CN1942519B - 具有隔离性能的容器及其制备方法 - Google Patents
具有隔离性能的容器及其制备方法 Download PDFInfo
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- CN1942519B CN1942519B CN2005800119861A CN200580011986A CN1942519B CN 1942519 B CN1942519 B CN 1942519B CN 2005800119861 A CN2005800119861 A CN 2005800119861A CN 200580011986 A CN200580011986 A CN 200580011986A CN 1942519 B CN1942519 B CN 1942519B
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- polyester
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Abstract
公开一种制备多层或单层塑料容器的方法。所述容器具有由以下材料制备的隔离层：(i)聚酯树脂，优选芳族聚酯树脂如聚对苯二甲酸乙二醇酯，(ii)聚酰胺材料，优选芳族聚酰胺材料，和(iii)氧清除材料，优选过渡金属。本发明也提供具有单层或多层壳体的容器。在隔离层的制备中，首先通过注塑法制备型坯，其中在注塑过程中，将包含稀释聚酯、聚酰胺材料和氧清除材料的预掺混料加入基础聚酯中。然后使型坯膨胀形成容器。
Description
发明领域
本发明涉及塑料容器及其制备方法。更具体来讲，本发明涉及具有优良隔离性能，并具有至少一个由聚酯树脂、聚酰胺材料和氧清除材料制备层的多层和单层容器。
发明背景
许多包装产品，尤其是食品和饮料产品，由于氧和/或水分通过包装壁吸收或损耗而容易变质。因此，容器-无论是刚性容器、半刚性容器、软包装容器、带盖容器、可折叠容器，或是其组合，不但用作产品包装，而且帮助防止不需要的物质从环境进入。
大气中的氧为最易与包装在容器中的产品反应的物质之一。增加1至4个电子后，氧分子(O2)被还原成各种高度活性中间体类物质。实际上所有食品和饮料中存在的碳-碳双键，特别容易与这些活性中间体类物质反应。所得氧化产物不利地影响产品的性能、气味和/或味道。
“氧敏感性”材料包括食品、饮料和药品，具有特殊的包装要求，包括防止外部的氧气进入包装内，和/或清除包装内存在的氧气。在一些情况中，尤其在橙汁和酿造工业中，通过真空、喷入惰性气体或这两种方法从产品中除去氧气。然而，这些方法除去最后微量的氧气是困难且昂贵的。
专门用玻璃或金属制备的容器提供优良的隔离性能，可防止容器内物质外溢，以及防止物质从环境进入容器。在大多数情况中，透过玻璃或金属容器的气体渗透可以忽略。全部或部分由聚合物制备的容器，通常不具有玻璃或金属容器的储存期或隔离性能。因此，尽管聚合物有很大优势，但是它们的不足限制了它们在容器中的应用。
聚合物的优点包括良好的机械、热和光学特性，以及容器制备技术的适应性，可提供均质、层压和/或涂层的容器。由聚合物制备的容器的其它优点包括重量轻、易破碎性降低和制备成本低。
由于这些优点，包装工业日渐转移至塑料容器。这种趋势涉及包括碳酸饮料的饮料容器和食品容器。在所有这些应用中，塑料材料的隔离性能不足，尤其是防止气体如氧气和二氧化碳以及汽化液体如水蒸汽通过的能力不足，导致包装在塑料容器中产品的储存期缩短。
已提出许多克服与塑料容器相关问题的方案。然而，所提出的解决方案未能符合低成本，并且高隔离性能以使塑料材料制备的容器可被实际使用的商业上确定的要求。所提出解决方案的实例包括：
a)层压，使用两层或多层聚合物材料，各层中的聚合物材料任选具有有利的隔离性能，例如透气、透光或透湿的隔离性能；
b)其中将金属如铝置于聚合物材料层之间，或形成容器内表面的结构；及
c)其中将非金属防渗透材料层置于聚合物材料层之间，或形成容器的内表面的结构。
其它提出的方案有：混合不同类型的塑料材料，然后模塑形成容器。例如，已知的制备包含聚对苯二甲酸乙二醇酯(PET)和聚酰胺混合物的聚合物材料的容器。见，如美国专利第4,501,781、4,837,115、5,034,252、5,258,233、5,281,360、5,641,825和5,759,653号。
尤其是，解决聚合物容器即塑料容器相关问题的尝试，导致了在包装材料中广泛使用不透氧物和/或防湿剂。典型的防湿剂包括聚乙烯和聚丙烯。不透氧物包括乙烯-乙烯醇共聚物(EVOH)、聚乙烯醇(PVOH)、尼龙及其掺混物。1，1-二氯乙烯/-氯乙烯共聚物和1，1-二氯乙烯/-丙烯酸甲酯共聚物用作防湿剂和不透氧物。
由于防渗透材料具有成本高、结构性质不稳定和其他缺点，因此难以单独由防渗透材料制备商业应用的塑料容器。例如，EVOH具有较好的不透氧性，但由于聚合物上的许多羟基而遭受水分问题。其他防渗透材料十分昂贵，这样单独由这些材料制备容器的花费令人望而却步。因此，制备多层结构成为普遍的实践方法，即将昂贵或敏感性防渗透材料的量减少制成薄层，便宜的聚合物置于隔离层的一面或双面上作为结构层。
尽管含隔离层的多层结构比防渗透材料单层便宜，且结构上更牢固，但这类容器比单层容器制备更复杂。此外，降低多层容器中隔离层的厚度经常会削弱容器的隔离性能。因此，除具有隔离层的多层容器之外，本领域需要具有高隔离性能和结构性能，但没有单独由防渗透材料所制备容器相应高成本的单层容器。
包装应用中常用的一种材料为聚对苯二甲酸乙二醇酯树脂，下文称为PET。PET在包装应用中有许多优良性能，但PET没有许多应用中必需或所需的阻气性。例如，尽管PET对碳酸果汁具有好的不透氧性，但PET尚没有用作其他产品的包装材料，如由于氧气进入瓶中会迅速失去味道的啤酒、柑橘属产品、番茄-基产品和防腐包装肉。具有类似于PET的物理性质的包装材料为聚萘二甲酸乙二醇酯(PEN)。PEN具有高于PET的隔离性能，但PEN显然比PET更昂贵。
存在相当不能渗透的聚合物，如乙烯和乙烯醇共聚物、1，1-二氯乙烯和氯乙烯共聚物以及间二甲苯二胺和己二酸共聚物(即MXD6)。但是由于实践原因或成本原因，这些共聚物一般作为薄层用于PET层上或PET层之间，或者在MXD6的情形下，以低重量百分比的量与PET掺混以达到可忽略的透气性。同样，以大于30％重量的量，使用含苯二甲基的聚酰胺树脂与PET，使得容器成为层压箔结构，从而提供容器箔层之间剥落的可能性。
根据上面所述，可认识到本领域需要具有优良的气体如氧气和二氧化碳隔离性能的改进塑料多层或单层容器。可满意地包装在这些容器中的产品包括如啤酒(尤其是熟啤酒)、葡萄酒(尤其是白葡萄酒)、果汁、碳酸软饮料、水果、坚果、蔬菜、肉制品、婴儿食品、咖啡、沙司和乳制品。本文公开具有优良隔离性能的多层和单层塑料容器，及其制备方法。
发明概述
本发明涉及制备具有优良隔离性能的多层或单层塑料容器的方法。该容器具有至少一个隔离层，该隔离层包含：(i)聚酯，(ii)聚酰胺材料和(iii)氧清除材料。使用注塑法或挤塑法制备多层容器或单层容器的隔离层，其中在注塑或挤塑过程期间，将包含稀释聚酯、聚酰胺材料和氧清除材料的预掺混料加入基础聚酯中。
更特别是，本发明涉及通过注塑法或挤塑法制备的塑料多层或单层容器，其中容器包含至少一个由芳族聚酯、芳族聚酰胺和过渡金属氧清除剂制备的隔离层。对于单层容器，隔离层为容器的唯一层。对于多层或单层容器，容器通过使具有隔离层的型坯膨胀而成型。型坯通过注塑法或挤塑法制备，其中在注塑或挤塑形成型坯之前，在模塑装置中，由混合基础聚合物的预掺混料形成隔离层。
因此，本发明一方面提供具有隔离层的型坯，隔离层通过注塑或挤塑基础聚酯制备，该基础聚酯中已经加入了含稀释聚酯、聚酰胺材料和氧清除材料的预掺混料。一般于注塑之前，以粒料或颗粒形式将预掺混料加入模塑装置中的基础聚酯中。
本发明另一方面提供预掺混料，该预掺混料包含(a)约25％至约75％重量稀释聚酯，(b)约25％至约75％重量聚酰胺材料，和(c)约20至约2000ppm过渡金属氧清除剂。在注塑法或挤塑法形成型坯的隔离层的注射步骤之前，将预掺混料加至基础聚酯中并与之混合。然后，使型坯膨胀，提供多层或单层容器。稀释聚酯和基础聚酯可为相同或不同的，例如聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)或其混合物。
本发明方法中使用的预掺混料显示优异的稳定性，即于25℃和40％相对湿度下储存6个月后，比于相同储存条件下储存的仅含聚酰胺材料和氧清除材料的掺混物，具有更高的稳定性。
预掺混料与基础聚酯按以下的量混合：约0.5％至约20％、优选约1％至约15％重量的预掺混料，和约80％至约99.5％、优选约85％至约99％重量的基础聚酯。预掺混料和基础聚酯更优选按以下的量混合：约2％至约12％重量的预掺混料，和约88％至约98％重量的基础聚酯。一般，预掺混料和基础聚酯以足量混合，以提供含约10至约80ppm，优选约20至约50ppm氧清除材料的型坯。
本发明另一方面提供具有由本发明方法制备隔离层的多层或单层容器，其中不透氧性在与水接触之后活化。
本发明另一方面提供通过型坯膨胀的多层容器，所述多层容器包含：(a)按本发明方法制备的含稀释聚酯、聚酰胺材料和氧清除材料的中间隔离层，和(b)可成型聚合物的内层和外层。
本发明再一方面提供通过注塑或挤塑含芳族聚酯的基础聚酯制备单层塑料容器的方法，其中基础聚酯中已经加入预掺混料，该预掺混料包含含芳族聚酯的稀释聚酯、聚酰胺和过渡金属氧清除材料。在优选的实施方案中，基础聚酯和预掺混料的芳族聚酯相同或不同，包含PET、PEN或其混合物；聚酰胺为芳族聚酰胺，如二甲苯聚酰胺；和过渡金属氧清除剂，包含铁、钴、镍、钌、铑、钯、锇、铱、铂的盐或络合物，或其混合物。
本发明还另一方面提供含聚酯、聚酰胺材料和氧清除材料的单层容器。该单层容器具有优异的结构强度，并由于容器用水性产品填充之后引发氧清除活性，因而在储存期间维持高隔离性能。该容器也具有优异的美学特性，尤其在容器的透明度方面。
根据以下优选实施方案的详细描述，本发明的这些和其他方面将是显而易见的。
优选实施方案的详述
用于产品如啤酒和果汁的容器需要足够的隔离性能，以维持产品的完整性。如前面所讨论的，塑料容器一般需要添加剂提供或增强隔离性能。通常通过提供具有隔离层的多层容器获得隔离性能。需要提供具有足够隔离性能的改进多层容器或单层容器来维持包装产品的完整性。
有几个因素影响含至少一层防渗透材料的聚合物-基容器的外观和性能。这些因素包括在模塑期间防渗透材料受到的剪切、在干燥和模塑期间材料的受热历程以及防渗透材料暴露于空气。空气暴露可通过氧化过程和接触水分使防渗透材料降解。这些变量可以解决，例如通过改变螺杆设计、树脂干燥和进料结构。本发明提供制备型坯的方法改进，将上述降解性因素最小化。
设想在单级或多级注塑设备上制备塑料容器的隔离层的几种方法。这些方法包括：
(1)将聚酰胺材料和氧清除材料以及聚酯如PET计量供至注射器螺杆中；
(2)混合聚酰胺材料和氧清除材料，然后将所得混合物与聚酯一起加入注射器螺杆中；和
(3)混合聚酰胺材料、氧清除材料和聚酯，然后用所得掺混物注塑。
方法(1)在实际操作上不可靠，因为需要将15ppm或更少，即约0.05％重量或更少的氧清除材料计量供应至注射器螺杆中，然后掺混提供均匀的混合物。方法(2)的缺点是聚酰胺材料/氧清除材料掺混物对温度、氧和水分敏感，因此在型坯制备期间掺混物一般进行明显的降解，导致容器不可接受的变朦胧且变黄。方法(3)的缺点是需要储存大量具有固定隔离水平的掺混材料，从而使该方法经济上无吸引力。
本发明方法克服先前方法的相关缺点，并提供制备具有改善隔离性能和外观的容器的更温和方法。制备型坯的本发明方法得到具有优异隔离性能的多层或单层容器，并减少不透氧性的削弱，从而提供更具美感的容器，例如改善光学特性如减少朦胧的容器。
本发明的一个重要特征是制备型坯，该型坯于25℃和_％相对湿度下储存至少六个月仍保持稳定。另一个重要特征是从本发明型坯制备容器，其中隔离层的氧清除能力直到容器被水性流体充满才被活化。因此，容器在充满之前具有长的储存期，充满水性流体之后，具有更长的不透氧能力。
本发明提供制备塑料容器的方法，该容器具有足够不透氧性以维持包装在容器中的氧敏感性产品如啤酒的完整性。容器也具有优异的外观。容器按本领域熟知的方法从型坯制备，并包含至少一个含聚酯、聚酰胺材料和氧清除材料的隔离层。
通过注塑法或挤塑法制备型坯。特别是，型坯的隔离层按以下方法制备。首先制备含稀释聚酯、聚酰胺材料和氧清除材料的预掺混料。在注塑或挤塑步骤之前，将预掺混料加至在注射螺杆中的基础聚酯中并与之混合。
特别是，型坯包含(a)约25％至约75％重量的稀释聚酯，(b)约25％至约75％重量的聚酰胺材料，和(c)约20至约2000ppm氧清除材料。组分(a)、(b)和(c)充分混合，优选形成粒料或颗粒，以便加入基础聚酯中。也设想可将颗粒状或粉末状的(a)、(b)和(c)预掺混料加入基础聚酯中。
更特别是，预掺混料包含约25％至约75％，优选约30％至约70％重量的稀释聚酯。在更优选的实施方案中，预掺混料包含约40％至约60％重量的稀释聚酯。
稀释聚酯为二元酸和二醇的缩合产物。二元酸一般包含芳族二元酸或其酯或酸酐，如间苯二甲酸、对苯二甲酸、萘-1，4-二甲酸、萘-2，6-二甲酸、邻苯二甲酸、邻苯二甲酸酐、四氢邻苯二甲酸酐、1，2，4-苯三酸酐、二苯氧基乙烷-4，4′-二甲酸、联苯-4，4′-二甲酸及其混合物。二元酸也可为脂族二元酸或酸酐，如己二酸、癸二酸、癸-1，10-二甲酸、富马酸、琥珀酸酐、琥珀酸、环己烷二乙酸、戊二酸、壬二酸及其混合物。也可使用本领域技术人员熟知的其他芳族和脂族二元酸。二元酸优选包含芳族二元酸，任选还包含占二元酸组分最高达约20％重量的脂族二元酸。
稀释聚酯的二醇或二元醇组分包含乙二醇、丙二醇、丁-1，4-二醇、二甘醇、聚乙二醇、聚丙二醇、新戊二醇、聚1，4-丁二醇、1，6-己二醇、戊-1，5-二醇、3-甲基戊二醇-(2，4)、2-甲基戊二醇-(1，4)、2，2，4-三甲基戊二醇-(1，3)、2-乙基己二醇-(1，3)、2，2-二乙基丙二醇-(1，3)、己二醇-(1，3)、1，4-二-(羟基乙氧基)苯、2，2-二-(4-羟基环己基)丙烷、2，4-二羟基-1，1，3，3-四甲基环丁烷、2，2-二-(3-羟基乙氧基苯基)丙烷、2，2-二-(4-羟基丙氧基苯基)丙烷、1，4-二羟基甲基-环己烷及其混合物。本领域技术人员熟知的其他二醇也可用作稀释聚酯的二醇组分。
两种优选的稀释聚酯为PET和PEN。PET和PEN可为均聚物或共聚物，其还含有最高达10mol％的不同于对苯二甲酸或萘二羧酸的二元酸，和/或最高达10mol％的不同于乙二醇的二醇。
本文中使用的术语“PEN”指聚萘2，6-二甲酸乙二醇酯、聚萘1，4-二甲酸乙二醇酯、聚萘1，6-二甲酸乙二醇酯、聚萘1，8-二甲酸乙二醇酯和聚萘2，3-二甲酸乙二醇酯。PEN优选为聚萘2，3-二甲酸乙二醇酯。
特别是，稀释聚酯优选包含PET(如未用瓶(virgin bottle)级PET或用过(postconsumer)级PET(PC-PET))、环己烷二甲醇/PET共聚物(PETG)、聚萘二甲酸乙二醇酯(PEN)、聚对苯二甲酸丁二醇酯(PBT)及其混合物。
适合的聚酯也可包含聚合物连接体、侧链和不同于先前指定简单聚酯的甲缩醛前体的端基。
用于本发明的合适聚酯一般具有约0.6至约1.2的特性粘度，更优选约0.7至约1.0(对于苯酚/四氯乙烷溶剂的60/40掺混物而言)。对于PET，0.6的特性粘度值大约对应于36,000的粘均分子量，1.2的特性粘度值大约对应于103,000的粘均分子量。
稀释聚酯任选可包含不会不利地影响预掺混料、或型坯或由其制备容器的添加剂。任选的添加剂包括但不限于稳定剂如抗氧化剂或紫外线掩蔽剂、挤塑助剂、干燥剂、填充剂、防阻塞剂、结晶助剂、冲击性改善剂、设计使聚合物更易降解或更易燃烧的添加剂、染料、颜料及其混合物。存在于稀释聚酯中的任选添加剂的量分别占稀释聚酯0％至约2％重量，总共占稀释聚酯0％至约10％重量。
除稀释聚酯外，预掺混料还包含约25％至约75％，优选约30％至约70％重量的聚酰胺材料。在更优选的实施方案中，预掺混料包含约40％至约60％重量的聚酰胺材料。
聚酰胺材料可为芳族聚酰胺或脂族聚酰胺。聚酰胺材料也可为均聚酰胺材料或共聚酰胺材料。优选芳族聚酰胺均聚物或共聚物。
优选的一类聚酰胺材料为MX尼龙。MX尼龙为含至少70mol％结构单元的聚合物，该结构单元得自单独的间二甲苯二胺，或含间二甲苯二胺与占总量小于30％的对二甲苯二胺的二甲苯二胺混合物，以及具有6-10个碳原子的α，ω-脂族二羧酸。
MX聚合物实例包括均聚物，如聚己二酰间苯二甲胺和聚癸二酰间苯二甲胺；共聚物，如己二酰间苯二甲胺/己二酰对苯二甲胺共聚物、间苯二甲基/对苯二甲基pyperamide共聚物和壬二酰间苯二甲胺/壬二酰对苯二甲胺共聚物；以及这些均聚物或共聚物组分与以下物质的共聚物：脂族二胺如1，6-己二胺、环状二胺如哌嗪、芳族二胺如对-二(2-氨基乙基)苯、芳族二羧酸如对苯二甲酸、内酰胺如ε-己内酰胺、ω-氨基羧酸如ω-氨基庚酸和芳族氨基羧酸如对-氨基苯甲酸。任选可将聚合物如尼龙6、尼龙66、尼龙610和尼龙11掺入至MX聚合物中。
尤其优选的芳族聚酰胺为通过间二甲苯二胺(即H2NCH2-m-C6H4-CH2NH2)和己二酸(即HO2C(CH2)4CO2H)聚合形成的聚合物，例如由Mitsubishi Gas Chemicals，Japan制备和销售的名称为MXD6的产品。也可得到各等级的MXD6，如6001、6007、6021级。优选的脂族聚酰胺材料为尼龙66。其他合适的聚酰胺包括如(如
G16和G21，为具有线型脂族单元和环状芳族组分的共聚酰胺，可得自EMS-Chemie公司)和
(脂族聚酰胺一般用作油墨树脂，可得自Cognis公司)。
除稀释聚酯和聚酰胺材料之外，预掺混料还包含氧清除材料。氧清除材料存在的量占预掺混料重量约20至约2000，优选约50至约1500ppm。在更优选的实施方案中，预掺混料包含占预掺混料重量约100至约1000ppm的氧清除材料。
“氧清除剂”为通过与捕获的氧反应或结合，或者通过促进产生无害产物的氧化反应，可从密闭包装的内部除去氧气或防止氧气进入包装内部的任何物质或化合物。
氧清除材料赋予高不透氧性，即有足够抵挡氧气进入容器中的能力。导致隔离性能能力的作用称为氧“清除”作用。尽管不受任何理论束缚，提出氧清除材料形成具有与氧键合能力的活性金属络合物。因此，氧清除材料赋予容器高不透氧性。
许多金属化合物可有效提供氧清除作用，基于成本和与预掺混料中稀释聚酯和聚酰胺材料的相容性，选择合适的氧清除材料。优选的氧清除材料为选自元素周期表中第一、第二和第三过渡元素系的金属或金属的络合物或盐。这些金属包括铁、钴、铜、锰、锌、镍、钌、铑、钯、锇、铱和铂。用于本发明的合适氧清除材料也包括铝粉、碳化铝、氯化铝、钴粉、氧化钴、氯化钴、锑粉、氧化锑、三乙酸锑、氯化锑III、氯化锑V、铁、电解铁、氧化铁、铂、披铂氧化铝、钯、披钯氧化铝、钌、铑、铜、氧化铜、镍和混合金属的纳米颗粒(如钴铁氧化物纳米颗粒)。合适纳米颗粒的平均粒度小于约200nm，优选小于约100nm，更优选约5至约50nm。
钴、铁、镍、铜或锰化合物为优选的氧清除材料。最优选钴化合物。氧清除材料一般以金属的盐或络合物形式存在。盐的阴离子可为无机的或有机的。阴离子实例包括卤离子尤其是氯离子、醋酸根、硬脂酸根和辛酸根。其他氧清除剂包括溴化钴(II)和羧酸钴。羧酸钴可以钴
(Akzo Chemie Nederland B.V.，Amersford，荷兰的商标)获得。羧酸钴为C8-C10羧酸钴的溶液，钴(金属)的浓度相对于溶液为约10％重量。
预掺混料中稀释聚酯、聚酰胺材料和氧清除材料的相对量，与变量如基础聚酯的特征、包装在容器中的产品和加入基础聚酯中的预掺混料量有关。预掺混料可为粒料、颗粒或粉末形式。
在双螺杆挤塑机上，制备含PET、MXD6和钴氧清除材料的一个本发明预掺混料实施方案的通用方法见下面描述。具体来讲，稀释聚酯(PET)在固定床干燥剂(dessicant)干燥机如Conair制备的干燥机中干燥。PET的一般干燥条件为于约160℃约4小时。MXD6可由制备时密封的箔袋提供使用，或者可于约140℃单独干燥或与PET一起干燥。钴氧清除材料可为液体形式或固体形式。钴催化剂可与PET和MXD6中之一或两者在Henschel混合机(Henschel Industrietecknik GmBH，Kassel，Germany)中预混，或者以液体形式单独泵入挤塑机的进料口。优选钴氧清除材料与PET和MXD6中至少一种同时加入挤塑机的第一进料区。
以下实施例1为预掺混料的非限定性实施例，所述预掺混料包含(a)46％重量PET，(b)54％重量MXD6，和(c)500ppm钴氧清除材料(如新癸酸钴)。
实施例1
将得自Mitsubishi Gas Corporation的6007级MXD6(16.2磅)与得自Voridian Chemical的13.8磅的9663级PET混合，所得掺混物于140℃下干燥四小时。向十磅该混合物中加入2.27g(500ppm重量)得自OMGroup，Inc.Cleveland，OH的新癸酸钴(即基于钴离子128ppm)。用手混合混合物，然后加入至配有容量加料器的Werner和Pfleiderer ZSK-25双螺杆挤塑机的进料口中。将挤塑机的加热区域维持在240℃-280℃。将掺混物挤出成线料，置于空气冷却的带上，然后制粒。将所得粒料于120℃、真空下，再结晶四小时。
如上述公开，在注塑法或挤塑法的注射步骤之前，将预掺混料的固体颗粒与基础聚合物的固体颗粒混合，以提供型坯的隔离层。在随后的加工步骤中将型坯转化为容器。特别是，在注射步骤之前，将预掺混料颗粒计量转入基础聚酯颗粒中并与之混合。
预掺混料加入基础聚合物中的量占预掺混料/基础聚酯混合物约0.5％至约20％，优选约1％至约15％重量。在更优选的实施方案中，预掺混料存在的量占预掺混料/基础聚酯混合物总重量约2％至约12％。
基础聚酯可与预掺混料的稀释聚酯相同或不同。基础聚酯可包含单一聚合物或两种或多种聚合物的混合物。合适的基础聚合物包括相对于稀释聚合物特征的上述聚酯。本领域技术人员熟知如预掺混料、基础聚酯或预掺混料/基础聚酯混合物可包含任选组分。
基础聚酯的选择没有特别限制。然而，要求基础聚酯与预掺混料组分之间的相容性。本领域技术人员能选择用于具体预掺混料的基础聚酯。此外，预掺混料组分可根据所需基础聚酯进行选择，以便提供物理和化学上相容的预掺混料/基础聚合物混合物。
预掺混料与基础聚合物的比例也取决于各种参数，如组分特征及其在预掺混料中的重量百分比、基础聚酯的特征、所需隔离效果、容器的具体终端用途、所需的容器储存期、再循环能力、经济状况和制备的难易程度。
存在许多多层型坯和容器的结构，其中每种结构适用于具体的产品和/或制备方法。一些代表性实例如下。
一种三层结构，该结构包含置于内层和外层之间的隔离层。例如，容器的三层侧壁结构可包含PET的内层和外层及芯隔离层。
一种五层结构，该结构可具有相对较薄的内部和外部中间层，以提供高不透氧性而不损失透明度。相对较厚的PET内层和外层提供必需的强度和透明度。按上述制备的薄隔离层提供必需的隔离效果。
在优选的实施方案中，多层容器的隔离层厚度占总容器壁厚度约1-10％，更优选约2-8％，最优选约3-6％。
采用几种不同的方法制备本发明容器。
在一种方法中，多层容器按以下步骤制备：(i)提供上述预掺混料和基础聚酯的混合物；(ii)提供合适的可成型聚合物的内层和外层材料；(iii)共注塑预掺混料/基础聚酯混合物以及内层和外层材料，形成多层型坯；和(iv)加热并使型坯膨胀，形成容器。
在替代方法中，多层容器按以下步骤制备：(i)提供上述预掺混料和基础聚酯的混合物；(ii)提供合适的可成型聚合物的内层和外层材料；(iii)挤塑成多层型坯管，该型坯管具有合适的可成型聚合物的内层和外层，及预掺混料/基础聚酯混合物的芯层；(iv)将型坯管夹住置于中空阴模模具中；(v)对着阴模向型坯管吹气成型；和(vi)将模塑容器修边。
在还一个替代方法(“超量注入(over-injected)型坯”方法)中，多层容器按以下步骤制备：(i)提供上述预掺混料和基础聚酯的混合物；(ii)提供合适的可成型聚合物的内层和外层材料；(iii)挤塑成多层型坯管，该型坯管具有合适的可成型聚合物的内层和外层，及由预掺混料/基础聚酯混合物制备的中心隔离层；(iv)在型坯上注塑一个或多个另外的聚合物层；(v)将超量注入型坯管夹住置于中空阴模模具中；(vi)对着阴模向超量注入的型坯吹气成型；和(vii)任选将模塑容器修边。
在再一个方法(称为“IOI”)中，多层容器按以下步骤制备：(i)提供上述的预掺混料和基础聚酯的混合物；(ii)提供合适的可成型聚合物；(iii)注塑预掺混料/基础聚酯混合物以形成型坯；(iv)紧靠型坯(如在外表面)注塑可成型聚合物的层；和(v)加热并使型坯膨胀，形成容器。
根据本发明，为了形成单层容器，通过注塑法或挤塑法，使用预掺混料和基础聚酯制备型坯。然后使用本领域技术人员熟知的方法，将型坯转变成容器。在本发明的注塑法或挤塑法中，将基础聚酯加入至注射器螺杆中。在进料口或沿着注射器螺杆长度的恰当位置，向基础共聚酯加入预掺混料。在使熔化的基础聚酯和熔化的预掺混料充分混合的点，将预掺混料加至基础聚酯，提供均匀的混合物。然后将基础聚酯/预掺混料的混合物注塑或挤塑形成型坯。然后将型坯加热并膨胀，如形成单层容器。
在制备单层容器或多层容器的隔离层中，一般不暴露于环境温度，将基础聚酯/预掺混料的混合物加至模塑装置中，根据传统技术，熔化混合物，并由熔化的掺混物注塑或挤塑成型坯。对于注塑，于约255℃至约280℃、优选约260℃至约275℃的温度下，将基础聚酯/预掺混料的混合物置于注塑装置的压缩部分内，一般也可于相同温度范围内，置于注料嘴中。迅速冷却型坯，以便保持无定形状态。
随后将无定形型坯再成型为容器。在某些物理应用中，在无定形材料的型坯沿轴向和/或其周围方向膨胀成中间体型坯时完成其再成型，该中间体型坯比型坯薄，优选为至少单轴向的材料。随后将中间体型坯进一步膨胀成容器的最终形状。在其他物理应用中，在一个成型阶段将型坯转变成容器。制备单层容器的本发明方法也允许使用用过的PET，以充分降低制备成本。
以下非限定性实施例举例说明本发明，但不应视为限定本发明的范围。
实施例2
由基础聚酯和预掺混料制备碳酸软饮料瓶，其中预掺混料含46％重量稀释聚酯、54％重量聚酰胺材料和500ppm钴离子如新癸酸钴。
如下表所列，向基础聚酯中加入预掺混料的量占总混合物约4％重量。检测由所得混合物制备容器的隔离和美学特性。在该实施例中使用的碳酸软饮料瓶一般按以下方法制备：
将预掺混料(如实施例1)在Conair干燥器中，于140℃干燥3小时，至最大水分含量为50ppm。将干燥的预掺混料装入容量加料器(可由Maguire Products，Aston PA购买获得)中，该加料器固定在Husky注塑机的进料口上。容量加料器的漏斗安装了氮气吹扫，以确保在加工期间，将干燥的预掺混料维持没有水分和氧气。容量加料器放料的同时，电子控制PET释放至注射螺杆的进料口。校准进料器，各循环释放预定量的预掺混料，一般对应于总组合物的约1％至约10％重量。然后，以本领域熟知的制备仅含PET型坯的同样方法，制备含预掺混料和基础聚合物的型坯。然后根据本领域熟知的方法，吹塑型坯，提供软饮料瓶，或者在吹塑之后，进行任选的热定形步骤，以提供热-填充果汁瓶。
按上述方法，从不同预掺混料和不同基础聚合物制备各种容器，然后测试其隔离性能和雾度，见表1总结。
1)两次重复试验。
由以下组分制备容器1-7。各预掺混料包含46％重量PET、54％重量MXD6和500ppm新癸酸钴。各容器所用预掺混料的PET和基础PET相同。所有容器使用4％重量预掺混料制备，该预掺混料分别提供20ppm钴离子(如得自Eastman Chemicals的新癸酸钴)。
容器1——高分子量PET(即TRAYTUF 8506，得自M&GPolymer USA，LLC，Houston，TX)、MXD6(6121级，得自Mitsubishi GasCorporation)；
容器2——TRAYTUF 8506PET、MXD6(6007级)；
容器3——Eastman 9663PET(得自Eastman Chemicals)、MXD6(6007级)；
容器4——Eastman 9663PET、MXD6(6007级)；
容器5——TRAYTUF 8506PET、MXD6(6007级)；
容器6——Eastman 9663PET、MXD6(6121级)；和
容器7——TRAYTUF 8506PET、MXD6(6121级)。
不同的PET组分基本上具有相同的特性粘度。不同的MXD6组分在分子量和粘度上不同。
表1中的数据总结未填充容器和用水冷填充的容器在48小时的透氧度。在Mocon Oxtran 2/20型ML和SM上进行氧传递测定，调节ML和SM使其在环境温度和湿度下用于10oz(295ml)瓶。在每次测试前，使容器适应条件24-48小时。该测试提供120小时试验时间的Mocon数据，以cc O2/包装/天说明透氧度。表1也包含雾度测试的数据，雾度测试使用Hunter实验室Color-quest装置进行。
表1中数据显示由根据本发明方法制备型坯制备的容器提供优异的不透氧性，尤其是在冷填充的容器中，其中钴/MXD6隔离系统已被活化。％雾度值显示除了高的隔离性能外，容器也呈现优异的外观。
特别是，未填充容器显示出比冷填充容器更大的透氧度，如增大约10倍。这说明根据本发明制备容器的不透氧性在容器被填充之后引发。因为活化之后不透氧性随时间降低，因此这是本发明的重要方面。与未填充储存期间相反，通过填充之后引发不透氧性，包装在容器中的产品被保护更长时间。
本发明方法克服了与制备含聚酯、聚酰胺材料和氧清除材料的容器的先前方法相关的问题。首先，在形成型坯之前，预掺混料在延长的时间内稳定。稀释聚酯的存在防止或延缓不透氧络合物的活化，使得在型坯制备之前预掺混料可储存几个月。这个特征对容器制造商具有重要的经济利益。其次，由于不透氧性直到容器被填充后才活化，所以本发明方法使得制备的容器在容器制成后的很长时间内，仍具有优异的隔离性能和美学特性。
本发明方法也使氧清除材料均匀分布至聚酯中，减少由于太早接触并活化聚酰胺-氧清除材料络合物导致的不透氧效果降低，提高PET/预掺混料混合物的热稳定性，导致稳定性提高，更容易操作且经济上更具吸引力。重要的是，预掺混料的制备使在加入至基础聚酯之前，聚酰胺材料和氧清除材料之间的接触被降到最小或消除。这又消除氧清除络合物的过早活化，即过早氧化，过早氧化降低单层容器的不透氧性。
使用本发明方法制备的容器显示出0.1-0.01之间的氧渗透系数。因此，这些容器非常适合用作要求高不透氧性产品的包装。
本发明多层或单层容器为包装产品如碳酸软饮料提供优异的不透氧性和美学特性。本发明容器在包装产品如啤酒、柑橘属产品、基于番茄的产品和防腐包装肉中特别有用，因为由于氧迁移进入瓶中，导致这些产品迅速失去味道。
显然，可对前述本发明进行许多修改和变化，而不会背离其宗旨和范围，因此，本发明范围只由权利要求书限定。
Claims (23)
1.一种制备具有隔离性能的容器的方法，所述方法包括步骤：
(a)形成预掺混料，该掺混料包含：
(i)稀释聚酯，该稀释聚酯为二元酸和二醇的缩合产物，
(ii)聚酰胺材料，和
(iii)20至2000ppm重量的氧清除材料，该氧清除材料包含过渡金属或其络合物或盐，所述过渡金属选自元素周期表中第一、第二或第三过渡金属系；
(b)提供基础聚酯；
(c)将步骤(a)的预掺混料和步骤(b)的基础聚酯加入模塑装置中，使其熔化，并混合所述预掺混料和所述基础聚酯；
(d)在所述装置中注塑或挤塑步骤(c)的混合物，提供型坯；和
(e)使步骤(d)的型坯膨胀，提供从步骤(c)的混合物形成的具有隔离层的塑料容器，
其中所述塑料容器在未填充储存期间是稳定的，并且所述隔离层的氧清除能力直到容器被水性流体充满才被活化。
2.权利要求1的方法，其中所述塑料容器为多层塑料容器。
3.权利要求1的方法，其中所述塑料容器为单层塑料容器。
4.权利要求1的方法，所述容器在填充水后48小时的cc O2/包装/天透氧度，比该容器填充水之前的透氧度小。
5.权利要求1的方法，其中于25℃和40％相对湿度储存六个月后，步骤(a)的预掺混料比在相同储存条件下储存的仅含聚酰胺材料和氧清除材料的掺混物，具有更高的稳定性。
6.权利要求1的方法，其中所述预掺混料为固体颗粒形式。
7.权利要求1的方法，其中所述预掺混料中存在的稀释聚酯量占该预掺混料25％至75％重量。
8.权利要求1的方法，其中所述稀释聚酯包含：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的均聚物或共聚物，环己烷二甲醇/聚对苯二甲酸乙二醇酯共聚物或其混合物。
9.权利要求8的方法，其中所述聚对苯二甲酸乙二醇酯包含未用瓶级聚对苯二甲酸乙二醇酯、用过级聚对苯二甲酸乙二醇酯或其混合物。
10.权利要求1的方法，其中所述预掺混料中存在的聚酰胺材料量占该预掺混料25％至75％重量。
11.权利要求1的方法，其中所述聚酰胺材料包含含间二甲苯二胺单体单元、对二甲苯二胺单体单元或其混合物的聚合物。
12.权利要求1的方法，其中所述聚酰胺材料包含间二甲苯二胺和己二酸的聚合产物。
13.权利要求1的方法，其中所述预掺混料中存在的氧清除材料的量为50至1500ppm重量。
14.权利要求1的方法，其中所述氧清除材料选自钴、铁、镍、铜、锰及其混合物或其盐或络合物。
15.权利要求1的方法，其中所述预掺混料包含30％至70％重量稀释聚酯，所述稀释聚酯包含聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二醇酯或其混合物；30％至70％重量芳族聚酰胺材料；和50至1500ppm重量的氧清除材料，该氧清除材料包含钴的盐或络合物。
16.权利要求1的方法，其中所述基础聚酯为固体颗粒形式。
17.权利要求1的方法，其中所述预掺混料与所述基础聚酯以0.5％至20％重量预掺混料，和80％至99.5％重量基础聚酯的量混合。
18.权利要求1的方法，其中所述基础聚酯选自聚对苯二甲酸乙二醇酯、聚对苯二甲酸萘酯、聚对苯二甲酸丁二醇酯、环己烷二甲醇/聚对苯二甲酸乙二醇酯共聚物或其混合物。
19.权利要求18的方法，其中所述聚对苯二甲酸乙二醇酯包含未用瓶级的聚对苯二甲酸乙二醇酯、用过级的聚对苯二甲酸乙醇酯或其混合物。
20.权利要求1的方法，其中所述型坯含有10至80ppm重量氧清除材料。
21.权利要求1的方法，其中所述基础聚酯是一种未用瓶级聚对苯二甲酸乙二醇。
22.一种塑料容器，所述容器按权利要求1的方法制备。
23.权利要求22的容器，所述容器在填充水后48小时，透氧度为0.035cc O2/包装/天或更小。
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- 2005-01-07 JP JP2006553123A patent/JP5161462B2/ja active Active
- 2005-01-07 KR KR1020067018563A patent/KR101186759B1/ko active IP Right Grant
- 2005-01-07 EP EP05705168A patent/EP1713860B1/en active Active
- 2005-01-07 AU AU2005217350A patent/AU2005217350A1/en not_active Abandoned
- 2005-01-07 CN CN2005800119861A patent/CN1942519B/zh not_active Expired - Fee Related
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Also Published As
| Publication number | Publication date |
|---|---|
| AU2005217350A1 (en) | 2005-09-09 |
| KR20070007096A (ko) | 2007-01-12 |
| US20120219670A1 (en) | 2012-08-30 |
| CN1942519A (zh) | 2007-04-04 |
| EP2272912A2 (en) | 2011-01-12 |
| KR101186759B1 (ko) | 2012-09-28 |
| JP5507530B2 (ja) | 2014-05-28 |
| JP2007522049A (ja) | 2007-08-09 |
| WO2005083003A2 (en) | 2005-09-09 |
| EP1713860A2 (en) | 2006-10-25 |
| US8192676B2 (en) | 2012-06-05 |
| KR20120094006A (ko) | 2012-08-23 |
| US20050181155A1 (en) | 2005-08-18 |
| EP2272912A3 (en) | 2012-02-29 |
| KR101258383B1 (ko) | 2013-04-30 |
| WO2005083003A3 (en) | 2005-10-20 |
| EP2272912B1 (en) | 2017-12-13 |
| JP5161462B2 (ja) | 2013-03-13 |
| EP1713860B1 (en) | 2012-06-13 |
| JP2012101546A (ja) | 2012-05-31 |
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