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CN101641201A - 多层聚酯容器及其生产方法 - Google Patents

多层聚酯容器及其生产方法 Download PDF

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Publication number
CN101641201A
CN101641201A CN200780052281A CN200780052281A CN101641201A CN 101641201 A CN101641201 A CN 101641201A CN 200780052281 A CN200780052281 A CN 200780052281A CN 200780052281 A CN200780052281 A CN 200780052281A CN 101641201 A CN101641201 A CN 101641201A
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CN
China
Prior art keywords
resin
functional resin
preform
multilayer
layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN200780052281A
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English (en)
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CN101641201B (zh
Inventor
笹井实佐
菊地淳
山田俊树
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toyo Seikan Group Holdings Ltd
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Toyo Seikan Kaisha Ltd
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Publication of CN101641201A publication Critical patent/CN101641201A/zh
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    • B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
    • B29C49/0005—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor characterised by the material
    • B29C49/0006—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor characterised by the material for heating or cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
    • B23B27/08—Cutting tools with blade- or disc-like main parts
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Abstract

一种多层聚酯容器，其包含聚酯树脂制成的内外层和至少一层功能性树脂或功能性树脂组合物制成的中间层，其中所述聚酯内层在0.5Hz下在动态粘弹性(DMS)测量中80℃和60℃之间的tanδ之差为0.035以下。即使当将具有高拉伸应力的功能性树脂或功能性树脂组合物用作中间层时，该容器也具有优良的透明性，和有效地展现由功能性树脂或功能性树脂组合物所具有的功能如阻挡性。

Description

多层聚酯容器及其生产方法
技术领域
本发明涉及具有功能性树脂中间层的多层容器。更具体地，本发明涉及特征在于即使通过使用具有大拉伸应力的功能性树脂作为中间层，透明性和阻挡性也优良的多层聚酯容器及其生产方法。
背景技术
为了改进塑料包装容器内容物的保存性，迄今习惯的作法是形成多层结构的容器壁，其使用聚酯树脂作为内外层和使用功能性树脂如用于改进气体阻挡性的乙烯/乙烯基醇共聚物或含亚二甲苯基的聚酰胺树脂或用于改进水蒸气(水)阻挡性的环状烯烃共聚物作为中间层。
为了进一步改进功能如气体阻挡性或进一步赋予任何其它功能，将功能性树脂与无机填料或任何其它树脂组合物共混也是切实可行的。例如，JP-A-2004-142444公开将含亚二甲苯基的聚酰胺与表面改性的粘土共混以进一步改进含亚二甲苯基的聚酰胺树脂的气体阻挡性。
发明内容
然而，如果在与用于使用以上功能性树脂作为中间层的单层聚酯瓶的那些相同的条件下进行双轴拉伸吹塑成型，出现的问题在于由于拉伸而在中间层中产生材料缺乏，各种尺寸的空隙产生，引起透明性和阻挡性降低。
此外，在通过将共混有表面改性粘土的含亚二甲苯基聚酰胺的树脂组合物作为在聚酯树脂内层和外层之间的中间层拉伸吹塑成型来获得的多层容器的情况下，展现这样的拉伸特性：在拉伸时趋于产生高负荷，对于拉伸比和对于共混有表面改性粘土的树脂组合物的用量施加限制，因此，对于改进气体阻挡性施加限制。
因此，本发明的目的是提供特征在于即使通过使用具有大拉伸应力的功能性树脂或功能性树脂组合物作为中间层，透明性和阻挡性也优良的多层聚酯容器。
本发明的另一目的是提供当将具有大拉伸应力的功能性树脂或功能性树脂组合物用作中间层时能够形成多层聚酯容器而不降低功能如透明性和阻挡性的方法。
根据本发明，提供多层聚酯容器，其包含聚酯树脂内外层和至少一层功能性树脂中间层，其中聚酯内层在0.5Hz下测量其粘弹性时在80℃和60℃下的tanδ之差为0.035以下。
在本发明的多层聚酯容器中，期望：
1.当功能性树脂的具有厚度为1.5mm的注射成型板在115℃下拉伸时，功能性树脂具有拉伸应力的最大值为50N以上；
2.功能性树脂包含乙烯/乙烯基醇共聚物或聚己二酰间苯二甲胺(polymetaxylylene adipamide)作为基础树脂；
3.功能性树脂包含分散于其中的粘土；和
4.功能性树脂为环状烯烃树脂。
根据本发明，进一步提供通过双轴拉伸吹塑成型包含聚酯树脂内外层和至少一层功能性树脂中间层的多层预制品来生产多层聚酯容器的方法，其中在进行双轴拉伸吹塑成型时，将多层预制品在温度105至120℃下加热，将多层预制品通过使用在300至600℃下加热的加热棒和/或在150至220℃下的热空气来内部加热。
在本发明多层聚酯容器的生产方法中，能优选使用功能性树脂，所述功能性树脂当其具有厚度为1.5mm的注射成型板在115℃下拉伸时具有拉伸应力的最大值为50N以上。
在本发明的包含聚酯树脂内外层和至少一层功能性树脂中间层的多层聚酯容器中，抑制由于拉伸而产生的空隙，由于使用功能性树脂而展示透明性和优良的功能。
此外，根据本发明的生产方法，使得能够生产包含聚酯树脂内外层和至少一层功能性树脂中间层的多层聚酯容器而不损害功能性树脂的透明性和优良的功能。
在本发明的包含聚酯树脂内外层和至少一层功能性树脂中间层的多层聚酯容器中，重要的特征在于所述聚酯内层在0.5Hz下测量其粘弹性时在80℃和60℃下的tanδ(损耗角正切)之差为0.035以下。
在如上所述的包含聚酯树脂内外层和至少一层功能性树脂中间层的多层聚酯容器中，构成中间层的功能性树脂通常具有高于构成内外层的聚酯树脂拉伸应力的拉伸应力。因此，如果拉伸吹塑成型以与用于普通多层聚酯容器成型相同的方式进行，中间层的拉伸不能追随内外层的拉伸。结果，空隙产生于中间层中，损害透明性。除此之外，未显示用作中间层的功能性树脂的功能至足够的程度。
根据本发明，即使通过使用上述功能性树脂作为中间层，聚酯内层在0.5Hz下测量其粘弹性时在80℃和60℃下的tanδ之差为0.035以下，也有效地防止空隙的产生，并能够使形成具有阻挡性的透明中间层的树脂展示其固有功能至足够的程度。
测量粘弹性时的tanδ值是通过弹性损失模量E”除以弹性储能模量E’得到的值，即，对损失分量有贡献的无定形部分与对储能分量有贡献的结晶部分的比例。因此，其绝对值小代表由拉伸引起的应力小，在80℃和60℃下的tanδ的差值小代表应变的残余量几乎不依赖于温度，应变在该温度区域中得到松弛。
本发明利用在80℃和60℃下的tanδ值。这是因为，通过实验发现，在上述温度下的值突出表现本发明的特征。
在本发明中，重要的是：在具有大拉伸应力的功能性树脂中间层中，应变在拉伸时得到松弛。因此，理想的是测量中间层的tanδ，以确保应变得到松弛。但是，通常中间层具有小的厚度，同时功能性树脂涉及由于其性质如高吸湿性而引起的难以正确测量其tanδ。因此，在进行根据本发明的双轴拉伸吹塑成型时，注意具有沿容器厚度方向的最大拉伸比和具有大应变的聚酯最内层。当然，当应变在聚酯最内层中松弛至足够的程度时，也认为应变在功能性树脂中间层中得到松弛。事实上，本发明人已测量聚酯内层中的tanδ值，观察在中间层中在该值处的空隙，并评价功能如透明性和阻挡性。结果，本发明人已发现聚酯内层中的tanδ值与中间层中松弛应变的程度之间的相关性。
此外，在双轴拉伸吹塑成型的容器中，主体部(body portion)在容器的部位中受到拉伸最多并且几乎不适于测量应变松弛效果。因此，tanδ值在能够易于测量应变松弛效果部位处更好地测量。因此，必要的是：在靠近颈部基本面(ground surface)或靠近颈部底部，特别是在靠近拉伸不太多的颈部底部进行测量。
本发明的多层聚酯容器的上述作用和效果从稍后示出的实施例结果变得显而易见。即，当聚酯内层在0.5Hz下测量其粘弹性时在80℃和60℃下的tanδ之差大于0.035时，透明性和阻挡性由于空隙而降低(比较例1至5和比较例7至9)。另一方面，当tanδ之差为0.035以下时，展现优良的透明性和阻挡性(实施例1至8)。
附图说明
图1是说明本发明多层聚酯容器的截面结构的图；和
图2是说明本发明多层聚酯容器的截面结构的图。
具体实施方式
(功能性树脂)
作为构成本发明中间层的功能性树脂，能使用已知的功能性树脂如具有气体阻挡性、水蒸气阻挡性、氧吸收性或氧吸收气体阻挡性的功能性树脂，或使用功能性树脂作为基质的树脂组合物。在本发明中，特别是能够优选使用具有当其具有厚度1.5mm的注射成型板在115℃下拉伸时拉伸应力最大值为50N以上的功能性树脂。所述具有大拉伸应力的功能性树脂易于在其拉伸时产生空隙，并当拉伸时易于损害功能性树脂的透明性和功能。然而，本发明使得可以即使当将具有大拉伸应力的功能性树脂用作中间层时也展现优良的透明性和功能。
作为用于本发明中间层的功能性树脂，能够例举作为气体阻挡性树脂的聚酰胺树脂例如聚己二酰间苯二甲胺或聚癸二酰间苯二甲胺(polymetaxylylene sebacamide)、乙烯/乙烯基醇共聚物和作为水蒸气阻挡性树脂的环状烯烃树脂。所有这些树脂具有在上述条件下测量的拉伸应力最大值为50N以上，并能够难以拉伸。
上述气体阻挡性树脂可含有分散于其中的有机粘土，以致用作气体阻挡性树脂组合物层，或者可在包含有机粘土或不包含有机粘土的情况下，含有氧化性有机组分和过渡金属催化剂，以致用作氧吸收气体阻挡性树脂组合物层。共混有机粘土等的功能性树脂组合物通常具有比其仅包含该功能性树脂时更大的拉伸应力，并趋于由于空隙产生而损害功能如透明性和气体阻挡性。
表面改性粘土是通过用有机化剂处理粘土以膨胀而获得的那些。在表面改性粘土中的粘土是云母、蛭石或绿土，优选具有电荷密度为0.25至0.6的2-八面体型或3-八面体型的层状硅酸盐。作为2-八面体型的粘土，能例举蒙脱石、贝得石和绿脱石，作为3-八面体型的粘土，能例举锂蒙脱石和皂石。其中，蒙脱石由于有机化剂渗入而进行层之间的膨胀因而高度膨胀，是特别期望的。
作为有机化剂，理想地使用季铵盐。然而，更理想地，能使用具有至少一种或多种具有不少于12个碳原子的烷基的季铵盐，具体地是三甲基十二烷基铵盐和三甲基十四烷基铵盐。
期望包含表面改性粘土的功能性树脂以基于100重量份功能性树脂为1至10重量份，特别是1至8重量份的比例共混有表面改性粘土。当表面改性粘土的量小于上述范围时，与当表面改性粘土以上述范围内的量共混时相比，不会获得气体阻挡性至足够的程度。另一方面，当表面改性粘土的量大于上述范围时，成型性变得劣于当表面改性粘土量在上述范围内时的成型性，这是不期望的。
氧化性有机组分和过渡金属催化剂的组合可以是迄今用于氧吸收性树脂组合物的组合。作为氧化性有机组分，能例举在侧链或在末端具有官能团并能被氧化的那些。具体地，能例举用酸或酸酐改性的多烯低聚物或聚合物，例如丁二烯和用马来酸酐改性的丁二烯。作为过渡金属催化剂，能使用元素周期表的第VIII族金属组分，例如铁、钴、镍等，当然，尽管不仅限于此。
期望氧化性有机组分以基于100重量份功能性树脂为2至10重量份的量共混。进一步期望过渡金属催化剂以作为金属计算的至少300ppm的量共混。
除了上述有机粘土、氧化性组分和过渡金属催化剂的组合之外，在不损害本发明目的的范围内，根据已知配方，用于本发明的功能性树脂可进一步共混已知的用于树脂的共混剂如脱氧剂、填料、着色剂、热稳定剂、耐候剂、抗氧化剂、老化稳定剂、光稳定剂、紫外线吸收剂、抗静电剂、润滑剂(如金属皂或蜡)和改造树脂(reforming resin)或橡胶。
(聚酯树脂)
用作本发明内外层的聚酯树脂可以是已知的包括二羧酸组分和二醇组分的聚酯树脂。
关于二羧酸组分，从机械性质和热性质的观点出发，期望50％以上，特别是80％以上的二羧酸为对苯二酸。然而，当然可以包含除对苯二酸之外的羧酸组分。作为除对苯二酸之外的羧酸组分，能够例举间苯二酸、萘二甲酸、对-β-氧代乙氧基苯甲酸、联苯基-4，4’-二羧酸、二苯氧基乙烷-4，4’-二羧酸、5-钠磺基间苯二酸(5-sodiumsulfoisophthalic acid)、六氢对苯二酸、己二酸和癸二酸。
关于二醇组分，从机械性质和热性质的观点出发，期望50％以上，特别是80％以上的二醇为乙二醇。作为除乙二醇之外的二醇组分，能够例举1，4-丁二醇、丙二醇、新戊二醇、1，6-己二醇、二甘醇、三甘醇、环己烷二甲醇、双酚A的环氧乙烷加成物、甘油和三羟甲基丙烷。
二羧酸组分和二醇组分可以含有三官能以上的高级官能多元酸和多元醇。其实例包括多元酸如偏苯三酸、1，2，4，5-苯四酸、苯连三酸、1，1，2，2-乙烷四甲酸、1，1，2-乙烷三甲酸、1，3，5-戊烷三甲酸、1，2，3，4-环戊烷四甲酸、联苯基-3，4，3’，4’-四甲酸，和多元醇如季戊四醇、甘油、三羟甲基丙烷、1，2，6-己三醇、山梨醇和1，1，4，4-四(羟甲基)环己烷。
期望用作本发明内外层的聚酯树脂具有通过使用重量比为1∶1的苯酚/四氯乙烷混合溶剂在温度30℃下测量的固有粘度在0.60至1.40dL/g范围内。进一步期望聚酯树脂具有熔点(Tm)200至275℃，从而改进多层容器的耐热性和加工性。进一步期望玻璃化转变点为30℃以上，特别是在50至120℃的范围内。
根据已知配方，用作本发明内外层的聚酯树脂能够以不损害最终成型体品质范围的量共混已知的用于树脂的共混剂，例如着色剂、抗氧化剂、稳定剂、各种抗静电剂、脱模剂、润滑剂和成核剂。
(多层聚酯容器)
本发明的多层聚酯容器可以利用各种层结构，只要其至少具有聚酯树脂内层和外层，以及功能性树脂中间层或使用功能性树脂作为基础树脂的功能性树脂组合物中间层即可。如图1所示，所述层结构可包含在聚酯树脂内层1和外层2之间的功能性树脂中间层3。或者，如图2所示，所述层结构可包含聚酯树脂的内层1和外层2，以及两层功能性树脂中间层3a和3b，其中之一位于聚酯树脂内层1和聚酯树脂中间层4之间，另一者位于聚酯树脂外层2和聚酯树脂中间层4之间。
在生产多层容器时，可将粘合剂树脂插入所述树脂层之间，然而，这通常并不要求。作为粘合剂树脂，能例举以每100g树脂为1至700毫当量(meq)的浓度，特别是以每100g树脂为10至500meq的浓度在主链或在侧链上包含基于羧酸、羧酸酐、羧酸盐、羧酸酰胺以及羧酸酯的羰基(-CO-)的热塑性树脂。粘合剂树脂的优选实例包括乙烯/丙烯酸共聚物、离子交联的烯烃共聚物、马来酸酐接枝聚乙烯、马来酸酐接枝聚丙烯、丙烯酸接枝聚烯烃、乙烯/乙酸乙烯酯共聚物和共聚聚酯。
在本发明的多层容器中，期望主体部的总厚度在200至600μm，特别是240至500μm的范围内，尽管其可能依赖于容器体积(重量)和容器用途而变化。
从容器透明性的观点出发，期望作为中间层的功能性树脂层具有厚度30μm以下，特别是在10至30μm的范围内，并且中间层在主体部总厚度的3至15％范围内。
当功能性树脂的中间层要以多数层形成时，期望各中间层具有厚度25μm以下，特别是在10至25μm范围内，并且整个中间层在主体部总厚度的3至25％范围内。
(多层容器的生产方法)
本发明的多层容器通过以下方式形成：形成具有上述多层结构的预制品，将所述预制品在105℃以上的高温下加热，沿轴向拉伸所述预制品，沿周向吹塑-拉伸所述预制品，必要时热固化所述预制品。
多层预制品能够通过已知成型法来生产，所述成型法例如：通过共挤出例如功能性树脂和聚酯树脂的共挤出成型法；通过同时将功能性树脂和聚酯树脂注射入金属模具的共注射成型法；通过将聚酯树脂、功能性树脂和聚酯树脂顺序地注射入金属模具的顺序注射法；或通过使用芯模具(core mold)和型腔模具(cavity mold)将功能性树脂和聚酯树脂的共挤出熔融树脂块压缩成型的压缩成型法。
当利用上述系统的任一种时，成型的预制品应当处于过冷状态，即处于无定形状态。进一步期望将功能性树脂中间层封入热塑性聚酯内层和外层之中的内部。
期望多层预制品成型和其拉伸吹塑成型通过上述冷型坯系统进行。然而，也可利用热型坯系统进行拉伸吹塑成型而不完全冷却成型的多层预制品。
在拉伸吹塑成型之前，将预制品通过此类手段如热空气、红外线加热器或高频感应加热预热至拉伸温度。然而，在本发明中，重要的是通过在高于普通拉伸吹塑成型温度的高温105至120℃，特别是108至118℃下进行拉伸吹塑。即，当预制品的温度低于上述温度时，功能性树脂中间层的拉伸应力增大，导致空隙易于产生，因而，损害所获得的多层容器的透明性。另一方面，当预制品的温度高于上述范围时，在拉伸吹塑成型时预制品被软化，引起偏心，劣化成型性，失去所获多层容器的厚度分布均匀性，使得预制品在拉伸吹塑成型前结晶化，并使得难以完成成型。
将由此加热的预制品供料至已知的拉伸吹塑成型机，将其置于金属模具内，通过挤压拉伸杆沿轴向拉伸，并通过吹塑流体沿周向拉伸。此处，在本发明中，重要的是通过使用在300至600℃加热的加热棒和/或150至220℃，特别是170至210℃的热空气加热多层预制品内部。
即，在双轴拉伸吹塑成型在上述温度范围内加热的预制品时，将在高温下加热的加热棒插入预制品中以加热其内部和/或将高温热空气强力引入其中。因此，预制品中的温度变高，并在拉伸吹塑成型松弛应变期间在预制品内部维持高温，将在包含具有大拉伸应力的功能性树脂中间层中的应变松弛，抑制空隙形成而不损害透明性和功能如气体阻挡性。
在本发明中，重要的是加热棒和热空气的温度在上述范围内。当该温度低于上述范围时，不会将预制品内部加热至足够的程度，应力不会得到有效地松弛。另一方面，当该温度高于上述范围时，聚酯内层或功能性树脂结晶化和泛白(whitened)或被不均匀地拉伸，或功能性树脂层被不均匀地拉伸，劣化成型性。
期望用于加热内部的时间根据预制品的预热温度和用于加热内部的加热棒的设定温度而变化。优选地，加热时间为8至20秒，特别地为10至15秒。进一步期望将用于拉伸吹塑成型的热空气强力引入放置在金属模具中的预制品中2至3秒。
期望作为最终制品的多层聚酯容器的拉伸比以面积比计为1.5至25倍，以沿轴向的拉伸比计为1.2至6倍，以沿周向的拉伸比计为1.2至4.5倍。
通过本发明的方法获得的多层聚酯容器具有25％以上的聚酯内层结晶度，这可与通过在普通条件下拉伸吹塑成型单层预制品所获容器的取向和结晶度相比。
拉伸吹塑成型瓶能通过已知方式热固化。所述热固化能通过单成型法(one-molding method)在吹塑成型金属模具中进行，或通过双成型法使用与吹塑成型金属模具分离的热固化金属模具进行。用于热固化的温度理想地在100至200℃的范围内。
作为另外的拉伸吹塑成型，可以例举两步拉伸吹塑成型，根据该两步拉伸吹塑成型，将该预制品通过使用初次(primary)吹塑金属模具成型为尺寸大于最终吹塑成型体的初次吹塑成型体，将该初次吹塑成型体在加热收缩后，接着通过使用二次吹塑金属模具进行双轴拉伸吹塑成型，以获得最终吹塑成型体，如在转让给本申请人的日本专利2917851中所教导。根据该拉伸吹塑成型，获得得以拉伸以具有降低至足够程度厚度的底部并且特征为在热充填和通过加热灭菌时优良的变形和冲击性的吹塑成型体。
当还根据本发明进行上述两步拉伸吹塑成型时，重要的是通过在初次吹塑时使用在300至600℃下加热的加热棒和/或使用150至220℃的热空气加热内部。
本发明的多层容器不只限于上述双轴拉伸吹塑成型瓶，而是可以为杯状等的拉伸成型多层容器，只要聚酯内层在0.5Hz下测量粘弹性时在80℃和60℃下的tanδ之差为0.035以下即可。即，通过利用用于在使用功能性树脂作为中间层和热塑性聚酯作为内外层生产多层片材时和在使多层片材进行真空成型、压缩空气成型、拉伸成型或模塞助压成型时，或在生产多层预制品和使多层预制品进行双轴拉伸吹塑成型时松弛聚酯内层中变形的方式，能生产至少具有拉伸主体部的杯状多层塑料容器。
依赖于用于中间层的功能性树脂，本发明的多层聚酯容器展现各种功能如气体阻挡性、氧吸收性和水蒸气阻挡性，并用作能够例如防止内容物的风味因氧而劣化的容器。能够充填的内容物可以是饮料如啤酒、葡萄酒、果汁、碳酸化软饮品和含果汁的碳酸化饮料，食品如水果、坚果、蔬菜、肉类、幼儿食品、咖啡、果酱、蛋黄酱、调味番茄酱、食用油、调味品、加味料、酱油中煮过的食品、奶制品，以及药品、化妆品和汽油，它们在氧存在下劣化，尽管并不仅限于此。
实施例
将通过下列实施例进一步描述本发明，然而，本发明绝不限于此。
[功能性树脂拉伸应力的测量]
将具有厚度1.5mm的功能性树脂注射成型板通过使用双轴拉伸试验仪(由Toyo Seiki Seisaku-sho.Ltd.制造)，在温度115℃下，以拉伸速度2.5m/分钟，以3倍长和3倍宽的比例双轴拉伸，从而通过使用连接至双轴拉伸试验仪的应力测量装置来测量拉伸应力。
[tanδ之差的测量]
将1cm宽和2cm长的试件从所形成的多层容器的颈部下端下方10mm的位置沿肩部形状切出，仅将厚度100μm的聚酯最内层剥掉。将由此剥掉的试件通过使用粘弹性测量设备[EXSTAR6000SERIES-DMS 6100，由SII NanoTechnology Inc.制造]，在以下测量条件下测量其tanδ，所述测量条件为：试件计量长度10mm，振动0.5Hz，应变振幅10μm，最小张力/压缩力200mN和以每分钟5℃的速率升温。在60℃和80℃下的tanδ值从所得的图谱中读取，得到其间的差值。
[内部雾度(haze)的测量]
将30mm宽和40mm长的试件从所形成的多层容器主体部中心切出。仅将功能性树脂中间层从试件剥离，将石蜡液体薄薄地施涂于其表面上，以去除外部雾度。其后，通过使用由SugaTestInstruments Co.，Ltd.制造的S&M Colour Computer，ModelSM-4来测量雾度(％)。
[氧透过系数的测量]
将13cm宽和9cm长的试件从所形成的多层容器主体部切出。仅将功能性树脂中间层从试件剥离，并通过使用由MoconInc.制造的氧透过分析系统OX-TRAN 2/20，在温度40℃和相对湿度90％RH的条件下测量其氧透过率(ml·mm/day·atm)，氧透过系数(ml·mm/m2·day·atm)由已预先测量的样品厚度(mm)计算。
[水蒸气透过系数的测量]
将13cm宽和9cm长的试件从所形成的多层容器主体部切出。仅将功能性树脂中间层从试件剥离，并通过使用由MoconInc.制造的水蒸气透过分析系统PERMATRAN-W 3/30，在温度40℃和相对湿度90％RH的条件下测量其水蒸气透过率(g·mm/day·atm)，水蒸气透过系数(g·mm/m2·day·atm)由已预先测量的样品厚度(mm)计算。
[实施例1]
通过使用设置有三台注射机，即，用于内外PET层的注射机(a)、用于中间PET层的注射机(b)和用于功能性树脂的注射机(c)的共注射成型机，将在150℃下干燥4小时的聚对苯二甲酸乙二酯(PET)树脂(RT543CTHP，由Japan Unipet Co.，Ltd.制造)进给至注射机(a)和(b)，将聚己二酰间苯二甲胺树脂(MXD6)(S6121，由Mitsubishi Gas Chemical Company Inc.制造)(拉伸应力：55N)作为功能性树脂进给至注射机(C)，以通过顺序注射成型来成型两种五层(a/c/b/c/a)的多层预制品，其具有内外层和中间层(都为PET层)，以及它们之中的功能性树脂的功能性树脂中间层。预制品称重为32g，其中功能性树脂的比例为总膜厚度的5％。
接着，通过使用石英加热器，将预制品从外侧预热至表面温度113℃，并通过使用在150℃下加热的压缩空气拉伸吹塑成型，以成型具有容量530ml和主体部中各种层，即最内层PET层(100μm)/内功能性树脂层(11μm)/中间PET层(180μm)/外功能性树脂层(11μm)/外PET层(150μm)的二种五层的多层瓶。
将样品从靠近所得瓶颈部的下部切出，以测量tanδ。此外，将样品从主体部切出，以测量内部雾度和氧透过系数。
[实施例2]
除了使用通过利用双轴挤出机将聚己二酰间苯二甲胺[T630，由Toyo B oseki Co.制造]和3重量％已进行有机化处理的天然蒙脱石熔融捏合获得的树脂组合物(拉伸应力：70N)作为功能性树脂，在预热该预制品时，将该预制品通过将在530℃下加热的铁芯插入预制品10秒来加热，并通过使用室温压缩空气吹入空气之外，以与实施例1相同的方式成型多层预制品和多层瓶。
将所得的瓶以与实施例1中相同的方式进行测量。
[实施例3]
除了将所得预制品通过使用石英加热器加热至116℃并通过使用在190℃下加热的热空气将预制品拉伸吹塑成型而不通过铁芯加热内部之外，以与实施例2中相同的方式成型多层预制品和多层瓶。
将所得的瓶以与实施例2中相同的方式进行测量。
[实施例4]
除了使用通过利用双轴挤出机将乙烯/乙烯基醇共聚物(EVOH)(Evar F101，由Kuraray-Eval Company制造)和3重量％已进行有机化处理的天然蒙脱石熔融捏合获得的树脂组合物(拉伸应力：65N)作为功能性树脂之外，以与实施例2中相同的方式成型多层预制品和多层瓶。
将所得的瓶以与实施例2中相同的方式进行测量。
[实施例5]
除了使用环状烯烃共聚物(COC)[APL 6509T，由MitsuiChemicals，Inc.制造](拉伸应力：100N以上)作为功能性树脂，并将所得的预制品通过将在530℃下加热的铁芯插入预制品15秒来加热之外，以与实施例3中相同的方式成型多层预制品和多层瓶。
将所得的瓶以与实施例3中相同的方式进行测量。
[实施例6]
除了通过使用石英加热器将预制品从外侧预热至表面温度105℃和通过使用在220℃下加热的热空气拉伸吹塑成型预制品之外，以与实施例3中相同的方式成型多层预制品和多层瓶。
将所得的瓶以与实施例2中相同的方式进行测量。
[实施例7]
除了通过使用石英加热器将预制品从外侧预热至表面温度112℃，在预热预制品时通过将在300℃下加热的铁芯插入预制品20秒来加热预制品和通过使用在150℃下加热的热空气拉伸吹塑成型预制品之外，以与实施例2中相同的方式成型多层预制品和多层瓶。
将所得的瓶以与实施例2中相同的方式进行测量。
[实施例8]
除了通过使用石英加热器将预制品从外侧预热至表面温度120℃，在预热预制品时通过将在600℃下加热的铁芯插入预制品8秒来加热预制品和通过使用在150℃下加热的热空气拉伸吹塑成型预制品之外，以与实施例2中相同的方式成型多层预制品和多层瓶。
将所得的瓶以与实施例2中相同的方式进行测量。
[比较例1]
除了通过使用石英加热器在98℃下加热预制品之外，以与实施例1中相同的方式成型多层预制品和多层瓶。所得的瓶的阻挡层泛白。
将所得的瓶以与实施例1相同的方式进行测量。
[比较例2]
除了通过使用石英加热器在100℃下加热预制品，而不进行通过将在530℃下加热的铁芯插入来加热预制品内部之外，以与实施例2中相同的方式成型多层预制品和多层瓶。所得的瓶的阻挡层泛白。
将所得的瓶以与实施例2中相同的方式进行测量。
[比较例3]
除了通过使用石英加热器在95℃下加热预制品之外，以与实施例4中相同的方式成型多层预制品和多层瓶。所得的瓶的阻挡层泛白。
将所得的瓶以与实施例4相同的方式进行测量。
[比较例4]
除了通过使用石英加热器在100℃下加热预制品之外，以与实施例5中相同的方式成型多层预制品和多层瓶。所得的瓶的阻挡层泛白。
将所得的瓶以与实施例5相同的方式进行测量。
[比较例5]
除了通过使用石英加热器在105℃下加热预制品，和在预热预制品时通过将在250℃下加热的铁芯插入预制品10秒来加热预制品之外，以与实施例2中相同的方式成型多层预制品和多层瓶。所得的瓶的阻挡层泛白。
将所得的瓶以与实施例2中相同的方式进行测量。
[比较例6]
通过使用石英加热器在130℃下加热预制品，并在预热预制品时通过将在530℃下加热的铁芯插入预制品10秒来进一步加热。然而，预制品结晶化和泛白，并且不能形成多层瓶。
[比较例7]
除了通过使用石英加热器在105℃下加热预制品，用在140℃下加热的热空气拉伸吹塑成型预制品而不通过使用铁芯加热内部之外，以与实施例3中相同的方式成型多层预制品和多层瓶。所得的瓶的阻挡层泛白。
将所得的瓶以与实施例3相同的方式进行测量。
[比较例8]
除了通过使用石英加热器在105℃下加热预制品，用在230℃下加热的热空气拉伸吹塑形成预制品而不通过使用铁芯加热内部之外，以与实施例3中相同的方式成型多层预制品和多层瓶。该瓶的阻挡层展现不均匀的厚度分布和降低的阻挡性。
将所得的瓶以与实施例3相同的方式进行测量。
[比较例9]
除了通过使用石英加热器在115℃下加热预制品，和在预热预制品时通过将在620℃下加热的铁芯插入预制品10秒来加热预制品之外，以与实施例2中相同的方式成型多层预制品和多层瓶。该瓶的阻挡层展现不均匀的厚度分布和展现降低的阻挡性。
将所得的瓶以与实施例2中相同的方式进行测量。
Figure G2007800522813D00191
Figure G2007800522813D00201

Claims (7)

1.一种多层聚酯容器，其包含聚酯树脂内外层和至少一层功能性树脂中间层，其中所述聚酯内层在0.5Hz下测量其粘弹性时在80℃和60℃下的tanδ之差为0.035以下。
2.根据权利要求1所述的多层聚酯容器，其中当所述功能性树脂的具有厚度1.5mm的注射成型板在115℃下拉伸时，所述功能性树脂具有拉伸应力的最大值为50N以上。
3.根据权利要求1所述的多层聚酯容器，其中所述功能性树脂含有乙烯/乙烯基醇共聚物或聚己二酰间苯二甲胺作为基础树脂。
4.根据权利要求1所述的多层聚酯容器，其中所述功能性树脂含有分散于其中的粘土。
5.根据权利要求1所述的多层聚酯容器，其中所述功能性树脂为环状烯烃树脂。
6.一种多层聚酯容器的生产方法，其通过双轴拉伸吹塑成型多层预制品而生产，所述多层预制品包含聚酯树脂内外层和至少一层功能性树脂中间层，其中在进行双轴拉伸吹塑成型时，将该多层预制品在温度105至120℃下加热，并且将该多层预制品通过使用在300至600℃下加热的加热体和/或150至220℃的热空气内部加热。
7.根据权利要求6所述的多层聚酯容器的生产方法，其中当所述功能性树脂的具有厚度1.5mm的注射成型板在115℃下拉伸时，所述功能性树脂具有拉伸应力的最大值为50N以上。
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