B CN111630112B CN201980009674.9A CN201980009674A CN111630112B CN 111630112 B CN111630112 B CN 111630112B CN 201980009674 A CN201980009674 A CN 201980009674A CN 111630112 B CN111630112 B CN 111630112B
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- resin composition
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Images
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Abstract
本发明提供一种具有高吸氧性能的吸氧性树脂组合物。本发明提供的吸氧性树脂组合物的特征在于,是含有包含铁粉及卤化金属的吸氧剂、和树脂的吸氧性树脂组合物,铝的含量为50质量ppm以下。
Description
技术领域
本发明涉及吸氧性树脂组合物及容器。
背景技术
作为包装容器,使用金属罐、玻璃瓶、各种塑料容器等,然而从轻量性、抗冲击性、成本等观点出发,在各种用途中尤其使用塑料容器。然而,就金属罐、玻璃瓶而言,基本上没有穿过容器壁的氧透过,而在塑料容器的情况下会轻微地产生穿过容器壁的氧透过,因此在内容物的保存性的方面存在有问题。因此,使用具备包含能够吸收氧的吸氧剂和树脂的吸氧层的塑料容器。
作为所述吸氧剂,一般使用铁系吸氧剂(例如专利文献1及2)。
现有技术文献
专利文献
专利文献1:日本特开平4-90848号公报
专利文献2:日本特开2007-284632号公报
发明内容
发明所要解决的问题
专利文献1及2中记载的铁系吸氧剂虽然具有高吸氧性能,然而在与树脂混合使用时存在其吸氧性能降低的情况,期望进一步的改良。
本发明的目的在于,提供具有高吸氧性能的吸氧性树脂组合物及容器。
用于解决问题的方法
本发明的吸氧性树脂组合物的特征在于,是含有包含铁粉及卤化金属的吸氧剂、和树脂的吸氧性树脂组合物,铝的含量为50质量ppm以下。
本发明的容器的特征在于,具有包含所述吸氧性树脂组合物的吸氧层。
发明效果
根据本发明,能够提供具有高吸氧性能的吸氧性树脂组合物及容器。
附图说明
图1是表示本发明的实施方式的容器的一例的剖视图。
图2是表示实施例1~3、比较例1~4的相对于铝含量而言的吸氧量的曲线图。
具体实施方式
[吸氧性树脂组合物]
本发明的吸氧性树脂组合物含有包含铁粉及卤化金属的吸氧剂、和树脂。此处,该吸氧性树脂组合物的铝的含量为50质量ppm以下。
就树脂、特别是烯烃系树脂而言,在其制造工序中通常使用包含铝的催化剂作为催化剂。在反应后该催化剂被使用中和剂等除去,然而在所得的树脂中作为催化剂残渣而包含一定量以上的铝。
本发明人等发现,在含有包含铁粉及卤化金属的吸氧剂、和树脂的吸氧性树脂组合物中,在树脂中超过给定量地包含铝的情况下,该铝会阻碍铁与氧的反应,使铁的吸氧性能降低。具体而言,由于铝与铁相比离子化倾向更高,因此铝比铁更优先地与氧及水反应,形成铝的氧化被膜。可以推测,一旦在铁粉上形成铝的氧化被膜,铁与氧的反应就受到阻碍,因此铁的吸氧性能降低。因而,本发明人等发现,在含有包含铁粉及卤化金属的吸氧剂、和树脂的吸氧性树脂组合物中,通过将该组合物中的铝的含量设为50质量ppm以下,能够抑制铝的氧化被膜形成,提高吸氧性能。
特别是,本发明的吸氧性树脂组合物中,由于铁能够发挥高吸氧性能,因此能够降低组合物中的吸氧剂的含量,能够降低制造成本。另外,作为树脂的制造中催化剂的除去工序中使用的中和剂,一般使用水滑石,然而由于在水滑石中包含铝,因此该组合物优选不包含水滑石。需要说明的是,作为水滑石以外的中和剂,例如使用金属皂系中和剂。以下,对本发明的详情进行说明。
(吸氧剂)
本发明中吸氧剂包含铁粉及卤化金属。作为该铁粉,可以使用还原铁粉、雾化铁粉、电解铁粉、羰基铁粉等公知的铁粉。它们当中,可以合适地使用多孔且比表面积较大的还原铁粉、特别是回转窑还原铁粉(日文原文:ロータリー還元鉄粉)。回转窑还原铁粉由于纯度高、比表面积大,因此吸氧性能优异。这些铁粉可以使用一种,也可以并用两种以上。吸氧剂中的铁粉的含量优选为3~40质量%,更优选为5~30质量%。
作为所述卤化金属,可以举出碱金属、碱土金属、铜、锌、铁等的卤化物。具体而言,可以举出氯化钠、溴化钠、碘化钠、氯化钾、溴化钾、碘化钾、氯化钙、氯化镁、氯化钡等。它们当中优选氯化钠。这些卤化金属可以使用一种,也可以并用两种以上。
所述卤化金属优选相对于作为吸氧剂的主剂的铁粉100质量份配合0.1~10质量份,更优选配合1~5质量份。通过相对于铁粉100质量份配合0.1质量份以上的卤化金属,能够获得充分的吸氧性能。另外,通过相对于铁粉100质量份配合10质量份以下的卤化金属,能够抑制由铁粉含量的降低所致的吸氧性能的降低,另外能够抑制由卤化金属的渗出所致的外观不良、向内容物的附着。
本发明的吸氧剂可以在铁粉及卤化金属以外还包含碱性物质。通过包含碱性物质,能够降低因铁与水的反应而生成的氢的产生量。作为所述碱性物质,例如可以举出氢氧化镁、氢氧化钙、氢氧化锶、氢氧化钡、碳酸镁、碳酸钙、碳酸锶、碳酸钡等。它们当中,优选氢氧化钙、作为氢氧化钙的脱水物的氧化钙。这些碱性物质可以使用一种,也可以并用两种以上。
在吸氧剂包含碱性物质的情况下,所述碱性物质优选相对于铁粉100质量份配合0.5~2质量份,更优选配合1~2质量份。通过相对于铁粉100质量份配合0.5质量份以上的碱性物质,能够充分地降低氢的产生量。另外,通过相对于铁粉100质量份配合2质量份以下的碱性物质,能够获得充分的吸氧性能。
吸氧剂例如可以利用以下的方法制备。首先,将铁粉粗粉碎后,加入卤化金属及根据需要使用的碱性物质并一边混合一边微粉碎。作为混合粉碎的方法,可以采用振动磨机、球磨机、管磨机、高速混合机等公知的机构。另外也可以不同时地进行粉碎和混合,而是采用向制备成适当的粒度的铁粉的表面喷雾并覆盖含有卤化金属及根据需要使用的碱性物质的溶液的方法。
然后,在以从微粉碎物中除去粗大粒子的方式分级后,进行热处理。分级操作可以通过筛分、风力分级等来进行。对于热处理而言,优选与氧(空气)存在下的热处理一起,组合非活性气体气氛下、适合为氮气氛下的热处理地进行。具体而言,优选在氧的存在下进行热处理,在该热处理工序前和/或后在氮气氛下进行热处理。氧气氛下的热处理温度优选为400~600℃,更优选为500~550℃。热处理时间优选为2~12小时,更优选为4~10小时。氮气氛下的热处理温度优选为400~600℃,更优选为500~550℃。热处理时间优选为0~6小时,更优选为0~2小时。热处理后根据需要可以以除去粗大粒子的方式分级,得到吸氧剂。
(树脂)
作为本发明的吸氧性树脂组合物中含有的树脂,没有特别限定,然而可以使用热塑性树脂。具体而言,可以举出低-、中-或高-密度的聚乙烯、聚丙烯、乙烯-丙烯共聚物、聚1-丁烯、乙烯-1-丁烯共聚物、丙烯-1-丁烯共聚物、乙烯-丙烯-1-丁烯共聚物、聚甲基-1-戊烯、乙烯-乙酸乙烯酯共聚物、乙烯-(甲基)丙烯酸共聚物、离子交联烯烃共聚物(离聚物)、乙烯-乙烯醇共聚物或它们的共混物等烯烃系树脂、聚苯乙烯、苯乙烯-丁二烯共聚物、苯乙烯-异戊二烯共聚物、ABS树脂等苯乙烯系树脂、聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、二醇类改性聚对苯二甲酸乙二醇酯、聚乳酸、聚丁二酸丁二醇酯等聚酯、尼龙6、尼龙66等聚酰胺、聚碳酸酯等。它们当中,优选烯烃系树脂,更优选聚丙烯。这些树脂可以使用一种,也可以并用两种以上。
(吸氧性树脂组合物的制造方法)
本发明的吸氧性树脂组合物可以通过将所述吸氧剂配合到所述树脂中并混合而得到。混合可以是熔融共混也可以是干式共混。在配合少量的吸氧剂的情况下,优选制备高浓度地含有吸氧剂的母料,将该母料混合到树脂中。
(铝的含量)
在本发明的吸氧性树脂组合物中,铝的含量为50质量ppm以下。若铝的含量大于50质量ppm,则吸氧性能降低。铝的含量优选为45质量ppm以下,更优选为40质量ppm以下,进一步优选为30质量ppm以下,特别优选为20质量ppm以下。需要说明的是,铝的含量的范围的下限没有特别限定,铝的含量更少时铁与氧的反应更不受阻碍,因此优选。需要说明的是,铝的含量是利用ICP分析装置(商品名:720-ES、Varian制)测定的值。
如前所述,在制造树脂时有时使用包含铝的催化剂作为催化剂、另外使用包含铝的水滑石作为中和剂。因而,可以通过使用催化剂残渣少的树脂、使用不包含水滑石的树脂等,将吸氧性树脂组合物的铝的含量调节为50质量ppm以下。
(吸氧剂的含量)
在本发明的吸氧性树脂组合物中,所述吸氧剂的含量优选为30质量%以下,更优选为10质量%以上且30质量%以下,进一步优选为20质量%以上且27质量%以下。本发明的吸氧性树脂组合物中,由于铁能够发挥高吸氧性能,因此能够使组合物中的吸氧剂的含量为30质量%以下,能够降低制造成本。另外,能够提高成形性、作为容器的特性。
[容器]
本发明的容器具有包含本发明的吸氧性树脂组合物的吸氧层。由于本发明的吸氧性树脂组合物具有高吸氧性能,因此具有包含该组合物的吸氧层的本发明的容器显示出高吸氧性能,并显示出高内容物保存性。特别是,由于该吸氧层具有高吸氧性能,因此本发明的容器能够降低阻氧层、吸氧层的厚度,能够降低制造成本。
本发明的容器只要具有包含本发明的吸氧性树脂组合物的吸氧层,其构成就没有特别限定,然而优选具有包含该吸氧层的多层结构,更优选具有包含该吸氧层作为中间层的多层结构。将本发明的容器的容器壁的构成的一例表示于图1中。图1所示的容器具有从外侧起依次为外层1/粘接层2a/阻氧层3/粘接层2b/吸氧层4/内层5的层构成。由于相对于吸氧层4在外侧设置有阻氧层3,因此能够在利用阻氧层3阻断来自外部的氧透过的同时,将没有完全阻断的氧也利用吸氧层4吸收。另一方面,能够利用吸氧层4吸收容器内的残存氧。另外,外层1及内层5优选含有二氧化钛。由此,能够遮盖由吸氧层4中含有的铁粉所致的着色。
(吸氧层)
吸氧层包含本发明的吸氧性树脂组合物。吸氧层的质量相对于容器整体的质量(100质量%)的比例(与厚度有关的质量比率)优选为20质量%以下,更优选为1质量%以上且15质量%以下,进一步优选为5质量%以上且10质量%以下。构成吸氧层的本发明的吸氧性树脂组合物中,由于铁能够发挥高吸氧性能,因此能够使该比例为20质量%以下,能够降低制造成本。另外,能够实现容器的轻量化。吸氧层的厚度优选为5μm以上且300μm以下,更优选为10μm以上且200μm以下。
(阻氧层)
作为阻氧层的材料,可以使用乙烯-乙烯醇共聚物、尼龙MXD6、聚乙醇酸等阻气性树脂。它们当中,从氧的阻断性高的观点出发,优选乙烯-乙烯醇共聚物。这些材料可以使用一种,也可以并用两种以上。另外,也可以使用所述材料与聚烯烃系树脂的混合物。也可以使用铝、钢等金属箔、无机薄膜蒸镀膜、将聚乙烯醇、聚丙烯酸等阻气性材料涂布于基材膜而得的阻气性涂布膜作为阻氧层。
从在从容器外部透过的氧到达吸氧层前有效地阻断该氧的观点出发,阻氧层优选相对于吸氧层设于外侧。在阻氧层包含乙烯-乙烯醇共聚物的情况下,阻氧层的质量相对于容器整体的质量(100质量%)的比例(与厚度有关的质量比率)优选为10质量%以下,更优选为1质量%以上且9质量%以下,进一步优选为2质量%以上且8质量%以下。构成吸氧层的本发明的吸氧性树脂组合物中,由于铁能够发挥高吸氧性能,因此能够使该比例为10质量%以下,能够降低制造成本。另外,能够实现容器的轻量化。阻氧层的厚度优选为5μm以上且200μm以下,更优选为5μm以上且150μm以下。
(内层、外层)
作为内层及外层的材料,没有特别限定,例如可以举出低-、中-或高-密度的聚乙烯、聚丙烯、乙烯-丙烯共聚物、聚1-丁烯、乙烯-1-丁烯共聚物、丙烯-1-丁烯共聚物、乙烯-丙烯-1-丁烯共聚物、聚甲基-1-戊烯、乙烯-乙酸乙烯酯共聚物、乙烯-(甲基)丙烯酸共聚物、离子交联烯烃共聚物(离聚物)或它们的共混物等烯烃系树脂、聚苯乙烯、苯乙烯-丁二烯共聚物、苯乙烯-异戊二烯共聚物、ABS树脂等苯乙烯系树脂、聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、二醇类改性聚对苯二甲酸乙二醇酯、聚乳酸、聚丁二酸丁二醇酯等聚酯、尼龙6、尼龙66等聚酰胺、聚碳酸酯等。这些材料可以使用一种,也可以并用两种以上。另外,内层的材料与外层的材料可以相同,也可以不同。内层及外层的厚度没有特别限定,例如可以为30~1000μm。
(粘接层)
作为粘接层的材料,没有特别限定,例如可以举出乙烯-丙烯酸共聚物、离子交联烯烃共聚物、马来酸酐接枝聚乙烯、马来酸酐接枝聚丙烯、丙烯酸接枝聚烯烃、乙烯-乙酸乙烯酯共聚物、共聚聚酯、共聚聚酰胺等。这些材料可以使用一种,也可以并用两种以上。粘接层的厚度没有特别限定,例如可以为1~20μm。
(容器的制造方法)
本发明的容器的制造方法没有特别限定。例如,可以是如下的多层同时挤出,即,将与各层对应的材料用挤出机熔融混炼后,穿过T-模头、圆板牙(日文原文:サーキュラーダイ)等多层多重模具而以给定的形状挤出。另外,也可以在用与各层对应的注射机将各材料熔融混炼后,向注射模具中共注射或逐次注射,制造多层容器或容器用的预制件。此外,也可以采用干式层压、夹心层压、挤出涂布等层叠方式。
成形物可以是膜、片、瓶或管子形成用型坯、或者管道、瓶或管子成形用预制件等。由型坯、管道或预制件开始的瓶的形成可以通过将挤出物用一对分割式模具夹断、并向其内部吹入流体而容易地进行。另外,在将管道或预制件冷却后,加热到拉伸温度,沿轴向进行拉伸,并且利用流体压力沿圆周方向进行吹塑拉伸,由此可以得到拉伸吹塑瓶。另外,通过对膜或片实施真空成形、压缩空气成形、胀形成形、柱塞助压成形等,可以得到杯状、托盘状等的容器。此外,在多层膜的情况下,也可以将其重叠或折叠为袋状,对周围进行热封而制成袋状容器。
(用途)
本发明的容器由于吸氧性能优异,因此能够作为例如米饭、咖啡、汤等的容器合适地使用。
实施例
以下,利用实施例对本发明进一步具体说明,然而本发明并不受这些实施例限定。利用以下的方法评价各实施例中得到的吸氧性树脂组合物颗粒及容器的吸氧性能。
[吸氧性树脂组合物颗粒的吸氧性能的评价]
在层叠有钢箔的内容积85ml的不透气性的塑料杯容器内部,以使两者不接触的方式设置吸氧性树脂组合物颗粒3g及蒸馏水1ml。其后,使用不透气性的金属箔层叠膜,将该容器在空气中热封,进行了密封。将该容器在50℃保管1天后,使用气相色谱(商品名:CP4900、Agilent制)测定出该容器内部的氧浓度。根据所得的测定结果,算出吸氧性树脂组合物颗粒的每单位质量的吸氧量。将结果表示于表1中。需要说明的是,表1中将吸氧量作为将实施例1的吸氧性树脂组合物颗粒(铝含量:7质量ppm)的吸氧量设为100.0%时的相对比率(单位:%)表示。
[容器的内容物保存性的评价]
向容器内部加入米饭,使用不透气性的金属箔层叠膜,将该容器在1%的氧浓度气氛下热封,进行了密封。此时,容器的有效面积为220cm2,容器内部的顶部空间为50ml。将该容器在23℃-50%RH下保管300天后,使用气相色谱(商品名:CP4900、Agilent制)测定出该容器内部的氧浓度。根据保管后的容器内的氧浓度依照以下的基准评价内容物保存性。将结果表示于表2中。
○:保管后的容器内的氧浓度小于1%。
△:保管后的容器内的氧浓度为1%以上且小于1.15%。
×:保管后的容器内的氧浓度为1.15%以上。
[实施例1]
(吸氧剂的制备)
将回转窑还原铁粉(金属铁量90质量%、平均粒径45μm)100质量份、氯化钠2质量份及氢氧化钙1质量份混合,使用振动球磨机进行10小时粉碎处理。其后,利用180目的筛子进行分级而除去90μm以上的粗大粒子,得到混合微粉碎物。将所得的混合微粉碎物50kg填充于内容积230L的间歇式回转炉内,在转速6rpm、氮气流量10L/分钟、550℃的条件下进行8小时热处理(升温2小时、冷却8小时)。需要说明的是,在热处理时,取代氮气而以10L/分钟的流量流入空气6小时,由此促进了表面氧化。其后,利用180目的筛子进行分级而除去90μm以上的粗大粒子,得到吸氧剂。
(吸氧性树脂组合物颗粒的制作)
将所述吸氧剂29质量份和无规聚丙烯(无规PP)(密度:0.91g/cm3、熔融指数(MI):0.6g/10min、230℃)71质量份利用双轴挤出机(商品名:TEM-35B、东芝机械制)熔融混炼,进行成形而制作出吸氧性树脂组合物颗粒。该吸氧性树脂组合物颗粒的铝含量为7质量ppm。需要说明的是,利用ICP分析装置(商品名:720-ES、Varian制)测定出该铝含量。对于所得的吸氧性树脂组合物颗粒,利用上述方法评价吸氧性能。将结果表示于表1及图2中。
[实施例2、3、比较例1~4]
除了在吸氧性树脂组合物颗粒的制作中通过变更所用的无规PP而将吸氧性树脂组合物颗粒的铝含量如表1所示地变更以外,与实施例1同样地制作、评价了吸氧性树脂组合物颗粒。将结果表示于表1及图2中。
[表1]
[实施例4]
在实施例1的吸氧性树脂组合物颗粒的制作中,通过变更所用的无规PP,而制作出实质上不包含铝的吸氧性树脂组合物颗粒(铝含量:小于10质量ppm)。另外,作为阻氧层的材料准备了乙烯-乙烯醇共聚物(EVOH、乙烯含量32摩尔%、皂化度99.6摩尔%),作为内层及外层的材料准备了含有8质量%的钛白颜料的白色嵌段聚丙烯(白色嵌段PP),作为粘接层的材料准备了马来酸酐改性聚丙烯(马来酸酐改性PP)(MI:1.0g/10min、230℃)。
使用这些材料,利用包含单轴挤出机、分流器、T-模头、冷却辊及片收卷装置的成形装置,制作出厚500μm的4种6层片(外层(40质量%)/粘接层(2质量%)/阻氧层(7质量%)/粘接层(2质量%)/吸氧层(7质量%)/内层(42质量%))。将所得的片在真空压缩空气成形机中使用多型腔模具进行深拉伸成形,成形出口外径140×105mm、高40mm、内容量330ml的多层深拉伸容器。对于所得的容器,利用上述方法评价内容物保存性。将结果表示于表2中。
[实施例5]
除了将层构成变更为外层(40质量%)/粘接层(2质量%)/阻氧层(6质量%)/粘接层(2质量%)/吸氧层(7质量%)/内层(43质量%)以外,利用与实施例4相同的方法制作、评价了容器。将结果表示于表2中。
[实施例6]
在吸氧性树脂组合物颗粒的制作中,除了使用所述吸氧剂26质量份、和所述无规PP 74质量份以外,利用与实施例4相同的方法制作、评价了容器。将结果表示于表2中。
[比较例5]
在吸氧性树脂组合物颗粒的制作中,通过变更所用的无规PP,制作出包含140质量ppm以上的铝的吸氧性树脂组合物颗粒。除了使用该吸氧性树脂组合物颗粒以外,利用与实施例4相同的方法制作、评价了容器。将结果表示于表2中。
[表2]
符号说明
1 外层,
2a、2b 粘接层,
3 阻氧层,
4 吸氧层,
5 内层。
Claims (6)
1.一种吸氧性树脂组合物,其特征在于,所述吸氧性树脂组合物含有烯烃系树脂和吸氧剂,
所述吸氧剂包含铁粉、卤化金属及碱性物质,
所述吸氧剂的含量为10质量%以上且30质量%以下,所述卤化金属相对于铁粉100质量份为0.1质量份~10质量份,
所述碱性物质相对于铁粉100质量份为0.5质量份~2质量份,
所述吸氧性树脂组合物中的铝的含量为7质量ppm~50质量ppm。
2.根据权利要求1所述的吸氧性树脂组合物,其中,
所述吸氧性树脂组合物不包含水滑石。
3.一种容器,其特征在于,
具有包含权利要求1所述的吸氧性树脂组合物的吸氧层。
4.根据权利要求3所述的容器,其中,
相对于所述吸氧层在外侧还具有包含乙烯-乙烯醇共聚物的阻氧层。
5.根据权利要求4所述的容器,其中,
所述阻氧层的质量相对于所述容器整体的质量的比例为10质量%以下。
6.根据权利要求3所述的容器,其中,
所述吸氧层的质量相对于所述容器整体的质量的比例为20质量%以下。
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KR20200103812A (ko) | 2020-09-02 |
EP3747952A1 (en) | 2020-12-09 |
PL3747952T3 (pl) | 2024-05-27 |
ES2973529T3 (es) | 2024-06-20 |
EP3747952A4 (en) | 2021-11-03 |
CN111630112A (zh) | 2020-09-04 |
JP7135327B2 (ja) | 2022-09-13 |
WO2019146491A1 (ja) | 2019-08-01 |
JP2019131632A (ja) | 2019-08-08 |
EP3747952C0 (en) | 2024-03-06 |
EP3747952B1 (en) | 2024-03-06 |
US20210053023A1 (en) | 2021-02-25 |
KR102498404B1 (ko) | 2023-02-09 |
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