CN1092352A - 具有低结晶内层的多层预成型坯和瓶子的成型方法 - Google Patents
具有低结晶内层的多层预成型坯和瓶子的成型方法 Download PDFInfo
- Publication number
- CN1092352A CN1092352A CN93109891A CN93109891A CN1092352A CN 1092352 A CN1092352 A CN 1092352A CN 93109891 A CN93109891 A CN 93109891A CN 93109891 A CN93109891 A CN 93109891A CN 1092352 A CN1092352 A CN 1092352A
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- Prior art keywords
- bottle
- polyester
- copolymer
- shaped portion
- preform
- Prior art date
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- Pending
Links
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Images
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Abstract
一种多层聚酯预成型坯和瓶子的成型方法,尤其
适合于可再灌装的PET碳酸饮料瓶,具有高共聚物
聚酯的内层,在预成型坯的注塑阶段上述内层材料能
阻止混浊,还具有至少一聚酯外层,在吹塑时外层可
获得提高的应变诱生的结晶度。该瓶子能承受较高
的碱洗温度,和具有减少从一产品至另一产品的夹带
气味。
Description
本申请是共同待批和共同拥有的下述美国专利的接续,即由W.Collette,S.Schmidt和S.KrishnaKumar于1992年7月7日申请的申请号为No 07/909,961名称为“多层可再灌装的瓶子、预成型坯及其成形方法”的美国专利。
本发明涉及对瓶子方面新的和有效的改进,特别涉及具有提高的表面侧壁结晶度的瓶子成形方法,同时保持高的透明度(清澈性)。该瓶子特别有效地作为可再灌装的碳酸饮料瓶,能耐高温咸洗,减少夹带产品气味并可作为热灌装瓶子。
自从1987年,由欧洲大陆引入PET技术后,对于PET可再灌装的碳酸软饮料(CSD)瓶的市场,在世界范围获得可喜的明显增长。这些瓶子已商品化,遍及欧洲,中美洲和南美洲,而现已进入远东市场。
再灌装瓶子减少与可处理的塑料饮料瓶关联的现存在的垃圾填埋和重复利用的问题。此外,在那些由玻璃支配的市场提供安全,较轻重量,可再灌装的塑料瓶子,上述的市场立法禁止使用不能重复利用的包装。目的在于生产具有必要的物理性能的可再灌装的瓶子,以耐多次再灌装循环,并且其生产仍然是经济的。
通常,可再灌装塑料瓶在最少10次,优选20次循环或是考虑经济可行的封闭系统次数下,必须保留其功能和美学性能。一个封闭系统包括:(1)空瓶的热咸洗;(2)污染检查和产品灌装/封口;(3)仓库储存;(4)分配到批发和零售点,和(5)由消费者购买,使用并储存空瓶,最终返回到制瓶厂。该循环见图1所示。在另一种循环中,污染检查发生在碱洗以前。
可再灌装瓶必须满足几个主要性能标准,以获得商业的可行性,包括:
1.高清澈性(透明度)以允许直观现场检查;
2.在瓶子使用寿命期间保持尺寸稳定性;
3.抗碱洗所引起的断裂应力和泄漏。
商品化成功的PET可再灌装CSD瓶,现由CoCa-Cola公司将其销售到欧洲(下文为“已有技术瓶子”)。该瓶子是由具有3-5%共聚单体的聚对苯二甲酸乙酯(PET)的单层所构成,所说共聚单体例如,1.4-环已烷-二甲醇(CHDM)或间苯二酸(IPA)。预成型坯(从其可吹塑拉伸成瓶)具有侧壁厚度大约为5-7mm,或是大约为用于可处理一次性瓶子的预成型坯厚度的2-2.5倍。基于二维拉伸比大约10∶1,这样提供较大的瓶子平均侧壁厚度(即0.5-0.7mm),可满足抗乱用和尺寸稳定性的要求。壁板(在商标下的圆筒形侧壁部分)的平均结晶度大约为15-20%。在注塑过程中,高共聚物含量防止在形成预成型坯时出现可见的结晶,即混浊。预成型坯的混浊是不希望的,因为它造成瓶子混浊,妨碍对商品化再灌装瓶所要求的直观的现场检查。现有技术的瓶子的各种情况描述在欧洲大陆PET技术(Continentul PET Techno-logy′s)的美国专利No.4,725,464,4,755,404,5,066,528,5,198,248中。
现有技术的瓶子的试验证明,在碱洗温度达到60℃,可经受超过20次再灌装试验。试验虽然是成功的,但商品化要求改进瓶子,即要允许清洗温度大于60℃,同时要降低夹带产品气味。而后者发生在,当气味成分从第一产品(例如,root啤酒)流入瓶子的侧壁,而接着在以后灌装循环中,进入第二产品(例如,club汽水),这样影响第二产品的味道。提高清洗温度也是所希望的,以便提高碱洗效率和/或减少碱洗时间,而且提高清洗温度对于某些产品,例如,果汁,牛奶是可以要求的。
因此,对于具有使用寿命至少10次再灌装,而优选20次再灌装的瓶子,要求提高碱洗温度高于60℃,并且要降低夹带产品气味。正如下面描述的本发明可达到这些和其它目的。
按照本发明的基本上透明的多层瓶子的成形方法,提供提高的诱生应变的外侧壁结晶度,并且通过低温热定形上述结晶度可得到进一步提高。该瓶子具有改进的抗碱洗断裂应力,同时保持高透明度和尺寸稳定性。因此,特别适合于可再灌装的碳酸饮料瓶。在碱洗温度达60℃和以上的温度下,该瓶具有至少10次再灌装循环的使用寿命。优选的至少20次再灌装循环的使用寿命。该瓶与上述可再灌装CSD现有技术瓶相比至少减少20%的夹带气味。
在一实施例中,提供的预成型坯包括一壁板成形部分,它具有第一共聚物聚酯的内层,和具有较低共聚物的第二聚酯的外层,并且其结晶速度至少比第一聚酯材料高大约20%。低共聚物的两外层(内和外)之间,最好在内层形成高共聚物的芯层。高共聚物防止芯层结晶(混浊),该芯层冷却较慢保持整个瓶子的清澈和可检查性。在注塑过程中,外层(内和外)冷却较快,并且结晶可能性小。它由均聚物或低共聚物聚酯制成,所说的材料具有较高速度的拉伸或产生应变的结晶度,因此,吹塑瓶提供提高的表面由碱洗引起的断裂应力阻力和减少的夹带气味。芯层一般可以包括大约50-80%预成型坯的壁板成形的壁的厚度,和相应的瓶子的壁厚,而更为优选的大约为60-70%。
在一实施例中,上述的预成型坯再加热拉伸吹塑以形成一件PET独立的可再灌装的增压饮料瓶,在其壁面,具有双轴取向,较薄的和高结晶的内层和外层。壁板的总平均厚度大约0.5至大约0.8mm,芯层占大约60-70%的总厚度。瓶底包括较低的定向和结晶度的变厚部分。壁的内层和外层具有产生应变的平均结晶度至少大约20%,而壁的芯层至少大约14%,均在二维拉伸比为大约7-13∶1而更优选为9-11∶1下取得的。所说的“平均”结晶度,意指是取各壁板部分,例如,侧壁的总面积的平均值。
多层PET瓶其壁板具有至少20%诱生应变的平均结晶度,通过低温热定形(例如,接触110-140℃的模子以保持透明度)可进一步提高至30-35%或甚至更高。在壁板的外层具有较高的结晶度,可允许清洗温度,例如,62℃,65℃或70℃。在壁板的芯层具有较低的结晶度,但是对于富有生命力的再灌装瓶来说,足以提供需要的强度(抗蠕变力,抗乱用和热稳定性)。总之,与上述的现有技术单层可再灌装的CSD饮料瓶相比,本发明的瓶子可以在60℃或更高的温度下清洗,并减少夹带气味(有20%或更多的改进),并且瓶子的性能没有明显的降低。
上述的两种材料三层PET预成型坯可通过计量,接着共注塑的方法制造,该方法包括第一次注塑均聚物或低共聚物,例如,0-12%共聚物。
在升高的温度下改进的抗混浊和抗断裂应力,使本发明的瓶子也特别适合作为热灌装瓶。
通过以下结合附图对实施例1的详细说明将对本发明的这些和其它特征做更详细地描述。
图1是一典型的循环或封闭系统示意图,可再灌装的瓶子必须通过该系统;
图2是本发明的PET可再灌装1.5升碳酸饮料瓶的正视简图,部分剖视,表示沿着瓶子的不同部位,高共聚物芯层与低共聚物内层、外层不同标高的结晶度;
图3是沿图2的3-3线剖面放大图,更具体地表示高共聚物PET芯层和低共聚物PET的内层和外层;
图4是通过一注模腔的剖面简图,表示聚酯树脂材料直接注入模腔内以形成按照本发明预定型坯;
图5是一部分放大简图,表示一定量的第一低共聚物材料注入模腔的底部,由于接触较冷的模壁表面而被冷却以形成预定型坯的内层和外层;
图6是一部分放大简图,表示一定量的第二高共聚物材料注入到模腔的底部,以形成芯层,其结果是第一和第二材料在腔道的流动以形成预定型坯;
图7是一用于构成本发明的瓶子的多层预定型坯的放大剖面简图;
图8是一部分放大图,表示由图7所示的预定型坯制造的瓶的底部截面;
图9是一另一种预定型坯的部分剖面图,在预定型的底部成形部分具有第三注入材料,它置于芯层材料中,它可以是类似于内层和外层的低共聚物材料;和
图10是一部分放大图,表示由图9所示的预定型坯制造的瓶的底部截面。
参照附图,特别是图1,商品化可再灌装的瓶子必须能承受多次再灌装循环,而同时能保持其美学和功能特性。用于模拟此种循环的试验步骤如以下所述。正如在说明书和权利要求书中,按照下列试验步骤确定可承受再灌装循环的指定次数而不破裂和/或有大的体积变化的能力。
每个瓶子用一般工业用碱洗液清洗,所说的碱洗液由3.5%重量的氢氧化钠和自来水制备。按照本发明该清洗液保持在指定的清洗温度,即60℃或更高。打开盖的瓶子浸没在清洗液中清洗15分钟,以模拟商品化瓶子清洗系统的时间/温度条件。经清洗液取出的瓶子再用自来水冲选,然后以4.0±0.2大气压下(模拟碳酸软饮料容器的压力)灌装碳酸水溶液,加盖并置于38℃的对流炉子。在50℃相对温度下24小时。选择高的炉温以模拟在较低环境温度下较长周期的商业储存。从炉子取出后,瓶子排空,并进行相同的再灌装循环,直至瓶子损坏。
所谓的损坏的定义是,破裂沿着瓶壁蔓延,以致泄漏和压力降低,确定体积的变化是通过比较在室温下瓶内液体体积的变化,即在每次再灌装循环前和后的变化。
下面描述的图2所示的瓶子,在清洗温度大于60℃下至少可承受20次再灌装循环而不损坏,而在20次循环后仅仅有约1.5%的体积变化。该瓶子也表示至少减小20%的夹带的产品气味,(与已有技术CDS瓶比较),它由气体色谱仪测定。
图2所示的是按照本发明制造的PET可再灌装的1.5升碳酸饮料瓶,具有较厚的香槟酒颜色的底。瓶10是整体吹塑的双轴取向的中空体,具有上部开口,在颈部精表面12具有外螺纹用以与盖的螺纹配合(未示出),并具有下端封闭的底18。在颈部精表面和底部之间是基本上垂直地设置的侧壁,它包括一上部倾斜的肩部14,和一基本上圆筒形的壁16(由瓶子的垂直轴线或中心线CL所限定)。香槟酒颜色底18具有中心向外中凹的拱形底22,并带有中心底座部分20,一向内中凹的瓶底凹边24,它包括一用于支承瓶子的立环,和一径向逐渐增加的弧形外底部26,用以使底平滑地过渡到侧壁16。瓶底凹边基本上是喇叭口形曲面围绕着立环,其厚度增加以抗断裂应力。拱形和瓶底凹边形成一厚度变厚的底部,是大约3-4倍的侧壁16的厚度。在瓶底凹边的上部,是较薄的外底部份,其厚度大约是50-70%的变厚底部的厚度,而结晶度逐渐增加直到增加到与侧壁的结合处。较薄的外底部分具有改善的抗冲击强度。
由于附图的比例小,因此,瓶10的多层侧壁没有在图2中详细地表示。图3表示壁16的侧壁横截面,具有一高共聚物的芯层30和低共聚物的内层32和外层34。芯层30大约0.015-0.024英寸(0.38-0.61mm)厚,而内层32和外层34各大约0.003-0.006英寸(0.077-0.15mm)厚,上述瓶子,基于具有侧壁厚度大约0.24英寸(6.1mm)的预成型坯及平面拉伸比大约10∶1而制成的。瓶子高度大约为13.2英寸(335mm),直径(最宽)大约3.6英寸(92mm)。
用于制造图2所示的瓶子的预成型坯具有壁板成形的壁厚大约0.24英寸(6.1mm),其中壁板16是在平均平面拉伸比大约为10∶1下拉伸而成。平面拉伸比是预成型坯的壁板成形部分平均厚度与瓶子的侧壁的平均厚度之比。对于大约0.5至2.0升/容积,壁厚大约为0.5至0.8mm的聚酯可再灌装碳酸饮料瓶,优选的平面拉伸比为大约7-15∶1,而更优选的是大约9-11∶1。环向的拉伸优选为3-3.6∶1,轴向拉伸为2-3∶1。这样制造的瓶子侧壁具有所希望的抗乱用性能,而预成型坯的侧壁具有要求的直观透明度。壁厚和拉伸比的选择是根据特定瓶子的尺寸,内压(例如,啤酒为2大气压,软饮料为4大气压)和特定材料的加工性能(例如,由内粘度确定)。
沿着瓶子从颈部精表面至底部的不同部位,不同的结晶度百分比见图2所示的。结晶度百分比是根据ASTM 1505按以下确定的:
%结晶度=[(ds-da)/(dc-da)]×100
其中:ds是试样的密度g/cm3,
da是非晶体薄片0%结晶度的密度(对于PET为1.333g/cm3),dc是晶体的密度,由单元晶粒参数计算(对于PET为1.455g/cm3)。
正如图2所示,在颈部精表面12芯层和内、外层的结晶度均很低(0-2%),因为瓶子的该部位基本上未受到延伸。倾斜的肩部14,该部位所受的延伸小于侧壁16,在芯层获得15-17%诱生应变的结晶度,而在内层和外层为22-24%的结晶度。在高拉伸的侧壁16,其芯层为16-18%诱生应变的结晶度,而在内层和外层为22-25%的结晶度。在底座口20和底的凹口部分22具有较厚的截面延伸比较小,另外在该处芯层和内层、外层的诱生应变的结晶度从0-2%。在瓶底凹边处24,其芯层诱生应变的结晶度为4-8%,而内层、外层为16-18%。
另一方面,通过热定形可以进一步提高结晶度等级,(诱生热的结晶度在低温下以保持结晶度,例如,对于PET,模子温度为110-140℃时与模子接触),为了诱生应变与诱生热的结晶度相结合。例如,结合的平均壁结晶度30-35%允许至少62℃的清洗温度清洗,20次循环,同时至少降低20%夹带气味。通常,诱生应变的结晶度沿着特定层的厚度基本上是均匀的,而诱生热的结晶度沿着壁是坡度分布。在本发明中,虽然沿着各自的层,获得的结晶度基本上是恒定的平均值,但只有在侧壁的表面的高结晶度是足够的。
根据上述的结晶度百分比,吹塑瓶基本上是透明的。另一透明度的度量是混浊度百分数,即用以通过壁(HT)来透光,上述HT由下式获得:
HT=[Yd+(Yd+Ys)]×100
其中Yd是通过样品的漫射光,Ys是样品的反射光。按照ASTM法D1003使用任何标准的色差计,例如由Hunterlab公司制造的型号为D25D3P,可以测定漫射光和反射光的值。再灌装瓶的混浊度百分比(通过壁)应该小于约15%,优选的小于约10%,而更为优选的小于约5%。
形成芯层30的高共聚物PET最好含有大约4-6%重量的共聚单体,例如1.4-环已烷-二甲醇(CHDM)和/或间苯二酸(IPA)。形成内层32和外层34的低共聚物PET最好含有约0-2%重量的共聚单体,例如CHDM和/或IPA。这些材料从市场可以得到,即从田纳西州的Kingsport的Eastman化学公司和俄亥俄州的AKron的Goodyear轮胎与橡胶公司获得。共聚单体(例如CHDM作为取代部分乙二醇,或IPA作为取代部份酸)断裂PET聚合物的主链(即酸和乙二醇的替代单元)以降低分子结晶速率,如果形成主链的一部分,共聚单体是最有效的,但也可能形成支链共聚物。
制造瓶子最好是经两步预成型注塑和随后的再加热吹塑。通常,瓶子的拉伸部分(在合适的温度下),沿着侧壁显示最大的结晶度。此外,在多层侧壁(见图3)中,不同的共聚物形成不同的结晶度,具有高共聚物的芯层30的结晶度比低共聚物的内层32,外层34低。这是因为增加的共聚物量在给定的温度下降低分子结晶速率。
一种测定结晶速率的方法是由结晶特性曲线确定△T,用差值扫描量热法(DSC)可以得到结晶特性曲线,即△T=Tie-Tp,其中Tp是结晶峰值温度,Ti是开始结晶温度(开始),而Tie是推定开始温度,由切线与放热峰值的高温侧的基线相义面获得。这是公知的技术,它描述于H.N,Beck和H.D,Ledbetter的J.Appl.Polym.Sci.,9,2131(1965)和Saleh A.Jabarin,的“树脂和加工性能对PET预成型坯的结晶影响”(“Recin and Process Parameters Affecting crystallization of PET Preforns,”),BEV-PAK 92第十六届饮料包装国际Ryder会议,1992年3月23-25,图6-11,该全文结合在本发明中参考。参数△T是整个结晶速率的函数,△T越小,结晶速率越大。对于PET高共聚物,通常认为其△T(它是由300℃以5℃/mm的冷却速度降到Tg(80℃)以下来确定)为21.5℃和以上,而低共聚物为低于21.5℃。最好在本发明的高共聚物和低共聚物层之间有不同的△T,至少大约为20%,例如,高共聚物△T大约为24℃,而低共聚物的△T为大约20℃。
用于吹塑瓶子的预成型坯应该基本上是非晶体的,对于PET达到约10%的结晶度,优选的不大于约5%的结晶度,更为优选的不大于约2%的结晶度。
另一方面,基本上非晶体的或半透明状的预成型坯可以用混浊度百分比来确定。沿着预成型坯壁的混浊度百分比应该是不大于约20%,优选的不大于约10%,而更优选的不大于约5%。
然后拉伸基本上非晶体的预成型坯,使在瓶子的侧壁产生定向和结晶。采用任何传统的技术可以将预成型坯拉伸成瓶子,该技术包括预成型坯的胀大,例如用真空或压力成型。两种公知的方法是,整体的注射吹塑方法和二步预成型坯注塑然后重新加热吹塑法。
胀大步骤应该在所用的聚酯材料分子定向温度范围内进行。一般说,可定向的热塑材料的分子定向发生在一温度范围,即从玻璃转化温度以上(该温度,即窄的温度范围,低于该温度聚合物成玻璃态)直至低于聚合物的熔解温度。正如实际情况,定向的瓶子是在很窄的湿度范围内成形,称为分子定向温度范围。其理由是,如果温度太接近于玻璃化温度,即材料太硬不能在传统的设备中进行拉伸。如果温度提高,可大大改进成型性能,但实际上有一上限温度,在或接近该温度开始形成叫做球粒的大集聚晶料,因为球粒成长对定向过程不利。对于基本上非晶体的聚酯材料,分子定向温度范围一般是从大约20至65°F(11至36℃)优选的从大约30至40°F(17-22℃),高于聚酯材料的玻璃转化温度。一般非晶体PET聚合物具有玻璃转化温度大约168°F(76℃),而通常定向温度范围大约195°F(91℃)至大约205°F(96℃)。
在优选的重新加热拉伸吹塑方法中,热注塑预成型坯在使用前急冷至室温,然后预成型坯在胀大步骤前重新加热到定向温度范围以内。重新加热的预成型坯置于拉伸吹塑组件中,其中一拉伸捧从预成型坯的开口端移入,并对着吹塑模具内腔的底拉伸棒延伸,以拉伸预成型坯,从而轴向地拉伸预成型坯的侧壁,同时或接着将吹塑介质通过开口进入或围绕棒进到预成型坯的内部,以便径向地向外拉伸型坯,与模具的内表面吻合。根据所要求瓶子形状和吹塑瓶子的壁厚拉伸的程度可以是不同的,由预定的开始型坯和最终瓶子的相对尺寸来控制。
在另一种整体的方法中,在用合适的吹塑或结合拉伸/吹塑设备,类似于以上所述的胀大之前,热注塑预成型坯被部分地冷却并允许平衡到定向温度范围内。
图4-6表示用于制造本发明多层预成型坯计量,共注塑设备。该设备描述在1987年12月1日授权的Krishnakumar等人的美国专利US No.4,710,118中,将其全文结合在本发明中参考。
正如图4所示,注塑模具40包括外模腔42,用以限定颈部的精表面的颈环44,以及型芯46,颈环44连同型芯46封闭模腔42的上端部,而其下端部具有开孔48,它与挤出机的旋转阀件52的像喷管端50密封连接。阀件52密封地安装在一阀体54内,在阀体54内形成第一通道56,它与注塑机或注塑头的一常用的喷口60相接通。通道56径向地通向旋转阀件52,后者具有通道62,其一端接在径向通道64上,它可与通道56对准。阀体54也连接第二材料分配器66,该分配器包括一分配活塞68和一流体通道70,其出口朝向阀体54。阀体54具有一径向通道72,它轴向地对准和连接通道70。阀件52具有另一通道74,它从通道62径向地延伸,它与通道64环形间隔,以致当通道64与通道56对准,而通道74与通道72相隔开。转动阀件52,使通道64不与通道56对准,而通道74与通道72接通。因此,材料可以有选择地或是从第一供料装置(注塑头60)供入或是从第二供料装置66供入。
按照优选的实施例,由第一供料装置60提供的材料将是用于内层和外层的低共聚物PET。由第二供料装置66提供的材料将是用于芯层的高共聚物PET。
参照图5,可以看到,预先选择一定量的第一低共聚物树脂76将被注塑到模腔42的底部,而当其流过模腔时,由于模具40,包括型芯46相对低的温度,树脂76将被固化以限定第一材料的外部内层78和外层80。
正如图6所示,接着将高共聚物芯层材料86注塑到模腔。可以看到,芯层材料86将流过在层78与80之间限定的腔道,同时超过先前已注塑入的材料76。内部芯材料冷却的比较慢,因为它不接触较冷模具壁,但是由于芯层具有较高共聚物含量,可抗混浊。
至于图7,按上述的方法制造预成型坯110,它包括一高共聚物芯层130,一连续的低共聚物内层132,一低共聚物外层134,它除了部分被芯层材料间断外是连续的,所述的芯层材料在底座120处可延伸通过外层。预成型坯110包括一上端颈部精表面112,一倾斜的肩部成形部分114,它从顶部到底部厚度增加,一侧壁成形部分116,它具有均匀的厚度,和一底部成形部分118。底部118包括一上圆筒形变厚部分121,其厚度比侧壁116厚,并在瓶底形成变厚的瓶的凹边,和一倾斜的下部119,它的厚度减小以形成瓶子的凹进的圆形底座。为了再灌装的应用,具有优选截面的预成型坯描述在1991年11月19日批准的。Krishnakumar等人的美国专利US 5,066,522中,其全文结合在本发明中参考。在侧壁116的芯层130大致上为每一内层132和外层134的两倍厚,以形成具有上述壁厚的优选的1.5升瓶子。
正如图8所示,吹塑瓶子具有香槟酒颜色型的底部150,它包括中心底座152,中心凹进的圆形底座154,瓶的凹边156以及外底158。沿着底部芯层160和内层162和外层164各自的厚度是不同的,它取决于特定的底部所受到相对的拉伸量,但是,从底座152往径向推移时,通常其壁厚是逐渐减小的。
图9所示是预成型坯底部成形部分218的另一个实施例,其中第三低共聚物材料被注塑到底部成形部分的至少一部分236,而优选的是注入减小壁厚的下底部219,因为该处厚度小,冷却较快,对混浊不敏感。低共聚物部分236置于芯层材料230中,而优选的是内层232和外层234具有相同的材料,这样在上述的共注过程中,在下一个型坯开始注塑前,喷管要清理高共聚物,以避免将任何高共聚物注入下一个型坯的内层和外层中。如图10所示,是由图9所示预成型坯吹塑而成的香槟酒杯颜色型的瓶底250,它包括底座252,圆形底座254,瓶的凹边256,以及外底258。横切壁截面,该底部包括内层262,和外层264,和芯层260。至少一部分芯层260被低共聚物266所替换,该低共聚物穿过底座和凹口区。
用于本发明的热塑性聚酯材料优选是以聚亚烷基为基础,尤其是聚对苯二甲酸乙酯(PET)。用聚对苯二酸或其构成酯的衍生物和乙烯可制备PET聚合物。该聚合物包含对苯二酸-乙二醇的重复单元,其结构式为:
本发明考虑使用小比例的聚对苯二甲酸乙酯共聚物,例如,达到约10%重量的对苯二酸-乙二醇被相容的单体所替换。因此,这里用的“PEET”表示适合于制造瓶子的PET均聚物和PET共聚物,所述的制造瓶子是公知的技术。乙二醇一部分单体可被脂族或脂环乙二醇的替换,例如,环已烷二甲醇(CHDM),亚丙基二醇,聚1,4丁二醇,1,6-已二醇,十二亚甲基二醇,二甘醇,聚乙二醇,聚丙二醇,丙烷-1,3-二醇,丁烷-1,4-二醇和新式二醇,双酚类和其它芳族二醇,例如对苯二酚和2,2-双(4-B-羟基-乙氧苯基)丙烷。可以置换成单体的二羧酚一部分样品,它包括芳族二羧酸,例如间苯二酸(IPA),苯二甲酸,萘-二羧酸,联苯二羧酸,联苯氧基乙烷二羧酸,联苯甲酸和脂族或脂环二羧酸,例如已二酸,癸二酸,壬二酸,癸烷二羧酸和环已烷二羧酸。此外,各种多功能化合物,例如,三羟甲基丙烷,季戊四醇,1,2,4-苯三酸和1,3,5-苯三酸可以与聚对苯二甲酸乙酯共聚合。
聚对苯二甲酸乙酯聚合物可含有其它相容的添加剂和配合剂,它们不会对瓶子的性能有不利的影响,例如,对包装在其中产品的味道或其它性能的不利影响。此种配合剂包括热稳定性剂,光稳定剂,染料,颜料,增塑剂,填料,解毒剂,润滑剂,压出助剂,残渣单体清除剂等。
内粘度(I,V.)影响聚酯树脂的加工性能。具有内粘度大约为0.8的聚对苯二甲酸乙酯广泛地应用于CSD工业。作为各种用途的树脂可以是大约0.55至大约1.04的范围,而更特别是从大约0.65至0.85。测定内粘度可根据ASTM D-2857方法,即在30℃下,用0.0050±0.0002g/ml的聚合物在包括0-氯苯的溶剂中(熔点为0℃)。可按下式获得内粘度(I、V):
I、V=(Ln(Vsoln/Vsol))/C
其中:
Vsoln.是任意单元的溶液粘度;
Vsol.是在同一单元的溶剂粘度;和
C是g聚合物/100mls溶液。
制造可再灌装聚酯饮料瓶的其它重要因素描述在1982年6月15日授权的Krishnakimer等人的美国专利4,334,627,1988年2月16日授权的Collerre的美国专利4,725,464和1991年11月19日批准的Krishnakumar等人的美国专利5,066,528,上述专利全文结合在本发明中参考。
正如以下所述,本发明的塑料瓶优选用聚对苯二甲酸乙酯(PET)制造,然而,其它热塑性聚酯树脂可用于制造本发明的多层瓶,其中内层在注塑或类似的热处理过程中,具有对诱生热的结晶有较大阻力,而外部第二层在吹塑或拉伸步骤中,获得较高的应变和/或诱生热的结晶,以便提供较高级的表面结晶。除了优选实施例的芯层、内层和外层外,可提供辅加层,例如阻挡层(氧,二氧化碳、光),高热稳定性,回收PET或消费者用后的PET或其它层。可以使用不同的底部结构,例如一种瓶底,具有基本上半球形底壁,带有多个向下延伸的腿,并接到最下端的支撑座上,在腿之间还带有辐射状的加强肋(作为底壁的一部分)。材料,壁厚,预成型坯、瓶的形状和加工技术,对于特定用途的瓶子是不同的,同时还要结合本发明的要点。瓶子可用于装其它压力的或不带压力的饮料;例如,啤酒,果汁或牛奶或其它非饮料产品。本发明的优点是,例如抗混浊和高温下改进的抗断裂应力,特别适用于热灌装瓶,例如,描述在1989年9月5日授权的Collette等人的美国专利No 4,863,046,将其全文结合在本发明中参考。一般热灌装瓶必须耐高温,大约180-185°F(产品灌装温度)和耐正内压在约2-5Psi(灌装线压力),而基本上不变形(即体积变化不大于约1%)。
虽然已对本发明的几个实施例做了详细描述,应该指出,在不违背本发明附加的权利要求书所限定的精神和范围下,在预成型结构,材料,瓶结构和瓶成形方法方面可以做出不同的更改。
Claims (43)
1、一种基本上透明的多层瓶成形方法,包括:
提供一第一共聚物聚酯和一第二聚酯,第二聚酯具有较少的共聚物,其结晶速度至少比第一聚酯高约20%,
在升高的温度下形成基本上非晶体和透明的多层预成型坯,它具有第一聚酯内层和至少一第二聚酯的外层,其特征是从外层和第一聚酯内层冷却预成型坯,阻止诱生热的结晶。
2、按权利要求1的方法,还包括:
在高于第一和第二聚酯的玻璃转化温度下,延伸预成型坯以形成双轴取向的基本上透明的多层瓶,基于聚酯的不同结晶速度,其外层的结晶度比内层高。
3、按权利要求1和2任意之一的方法,其特征是在两外部的内层和外层之间的内层是芯层。
4、按权利要求3的方法,其特征是第一和第二聚酯基本上是聚对苯二甲酸乙酯(PET)。
5、按权利要求4的方法,其特征是第一聚酯是具有从大约4至大约6%的共聚物,而第二聚酯具有不大于大约2%的共聚物。
6、按权利要求1的方法,其特征是该预成型坯具有颈部精表面侧壁成形部分和底成形部分,其中侧壁成形部分具有平均结晶度不大于大约10%。
7、按权利要求1的方法,其特征是该预成型坯具有颈部精表面侧壁成形部分和底成形部分,其中侧壁成形部分具有平均结晶度不大于约20%。
8、按权利要求1的方法,其特征是该预成型坯具有颈部精表面侧壁成形部分和底成形部分,其中侧壁成形部分具有第一聚酯的内芯层,其厚度为大约50-80%的侧壁厚度,还具有第二聚酯的外部内和外层。
9、按权利要求8的方法,其特征是侧壁成形部分包括壁板成形部分,具有壁厚从约5至约7mm。
10、按权利要求9的方法,其特征是壁板成形部分是在拉伸比大约9-11∶1下延伸的。
11、按权利要求10的方法,其特征是壁板成形部分是在面积拉伸比大约9-11∶1下延伸的。
12、按权利要求11的方法,其特征是第一和第二聚酯基本上是聚对苯二甲酸乙酯(PET),而第一聚酯是从大约4%至大约6%共聚物,第二聚酯是不大于大约2%共聚物。
13、按权利要求2的方法,还包括提高瓶子的平均结晶度,同时通过低温热定形保持基本上的透明度。
14、按权利要求2的方法,其特征是预成型坯具有一颈部精表面,一侧壁成形部分和一底成形部分,所述的侧壁成形部分包括一壁板成形部分,它具有壁厚度从大约5至大约7mm,而平均混浊度不大于约10%,壁板成形部分在拉伸比大约7-11∶1下拉伸的,以形成的壁板具有平均混浊度不大于约10%,并且在外层平均结晶度至少大约20%,在内层至少大约14%,其中第一和第二聚酯基本上是聚对苯二甲酸乙酯(PET),第一聚酯具有从大约4%至大约6%的共聚物,第二聚酯不大于大约2%的共聚物。
15、按权利要求14的方法,还包括通过低温热定形提高壁板的外层的平均结晶度至少30%。
16、一种按照权利要求2,13,14,和15之一的方法制造的瓶子,其特征是瓶子在碱洗温度高于60℃下能承受至少10次再灌装循环,而没有断裂损坏。
17、按权利要求16的瓶子,其特征是瓶子能承受指定的再灌装循环次数,其最大体积变化大约±1.5%。
18、按权利要求16的瓶子,其特征是瓶子能承受至少20次再灌装循环。
19、按权利要求18的瓶子,其特征是瓶子能承受指定的再灌装循环次数,其最大体积变化大约±1.5%。
20、按权利要求2的瓶子,其特征是瓶子是独立的,增压的PET饮料瓶。
21、按权利要求2的瓶子,其特征是瓶子热灌装瓶。
22、按权利要求16的瓶子,其特征是瓶子包括至少一附加层,它选自阻挡层,高热稳定性,回收PET和消费者用后的PET。
23、一种瓶子,它包括具有基本上透明的双轴取向的多层整体侧壁的瓶体,所说的侧壁包括第一共聚物聚酯的内层和至少一第二聚酯的外层,所说的第二聚酯具有的共聚物少于第一聚酯,而其结晶速率至少比第一聚酯高20%,所说的侧壁包括基本上圆筒形壁板,它具有平均诱生应变的结晶度,外层至少大约20%,内层至少大约14%。
24、按权利要求23的瓶子,其特征是第一聚酯具有大约4%至大约6%的共聚物。
25、按权利要求24的瓶子,其特征是第二聚酯具有不大于大约2%的共聚物。
26、按权利要求25的瓶子,其特征是第一和第二聚酯基本上是聚对苯二甲酸乙酯((PET)。
27、按权利要求26的瓶子,其特征是通过诱生热的结晶度使壁板的外层平均结晶度可提高到至少大约30%,同时保持基本上透明。
28、按权利要求26的瓶子,其特征是壁板的厚度为大约0.5至0.7mm。
29、按权利要求28的瓶子,其特征是壁板是在二维拉伸比大约7-13∶1下拉伸而成。
30、按权利要求29的瓶子,其特征是壁板是在二维拉伸比大约9-11∶1下拉伸面成。
31、按权利要求23和26任意之一的瓶子,其特征是内层是芯层为大约50%至大约80%的壁板厚。
32、按权利要求26的瓶子,其特征是:瓶子在碱洗温度高于60℃下能承受至少10次再灌装循环而不断裂损坏。
33、按权利要求32的瓶子,其特征是瓶子在碱洗温度高于60℃下能承受至少20次再灌装循环而不断裂损坏。
34、按权利要求32至33任意之一的瓶子,其特征是瓶子能承受指定的再灌装循环次数,其最大体积变化大约±1.5%。
35、按权利要求26的瓶子,其特征是共聚物选自包括1.4-环已烷二甲醇和间苯二酸。
36、按权利要求23的瓶子,其特征是瓶子是独立的增压的PET饮料瓶。
37、按权利要求23的瓶子,其特征是瓶子是热灌装瓶子。
38、按权利要求26的瓶子,其特征是侧壁的混浊度百分数不大于约15%。
39、按权利要求23的瓶子,其特征是第一和第二聚酯是每个瓶子是不同等级的PET。
40、按权利要求23的瓶子,其特征是瓶子包括一材料层,它选自包括阻挡层,高热稳定性,回收PET和消费者用后的PET。
41、一种预成型坯,它包括具有基本上透明和非晶体的多层整体侧壁的坯体,所说的侧壁包括一第一共聚物的内层和至少一第二聚酯的外层,所说的第二聚酯具有的共聚物少于第一聚酯,而其结晶速率至少比第一聚酯高20%。
42、按权利要求41的预成型坯,其特征是内层是芯层为大约50%至大约80%的侧壁厚度,外层包括内层和外层。
43、按权利要求41的预成型坯,其特征是第一和第二聚酯基本上是聚对苯二甲酸乙酯,第一聚酯是具有从大约4%至大约6%的共聚物,而第二聚酯具有不大于2%的共聚物。
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
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US90996192A | 1992-07-07 | 1992-07-07 | |
US07/909,961 | 1992-07-07 | ||
US8217193A | 1993-06-30 | 1993-06-30 | |
US08/082,171 | 1993-06-30 |
Publications (1)
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CN1092352A true CN1092352A (zh) | 1994-09-21 |
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CN93109891A Pending CN1092352A (zh) | 1992-07-07 | 1993-07-07 | 具有低结晶内层的多层预成型坯和瓶子的成型方法 |
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US (3) | US5728347A (zh) |
EP (1) | EP0653981B1 (zh) |
CN (1) | CN1092352A (zh) |
AT (1) | ATE177049T1 (zh) |
AU (1) | AU674528B2 (zh) |
CA (1) | CA2139764C (zh) |
DE (1) | DE69323751T2 (zh) |
HU (1) | HU213531B (zh) |
SG (1) | SG45429A1 (zh) |
SK (1) | SK1495A3 (zh) |
WO (1) | WO1994001268A1 (zh) |
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CN111032519A (zh) * | 2017-08-31 | 2020-04-17 | 宝洁公司 | 具有良好限定的拐角的刚性制品 |
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1993
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- 1993-07-02 SG SG1996007595A patent/SG45429A1/en unknown
- 1993-07-02 CA CA002139764A patent/CA2139764C/en not_active Expired - Fee Related
- 1993-07-02 SK SK14-95A patent/SK1495A3/sk unknown
- 1993-07-02 AU AU46642/93A patent/AU674528B2/en not_active Ceased
- 1993-07-02 WO PCT/US1993/006335 patent/WO1994001268A1/en active IP Right Grant
- 1993-07-02 DE DE69323751T patent/DE69323751T2/de not_active Expired - Fee Related
- 1993-07-02 EP EP93916962A patent/EP0653981B1/en not_active Expired - Lifetime
- 1993-07-02 HU HU9500018A patent/HU213531B/hu not_active IP Right Cessation
- 1993-07-07 CN CN93109891A patent/CN1092352A/zh active Pending
-
1995
- 1995-03-31 US US08/415,149 patent/US5728347A/en not_active Expired - Fee Related
-
1997
- 1997-05-19 US US08/858,132 patent/US5759656A/en not_active Expired - Fee Related
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CN101743113A (zh) * | 2007-06-07 | 2010-06-16 | 西德尔合作公司 | 具有结晶梯度的聚合物制的容器 |
CN101743113B (zh) * | 2007-06-07 | 2013-08-07 | 西德尔合作公司 | 具有结晶梯度的聚合物制的容器 |
CN110769994A (zh) * | 2017-06-23 | 2020-02-07 | 赫斯基注塑系统有限公司 | 具有选择性变化的芯层几何形状的模制品以及用于制造该模制品的热流道喷嘴 |
CN113524495A (zh) * | 2017-06-23 | 2021-10-22 | 赫斯基注塑系统有限公司 | 适合于随后吹塑成最终成形容器的模制品 |
CN110769994B (zh) * | 2017-06-23 | 2022-06-24 | 赫斯基注塑系统有限公司 | 具有选择性变化的芯层几何形状的模制品以及用于制造该模制品的热流道喷嘴 |
CN113524495B (zh) * | 2017-06-23 | 2023-04-21 | 赫斯基注塑系统有限公司 | 适合于随后吹塑成最终成形容器的模制品 |
US11850779B2 (en) | 2017-06-23 | 2023-12-26 | Husky Injection Molding Systems Ltd. | Molded article with selectively varied core layer geometry and hot runner nozzles for producing same |
CN111032519A (zh) * | 2017-08-31 | 2020-04-17 | 宝洁公司 | 具有良好限定的拐角的刚性制品 |
CN111032519B (zh) * | 2017-08-31 | 2022-05-31 | 宝洁公司 | 具有良好限定的拐角的刚性制品 |
CN111907854A (zh) * | 2019-05-08 | 2020-11-10 | 宝洁公司 | 具有着色剂的一件式多层热塑性容器 |
CN111907854B (zh) * | 2019-05-08 | 2022-07-01 | 宝洁公司 | 具有着色剂的一件式多层热塑性容器 |
Also Published As
Publication number | Publication date |
---|---|
DE69323751T2 (de) | 1999-07-01 |
ATE177049T1 (de) | 1999-03-15 |
US5728347A (en) | 1998-03-17 |
DE69323751D1 (de) | 1999-04-08 |
WO1994001268A1 (en) | 1994-01-20 |
HUT71921A (en) | 1996-02-28 |
CA2139764C (en) | 1999-02-23 |
US6090460A (en) | 2000-07-18 |
AU4664293A (en) | 1994-01-31 |
SG45429A1 (en) | 1998-01-16 |
AU674528B2 (en) | 1997-01-02 |
EP0653981A1 (en) | 1995-05-24 |
HU9500018D0 (en) | 1995-03-28 |
HU213531B (en) | 1997-07-28 |
SK1495A3 (en) | 1995-08-09 |
US5759656A (en) | 1998-06-02 |
EP0653981B1 (en) | 1999-03-03 |
CA2139764A1 (en) | 1994-01-20 |
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