CN103260854B - 用于容器的单步成形和充填的过程 - Google Patents
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Abstract
一种用于塑料容器的制造和充填的过程,所述过程包括以下步骤:a.使预成形坯(1)相对于两个或更多个部件的模具组件(20,21,22)安置,所述预成形坯一般由塑料制成并设置有纵向轴线(17)且具有可拉伸部分(13)和不可拉伸部分(11);b.使所述预成形坯沿其纵向轴线(17)拉伸;c.将流体(29)添注到所述预成形坯(1)的内部容积(6)中,所述流体(29)处在使所述预成形坯(1)发生塑性变形直至达到期望的尺寸和形状的压力下;和d.将所述容器从所述模具组件(20,21,22)取出并密封所述容器,并且其中,所述预成形坯(1)的可拉伸部分(13)的至少一部分处于比其玻璃化转变温度(Tg)低的温度,且优选地处于环境温度。
Description
技术领域
本发明涉及一种用于制造和充填塑料容器的方法。更特别地,本发明涉及利用经加热的加压空气使例如已通过注塑成型制成的预成形坯扩张而形成容器的技术。
背景技术
上述技术在塑料成形领域内被通常已知为“吹塑(模制)”。特别地,吹塑是一种用于形成容器(如用于食品、饮料或化学物质的容器)的常用技术。用于吹塑的常见塑料树脂包括聚对苯二甲酸乙二醇酯(PET)、高密度聚乙烯(HDPE)和聚丙烯(PP),但是也可采用具有适于所述过程和应用的特性的其它树脂。
用于吹塑过程的典型原料是通过注塑成型形成的大致管状的中空热塑性预成形坯。所述预成形坯一般在一端封闭,在另一端敞开,具有试管或类似容器的外观。预成形坯的敞开端一般呈大致最终成品的形式,可选地包括诸如螺纹、管嘴等的结构特征。然而,预成形坯也可在两端都敞开和未最终定形,具有后来要添加的封闭部和结构特征。
在典型的吹塑过程中,一般使用烤炉或辐射加热器首先对预成形坯进行预加热。预成形坯被加热到的温度是高于材料的玻璃化转变点的温度。这使得预成形坯变软和柔顺,且由此能够流入模具的凹部中。这样吹塑过程的工作温度根据所用材料的性质在55℃至135℃的范围内。
预成形坯一旦被均匀地加热到期望温度便被设置在模具内。模具型腔的廓形被设定成限定成品容器的外形。处在预成形坯的敞开端处的颈部一般从模具的顶部伸出。一拉伸杆被插入到预成形坯的开口中,并且吹塑设备安置在预成形坯的开口周围。在模塑过程中,拉伸杆以这样的方式向预成形坯中前移,以便压入预成形坯的封闭端并使其在其纵向轴线的方向上变形。同时,处在高压下的空气被吹入预成形坯中,使得预成形坯扩张并充满模具型腔。然后使容器冷却,这是通过在弹出容器之前使冷却剂循环流过模具体部或通过将低温流体如液氮喷入容器中来完成的。一旦已充分冷却,便将容器从模具中取出,用产品充填并密封。
如上所述的当前方法在几个方面是不利的。首先,必须对塑料预成形坯进行预加热,以便将塑料维持在用于成形的适当温度,该步骤以能量成本的形式给所述过程增加了相当大的成本。这些成本在大批量的操作中会更令人关切,其中必须使大量的预成形坯非常快地达到工作温度并且需要加热设备的大型设施。其次,由于容器是使用气体来模制的,所以对模塑过程的控制因气体的可压缩性而减弱。第三,容器在模制后必须冷却,并且在其温度已充分降低之前不能进行充填,这限制了吹塑设备可操作的速度并且给所述过程总地增加了另一层复杂性和开销。第四,由于塑料的温度在成形过程中被维持在材料的玻璃化转变点以上,所以最终形成的容器的分子结构仍主要保持为非晶态的,无法获益于强度及源于结晶和应变硬化的其它物理性质的提高。
发明内容
本发明的一个目的可以是通过减少在模制之前预成形坯的加热量来减少完成该过程所需的能量。
本发明的另一个目的可以是为预成形坯提供在不加热到材料的玻璃化转变点以上的情况下实现材料流动的替代手段。
本发明的又一个目的可以是提供可缩短容器吹塑和充填操作的循环时间的手段。
本发明的再一个目的可以是通过减少或消除在目前的吹塑技术中存在的气态流体的不精确和不可控的方面来改善当前的吹塑过程控制手段。
本发明的又一个目的可以是通过增大由吹塑过程生产的容器的结晶度来改善由这种过程生产的容器的晶体结构。
根据第一个方面,本发明涉及一种如在权利要求1中限定的新的过程(工艺流程,方法,process)。相关地,本发明还涉及如在权利要求15中限定的一种用于塑料容器的制造和充填的新系统。根据另一个方面,流体是不可压缩的流体。根据该另一个方面的过程和系统的有利之处在于,通过使用不可压缩的流体而非空气来实现预成形坯的扩张。这是有利的,因为它避免了对添注到扩张的预成形坯中的气体的量和压力的控制中存在的不可预测性和差异。例如,预成形坯可由热塑性树脂制成。
根据本发明的另一个方面,拉伸预成形坯的步骤和添注流体的步骤基本上顺次进行。这具有这样的优点,即允许本发明的实施者通过将所述过程分离成各个不同的可控步骤而对模制过程具有更大的控制。这也更好地允许本发明的实施者针对特定的容器设计优化模制过程:由于模制在几个不同的步骤中发生,因而实施者更能够将特定缺陷的原因限定在所述过程中的某个步骤中并相应地修正它。
根据本发明的一个另选方面,拉伸预成形坯的步骤和添注流体的步骤基本上同时进行。这具有的优点是,使模制过程相对于使用顺次拉伸和添注的过程加快,从而提高吹塑操作的生产能力。
根据本发明的又一个方面,拉伸预成形坯的步骤和添注流体的步骤在添注步骤在拉伸步骤结束之前开始的情况下基本上顺次进行。这结合了本发明的前两个方面的优点,因为各个步骤的开始在时间上错开,且因此构成不同的可控步骤。此外,由于添注步骤不等到拉伸步骤结束就开始,由此获得了制造过程的时间效益。
在本发明的再一个方面中,用于施行容器模制的流体(例如,不可压缩的流体)是将被容器包封并配销给顾客的流体。这是有利的,因为它免除了与获取和操作单独的模制和充填设备相关的资金开销和增加的处理时间。同时,大大改善了容器的消毒过程,因为在该过程中进行消毒的是预成形坯而不是成品容器。具体地,预成形坯的更小的尺寸和更简单的几何形状(相对于成品容器而言)允许消毒过程比现有方法快得多地进行。该方面也能可选地包括这样的步骤,其中在模制过程完成之后在容器上施加密封装置,例如常用来防止变质或调换的那些密封装置。
根据另一个方面,流体处于环境温度。这使得能散除由拉伸步骤产生的热。另外,这是有利的,因为加热或冷却能这样使用的流体不会浪费能量,原因是它储存在或可得自于流体源(在环境温度下)。
本发明的又一个方面是,所述过程所需的能量的量相对于当前的方法大大减少。这种能量减少导致相当大的单位成本节省和总成本节省。所述减少是通过用温度低于其玻璃化转变温度(Tg)、优选地处于环境温度的预成形坯进行吹塑操作来实现的。本发明的该方面的优点在于,由于在对预成形坯进行模制之前有限地进行加热或甚至不加热,在后模制的冷却时间大大缩短或甚至免除。这缩短了总的循环时间并提高了给定吹塑操作的生产能力,从而使容器制造商获得经济利益。有利地,预成形坯的至少一部分、更具体地说是预成形坯的在所述过程中能被拉伸的部分处于比其玻璃化转变温度(Tg)低的温度,最优选地处于环境温度。因此,预成形坯的可拉伸部分的至少30%、优选至少50%、更优选至少70%、最优选90%在预成形坯的拉伸之前处于比其玻璃化转变温度(Tg)低的温度。
优选地,在制造和充填塑料容器的过程中,预成形坯处于环境温度,并且预成形坯的可拉伸部分的具有减小的横截面积的至少一个区域能被加热,以有利于在模制期间开始(促发)变形。
本发明还涉及一种根据权利要求10的预成形件,其旨在用于上述的吹塑过程中。该预成形坯设置有沿其纵向轴线定位的一个或多个横截面积减小的区域。所述横截面积减小的区域用作纵向和径向应力的集中部,从而导致在模制过程中塑性变形始终一致地在所述区域中开始。所述一个或多个区域的横截面积的减小可通过沿预成形坯纵向轴线的平滑的几何形状变化(例如,弯曲的几何形状)、沿预成形坯纵向轴线的尖锐角部(例如,有角的几何形状)或它们的组合来实现。
因此,本发明的另一个方面在于,成品容器的结晶度相对于由根据现有技术的方法生产的容器中发现的结晶度增大。这种结晶度的增大是由于在吹塑过程中预成形坯在比制造其的材料的玻璃化转变温度(Tg)低的温度被模制。这归因于使用了具有良好导热性的不可压缩流体(例如,水尤其具有高的导热性),且因此该流体快速散除了由拉伸步骤产生的热。由此,可用水作为不可压缩的流体获得高水平的结晶度(30-35%)。这导致模制过程中改善的应变硬化,因为使预成形坯变形为期望形状的行为促进了塑料树脂分子的排列和结晶。这种结晶度的增大改善了成品容器的机械和化学特性。
根据权利要求13,本发明的另一个目的是一种控制如上简述的用于制造和充填塑料容器的过程的方法。该方法是有利的,因为与本发明的任意其它方面组合,它允许本发明的实施者通过使用自动化的过程控制系统来优化过程控制和生产能力。
附图说明
图1是用于本发明的预成形坯的图示,包括对图2和3中的单独详细视图的指示;
图2是图1的预成形坯上的变形区域的详细视图,其中该区域包括弯曲的几何形状;
图3是图1的预成形坯上的变形区域的另选的详细视图,其中该区域包括有角的几何形状;以及
图4是可实施本发明的设备的图示。
图5是由根据本发明的过程生产的成品容器的图示。
图6示意性地示出通过根据本发明的过程的一示例获得的实验曲线。
具体实施方式
从下面关于一优选实施例的描述将更好地理解本发明,该优选实施例作为非限制性示例给出,并且参照示出了根据本发明的预成形坯和模制设备的附图1-4加以说明。
用于由塑料、更特别地为热塑性树脂(如PET)吹塑出容器的过程以图1所示的预成形坯1开始。在该优选实施例中,预成形坯1由PET树脂以传统的注塑成型工艺制成。预成形坯1理想地为绕纵向轴线17轴对称的。预成形坯1是大体长形的管状体,包括上部11和下部13。预成形坯1的下部13大体由一起形成壁厚度5的外表面3和内表面4限定而成。所述厚度5不必一定是固定的;它可按照需要沿预成形坯1的体部(沿纵向)稍有差异,以优化成品容器的模制。预成形坯1的上部11设置有台肩9、螺纹10和开口12,它们以这样的方式配置成提供与盖子的简便装配。颈部14包括上部11和下部13之间的过渡部。
上部11是在制造容器的过程中和在沿预成形坯的纵向轴线拉伸预成形坯1的步骤期间不被拉伸的部分。因此它被指定为不可拉伸部分。相反,下部13被限定为可拉伸部分并且在达到容器的期望尺寸和形状之前被拉伸和变形。
预成形坯1还由底部2限定,底部2包括具有内半径7和外半径为8的半球壳。底部2与上部11和下部13结合的作用是使预成形坯具有限定了内部容积6的管状结构。
颈部14设置有相对于预成形坯1的其余部分具有局部减小的壁厚度15的区域16。区域16是在预成形坯1的壁中轴向和径向应力的集中部,用于提供模制期间的始终一致的变形开始部位并由此有利于模制期间预成形坯1的流动。图2和3示出减小的厚度15的两种可能的构型。在图2中,减小的厚度15通过可具有恒定或可变半径的平滑曲线18来实现。而在图3中,预成形坯设置有角部19(尖角),其与曲线18实现相同的目的。虽然在该优选实施例中只采用了一个这样的区域16,但根据所用材料的性质和所形成容器的几何形状也能可选地采用多个这样的区域。
优选地,预成形坯作为一个整体处于环境温度。更具体地说,预成形坯的可拉伸部分的至少一部分处于环境温度,且最优选地处于比预成形坯的玻璃化转变温度(Tg)低的温度。
如所提出,预成形坯的可拉伸部分的至少30%、优选至少50%、更优选至少70%、最优选90%在预成形坯的拉伸之前处于比其玻璃化转变温度(Tg)低的温度。
然而,为了有利于预成形坯的可拉伸部分沿其纵向轴线的拉伸,计划在某些部位对可拉伸部分进行局部加热。有利地,预成形坯能在具有局部减小的壁厚度15的区域16的位置被加热以在模制期间开始可拉伸部分的变形。区域16能在接近玻璃化转变温度(Tg)或高于玻璃化转变温度(Tg)的温度被加热,而预成形坯作为整体保持在比玻璃化转变温度(Tg)低的温度或优选保持在环境温度。
图4示出施行模制过程的设备的优选实施例。该设备包括模具,具有底部20和左、右半部21和22(统称为模具部件),以及带有拉伸元件(如由缸体26驱动的拉伸杆25)的成形头27。模具半部21和22沿模具中心线35相接,并沿模具底部接缝34靠接模具底部20。由此各模具部件的内表面23限定出模具型腔30。应指出,可替换使用具有不同数量的部件的模具。模具还可设置有一个或多个通气口38,以排出在模制操作过程中由预成形坯1排开的空气。
模具半部21和22设置有上开孔36。开孔36的尺寸设定为使得预成形坯的颈部14可穿过开孔36,而预成形坯的台肩9靠接于模具半部21和22的上表面。结果,预成形坯的下部13定位在模具型腔30内,而预成形坯的上部11靠在模具型腔的外部。
在模制操作之前,为模制过程制备预成形坯1。在优选实施例中,对预成形坯清除任何潜在的残留物并消毒杀菌,以防止其未来的内容物变质。优选地,预成形坯处于环境温度。所制备的预成形坯1相对于模具部件20、21和22安设成被如上所述地包围。在实际操作中,预成形坯1被插入到组装好的模具结构中,或者预成形坯1可在模具部件靠到一起并在其周围封闭的同时保持就位。一旦适当地安置定位,模具部件便通过夹具或锁定装置保持就位。该设备与预成形坯1一起形成用于制造和充填塑料容器的系统。然后使成形头27绕预成形坯1的口部28定位,并通过施加外力41保持就位。成形头27能可选地设置有用于与预成形坯的螺纹10接合以改善连接和密封的装置。
在模制操作的准备过程中,预成形坯1处于环境温度或者至少在比其玻璃化转变温度(Tg)低的温度。
预成形坯的可拉伸部分13的局部区域16能在接近其玻璃化转变温度(Tg)或比预成形坯1的玻璃化转变温度(Tg)高的温度被加热,以帮助在模制操作过程中开始预成形坯1的塑性变形。
模制操作这样开始,即,将拉伸杆25前移到预成形坯的内部容积6中,从而通过使其沿其纵向轴线17拉伸而使其发生塑性变形。拉伸杆25借助于气动缸26来驱动,气动缸26由从来源32供给并用阀33调节的压缩空气来操作。或者,也可使用其它驱动装置来驱动拉伸元件的移位。这种变形一直持续到拉伸杆25在底部点37与模具底部20接触,在该点拉伸杆25停下并保持就位,直至模制操作完成。
在拉伸杆25通过拉伸使预成形坯变形时,从来源31供给并用阀39调节的处在压力下的不可压缩流体29(例如,水)被添注到预成形坯的内部容积6中。更特别地,添注在拉伸已开始之后并在其结束之前开始。这使得能沿预成形坯的高度获得规则的结晶度分布。应指出,对最初为非晶态的PET预成形坯进行拉伸会在预成形坯中引起结晶。然而,由拉伸步骤产生的热会破坏所引起的这种结晶。使用不可压缩的流体、特别是具有良好的或甚至是很高的导热性的流体(例如,水)使得能排出拉伸步骤所产生的热并将结晶度保持在很高的水平,例如在30%和35%之间。此外,为了结晶的目的,在添注步骤中使用处于环境温度的水。然而,也可替换使用其它流体(例如,液体),特别是具有在0℃和100℃之间的任何温度的流体。能可选地设置用于在添注不可压缩的流体29之前从预成形坯1的内部除去空气的装置。由拉伸杆25引起的纵向应力以及由不可压缩的流体29的压力引起的纵向和径向应力使得在产生于预成形坯1中的位于区域16的应力集中部处开始塑性变形。
一旦塑性变形开始,预成形坯1持续向模具型腔30中扩张,直至其已大致达到模具内表面23的形状。这种扩张由设备的控制系统借助于适当安置的传感器40来监测。所需要的传感器40的确切数量将根据模具型腔30的形状而不同;这里为了简明起见只示出了两个。应指出,对模制过程的控制是通过控制此过程中模具内的体积(量,volume)增大(速)率来实现的。控制添注到预成形坯中的不可压缩流体(例如,水)的体积(例如,通过流量计或其它适当的装置进行)比控制诸如空气等的可压缩流体的体积容易得多。控制体积增大率使得能控制在模具内预成形坯扩张期间的表面增大率。以这样的方式监控体积增大率,以便获得基本恒定的PET气泡表面增大率,从而趋于在PET预成形坯中尽可能获得最大的结晶度。
如所述,在制造过程中,用预成形坯1使容器成形。所述预成形坯的可拉伸部分13的至少一部分处于比制造其材料的玻璃化转变温度Tg低的温度,优选地处于环境温度。
根据所提出的过程,预成形坯1的可拉伸部分13的至少30%、优选至少50%、更优选至少70%、最优选90%处于比其玻璃化转变温度(Tg)低的温度,从而使得所述过程中所需的能量可减少。
图6示出在实施根据本发明的制造过程的一个示例的过程中获得的示意性曲线(a)、(b)和(c)。曲线(a)表示在模制过程中拉伸位置随时间的幅度。曲线(b)表示在预成形坯被拉伸时添注到预成形坯中的不可压缩流体(例如,水)的体积的大小。从图中可清楚看到,流体在预成形坯的拉伸正在进行时开始添注。最后,呈虚线的曲线(c)表示水体积的设定值的大小。
一旦扩张已结束,便打开模具半部21和22并移除容器而不排空不可压缩的流体29。最后优选通过螺纹盖将不可压缩的流体29(例如,水或其它液体)密封在容器的内部,然后准备好通过配销其中所容纳的流体来使用容器。借助于所述优选实施例生产的成品容器在图5中示出,其中为了简明起见略去了盖子。
当然,本发明不限于上面所述和在附图中所示的实施例。变型是可能的,特别是关于各种要素的构造或通过技术等同物的替换,而由此不会脱离本发明的保护范围。因此,本公开的范围意在示例性而非限制性的,本发明的范围由至少部分地源自本公开的任何权利要求来限定。
Claims (16)
1.一种用于塑料容器的制造和充填的方法,所述方法包括以下步骤:
a.使预成形坯(1)相对于至少两个部件的模具组件(20,21,22)安置,所述预成形坯由塑料制成并设置有纵向轴线(17)且具有可拉伸部分(13)和不可拉伸部分(11),所述可拉伸部分(13)设置有具有局部减小的壁厚度(15)的至少一个区域(16);
b.使所述预成形坯沿其纵向轴线(17)拉伸;
c.将流体(29)添注到所述预成形坯(1)的内部容积(6)中,所述流体(29)处在使所述预成形坯(1)发生塑性变形直至达到期望的尺寸和形状的压力下;和
d.将所述容器从所述模具组件(20,21,22)取出并密封所述容器;
并且其中,所述至少一个区域(16)在高于玻璃化转变温度的温度被加热,而所述预成形坯(1)的可拉伸部分(13)的与所述至少一个区域不同的至少一部分处于比其玻璃化转变温度低的温度。
2.根据权利要求1所述的方法,其特征在于,所述流体是不可压缩的流体(29)。
3.根据权利要求1所述的方法,其特征在于,所述预成形坯由热塑性树脂制成。
4.根据权利要求1所述的方法,其特征在于,拉伸所述预成形坯(1)的步骤和添注所述流体(29)的步骤顺次进行。
5.根据权利要求4所述的方法,其特征在于,添注所述流体(29)的步骤在拉伸所述预成形坯(1)的步骤结束之前开始。
6.根据权利要求1所述的方法,其特征在于,拉伸所述预成形坯(1)的步骤和添注所述流体(29)的步骤同时进行。
7.根据权利要求1所述的方法,其特征在于,添注到所述预成形坯(1)中以形成所述容器的流体(29)被包封在所述容器内并与所述容器一起配销。
8.根据权利要求1所述的方法,其特征在于,所述流体处于环境温度。
9.根据权利要求1所述的方法,其特征在于,所述预成形坯(1)的可拉伸部分(13)的至少30%处于比其玻璃化转变温度低的温度。
10.根据权利要求1所述的方法,其特征在于,所述预成形坯(1)的可拉伸部分(13)的至少50%处于比其玻璃化转变温度低的温度。
11.根据权利要求1所述的方法,其特征在于,所述预成形坯(1)的可拉伸部分(13)的至少70%处于比其玻璃化转变温度低的温度。
12.根据权利要求1所述的方法,其特征在于,所述预成形坯(1)的可拉伸部分(13)的至少90%处于比其玻璃化转变温度低的温度。
13.一种控制根据权利要求1至12中任一项所述的方法的方法,包括:在模制过程中监控拉伸元件(25)的位置、所述流体(29)的体积流量、流体(29)的压力、拉伸元件(25)的力、和变形模式;以及,根据拉伸元件(25)的位置、所述流体(29)的体积流量、流体(29)的压力、拉伸元件(25)的力、和变形模式之间的预定关系来调节所述拉伸元件(25)的位置和流体(29)的体积流量,所述关系配置成优化被制造的特定类型容器的制造。
14.根据权利要求13所述的方法,其特征在于,所述流体(29)是不可压缩的流体。
15.一种用于塑料容器的制造和充填的系统,所述系统包括:
a.至少两个部件的模具组件(20,21,22);
b.相对于所述模具组件安置的预成形坯,所述预成形坯(1)由塑料制成并设置有纵向轴线(17);
c.用于使所述预成形坯(1)沿其纵向轴线(17)拉伸的拉伸元件(25);
d.用于将流体(29)添注到所述预成形坯(1)中的装置,所述流体(29)处在使所述预成形坯(1)发生塑性变形直至达到期望的尺寸和形状的压力下;
e.用于将所述容器从所述模具组件取出的装置;和
f.用于密封所述容器的装置,
其特征在于,所述预成形坯具有可拉伸部分(13)和不可拉伸部分(11),所述可拉伸部分(13)设置有具有局部减小的壁厚度(15)的至少一个区域(16),并且
所述系统还包括加热装置,用于在接近玻璃化转变温度或高于玻璃化转变温度的温度加热所述至少一个区域(16),而所述预成形坯(1)的可拉伸部分(13)的与所述至少一个区域不同的至少一部分处于比其玻璃化转变温度低的温度。
16.根据权利要求15所述的系统,其特征在于,所述流体(29)是不可压缩的流体。
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PCT/EP2011/072011 WO2012076576A2 (en) | 2010-12-10 | 2011-12-07 | A process for single-step forming and filling of containers |
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DE102013101775A1 (de) * | 2013-02-22 | 2014-08-28 | Khs Gmbh | Verfahren und Vorrichtung zur Herstellung und Füllen von Behältern |
PL3024335T3 (pl) * | 2013-07-25 | 2018-02-28 | Air Products And Chemicals, Inc. | System chłodzenia kriogenicznego drobiu i sposób |
EP2883800B1 (en) * | 2013-12-13 | 2017-08-16 | Discma AG | Piston device comprising a valve controlling the inlet of the piston device |
EP2930005B1 (en) * | 2014-04-08 | 2017-06-07 | Discma AG | Rotary machine and method for hydraulic forming of shaped containers |
EP2942177B1 (en) | 2014-05-05 | 2017-07-12 | Discma AG | Method for hydroforming a container from a preform |
FR3029133B1 (fr) * | 2014-11-27 | 2016-12-30 | Sidel Participations | Procede de fabrication de recipient a boxage cale sur le soufflage |
BR112017028189A2 (pt) * | 2015-06-26 | 2018-09-04 | Procter & Gamble | recipiente lustroso |
FR3063926B1 (fr) * | 2017-03-17 | 2019-04-12 | Sidel Participations | Procede de reglage automatique de la course d'une tige d'etirage d'un dispositif de formage de corps creux |
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BR112013014378B1 (pt) | 2020-10-06 |
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JP5985501B2 (ja) | 2016-09-06 |
RU2013131730A (ru) | 2015-01-20 |
MX2013006513A (es) | 2013-06-28 |
BR112013014378A2 (pt) | 2016-09-27 |
CA2819873A1 (en) | 2012-06-14 |
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US20130326998A1 (en) | 2013-12-12 |
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