CN102933369A - 注坯拉伸吹塑方法,预成型件和容器 - Google Patents
注坯拉伸吹塑方法,预成型件和容器 Download PDFInfo
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Abstract
本发明涉及一种由聚乙烯材料制成的固体预成型件,其中预成型件包括颈部区域、侧壁和基座区域,并且包括具有内壁的内部和具有外壁的外部;其特征在于按聚乙烯材料的总重量计,至少65%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值,其中Mn为数均分子量,并且Mz/Mn为Mz值除以Mn值。
Description
发明领域
注坯拉伸吹模法是一种广泛实用的制造瓶子的方法,所述瓶子由聚酯制成,具体地由聚对苯二甲酸乙二酯制成。除了其它用途之外,此类瓶子常用于软饮料的包装。
发明背景
相对于其它材料来讲,使用聚乙烯材料来制造容器具有许多优点。一个优点是,它们容易回收利用并且与现有的回收利用基础设施是相容的,这不同于某些其它材料诸如聚丙烯的情况。另一个优点是,与其它材料诸如对高pH敏感的聚对苯二甲酸乙二醇酯相比,它们不太容易发生“pH劣化和脱色”(裂化和结构损失)。这意味着在成品容器中能够储存具有一系列pH的更宽系列的材料。另一个优点是,由聚乙烯材料制成的容器更适用于对容器进行进一步的下游加工,诸如结合需要广泛变形的一体式柄部。
注坯拉伸吹塑技术获得了聚乙烯材料的优先分子取向,这超过了用传统生产容器的方法诸如挤坯吹塑所能够获得的效果。因此,其导致更高效的材料利用率,因为其改善了诸如拉伸模量(对弹性材料的“硬度”的量度)之类的特性。例如,相比于不能赋予同样多分子取向的更传统的方法来讲,在拉伸吹塑中所获得的聚乙烯取向可允许少使用25%的材料。因此,注坯拉伸吹塑提供了一种更经济且更高效的制造容器的方法的可能性。
注坯拉伸吹塑包括如下步骤:首先注塑预成型件,将其拉伸,然后增加拉伸过的预成型件中的内部压力以产生最终容器形状。预成型件也能够通过压塑或热成型来形成。
以商业速度注塑某种材料的能力要求材料具有良好的“剪切致稀特性”。剪切致稀为当材料处于熔融相期间向所述材料上施加应力时所表现出的典型的流变行为。换句话讲,处于熔融状态的材料必须流动使得其能够适形于模具的所有轮廓并且不产生过厚或过薄的材料区域。
在拉伸吹塑步骤中拉伸材料的能力要求材料表现出“应变硬化”,所述应变硬化被定义为拉伸阻力随着增加的延伸变形而产生的增加。该特性确保了良好的材料分布,因此所形成的容器不具有洞或其中材料被拉伸得太薄的区域。这意味着当材料达到一定厚度时,其会阻抗进一步的延伸,因此防止洞的最终形成。
高分子量聚乙烯材料表现出应变硬化,因而适用于拉伸吹塑。因此,由高分子量聚乙烯材料制成的预成型件能够被拉伸吹塑成具有良好材料分布并因此不具有洞或者薄或厚材料区域的容器。然而,高分子量材料的使用会导致较差的剪切致稀。
高分子量聚乙烯材料是存在的并且已用于注坯拉伸吹塑,如公布于2000年3月28日的JP-A-2000/086722所提及的那样。JP-A-2000/086722公开了一种经受注坯拉伸吹塑的高密度聚乙烯树脂。上述材料趋于因应变硬化特性而拉伸性能良好,但会因缺乏剪切致稀特性而在注塑中表现不佳。
此外,塑料部件在它们受到拉伸应力以及接触到包含氧化剂和表面活性剂的液体时会因环境应力而裂化。在容器中,应力断裂仅会在处于拉伸变形及接触液体的区域中发生。该拉伸应力导致“局部裂缝”(细小裂缝)的形成,所述局部裂缝在某些情况下会变成连续裂缝。聚乙烯作为规则有序的结晶片段的复合材料存在于无序聚合物基质中。从化学方面来讲,这两个相是彼此不能够区分的,但它们形成独立的离散相。接合分子将所述各种微晶连接在一起。当聚乙烯材料处于拉伸载荷下时,微晶处于应力下并且它们随着接合分子被拉伸而开始彼此远离。液体中的氧化剂(例如漂白剂)会裂解接合分子,从而导致其在材料暴露于水或空气之前就会失效。此外,液体中的表面活性剂还用作增塑剂,并且起着润滑作用以有利于解开接合分子的纠缠以及它们与微晶的分离(增塑作用为增加材料流动性的方法)。高分子量材料的存在提供了良好的环境应力抗裂性,因为这些长链会提供与接合分子的更多的相互作用。增加较低分子量材料的量以便获得剪切致稀将会降低环境应力抗裂性。
因此,需要提供一种用于制造聚乙烯容器的预成型件,其中该预成型件由如下聚乙烯材料制成,所述聚乙烯材料同时表现出用于注塑的剪切致稀特性和用于注坯拉伸吹塑方法的拉伸吹塑过程的应变硬化。也需要使预成型件生产出保持良好环境应力抗裂性的最终容器。也需要提供一种用于制造聚乙烯容器的方法,其中预成型件由如下聚乙烯材料制成,所述聚乙烯材料同时表现出剪切致稀和应变硬化特性,并且也提供最终产品的良好的环境应力抗裂性。
已令人惊讶地发现,由具有特定分子量特性的聚乙烯材料制成的预成型件解决了上述技术问题。这些材料表现出用于注塑的剪切致稀特性,这些预成型件在拉伸吹塑步骤期间具有良好的应变硬化特性,并且最终容器具有良好的环境应力抗裂性。
发明概述
本发明的第一方面为一种由聚乙烯材料制成的固体预成型件,其中预成型件包括颈部区域、侧壁和基座区域,并且包括具有内壁的内部和具有外壁的外部;其特征在于按聚乙烯材料的总重量计,至少65%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值,其中Mn为数均分子量,并且Mz/Mn为Mz值除以Mn值。
本发明的第二方面为一种用于注塑固体预成型件的方法,其中固体预成型件由聚乙烯材料制成,并且其中预成型件包括颈部区域、侧壁和基座区域,并且包括具有内壁的内部和具有外壁的外部;其特征在于按聚乙烯材料的总重量计,至少65%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值,其中Mn为数均分子量,并且Mz/Mn为Mz值除以Mn值,并且注塑过程中的峰值压力小于500巴。
本发明的第三方面为一种用于吹塑聚乙烯容器的方法,所述方法包括以下步骤:
a)提供由聚乙烯材料制成的固体预成型件,其中预成型件包括颈部区域、侧壁和基座区域,并且包括具有内壁的内部和具有外壁的外部;
b)任选地再加热预成型件,以便再加热过的预成型件的侧壁和基座区域的最热与最冷区域之间的最大温差小于4℃;
c)将预成型件传送至吹模腔体中;
d)以低于15巴的压力拉伸预成型件;以及
e)增加再加热过的预成型件内的压力,以便使得拉伸过的预成型件的壁膨胀至吹模腔体内部的形状和尺寸;
其特征在于按聚乙烯材料的总重量计,至少65%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值,其中Mn为数均分子量,并且Mz/Mn为Mz值除以Mn值。
附图简述
图1A和图B示出了用于本发明的预成型件的尺寸。
发明详述
用于本发明的方法的预成型件包括颈部区域、侧壁和基座区域,从而形成在其外部尺寸上从靠近封闭端的点至靠近开口端的点基本上对称的管。预成型件包括具有内壁的内部和具有外壁的外部。优选地,处于颈部区域和基座区域之间的预成型件的侧壁具有基本上直的且平行的外壁表面。已发现,具有平行且直的外壁的预成型件设计允许均匀地再加热和均匀地拉伸聚乙烯,从而有助于吹塑最终容器。平行且直的壁预成型件设计的另一种有益效果是,其在拉伸吹塑过程中最大化了能够装填在给定颈部设计中的材料量,并且最小化了拉伸比率(对材料的延伸量)。这意味着任何一个给定区域中的材料均不会被拉伸得太多或太少,因此允许材料更好地分布在最终容器中。
本发明的聚乙烯材料包括一个或多个聚合物种类。本发明的每个聚合物种类均可为由乙烯单体单元组成的均聚物,或可为包括与其它单体单元共聚合的乙烯单元的共聚物,优选地C3-C20α-烯烃,但可包括其他物质,诸如乙酸乙烯酯、马来酸酐等。因此,该聚乙烯材料包括不同的聚合物种类,每个聚合物种类均包括乙烯的单体单元、C3-C20α-烯烃、和其它共聚单体。聚合物种类的每种组合均表现出该特定聚乙烯材料所特有的不同的物理特性。本发明的聚乙烯材料也优选地为中密度或高密度聚乙烯。高密度聚乙烯被定义为具有0.941g/cm3至0.960g/cm3的密度。中密度聚乙烯被定义为具有0.926g/cm3至0.940g/cm3的密度。在一个实施方案中,本发明的聚乙烯材料具有0.926g/cm3至0.960g/cm3的密度。在另一个实施方案中,本发明的聚乙烯材料具有0.926g/cm3至0.940g/cm3的密度。在另一个实施方案中,本发明的聚乙烯材料具有0.941g/cm3至0.960g/cm3的密度。
在一个实施方案中,该聚乙烯材料为“生物源聚乙烯”,即,其来源于可再生资源而非油品。在一个实施方案中,甘蔗被发酵以产生醇。使醇脱水以制备乙烯气体。然后使该乙烯气体穿过聚合反应器(反应器的类型与用于来源于油品的乙烯气体的相同)。生物源聚乙烯能够由其它植物和植物材料例如糖用甜菜、糖浆或纤维素制成。生物源聚乙烯具有与油基聚乙烯相同的物理特性,前提条件是其已在与油源聚乙烯相同的反应器条件下聚合。
已令人惊讶地发现,由至少65%的具有介于300,000g/mol和6,000,000g/mol之间的特定分子量特性Mz和大于28的Mz/Mn的聚乙烯材料制成的预成型件表现出了注塑所需的剪切致稀特性,在拉伸吹塑步骤期间具有良好的应变硬化特性,并且最终容器具有良好的环境应力抗裂性。
在每种聚乙烯材料内,所述各种单个聚合物种类具有某个范围内的聚合度和分子质量。换句话讲,存在长链和短链聚合物种类的混合物,每种聚合物种类均具有不同的分子量。该分布通过一系列“平均”分子量公式来量化。用于聚乙烯材料的两种常见的分子量平均量为:
-数均分子量Mn,其为所述单个聚合物种类的分子量的平均值;
-Z-平均分子量Mz,其为每个聚合物种类的重量乘以每个聚合物种类的分子量。
对于某一聚合物种类,该聚乙烯材料中的聚合物种类的Mz能够被计算出来。Mz值使用公式1来定义;
MWi为特定聚合物种类的分子量,i.ni为具有MWi的该特定种类的数目,并且#为该聚乙烯材料中的种类的总数目。以上计算不包括MWi小于1500g/mol或大于7,000,000g/mol的种类。小于1500g/mol的低分子量种类将表示污染物,因而不利于该方法的拉伸部分。大于7,000,000g/mol的高分子量种类将代表不利于该方法的拉伸或注射部分的“凝胶”颗粒或其它不可熔/不流动的材料。
对于某种聚合物,该聚合物种类的数均分子量能够被计算为数均分子量(Mn)。数均分子量由公式2定义;
MWi为特定聚合物种类的分子量,i.ni为具有MWi的该特定种类的数目,并且#为该聚乙烯材料中的种类的总数目。实质上,Mn是通过如下方式测定的:测量n种聚合物分子的分子量、合计(Σ)这些分子量并除以n。出于上述原因,以上计算不包括MWi小于1500g/mol或大于7,000,000g/mol的种类。
为便于理解,可认为Mz值反映了该聚乙烯材料中的高分子量聚合物种类的量。因此可认为该值对应于该聚乙烯材料的应变硬化特性。
为便于理解,可认为Mz/Mn值反映了该聚乙烯材料中的高分子量聚合物种类和低分子量聚合物种类的比率。因此,可认为该值对应于该聚乙烯材料的剪切致稀特性。
按聚乙烯材料的总重量计,至少65%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Mz和大于28的Mz/Mn。在另一个实施方案中,按聚乙烯材料的总重量计,至少80%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Mz和大于28的Mz/Mn。在另一个实施方案中,按聚乙烯材料的总重量计,至少90%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Mz和大于28的Mz/Mn。
包括至少65%的Mz具有小于300,000g/mol的Mz的材料的预成型件由于缺乏应变硬化而在拉伸吹塑时产生了具有洞的容器。分子量大于6,000,000g/mol的材料为超高分子量聚乙烯。由于它们的分子量极高,它们会产生脆性容器。因此,包括至少65%的具有大于6,000,000g/mol的Mz的材料的预成型件是不合适的。
已令人惊讶地发现,为了使该材料生产出由预成型件制成的容器而所述预成型件不具有洞(应变硬化),但也具有注塑所需的剪切致稀特性,该聚乙烯材料也需要大于28的Mz/Mn。具有介于300,000g/mol和6,000,000g/mol之间的Mz但具有小于28的Mz/Mn在注射步骤中要求极高的压力。这意味着它们的剪切致稀特性较差,因此要求高压力来分配该材料以填充模具,或它们不能够填充模具。
由包括具有这些特性的材料的预成型件制成的最终容器也表现出了良好的环境应力抗裂性。
使用尺寸排阻色谱法(SEC)(也称为凝胶渗透色谱法(GPC))来分离并测量这些聚乙烯材料的Mz、Mw和Mn值。所使用的SEC仪器为聚合物实验室PL-GPC 220高温液体色谱法系统,该系统配备有三个聚合物实验室300×7.5mm PL-Gel混合的B交联聚苯乙烯柱、示差折光率检测器、以及在线Wyatt DAWN EOS 18角多角度激光散射检测器。色谱法洗脱液由用0.125g/L丁基化羟基甲苯(BHT)稳定的液体色谱法等级的1,2,4-三氯苯(TCB)组成。使用聚合物实验室PL-DG 802在线脱气器将洗脱液脱气,并且通过该液体色谱法系统以1.0mL/min进行计量。通过将大约10-20mg的该聚乙烯材料在150℃下溶解于5-20mL的TCB并持续大约24小时制备了聚乙烯材料样品溶液。在溶解之后,通过平均孔径为10μm的预热的铝玻璃料来过滤样品。将样品溶液保持在150℃下,然后加载到PG-GPC 220系统的自动取样机中以进行分析。由于该SEC系统配备有多角度激光散射检测器,因此不要求用已知的标准物来校准。然而,通过运行具有已知分子量的单分散和多分散聚乙烯标准物证实了该系统的精度和再现性。然后该设备的软件会转换出每种聚乙烯材料中的所述不同聚合物种类的分子量峰值,并且基于公式1和2计算出Mz和Mz/Mn值。
在本发明的一个实施方案中,本发明的聚乙烯材料包括具有添加剂的聚乙烯材料。添加剂优选地选自包括以下物质的组:颜料、UV滤光剂、遮光剂、抗氧化剂、表面改性剂、加工助剂或它们的混合物。优选地,添加剂为颜料。表面改性剂优选地选自包括以下物质的组:增滑剂、抗粘连剂、增粘剂以及它们的混合物。抗氧化剂优选地选自包括以下物质的组:主或副抗氧化剂或它们的混合物。在一个实施方案中,添加剂为颜料,优选地选自包括以下物质的组:TiO2或抚慰剂或它们的混合物。加工助剂优选地选自包括以下物资的组:蜡、油、含氟弹性体或它们的混合物。在另一个实施方案中,添加剂选自包括以下物质的组:阻燃剂、防静电剂、清除剂、吸收剂、气味增强剂、以及降解剂或它们的混合物。
在本发明的一个实施方案中,聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值,该聚乙烯材料包括消费后回收利用的高密度聚乙烯。消费后回收利用的是指从丢弃的消费品中回收利用的聚乙烯材料。优选使用这些材料,因为这样对环境会更加友好。然而,它们常常不表现出所期望的特性,所述特性是它们所必备的以具有如上所详述的应变硬化和剪切致稀特性。已令人惊讶地发现,加入聚乙烯蜡使所述消费后回收利用的高密度聚乙烯具有本发明所期望的分子量特性(Mz&Mz/Mn)值。
聚乙烯蜡为极低分子量聚乙烯。它们通常具有小于60,000的Mz和小于12的Mz/Mn。所述消费后回收利用的材料通常具有>500,000的Mz和小于20的Mz/Mn。
优选地,介于1%和40%之间,更优选介于15%和25%之间的聚乙烯材料包括聚乙烯蜡,所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值。优选地,介于40%和60%之间,更优选介于20%和80%之间,最优选介于10%和90%之间的聚乙烯材料包括消费后回收利用的高密度聚乙烯材料,所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值。
注坯拉伸吹塑包括以下步骤:
-注塑预成型件;
-将其拉伸并且随后
-增加拉伸过的预成型件中的内部压力以产生最终容器形状。
在第一工序中提供聚乙烯预成型件。高气穴注塑为目前广泛使用的用以产生预成型件的方法,然而也可使用任何合适的方法。用于聚乙烯的注射压力(在峰值压力时)为大约500至800巴。当该材料处于熔融相时,在更高的温度下进行注射。在一个实施方案中,可将液体着色剂加入熔融聚乙烯材料中。优选地,用于这些聚乙烯材料的峰值注射压力小于500巴的压力。
在另一个工序中,预成型件被任选地再加热,优选地在红外线烘箱中再加热。再加热是任选的,如在至少一个实施方案中那样,预成型件在预成型件的制造过程之后将不足以冷却,因为其要求再加热。通常,将预成型件自身再加热至约120℃至约140℃的温度。再加热过的预成型件的侧壁和基座区域的最热与最冷区域之间的最大温差优选小于4℃,更优选小于2℃。在另一个实施方案中,预成型件的侧壁和基座区域之间的温差在退出烘箱之前为+/-1℃。
将再加热过的预成型件传送到吹模中,并且首先拉伸,然后吹塑。该预成型件优选借助拉伸杆拉伸。预成型件优选以大于1m/s的速度拉伸。然后将拉伸过的预成型件内的压力增加至高于环境压力但低于15巴,优选低于10巴,更优选低于5巴,最优选低于2巴,以便使得拉伸过的预成型件的壁膨胀至吹模内部的形状和尺寸。
在拉伸吹塑工艺结束时,将成品容器由吹模腔体中倒出。
根据本发明制备的容器优选地具有200微米的最小容器壁厚,并且空容器的重量与体积比小于50克/升,优选小于40克/升,并且更优选小于30克/升。
顶部负载阻抗为容器耐受压缩性‘顶部’外加负载的能力,如例如在仓库储存期间所遇到的情况。可测量两种不同类型的顶部负载阻抗。第一种类型测量的是使瓶子发生某种位移例如凸出侧面所需的顶部负载。第二种类型测量的是使容器损坏例如‘颈部’区域塌陷或容器拐角被压裂所需的负载。这通常导致容器的材料发生损坏,诸如塑料裂化或分裂。测试方法和数据提供于实施例部分中。在注坯拉伸吹塑方法之后,由于分子重新取向的继续进行,容器需要经过一段时间才能够阻抗其最大顶部负载。根据本发明生产的聚乙烯容器具有如下属性:它们对顶部负载/压裂的抗性的充分形成速度快于其它材料诸如聚丙烯。因此,按本发明制造的聚乙烯容器在吹塑之后不要求小心地处理,因而能够以超过600个容器/小时/模具的高速来生产。
与通过传统的挤坯吹塑方法制备的聚乙烯容器相比,通过本发明所述的方法制备的所得聚乙烯容器表现出了增强的机械特性。这意味着使用本发明的方法制造的容器更耐受顶部外加力,例如当容器被堆叠在仓库中时所遇到的情况。
实施例
制备了表1的聚乙烯材料。材料1-2为根据本发明的材料(100%聚乙烯材料,无添加剂),而材料A-D为比较材料(100%聚乙烯材料,无添加剂)。
表1
材料 | Mz | Mz/Mn |
材料1 | 500,000 | 31.1 |
材料2 | 740,000 | 31.2 |
材料A | 740,000 | 18.8 |
材料B | 190,000 | 7.9 |
材料C | 270,000 | 10.9 |
材料D | 220,000 | 11.4 |
适用于本发明的预成型件的一般形状先前已在本专利申请中描述过。参见图1A和1B,用来收集数据以支持本发明的具体预成型件1的尺寸如下:长度2为120.87mm;长度3为118mm;直径4为35mm,长度5为19.48mm,宽度6为2.7mm,并且宽度7为2.6mm。
评估了以下方面:
1.表1的聚乙烯材料的剪切致稀特性。这是通过使用表1的聚乙烯材料注塑出预成型件来评估的。峰值注射压力(该注塑方法中所要求的最大压力)被用作对剪切致稀特性的指示。所需的峰值压力越高,则剪切致稀特性就越差,因为需要更高的压力来确保该材料在模具内的分布。
2.由表1的聚乙烯材料制成的预成型件的应变硬化。这是通过拉伸吹塑出由表1聚乙烯材料制成的预成型件来评估的。该性能是通过检查最终容器是否存在洞并且也检查壁厚的可变性来评估的。洞的存在和较差的材料分布指示较差的应变硬化,因为该材料不具有阻抗拉伸的能力。
3.由包括表1中的材料的预成型件制成的最终容器的环境应力抗裂性。这是通过测量填充有洗涤剂并且具有施加在顶部上的负载的容器在它们开始裂漏之前所需的时长来评估的。
4.由包括表1中的材料的预成型件制成的最终容器的机械特性。这是使用标准方法ASTM International,D2659-95通过使用12.7mm/min的恒定压缩速度来评估的。该方法评估的是使瓶子发生结构损坏所需的顶部外加力的量。比较了使用本发明的方法制造的容器与使用另一种容器制造方法即挤坯吹塑制造的容器。
注塑
注塑由表1所详述的材料制成的预成型件的能力是通过如下方式来评价的:使用Arburg 370C单腔注坯机模塑出具有图1A和1B所详述的给定几何形状的预成型件。操作该Arburg 370C单腔注坯机所需的例行步骤是本领域的技术人员已知的。用于所有材料的方法参数示出于表2中。本领域的技术人员了解如何将以下参数输入到该Arburg 370C单腔注坯机中。
表2
其中“速率”为对应于所述四种不同的受控速率级的螺杆的线性注射速度;“结束步长”为螺杆在适当级的给定注射速度下的位移;“保持压力”为在所述各种受控压力级期间施加的液压压力的量;“保持时间”为在所述各种受控压力级上施加“保持压力”的时间量;“剂量”为所注射的材料体积或注入量;“反压力”为当螺杆在注射之后被再填装时施加到螺杆上的压力量,“减压流速”为如下线速度,材料的注射一旦发生之后螺杆即以所述线速度回缩;“减压体积”为材料的注射一旦发生之后在螺杆中减压的体积量;“循环时间”为注入材料、冷却材料、顶出材料、再填装螺杆并且封闭模具所需的总循环时间;“温度”为用于所述各种挤出机区段、热流道、和热尖端的设定值温度;并且“峰值注射压力”为在前述循环期间所经历的峰值液压压力。
特定聚乙烯材料注塑的良好程度是通过比较所有这些聚乙烯材料的峰值注射压力来测定的。峰值注射压力为快速填充模具过程中的一种限制因素。具有更高峰值注射压力的材料对于给定注射速度和温度来讲将会更加难以在类似的多腔设备上进行加工(即,具有较差的剪切致稀特性)。材料D为一种标准注塑材料,其已在众多应用中以商业规模被成功地用于多腔注射设备。因此,用于该材料的峰值注射压力即340巴在具有类似预成型件几何形状的多腔设备中被用作商业模具条件中的一个标准条件。峰值注射压力在340巴(476巴)的40%以内的材料被标定为具有“良好”剪切致稀特性。这意味着它们适用于注塑。结果总结于表3中。
表3
拉伸吹塑
拉伸预成型件的能力是通过使用Sidel SBO机器拉伸由表1所述的聚乙烯材料制成的图1A和1B的预成型件来评估的。对于每种聚乙烯材料进行了拉伸参数的例行优化以便产生最佳瓶子。该优化是对任何聚乙烯材料进行的例行步骤。本领域的技术人员将能够进行该例行优化而不需要任何创造性活动。用以优化的参数包括再加热温度特征图和吹塑压力。一旦对于每种材料获得了最佳条件,就从预成型件生产出了至少200个瓶子。如果材料满足两个要求,就将它们归类为“良好”的。首先,该材料必须能够生产出在壁、颈部或基座中不具有任何洞的瓶子。其次,该材料必须能够生产出在瓶子的所有区域中具有最小厚度的瓶子。否则的话,该材料就被标定为具有“较差”应变硬化。
最终容器的壁、颈部或基座中的洞的存在是以视觉方式评估的。
厚度可变性使用Magna Mike来测量。该标准测试方法将3.2mm直径的磁球用于容器。因而该Magna Mike设备也包含磁体,所述磁体吸引容器内侧上的磁球。因而使用者能够围绕容器移动该Magna Mike装置,所述装置测量壁的厚度,所述厚度取决于所述球和传感器之间的磁引力差值。当容器具有24g的总体重量时,对于容器的任何部分可优选地获得0.2mm的最小厚度。这确保结构完整性。未获得0.2mm的最小厚度的任何容器均被标定为具有较差的材料分布。结果可见于表4。
表4
环境应力抗裂性
环境应力抗裂性是在密封的注射拉伸吹塑的瓶子上测试的,所述瓶子填充有49℃(120℉)的液体洗涤剂,并且具有4.5kgf(10lbf)的外加顶部负载。在四星期的时段内监测了这些瓶子的裂漏情况。如果瓶子在四星期的时段之后未发生裂漏,则称该材料具有“良好”环境应力抗裂性(否则就是“较差”的)。结果可见于表5。
表5
材料 | 环境应力抗裂性 |
材料1 | 良好 |
材料2 | 良好 |
材料A | 良好 |
材料B | 良好 |
材料C | 良好 |
材料D | 较差 |
机械特性
相比于使用挤坯吹塑由标准挤坯吹塑材料制成的容器,使用注坯拉伸吹塑由根据本发明的预成型件制成的容器表现出了改善的顶部负载阻抗。顶部负载阻抗测试是根据ASTM International,D2659-95使用12.7mm/min的恒定压缩速度来进行的。测试了导致容器的任何部分中发生4mm位移所需的顶部负载(或压裂屈服负载)和最大顶部负载(损坏时的压裂负载)。结果可见于表6。如由表6可见,与通过挤坯吹塑制造的参考容器相比,根据本发明制造的容器具有增加的顶部负载阻抗。
表6
对聚乙烯进行注坯拉伸吹塑具有通过分子取向获得更好的机械特性的优点。聚乙烯通常用于挤坯吹塑方法以产生大的三维容器。这些挤坯吹塑的聚乙烯容器缺乏显著的分子取向,这是由于它们实际上是在远远高于该材料的熔融温度下被拉伸的。由于注坯拉伸吹塑发生在较低温度下,因此分子取向能够被锁定并且一直保持到固态中。在最佳情况下,注坯拉伸吹塑方法能够使用按25%减少的材料生产出类似于挤坯吹塑的瓶。因此,注坯拉伸吹塑提供了一种更经济且更高效的制造三维容器的方法。
发明概述
表7总结了如上所述的数据。如可见到的那样,仅本发明的材料具有良好的剪切致稀特性,生产出了具有良好应变硬化特性的预成型件,并且生产出了具有良好环境应力抗裂性的最终容器。对于注塑、拉伸吹塑中的至少一种或环境应力抗裂性,所有其它预成型件均为“较差”的。
表7
本文所公开的量纲和数值不应被理解为严格限于所述确切数值。相反,除非另外指明,每个上述量纲旨在表示所述值以及该值附近的功能等效范围。例如,公开为“40mm”的量纲旨在表示“约40mm”。
除非明确地不包括在内或换句话讲限制,本文所引用的每篇文献,包括任何交叉引用或相关的专利或专利申请,均特此以引用方式全文并入本文。任何文献的引用不是对其作为本文所公开的或受权利要求书保护的任何发明的现有技术,或者其单独地或者与任何其它参考文献的任何组合,或者参考、提出、建议或公开任何此类发明的认可。此外,当本发明中术语的任何含义或定义与以引用方式并入的文件中术语的任何含义或定义矛盾时,应当服从在本发明中赋予该术语的含义或定义。
尽管已用具体实施方案来说明和描述了本发明,但是对本领域的那些技术人员显而易见的是,在不脱离本发明的实质和范围的情况下可作出许多其它的改变和变型。因此,随附权利要求书旨在涵盖本发明范围内的所有这些改变和变型。
Claims (9)
1.一种由聚乙烯材料制成的固体预成型件,其中所述预成型件包括颈部区域、侧壁和基座区域,并且包括具有内壁的内部和具有外壁的外部;其特征在于按所述聚乙烯材料的总重量计,至少65%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值,其中Mn为数均分子量,并且Mz/Mn为Mz值除以Mn值。
2.如权利要求1所述的固体预成型件,其中所述聚乙烯材料具有0.926至0.960g/cm3的密度。
3.如任一项前述权利要求所述的固体预成型件,其中所述聚乙烯材料包括含有添加剂的聚乙烯材料,所述添加剂选自包括以下物质的组:着色剂、UV滤光剂、遮光剂、抗氧化剂、加工助剂或它们的混合物。
4.一种用于注塑固体预成型件的方法,其中所述固体预成型件由聚乙烯材料制成,并且其中所述预成型件包括颈部区域、侧壁和基座区域,并且包括具有内壁的内部和具有外壁的外部;其特征在于按所述聚乙烯材料的总重量计,至少65%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值,其中Mn为数均分子量,并且Mz/Mn为Mz值除以Mn值,并且在所述注塑过程中的峰值压力小于500巴。
5.一种用于吹塑聚乙烯容器的方法,包括以下步骤:
a)提供由聚乙烯材料制成的固体预成型件,其中所述预成型件包括颈部区域、侧壁和基座区域,并且包括具有内壁的内部和具有外壁的外部;
b)任选地再加热所述预成型件,以便所述再加热过的预成型件的侧壁和基座区域的最热与最冷区域之间的最大温差小于4℃;
c)将所述预成型件传送至吹模腔体中;
d)以低于15巴的压力拉伸所述预成型件;以及
e)增加所述再加热过的预成型件内的压力,以致使所述拉伸过的预成型件的壁膨胀至所述吹模腔体内部的形状和尺寸;
其特征在于按所述聚乙烯材料的总重量计,至少65%的所述聚乙烯材料具有介于300,000g/mol和6,000,000g/mol之间的Z-平均分子量(Mz)和大于28的Mz/Mn值,其中Mn为数均分子量,并且Mz/Mn为Mz值除以Mn值。
6.如权利要求5所述的方法,其中所述预成型件借助拉伸杆以大于1m/s的速度拉伸。
7.如任一项前述权利要求所述的方法,其中所述预成型件通过选自注塑、挤坯吹塑和压塑的方法在步骤a)中形成。
8.如任一项前述权利要求所述的方法,其中所述预成型件在步骤b)中被再加热,并且其中所述再加热过的预成型件的侧壁和基座区域的最热与最冷区域之间的最大温差小于2℃。
9.一种根据任一项前述权利要求所述的方法制成的聚乙烯容器。
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PCT/US2011/025980 WO2011106471A2 (en) | 2010-02-24 | 2011-02-24 | Injection stretch blow molding process |
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CN102933369A true CN102933369A (zh) | 2013-02-13 |
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Family Applications (1)
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CN2011800106509A Pending CN102933369A (zh) | 2010-02-24 | 2011-02-24 | 注坯拉伸吹塑方法,预成型件和容器 |
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US (1) | US20110206882A1 (zh) |
EP (1) | EP2539132A2 (zh) |
JP (2) | JP2013520334A (zh) |
CN (1) | CN102933369A (zh) |
BR (1) | BR112012021344A8 (zh) |
CA (1) | CA2789469A1 (zh) |
MX (1) | MX2012009868A (zh) |
RU (1) | RU2012133344A (zh) |
WO (1) | WO2011106471A2 (zh) |
Cited By (3)
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CN107148385A (zh) * | 2014-08-01 | 2017-09-08 | 可口可乐公司 | 具有增强的贮藏寿命特性的小碳酸饮料包装 |
CN113165213A (zh) * | 2018-12-19 | 2021-07-23 | 宝洁公司 | 具有视觉效应的制品 |
US11634248B2 (en) | 2018-12-19 | 2023-04-25 | The Procter & Gamble Company | Mono-layer blow molded article with functional, visual, and/or tactile effects and method of making such articles |
Families Citing this family (6)
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EP2147721A1 (de) | 2008-07-08 | 2010-01-27 | Lanxess Deutschland GmbH | Katalysator-Systeme und deren Verwendung für Metathese-Reaktionen |
GB2486647B (en) * | 2010-12-20 | 2013-06-19 | Peter Reginald Clarke | Preforms for blow moulding |
US20150335778A1 (en) * | 2014-05-21 | 2015-11-26 | The Procter & Gamble Company | Freshening product comprising an aqueous perfume composition contained in a pressurized plastic container |
DE102014119563A1 (de) | 2014-12-23 | 2016-06-23 | Krones Ag | Verfahren zum Umformen von Kunststoffvorformlingen |
CN113825617A (zh) * | 2019-04-09 | 2021-12-21 | 日精Asb机械株式会社 | 树脂容器制造方法 |
NO347909B1 (en) * | 2022-09-30 | 2024-05-13 | Delta Eng Bvba | Top load testing method and device for blow moulded containers |
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-
2011
- 2011-02-23 US US13/033,091 patent/US20110206882A1/en not_active Abandoned
- 2011-02-24 JP JP2012554108A patent/JP2013520334A/ja active Pending
- 2011-02-24 RU RU2012133344/05A patent/RU2012133344A/ru not_active Application Discontinuation
- 2011-02-24 BR BR112012021344A patent/BR112012021344A8/pt not_active IP Right Cessation
- 2011-02-24 WO PCT/US2011/025980 patent/WO2011106471A2/en active Application Filing
- 2011-02-24 CN CN2011800106509A patent/CN102933369A/zh active Pending
- 2011-02-24 EP EP11710586A patent/EP2539132A2/en not_active Withdrawn
- 2011-02-24 CA CA2789469A patent/CA2789469A1/en not_active Abandoned
- 2011-02-24 MX MX2012009868A patent/MX2012009868A/es unknown
-
2015
- 2015-01-05 JP JP2015000533A patent/JP2015120351A/ja active Pending
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EP1287969A1 (en) * | 2001-08-24 | 2003-03-05 | Atofina Research S.A. | Injection blow moulded metallocene polyethylene container |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107148385A (zh) * | 2014-08-01 | 2017-09-08 | 可口可乐公司 | 具有增强的贮藏寿命特性的小碳酸饮料包装 |
CN113165213A (zh) * | 2018-12-19 | 2021-07-23 | 宝洁公司 | 具有视觉效应的制品 |
US11485535B2 (en) | 2018-12-19 | 2022-11-01 | The Procter & Gamble Company | Article with visual effect |
US11618606B2 (en) | 2018-12-19 | 2023-04-04 | The Procter & Gamble Company | Method of making article with visual effect |
US11634248B2 (en) | 2018-12-19 | 2023-04-25 | The Procter & Gamble Company | Mono-layer blow molded article with functional, visual, and/or tactile effects and method of making such articles |
Also Published As
Publication number | Publication date |
---|---|
MX2012009868A (es) | 2012-09-12 |
WO2011106471A2 (en) | 2011-09-01 |
RU2012133344A (ru) | 2014-03-27 |
CA2789469A1 (en) | 2011-09-01 |
JP2013520334A (ja) | 2013-06-06 |
WO2011106471A3 (en) | 2012-11-22 |
JP2015120351A (ja) | 2015-07-02 |
BR112012021344A2 (pt) | 2016-10-25 |
US20110206882A1 (en) | 2011-08-25 |
EP2539132A2 (en) | 2013-01-02 |
BR112012021344A8 (pt) | 2017-09-19 |
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