CN107002234B - 具有增强的二氧化硅屏蔽涂层的pet容器的制造方法 - Google Patents

具有增强的二氧化硅屏蔽涂层的pet容器的制造方法 Download PDF

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CN107002234B
CN107002234B CN201580061321.5A CN201580061321A CN107002234B CN 107002234 B CN107002234 B CN 107002234B CN 201580061321 A CN201580061321 A CN 201580061321A CN 107002234 B CN107002234 B CN 107002234B
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pet container
coating
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temperature
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CN107002234A (zh
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谢尔盖·B·波布罗夫
马克·D·施奈德
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Graham Packaging Co LP
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Abstract

本发明提供了一种用于向PET容器施加氧化硅屏蔽涂层的方法，其中所述PET容器包含具有内表面和外表面的壁，所述方法包括下述步骤：(a)加热PET容器以使得至少所述外表面处于约200℉至约383℉的温度；(b)在所述PET容器的至少所述外表面的温度处于约200℉至约383℉的温度时，通过在所述PET容器的至少所述内表面上施加至少一层氧化硅屏蔽层，形成涂层的PET容器；以及(c)在步骤b后冷却所述涂层的PET容器。

Description

具有增强的二氧化硅屏蔽涂层的PET容器的制造方法
发明背景
技术领域
本发明涉及具有增强的屏蔽性质的塑料容器，特别是在热处理后例如在将容器及其内含物加热至高达270℉的应用中保留有增强的屏蔽性质的塑料容器。这些应用包括灭菌、巴氏消毒或釜式灭菌过程。本发明还涉及制造这些塑料容器的方法。
背景技术
用于形成PET容器的吹塑模制法在本领域中是公知的。对于许多应用来说，PET塑料容器已代替玻璃容器或提供了玻璃容器的可替代物。某些包装在吹塑模制的PET容器中的食品必须至少在高温即高达195℉下装填，并且在某些情况下，必须在高达230℉和更高温度下使用巴氏消毒或釜式灭菌进行处理。巴氏消毒和釜式灭菌方法通常用于消毒固体或半固体食品例如腌菜和泡菜。所述食品可以在低于180℉的温度下与液体一起包装在容器中，然后密封并加盖，或者可以将所述食品置于容器中，然后装填以前可能已加热过的液体，随后将密封并加盖的容器的整个内含物加热至较高温度。当在本文中使用时，“高温”巴氏消毒和釜式灭菌是将产品暴露于约176℉至约270℉的温度下的灭菌过程。
巴氏消毒和釜式灭菌与热填充加工的区别在于包括将所述装填的容器加热至通常高于200℉的指定温度，直至所述装填的容器的内含物达到指定温度例如175℉预定的时间长度。也就是说，热填充的容器的外部温度可能高于200℉，使得固体或半固体产品的内部温度达到约175℉。巴氏消毒和釜式灭菌过程也可以包括向容器施加超压。对于对流体例如氧(进入)和二氧化碳(外出)具有高的气体屏蔽要求的塑料容器的使用来说，这种加工的苛刻性提出了显著挑战。一种出色的屏蔽材料是基于氧化硅的屏蔽涂层，其通常使用商业上可用的真空化学气相沉积方法施加到容器的内部。与没有所述氧化硅涂层的相同容器相比，这些新鲜涂层的容器的屏蔽改善因子(BIF)可以高达200X或更高。在巴氏消毒和釜式灭菌过程中，容器通常被容器内的高温和内部压力扭曲，这可以对所述氧化硅涂层施加应力并在所述涂层中形成微裂缝。这导致BIF劣化了20X或更多，由此产生BIF不超过10X的净结果。当然，劣化的BIF最终反映到被包装产品的保质期缩短。
因此，在本领域中，对具有基于氧化硅的屏蔽涂层的吹塑模制的PET容器的生产方法，存在着需求，其中所述屏蔽涂层能够抵抗巴氏消毒或釜式灭菌过程的苛刻性而不牺牲显著部分的通过施加所述涂层获得的BIF。
发明概述
一方面，本发明提供了一种用于向PET容器施加氧化硅屏蔽涂层的方法，其中所述PET容器包含具有内表面和外表面的壁，所述方法包括下述步骤：(a)加热PET容器以使得至少所述外表面处于约200℉至约383℉的温度；(b)在所述PET容器的至少所述外表面的温度处于约200℉至约383℉的温度时，通过在所述PET容器的至少所述内表面上施加至少一层氧化硅屏蔽层，形成涂层的PET容器；以及(c)在步骤b后冷却所述涂层的PET容器。
另一方面，本发明提供了一种包含氧化硅屏蔽涂层并且作为所述氧化硅屏蔽涂层的结果而具有屏蔽改善因子(BIF)的PET容器，其中所述PET容器在暴露于热灭菌过程后保留至少17％的BIF。
另一方面，本发明提供了一种涂层的PET容器，其中所述PET容器包含具有内表面和外表面的壁，并通过包含下述步骤的方法来制造：(a)加热PET容器以使得至少所述外表面处于约200℉至约383℉的温度；(b)在所述PET容器的至少所述外表面的温度处于约200℉至约383℉的温度时，在所述PET容器的至少所述内表面上施加至少一层氧化硅屏蔽层，以形成所述涂层的PET容器；以及(c)在步骤b后冷却所述涂层的PET容器，其中所述涂层的PET容器对氧具有屏蔽改善因子(BIF)，并且其中在所述涂层的PET容器暴露于热灭菌过程后，所述对氧的BIF基本上得以保留。
附图简述
正如在附图中说明的，从下面本发明的优选实施方式的更具体的描述，本发明的上述和其他特点和优点将显而易见，在所述附图中相似的指称数字通常指示一致的、功能上相似的和/或结构上相似的要素。
图1是符合本发明的罐型PET容器的透视图；
图2是形成15oz容器的圆筒段的PET材料的DSC热谱图；并且
图3是从其获取图3中所分析的样品的同一容器的门附近的底部区的DSC热谱图。
发明详述
下面详细讨论本发明的实施方式。在描述实施方式中，为清楚起见使用了特定术语。然而，本发明不打算受限于所选的特定术语。尽管讨论了特定示例性实施方式，但应该理解这样做仅仅是出于说明的目的。相关领域的技术人员将会认识到可以使用其他组分和配置，而不背离本发明的精神和范围。本文中引用的所有参考文献通过参考并入本文，如同每个参考文献被单个地并入。
本发明提供了一种用于向PET容器施加氧化硅屏蔽涂层的方法，其中所述PET容器包含具有内表面和外表面的壁，所述方法包括下述步骤：(a)加热PET容器以使得至少所述外表面处于约200℉至约383℉的温度；(b)在所述PET容器的至少所述外表面的温度处于约200℉至约383℉的温度时，通过在所述PET容器的至少所述内表面上施加至少一层氧化硅屏蔽层，形成涂层的PET容器；以及(c)在步骤(b)后冷却所述涂层的PET容器。
本发明的方法可以在由具有增强的热性能并同时为容器提供高澄清度的聚酯树脂例如聚对苯二甲酸乙二酯(PET)制成的任何容器上进行。适合的聚酯树脂包括例如聚邻苯二甲酸乙二酯的均聚物、聚对苯二甲酸乙二酯、聚间苯二甲酸乙二酯、聚萘二甲酸乙二酯和聚对苯二甲酸二甲酯、聚对苯二甲酸丁二酯的共聚物。在优选实施方式中，本发明的容器包含PET。优选地，所述PET具有约0.72dL/g至约0.86dL/g的特性粘度。适合的PET树脂包括制瓶级PET树脂例如由DAK Americas销售的任何树脂和由M&G Polymers销售的CLEAR 树脂。
本发明的PET容器可以具有任何几何构造、形状或尺寸。例如，符合本发明的PET容器可以是圆的、椭圆的、多边形的和不规则的。适合的容器可以是坛型、罐型、滤酒器型、广口和本领域普通技术人员已知的任何其他类型的容器。容器的适合的特点可以包括压力吸收特点、抓握加强特点、肩、减震器、表面漆、谐音(chime)、固定环(standing ring)、颈和本领域普通技术人员已知的其他特点。这些容器包含具有被所述PET聚合物的厚度分隔开的内表面和外表面的壁。
本发明的方法可以在新鲜制造的PET容器上或在已被制造、冷却、储存和/或运输的PET容器上进行。在优选实施方式中，本发明的方法利用按照美国专利申请公开号2012/0076965和美国专利号8,507,063制造的在结构上抵抗巴氏消毒和釜式灭菌过程的吹塑模制的PET容器，所述专利申请和专利的内容整体通过参考并入本文。这些容器通常包含密度在约1.370g/cc至1.385g/cc之间、热诱导的结晶度为约18％至约25％并且应变诱导的结晶度为约55％至约75％的壁，其在装填有温度为约212℉至约270℉的液体之后，经历的体积变化不超过3％，更优选地不超过2％，最优选地不超过1％。
本发明的方法包括在施加氧化硅屏蔽涂层之前将PET容器加热到约200℉至约383℉的表面温度的步骤。这个步骤在本文中也被称为“调制”步骤。用于所述调制步骤的热可以通过本领域技术人员已知的任何手段来施加，例如由热风枪产生的热空气、红外加热器或其组合。在本发明的方法的加热步骤中使用的热的优选来源是“通道”或仓室中的红外加热器或一系列红外加热器，以更好地包容发射出的热。适合与本发明相结合使用的示例性红外加热装置包括例如可以从ProthermTM(Brandon,MN)商购的红外加热装置和Axon的辐射ThermoRayTM热通道(Axon Styrotech(USA),Raleigh,NC)。
在优选实施方式中，在施加氧化硅涂层之前，可以将所述PET容器加热以将所述容器的壁的至少外表面温度升高到至少200℉，更优选地高达383℉。在一个优选实施方式中，将热均匀地施加在容器周围。为了实现这种加热，可以利用装备有旋转元件的加热通道为所述容器提供旋转，以确保围绕容器周边的热暴露的均匀性。在其他优选实施方式中，所述加热(即调制)步骤包括将所述PET容器加热到整个壁优选地约200℉至约383℉的温度，更优选地加热到整个壁约225℉至约383℉的温度，最优选地加热到整个壁约250℉至约383℉的温度。当在本文中使用时，短语“整个壁”意味着对于特定温度区来说，从所述壁的外表面到所述壁的内表面均实现该温度。
所述加热元件可以被设定到相同温度或沿着所述容器的竖直轴不同的温度，以产生不同的加热“区”。不同的加热区可以允许为容器的不同区段“定制”加热，以最终产生实现最大BIF保留所需的最大益处。例如，参考图1，PET“坛”容器10可以包含表面漆12、肩14、圆筒16、后跟18和底面20。较厚的区段例如肩14、圆筒16和后跟18可能需要较高的表面温度以更好地调制所述容器，以备施加氧化硅涂层。例如，肩14、圆筒16和后跟18区段可以暴露于超过275℉且最高383℉的温度，而所述底面只能被加热到212℉，并且所述表面漆只能被加热到140℉。其他包装物品可能需要不同的温度区，这可以由普通技术人员确定。
作为指导，优选地将所述区加热至不超过利用差示扫描量热术(DSC)通过焓变所测量的显著分子变化的起始温度的温度。当在本文中使用时，术语“焓变”是指当发生分子变化时被所述物质释放(放热，负值)或吸收(吸热，正值)的能量的量。这种焓变的实例是聚合物的熔点和/或玻璃化转变温度，其作为每个区段中聚合物形态差异的结果，在同一PET容器的不同区段中可以不同。
DSC是可用于确定容器的不同区中的目标调制温度、使得所述调制温度不超过所述PET容器的相应区段的显著焓变的工具。例如，图2是形成按照美国专利申请公开号2012/0076965中公开的方法制造的15oz容器的圆筒区段的PET材料的DSC热谱图。图2示出了聚合物中第一次可察觉的转变(通常为熔化开始)发生在约383℉(显示为194.79℃)；因此，该区域可以被加热至最高383℉而不影响所述容器的完整性。图3是从其获取图2中分析的样品的相同容器的门周围的底部区的DSC热谱图。图3的热谱图示出了聚合物中第一次可察觉的转变、即玻璃化转变，发生在约212℉(显示为100.22℃)；因此，容器的该区域可以被加热至约212℉或更低，而不影响所述容器的完整性。沿着所述PET容器的竖直区段的这种“剖面分析”的目的是在施加所述氧化硅屏蔽涂层之前最大化所述PET容器的每个区段中所述聚合物的热膨胀，正如在下面解释的。
本发明的方法包括在所述PET容器的至少所述外表面的温度处于约200℉至约383℉的温度时在所述PET容器的壁的至少所述内表面上形成至少一层氧化硅屏蔽涂层的步骤。通常，通过化学气相沉积(CVD)方法，优选地通过等离子体增强化学气相沉积(PECVD)方法这种沉积氧化硅屏蔽薄膜的技术，将氧化硅屏蔽涂层施加到PET容器。所述方法通常包括将所需屏蔽材料或所需屏蔽材料的前体以气体形式导向PET容器附近并添加能量，直至所述屏蔽气体或前体气体解离成等离子体状态。可以存在真空条件以允许所述过程在低得足以防止PET容器热损坏的温度下发生。不打算受到任何特定理论限制，据信解离的粒子在撞击PET容器的表面后，由于与试剂的化学反应而固化并附着于容器表面，并且受到聚合物极性的促进以产生所述氧化硅屏蔽层。另外，也可以使用其他适合类型的沉积方法向所述容器施加屏蔽涂层。
所述氧化硅屏蔽涂层优选被沉积在所述PET容器的内壁上。然而，也可以提供外部屏蔽涂层。另外，优选地向所述容器提供氧化硅屏蔽薄膜，尽管也可以使用其他类型的薄膜，例如利用乙炔或多种环氧热固性材料生产的薄膜。
在本发明中可以利用本领域中已知的任何适合的手段来引发等离子体。适合用于本发明的一种PECVD方法描述在美国专利号5,670,224中，所述专利通过参考并入本文。美国专利号5,670,224中描述的方法包括通过微波等离子体增强化学气相沉积将改性的氧化硅屏蔽涂层沉积在PET容器基材上的方法。所述方法包括下述步骤：1)提供可抽空的沉积仓室，其具有限定在其中的沉积区；2)提供微波能量源；3)将PET基材(例如容器)提供在所述沉积仓室中的沉积区内；4)抽空所述沉积仓室至低于大气压；5)进行所述PET基材的等离子体预处理；6)将前体气态混合物引入到所述沉积仓室内的沉积区中，所述混合物至少包含含有硅-氢的气体、含有氧的气体和含有选自锗、锡、磷和硼的至少一种元素的气体；7)将微波能量从所述微波能量源导向所述沉积区，由此在所述沉积区中通过所述微波能量与所述前体气态混合物的相互作用产生等离子体；8)将材料涂层从所述等离子体沉积在所述PET基材上，所述材料涂层为涂层的基材提供了比未涂层的基材更好的屏蔽性质；以及9)将足够流速的含氧气体引入到所述前体气态混合物中，以消除所述沉积的涂层中包含的硅-氢键。然而，美国专利号5,670,224公开了由于等离子体沉积固有地是高温过程，因此基材必须被间歇地冷却以便避免基材的破坏。此外，美国专利号5,670,224没有提到在施加所述屏蔽涂层之前基材的表面温度。
适合用于本发明的另一种PECVD方法描述在美国专利申请公开号2012/0231182中，所述申请通过参考并入本文。美国专利申请公开号2012/0231182公开了一种处理容器的方法，所述方法使用射频能量来解离化学前体，其重新结合将薄膜沉积在所述反应附近的表面上或处理所述容器的表面(例如灭菌、组织化处理等)。开发了一种仓室，其整合了将化学前体递送到仓室容积内的方法、从仓室空间内排气的机构、解离所述化学前体并产生化学反应的电极组件，通过所述化学反应将薄膜沉积在所述容器的内表面上。
用于执行屏蔽涂层方法的制造设备可以通过多个商业化来源购买。例如，下述公司制造商品化屏蔽涂层设备(后面跟随的，如果有的话，是每个公司为它们相应的屏蔽涂层设备和/或过程所命名的商品名)：Sidel(ACTIS)，Krones/Leybold(BestPet)，Tetra Pak(Glaskin)，Nissei，PPG(Bairocade)和KHS Plasmax。
本发明的方法还包括在施加屏蔽涂层后冷却所述PET容器的步骤，其中所述涂层的PET容器具有屏蔽改善因子(BIF)。所述冷却优选地通过简单地允许所述容器在环境空气中平衡到室温来实现。
按照本发明的方法制造的涂层的PET容器的BIF，可以提供针对氧进入或针对二氧化碳外出的屏蔽改善。针对例如氧的BIF，优选地通过下述方法来测量。
BIF/氧
瓶子样品在环境相对湿度、一个大气压和23℃下的透氧率，可以使用MoconOxTran 2/60型(MOCON Minneapolis,Minn.)或Oxygen Permeation Analyzer 8701型(SysTech/Illinois Instruments)(Chicago,Illinois)来测量。使用超高纯(UHP)氮气作为载样气体，并使用环境空气(20.9％氧气)作为试验气体。在试验之前，将样本用UHP氮气调制。试验继续进行直至获得稳态基线，其中对于20分钟的循环来说透氧率变化小于1％。当所述透氧率达到稳态时停止试验，在所述稳态中，当在正常大气条件下进行时，所述透氧率在20分钟的试验循环期间的变化小于1％。氧渗透结果被测量并记录为cm3/包装/天。为了测量屏蔽改善因子或“BIF”，将不含氧屏蔽层的对照瓶在与试验瓶相同的时间，在一致的条件下进行测量。通过用所述对照瓶的氧渗透除以所述试验瓶的氧渗透，来计算BIF。因此，例如，如果未涂层的单层PET容器表现出0.030cm3/包装/天的透氧度(进入)，并且现在涂层有氧化硅涂层的相同容器表现出0.003cm3/包装/天的透氧度(进入)，则BIF为0.030/0.003＝10。
根据本发明，对已暴露于热灭菌过程例如巴氏消毒或釜式灭菌的容器重复所述程序。
不打算受到任何特定理论限制，据信所述加热或调制步骤在沉积所述氧化硅屏蔽层之前使所述PET容器膨胀或延长，以便将所述氧化硅屏蔽层沉积在所述膨胀的容器上。这产生了一种构建物，其中所述PET容器基材与所述树脂的热膨胀系数成比例地膨胀，但所述氧化硅屏蔽涂层在涂层被沉积时不膨胀。在冷却后，PET容器“收缩”到其“正常”尺寸，并且在这样做时，氧化硅屏蔽层被压缩并变得更加紧密堆积或致密。因此，据信压缩的氧化硅屏蔽涂层能够吸收部分由包装内含物对巴氏消毒或釜式灭菌过程期间经历的高温的响应而产生的应力，因为所述PET容器再次与容器中的内部压力引起的热膨胀系数成比例地膨胀。
在实践中，本发明的方法的结果是所述PET容器在暴露于热灭菌过程(例如巴氏消毒或釜式灭菌)后，相对于通过施加氧化硅屏蔽涂层和冷却容器而首次获得的、即在暴露于热灭菌过程之前的BIF，保留了至少17％的所述BIF。本发明人发现，PET容器在暴露于热灭菌过程后的BIF保留率依赖于调制步骤的温度。例如，已发现，BIF保留率对于调制到200℉的PET容器来说为至少17％并高达35％，对于调制到225℉的PET容器来说为至少61％并高达121％，对于调制到250℉的PET容器来说为至少64％并高达125％，并且对于调制到275℉的PET容器来说为至少82％并高达160％，正如在下面的表1中示出的。当在本文中使用时，“125％”意味着BIF不仅完全保留，而且比新鲜涂层的容器、即在暴露于热处理例如巴氏消毒或釜式灭菌之前好25％。当在本文中使用时，“160％”意味着BIF不仅完全保留，而且比新鲜涂层的容器、即在暴露于热处理例如巴氏消毒或釜式灭菌之前好60％。
表1：对于200℉至275℉范围内的每种预加热温度来说，4个容器的平均保留BIF，其随着每单位时间的氧扩散的减少而变。
200℉ 225℉ 250℉ 275℉
最大值 35％ 121％ 125％ 160％
平均值 21％ 76％ 79％ 102％
最小值 17％ 61％ 64％ 82％
按照本发明的方法，通常在暴露于温度高达约356℉的热灭菌过程例如巴氏消毒和釜式灭菌后经历上面提到的BIF保留率。优选地，所述热灭菌的温度在约212℉至约356℉的范围内。
实施例
表1的容器是15oz PET耐热吹塑模制容器，其按照美国专利申请公开号2012/0076965中公开的方法制造。表1的容器在施加氧化硅涂层之前被预加热(即调制)到所陈述的温度，并且在冷却后进行热灭菌过程。热灭菌过程在高压锅中进行，所述高压锅在1.1-1.2atm的压力下在20分钟后达到235℉。表1中列出的结果是为每个调制温度分析的4个样品的平均值。
在本说明书中示出并讨论的实施方式仅仅旨在向本领域技术人员教示本发明人已知的制造和使用本发明的最佳方式。本说明书中的任何描述都不应被当作限制本发明的范围。提出的所有实例都是代表性而不是限制性的。正如本领域技术人员根据上述教示所认识到的，上面描述的本发明的实施方式可以被修改或改变而不背离本发明。尽管本发明参考广口容器进行描述，但符合本发明的嵌板曲率的功能应该对标准表面漆(即不是带有表面漆的广口颈)有效。因此应该理解，在权利要求书及其等同性范围内，本发明可以以具体描述的之外的其他形式实践。

Claims (13)

1.一种用于向PET容器施加氧化硅屏蔽涂层的方法，其中所述PET容器包含具有内表面和外表面的壁，所述方法包括下述步骤：
a.将所述PET容器加热到整个所述壁达到225℉至383℉的温度；
b.在所述PET容器的整个所述壁处于225℉至383℉的温度时，通过在所述PET容器的至少所述内表面上施加至少一层氧化硅屏蔽层，形成涂层的PET容器；以及
c.在步骤b后冷却所述涂层的PET容器，其中步骤a包括使用加热通道，所述PET容器移动穿过所述加热通道，并且其中所述加热通道包含沿着所述容器的竖直轴设置的2至6个不同温度的加热区。
2.权利要求1的方法，其中步骤a包括将所述PET容器加热到整个所述壁达到250℉至383℉的温度。
3.权利要求1的方法，其中步骤b包括：
i.在其中放置有至少一个PET容器的仓室中形成真空；
ii.向所述PET容器的壁的至少所述内表面添加形成氧化硅的单体反应气体；以及
iii.将所述PET容器暴露于等离子体能量，以在所述PET容器的壁的至少所述内表面上沉积至少一层氧化硅。
4.权利要求1的方法，其中所述加热通道包含旋转元件以使所述容器旋转，以便确保周边均匀的热暴露。
5.一种涂层的PET容器，其中所述PET容器包含具有内表面和外表面的壁，并通过包含下述步骤的方法来制造：
a.将所述PET容器加热到整个所述壁达到225℉至383℉的温度；
b.在所述PET容器的整个所述壁处于225℉至383℉的温度时，通过在所述PET容器的至少所述内表面上施加至少一层氧化硅屏蔽层，形成所述涂层的PET容器；以及
c.在步骤b后冷却所述涂层的PET容器，
其中步骤a包括使用加热通道，所述PET容器移动穿过所述加热通道，并且其中所述加热通道包含沿着所述容器的竖直轴设置的2至6个不同温度的加热区，其中在所述涂层的PET容器暴露于热灭菌过程后，所述PET容器保留至少125％的屏蔽改善因子，所述屏蔽改善因子是通过用不含氧屏蔽层的对照瓶的氧渗透除以试验瓶的氧渗透来计算的，其中所述对照瓶在与所述试验瓶相同的时间，在一致的条件下进行测量。
6.权利要求5的涂层的PET容器，其中所述热灭菌过程的温度为212℉至356℉。
7.权利要求5的涂层的PET容器，其中所述热灭菌过程的温度为235℉。
8.权利要求5的涂层的PET容器，其中所述PET具有0.72dL/g至0.86dL/g的特性粘度。
9.权利要求5的涂层的PET容器，其中所述壁的密度在1.370g/cc至1.385g/cc之间、热诱导的结晶度为18％至25％并且应变诱导的结晶度为55％至75％。
10.权利要求5的涂层的PET容器，其中所述热灭菌过程是巴氏消毒过程。
11.权利要求5的涂层的PET容器，其中所述热灭菌过程是釜式灭菌过程。
12.权利要求5的涂层的PET容器，其中在所述涂层的PET容器暴露于热灭菌过程后，保留125％的屏蔽改善因子。
13.权利要求5的涂层的PET容器，其中在所述涂层的PET容器暴露于热灭菌过程后，保留160％的屏蔽改善因子。
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