CN101678935A - 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 PDFInfo
- Publication number
- CN101678935A CN101678935A CN200880018883A CN200880018883A CN101678935A CN 101678935 A CN101678935 A CN 101678935A CN 200880018883 A CN200880018883 A CN 200880018883A CN 200880018883 A CN200880018883 A CN 200880018883A CN 101678935 A CN101678935 A CN 101678935A
- Authority
- CN
- China
- Prior art keywords
- interlayer
- amilan
- polyester container
- multilayered polyester
- polyamide resin
- 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
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Images
Classifications
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D1/00—Containers having bodies formed in one piece, e.g. by casting metallic material, by moulding plastics, by blowing vitreous material, by throwing ceramic material, by moulding pulped fibrous material, by deep-drawing operations performed on sheet material
- B65D1/40—Details of walls
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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Abstract
一种多层聚酯容器，其具有聚酯树脂内外层和至少一层聚酰胺树脂中间层，所述多层聚酯容器的特征在于，在容器体部中，所述聚酰胺树脂中间层具有在差示扫描量热法中伴随结晶的放热峰的开始温度96℃以上，并将粘土分散于聚酰胺树脂中。即使当将由加入有粘土的聚酰胺树脂组成的聚酰胺树脂组合物用于中间层时，也能够有效地防止因老化而产生的中间层白化。因而，能够提供具有优良透明性的多层聚酯容器。
Description
技术领域
本发明涉及多层聚酯容器，其具有通过将粘土分散于聚酰胺树脂获得的聚酰胺树脂组合物中间层。更具体地，本发明涉及能够长期维持优良透明性的多层聚酯容器和用于生产其的方法。
背景技术
为了改进在塑料包装容器中内容物的保存性，迄今已将多层结构用于容器壁，其内外层通过使用聚酯树脂形成，，其中间层通过使用用于改进气体阻隔性的乙烯/乙烯醇共聚物或含亚二甲苯基的聚酰胺树脂气体阻隔性形成或通过使用用于改进水蒸气(水)阻隔性的功能性树脂如环烯烃共聚物水蒸气(水)阻隔性形成(专利文献1)。
此外，已进行努力将功能性树脂与无机填料或其他树脂组合物共混，以进一步改进功能如气体阻隔性或赋予其他功能。例如，以下专利文献2教导了将含亚二甲苯基的聚酰胺与有机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隔性。
专利文献1：JP-A-2005-067637
专利文献2：JP-A-2004-142444
发明内容
本发明要解决的问题
然而，如果在与用于单层聚酯容器的那些相同的条件下将具有上述功能性树脂中间层的多层结构的聚酯容器双轴拉伸吹塑成型，则该容器在长期保存后经历白化，并损害透明性。
特别地，包括通过将粘土分散于聚酰胺树脂中获得的功能性树脂组合物中间层的多层聚酯容器具有拉伸特性，以致在拉伸时产生大的负荷，因此，趋于在该中间层中形成空洞(void)，从成型开始起白化。
因此，本发明的目的是提供多层聚酯容器及其生产方法，尽管使用通过将聚酰胺树脂与粘土共混获得的聚酰胺树脂组合物作为中间层，但所述多层聚酯容器即使随时间流逝后也有效防止白化，并以优良的透明性为特色。
用于解决问题的方案
根据本发明，提供多层聚酯容器，其包括聚酯树脂内外层和至少一层聚酰胺树脂中间层，其中在容器体部中，所述聚酰胺树脂中间层具有通过差示扫描量热法测量的由于结晶导致的放热峰开始温度不低于96℃，并将粘土分散于聚酰胺树脂中。
在本发明的多层聚酯容器中，期望以下：
1.聚酰胺树脂中间层具有不高于9J/g的由于结晶导致的放热峰；
2.聚酰胺树脂为聚己二酰间苯二甲胺；
3.聚酰胺树脂中间层具有厚度小于20μm；和
4.聚酯树脂内层具有结晶度为不小于23％，其外层具有结晶度不小于18％，内层结晶度和外层结晶度的平均值不小于24％。
此外，根据本发明，提供通过双轴拉伸吹塑成型多层预制品来生产多层聚酯容器的方法，所述多层预制品包括聚酯树脂内外层和至少一层分散粘土的聚酰胺树脂中间层，在所述方法中将所述多层预制品在110至120℃的温度加热下双轴拉伸吹塑成型，从而将多层聚酯容器成型，所述聚酰胺树脂中间层具有通过差示扫描量热法测量的由于结晶导致的放热峰开始温度不低于96℃。
发明的效果
根据本发明的多层聚酯容器，用作中间层的含粘土聚酰胺树脂组合物显示优良气体阻隔性，即使经过时间流逝后也有效地防止白化并且长期维持优良的透明性。
此外，根据用于生产本发明的多层聚酯容器的方法，不需要用于生产耐热性聚酯容器的方法所需要的热定形步骤，可将在容器体部中含粘土聚酰胺树脂组合物中间层的通过DSC测量的放热峰开始温度设定为不低于96℃，并使得可以生产有效防止由老化导致的白化的多层聚酯容器。
附图说明
[图1]为说明本发明多层聚酯容器的截面结构的图。
[图2]为说明本发明多层聚酯容器的截面结构的图。
具体实施方式
根据本发明，重要的特征在于，多层聚酯容器具有包括聚酯树脂内外层和至少一层含粘土聚酰胺树脂组合物中间层的多层结构，在所述多层聚酯容器中，在容器体部中，所述含粘土聚酰胺树脂组合物中间层具有通过差示扫描量热法(DSC)测量的由于结晶导致的放热峰开始温度不低于96℃。
如上所述，通过将聚酰胺树脂与粘土共混获得的含粘土聚酰胺树脂组合物具有如拉伸时产生大的负荷等特性。因此，如果多层聚酯容器通过与生产常规多层聚酯容器相同的方法成型，则所述容器趋于从成型开始起白化，当容器长期保存时白化进一步发生，损害透明性。
由于认为上述问题起因于在多层聚酯容器中的中间层的结晶，本发明人已尝试将在容器体部中通过差示扫描量热法测量的由于含粘土聚酰胺树脂组合物中间层的结晶导致的放热峰开始温度设定为不低于96℃。结果，本发明人已发现，即使在上述多层聚酯容器中，也不发生上述问题。
即，根据本发明的多层聚酯容器，含粘土聚酰胺树脂组合物中间层具有通过差示扫描量热法测量的由于结晶导致的放热峰开始温度不低于上述值，由此可知结晶在多层聚酯容器的中间层中得到促进，因此，留下很少的在随后的环境条件下能够结晶的无定形部分，即，中间层具有很少的能够结晶的结构。因此，即使在长期保存后，也抑制在本发明的多层聚酯容器中的中间层结晶，因此，能够长期维持成型时的起始透明性。
从稍后描述的实施例的结果，本发明的作用和效果将变得显而易见。
即，在含粘土聚酰胺树脂组合物中间层具有通过DSC测量的放热峰开始温度不低于上述值的本发明的多层聚酯容器中，容器的雾度降低或抑制增大，在50℃、80％RH、72小时下进行的老化测试中维持透明性(实施例1至5)，同时在通过DSC测量的放热峰开始温度低于上述值的多层聚酯容器中，雾度增大并损害透明性(比较例1至3和5)。
此外，在本发明的多层聚酯容器中，期望由于含粘土聚酰胺树脂组合物中间层的结晶导致的放热峰为不高于9J/g。即，不高于9J/g的由于结晶导致的放热峰表示在通过结晶温度时能够结晶的无定形组分的量，即，表示能够结晶的无定形组分的量。即，不高于9J/g的值意味着在聚酰胺树脂的无定形组分中相当大部分能够结晶的那些已结晶，或推测为像当结晶开始温度为不低于96℃时的情况一样几乎不结晶的结构。
此外，在本发明的多层聚酯容器中，特别期望在容器体部中，聚酯容器的内层具有结晶度不小于23％，其外层具有结晶度不小于18％，并且所述内层的结晶度与所述外层的结晶度的平均值不小于24％。即，具有不小于上述值的结晶度的聚酯树脂内层和外层几乎不允许水渗透入中间层中。因此，在中间层中的分子移动得到抑制，有效地抑制长期保存后由于结晶导致的中间层的白化，并能够维持更优良的透明性。
根据本发明，形成内外层的聚酯树脂的结晶度χc通过密度法测量，即，根据下式计算，
χc＝[dc(d-da)/d(dc-da)]×100
其中da为完全无定形的聚酯树脂的密度，dc为理论上完全结晶的聚酯树脂的密度，d为样品的密度。
当具有上述特征的本发明的多层聚酯容器通过用于生产多层聚酯容器的方法通过双轴拉伸吹塑成型多层预制品并通过在110至120℃的温度下加热该多层预制品来获得时，在拉伸时将应力释放在含粘土聚酰胺树脂组合物中，并且由于添加粘土导致促进结晶，所述多层预制品包括聚酯树脂内外层和至少一层含粘土聚酰胺树脂组合物中间层。
即，当本发明的多层聚酯容器通过双轴拉伸吹塑成型预制品同时在上述温度范围内将其加热来获得时，含粘土聚酰胺树脂组合物内层显示通过差示扫描量热法测量的由于结晶导致的放热峰开始温度不低于上述值(实施例1至5)。当多层聚酯容器通过根据生产多层聚酯容器的常规方法双轴拉伸吹塑成型预制品同时在低于110℃的温度下将其加热来获得时，中间层显示通过差示扫描量热法测量的由于结晶导致的放热峰开始温度低于上述值。结果，长期保存后损害透明性(比较例1、2、3和5)。
(中间层)
本发明的聚酯容器的中间层使用通过将粘土分散于聚酰胺树脂中获得的含粘土聚酰胺树脂组合物。
即，聚酰胺树脂显示优良的气体阻隔性，但也在伸长时产生大的应力，在伸长时趋于损失功能如透明性和气体阻隔性。此外，如果将粘土分散于聚酰胺树脂中，则比单独聚酰胺树脂在伸长时产生更大的应力，由于形成空洞而损害功能如透明性和气体阻隔性。因此，如本发明预期的，特别期望实现改进。
作为用于本发明的聚酰胺树脂，可优选使用以下聚酰胺，所述聚酰胺通过包括己二酰间苯撑二甲胺作为主要组分的二胺组分与包括具有4至20个碳原子的α，ω-直链脂肪族二羧酸作为主要组分的二羧酸组分的缩聚来获得。作为具有4至20个碳原子的α，ω-直链脂肪族二羧酸，可示例脂肪族二羧酸如琥珀酸、戊二酸、庚二酸、辛二酸、壬二酸、己二酸、癸二酸、十一烷二酸和十二烷二酸。
在本发明中，特别当使用在伸长时产生大应力并具有优良气体阻隔性的聚己二酰间苯二甲胺或聚癸二酰间苯二甲胺(polymetaxylylenesebacamide)时，特别明显地显示优良的作用和效果。
作为粘土，可使用云母、蛭石和绿土，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2-八面体型的层状硅酸盐，可示例蒙脱石、贝得石和囊脱石。作为3-八面体型的层状硅酸盐，可示例锂蒙脱石和三八面体蒙脱石(suponite)。
从气体阻隔性角度，用于本发明的粘土特别期望为用有机性赋予剂(organic property-imparting agent)溶胀化处理的粘土。在此情况下，在上述粘土中，蒙脱石具有高溶胀性，由于有机性赋予剂的浸透，溶胀在该层间扩展。
作为有机性赋予剂，可优选使用季铵盐。更优选地，可使用具有至少一个或多个包含有不少于12个碳原子的烷基的季铵盐，如三甲基十二烷基铵盐和三甲基十四烷基铵盐。
期望含粘土聚酰胺树脂组合物以每100重量份聚酰胺树脂功能性树脂为1至10重量份，特别地1至8重量份的比例包含粘土。如果粘土的量小于上述范围，与当以在上述范围内的量添加粘土时相比，通过添加粘土不能充分获得气体阻隔性。另一方面，如果粘土的量大于上述范围，成型性变得比当以上述范围内的量添加粘土时差。
此外，可将所述含粘土聚酰胺树脂组合物与氧化性有机组分和过渡金属催化剂组合共混，以赋予其氧吸收性。
作为氧化性有机组分，可示例在侧链上或在其末端具有官能团并且能够被氧化的那些。具体地，可示例用酸或酸酐改性的多烯低聚物或聚合物，如丁二烯和用无水马来酸改性的丁二烯。作为过渡金属催化剂，可使用元素周期表第VIII族的金属组分，如铁、钴和镍，然而，本发明绝不仅限于这些。
期望氧化性有机组分以每100重量份功能性树脂为2至10重量份的量共混，过渡金属催化剂以作为金属计算的至少300ppm的量共混。
用于本发明的聚酰胺树脂可根据已知配方与以下物质在它们不损害本发明目的的范围内共混：粘土以及氧化性组分与过渡金属催化剂组合，和已知树脂共混剂(blending agents)如脱氧剂(disoxidant)、填料、着色剂、热稳定剂、老化稳定剂、抗氧化剂、防老剂、光稳定剂、紫外线吸收剂、抗静电剂、润滑剂如金属皂或蜡，以及改质(reforming)树脂或橡胶。
(内外层)
作为用于本发明的内外层的聚酯树脂，可使用已知包括二羧酸组分和二醇组分的聚酯树脂。
作为二羧酸组分，从机械性质和热性质的观点，期望不低于50％，特别地，不低于80％的二羧酸组分为对苯二甲酸。然而，自然，可包含除了对苯二甲酸之外的羧酸组分。作为除了对苯二甲酸之外的羧酸组分，可示例间苯二酸、萘二羧酸、对-β-氧乙氧基苯甲酸、联苯基-4，4’二羧酸、二苯氧基乙烷-4，4’-二羧酸、间苯二酸5-磺酸钠(5-sodiumsulfoisophthalic acid)、六氢对苯二甲酸、己二酸和癸二酸。
作为二醇组分，从机械性质和热性质的观点，期望不低于50％，特别地，不低于80％的二醇组分为乙二醇。作为除乙二醇之外的二醇组分，可示例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的环氧乙烷加合物、甘油和三羟甲基丙烷。
此外，上述二羧酸组分和二醇组分可包含三官能以上的高官能多元酸和多元醇；即，多元酸如偏苯三酸、均苯四酸、苯三甲酸、1，1，2，2-乙烷四羧酸、1，1，2-乙烷三羧酸、1，3，5-戊烷三羧酸、1，2，3，4-环戊烷四羧酸和联苯基-3，4，3’，4’-四羧酸，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。
期望用于本发明的内外层的聚酯树脂具有通过使用重量比1∶1的苯酚/四氯乙烷混合溶剂在30℃下测量的固有粘度在0.60至1.40dL/g范围内。此外，期望聚酯树脂具有200至275℃的熔点(Tm)，以改进多层容器的耐热性和加工性。此外，期望聚酯树脂具有不低于30℃，特别地，在50至120℃的范围内的玻璃化转变点。
用于本发明的内外层的聚酯树脂可根据已知配方，与例如以下的已知树脂用共混剂在它们不损害最终成型制品的品质范围内共混：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。
(多层结构)
本发明的多层聚酯容器可采用各种层构造，只要其包括聚酯树脂内外层和至少一层共混有粘土的功能性树脂组合物中间层即可。该层构造可具有如图1所示在聚酯树脂内层1与外层2之间的含粘土聚酰胺树脂组合物中间层3。或者，如图2所示，该层构造可包括聚酯树脂内层1和外层2，以及插入聚酯树脂内层1与聚酯树脂中间层4之间，和聚酯树脂的外层2与聚酯树脂中间层4之间的两层含粘土聚酰胺树脂组合物中间层3a、3b。
在生产多层容器中，虽然通常不需要，但可将粘结剂树脂插入树脂层之间。作为粘结剂树脂，可示例热塑性树脂，所述热塑性树脂以1至700毫当量(meq)/100g树脂，特别地，10至500meq/100g树脂的浓度在主链或侧链上包含基于羧酸、羧酸酐、羧酸盐、羧酸酰胺或羧酸酯的羰基(-CO-)。粘结剂树脂的优选实例包括乙烯/丙烯酸共聚物、离子化交联的烯烃共聚物、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合的聚酯。
在本发明的多层聚酯容器中，期望容器体部具有200至600μm，特别地，240至500μm的总厚度，尽管其可依赖于容器的体积(重量)和容器的用途而改变。
重要的是，从容器的透明性的观点，作为中间层的包括含粘土聚酰胺树脂组合物的层的厚度小于20μm，特别地为5至15μm，并且该中间层的厚度为容器体部总厚度的3至10％。
如果使多个包括含粘土聚酰胺树脂组合物中间层存在，期望各中间层具有厚度小于20μm，特别地为5至15μm，中间层作为整体具有容器体部总厚度的3至20％的厚度。
(生产方法)
可通过以下方式生产本发明的多层聚酯容器：使具有上述多层结构的预制品成型，在110至120℃，特别是112至118℃的高温下加热该预制品，沿轴向拉伸牵引该预制品，同时，沿周向吹塑拉伸该预制品。
多层预制品可通过例如以下的已知成型方法来生产：共挤出成型法，其将含粘土聚酰胺树脂组合物和聚酯树脂一起共挤出；同时注塑成型法，其将含粘土树脂组合物和聚酯树脂同时注入金属模具中；顺序注塑法，其将聚酯树脂、含粘土聚酰胺树脂组合物和聚酯树脂顺序注入金属模具中；压缩成型法，其通过使用芯金属模具和腔金属模具将含粘土聚酰胺树脂组合物和聚酯树脂的共挤出产物压缩成型。
当采用这些体系的任何一种时，成型的预制品应在过冷状态下，即，在无定形状态下，期望将包括含粘土聚酰胺树脂组合物中间层封入热塑性聚酯内外层中。
期望通过如上所述的冷型坯体系进行成型多层预制品和拉伸吹塑成型多层预制品。然而，也允许通过热型坯体系进行拉伸吹塑成型而不完全冷却成型的多层预制品。
在进行拉伸吹塑成型之前，通过如热风、红外线加热器或高频诱导加热等手段将预制品预热至拉伸温度。此处，根据本发明，将预制品通过在高于常规拉伸吹塑成型温度的温度下，即，在110至120℃下，特别地在112至118℃下加热来拉伸吹塑是特别重要的。如果预制品的温度低于上述温度，包括含粘土聚酰胺树脂组合物中间层在伸长时产生大的应力，因此，不能预期由于拉伸取向导致结晶的促进，长期保存后透明性降低，容易产生空洞，并且获得的聚酯容器的透明性劣化。另一方面，如果预制品的温度高于上述范围，则预制品软化，在拉伸吹塑成型时偏离预制品的中心，劣化成型性。因此，获得的聚酯容器的厚度变得不均匀，预制品在拉伸吹塑成型前结晶，不能再成型。
将已加热的预制品进给至公知的拉伸吹塑成型机中，并设置在金属模具中，通过推入拉伸棒而沿轴向牵引和拉伸，并通过吹动流体沿周向拉伸。此处，在本发明中，期望通过使用在300至600℃下加热的加热体和/或通过使用150至220℃、特别是170至210℃的热风加热多层预制品内部。
即，在双轴拉伸吹塑成型在上述范围内的温度下加热的预制品时，预制品的内部通过插入在高温下加热的加热体和/或通过吹送高温热风来加热，由此预制品内部的温度变得更高，预制品中的温度在拉伸吹塑成型时维持得很高，促进其应变的松弛以及松弛在伸长时产生大的应力的包括含粘土聚酰胺树脂组合物中间层应变，抑制空洞形成，而不损害功能如透明性和气体阻隔性气体阻隔性。
在本发明中，期望加热体和热风的温度在上述范围内。如果该温度低于上述范围，则预制品的内部没有加热到足够的程度，不能够有效地促进应变的松弛。另一方面，如果该温度高于上述范围，内聚酯层和含粘土聚酰胺树脂组合物层由于结晶导致白化并且不均匀地拉伸，或含粘土聚酰胺树脂组合物层不均匀地拉伸，成型不良。
期望用于内部加热的时间依赖于预热预制品的温度和用于内部加热的加热体的设定温度而改变，并优选8至20秒，特别地10至15秒。此外，期望将用于拉伸吹塑成型的热风吹入设置在金属模具中的预制品2至3秒。
作为最终产品的多层聚酯容器的拉伸比优选作为面积比为1.5至25倍，作为沿轴向的拉伸比为1.2至6倍，作为沿周向的拉伸比为1.2至4.5倍。
当用于需要耐热性的用途时，拉伸吹塑成型瓶可通过已知手段热定形。热定形可在基于一步成型方法的吹塑成型金属模具中进行，或者也可在基于两步成型方法的与吹塑成型金属模具分离的热定形用金属模具中进行。用于热定形的温度期望为100至200℃。
作为其它拉伸吹塑成型，可示例与本申请相关的已审专利文献：JP-B-2917851中的两步拉伸吹塑成型，其中通过使用初次吹塑金属模具将预制品成型为比最终吹塑成型体尺寸大的初次吹塑成型体，接着，将初次吹塑成型体加热收缩，其后，通过借助于使用二次吹塑金属模具的双轴拉伸吹塑成型将其成型为最终吹塑成型体。拉伸吹塑成型使得可以通过拉伸来降低底部的厚度至充分的程度，并获得具有特征为在热填充(hottingfiting)和通过加热灭菌时优良抗变形性和抗冲击性的底部的吹塑成型体。
根据本发明，重要的是：即使当采用两步拉伸吹塑成型时，在初次吹塑成型期间在高达110至120℃的温度下加热预制品。
本发明的多层聚酯容器具有气体阻隔性，可用作防止内容物味道通过例如氧导致降低的容器。作为可填充的内容物，可示例以下：饮料，如啤酒、葡萄酒、果汁、碳酸软饮料、含果汁的碳酸饮料等；食物，如水果、坚果、蔬菜、肉类制品、婴儿食品、咖啡、果酱、蛋黄酱、番茄酱、食用油、调料、酱油、大豆煮制食品、牛奶制品等；以及在氧存在下经历劣化的药品、化妆品、汽油等，然而，用途绝不仅限于这些。
实施例
将通过以下实施例进一步描述本发明，然而，该实施例不限制本发明。
[测量放热峰开始温度和放热峰]
将包括含粘土聚酰胺树脂组合物中间层从获得的多层容器的体部中央和从其肩部剥离。精确地称量其约8mg，并密封在由该设备规定的铝盘中。通过使用差示扫描量热计[DSC7差示扫描量热计：由PERKIN ELMER Co.制造]，将该铝盘在10℃/分钟的速率下从20℃加热至280℃，以获得显示由于结晶导致的放热峰的图表。从该图表，读取放热峰开始温度。此外，从该峰面积得到放热峰(J/g)。
[测量结晶度]
将宽度5mm和长度5mm的试验片从获得的多层瓶的容器体部中央切出。将内聚酯层和外聚酯层从试验片剥离。将样品浸渍于在20℃下的水/硝酸钙型密度梯度管中2小时，其后，读取样品的位置以求得试验片的密度d(g/cm3)。结晶度χc(％)根据下式从获得的密度求得，
χc＝[1.455×(d-1.335)/(d×(1.455-1.335))]×100
其中1.335为完全无定形的聚对苯二甲酸乙二酯树脂的密度，1.455为理论上完全结晶的聚对苯二甲酸乙二酯树脂的密度。
[测量雾度]
将宽度30mm和长度40mm的试验片从刚成型后的多层瓶和在50℃和80％RH的环境中保存72小时后的多层瓶的体部中央切出。通过使用彩色(color)计算机[S & M COLOURCOMPUTER MODEL SM-4：由Suga Shikenki Co.制造]测量它们的多层形式试验片的雾度。
[实施例1]
通过使用装配有三个注塑机，即，用于PET内外层的注塑机(a)，用于中间PET层的注塑机(b)和用于含粘土聚酰胺树脂组合物的注塑机(c)的共注塑成型机，通过将在150℃下干燥4小时的聚对苯二甲酸乙二酯(PET)树脂[BK6180，由Nihon UnipetCo.制造]进给至注塑机(a)和(b)中，并通过将通过借助于使用双轴挤出机熔融捏合聚己二酰间苯二甲胺树脂(MXD6)[T620，由Nihon Unipet Co.制造]和3重量％的溶胀化处理的天然蒙脱石获得的含粘土聚酰胺树脂组合物进给至注塑机(c)，通过顺序注塑成型法获得具有PET的内外层和中间层以及在它们中的含粘土聚酰胺树脂组合物的层的两种五层(a/c/b/c/a)多层预制品，其重量为33g。
通过使用石英加热器，将预制品从其外部预热至119℃的表面温度，并在纵向为3.0倍和横向为3.0倍的拉伸比下双轴拉伸吹塑成型，从而获得多层瓶，所述多层瓶具有体积为516ml，以及在体部中各层的厚度，即内PET层(110μm)/内含粘土聚酰胺树脂组合物层(18μm)/中间PET层(80μm)/外含粘土聚酰胺树脂组合物层(17μm)/外PET层(140μm)。
测量获得的瓶的内含粘土聚酰胺树脂组合物层的放热峰开始温度和放热峰、内PET层和外PET层的结晶度及其雾度。
[实施例2]
除了在111℃下预热多层预制品，以致在其容器体部中的层具有厚度为内PET层(100μm)/内含粘土聚酰胺树脂组合物层(9μm)/中间PET层(110μm)/外含粘土聚酰胺树脂组合物层(11μm)/外PET层(130μm)之外，以与实施例1相同的方式成型多层瓶，并测量其结晶峰、结晶度和雾度。
[实施例3]
除了在113℃下预热多层预制品，以致在其容器体部中的层具有厚度为内PET层(110μm)/内含粘土聚酰胺树脂组合物层(17μm)/中间PET层(80μm)/外含粘土聚酰胺树脂组合物层(15μm)/外PET层(140μm)之外，以与实施例1相同的方式成型多层瓶，并测量其结晶峰、结晶度和雾度。
[实施例4]
除了在116℃下预热多层预制品，以致在其容器体部中的层具有厚度为内PET层(100μm)/内含粘土聚酰胺树脂组合物层(10μm)/中间PET层(110μm)/外含粘土聚酰胺树脂组合物层(10μm)/外PET层(130μm)之外，以与实施例1相同的方式成型多层瓶，并测量其结晶峰、结晶度和雾度。
[实施例5]
除了在117℃下预热多层预制品，以致在其容器体部中的层具有厚度为内PET层(100μm)/内含粘土聚酰胺树脂组合物层(7μm)/中间PET层(110μm)/外含粘土聚酰胺树脂组合物层(6μm)/外PET层(130μm)之外，以与实施例1相同的方式成型多层瓶，并测量其结晶峰、结晶度和雾度。
[比较例1]
除了在109℃下预热多层预制品，以致在其容器体部中的层具有厚度为内PET层(100μm)/内含粘土聚酰胺树脂组合物层(15μm)/中间PET层(100μm)/外含粘土聚酰胺树脂组合物层(14μm)/外PET层(130μm)之外，以与实施例1相同的方式成型多层瓶，并测量其结晶峰、结晶度和雾度。
[比较例2]
除了在其容器体部中的层具有厚度为内PET层(100μm)/内含粘土聚酰胺树脂组合物层(22μm)/中间PET层(80μm)/外含粘土聚酰胺树脂组合物层(24μm)/外PET层(100μm)之外，以与实施例1相同的方式成型多层瓶，并测量其结晶峰、结晶度和雾度。
[比较例3]
除了在106℃下预热多层预制品，以致在其容器体部中的层具有厚度为内PET层(100μm)/内含粘土聚酰胺树脂组合物层(10μm)/中间PET层(110μm)/外含粘土聚酰胺树脂组合物层(8μm)/外PET层(130μm)之外，以与实施例1相同的方式成型多层瓶，并测量其结晶峰、结晶度和雾度。
[比较例4]
除了在123℃下预热多层预制品之外，试图以与实施例1相同的方式成型多层瓶。然而，由于预制品的结晶不能成型该多层瓶。
[比较例5]
通过使用装配有以下两个注塑机，即，用于内PET层和外PET层的注塑机(a)和用于含粘土聚酰胺树脂组合物中间层的注塑机(b)的共注塑成型机，通过将在150℃下干燥4小时的聚对苯二甲酸乙二醇酯(PET)树脂[BK6180，由Nihon Unipet Co.制造]进给至注塑机(a)中，并通过将通过借助于使用双轴挤出机熔融捏合聚己二酰间苯二甲胺树脂(MXD6)[T620，由Nihon UnipetCo.制造]和3重量％的溶胀化处理的天然蒙脱石获得的含粘土聚酰胺树脂组合物进给至注塑机(b)，通过顺序注塑成型法获得具有PET的内外层和在它们之间的含粘土聚酰胺树脂组合物中间层的两种三层(a/b/a)多层预制品，其重量为28g。
通过使用石英加热器，将预制品从其外部预热至105℃的表面温度，并在纵向为2.0倍和横向为3.1的拉伸比下双轴拉伸吹塑成型，从而获得多层瓶，所述多层瓶具有体积为523ml，在容器体部中各层的厚度，即内PET层(200μm)/内含粘土聚酰胺树脂组合物层(25μm)/外PET层(180μm)。
测量获得的瓶的内含粘土聚酰胺树脂组合物层的放热峰开始温度和放热峰、内PET层和外PET层的结晶度和雾度。
[比较例6]
除了不将聚己二酰间苯二甲胺树脂(MXD6)[T620，由NihonUnipet Co.制造]与粘土共混，并如此成型预制品，以具有厚度为内PET层(100μm)/内MXD层(12μm)/中间PET层(100μm)/外MXD6层(12μm)/外PET层(120μm)之外，以与实施例3相同的方式成型多层瓶，并测量其结晶峰、结晶度和雾度。
Claims (6)
1.一种多层聚酯容器，其包括聚酯树脂内外层和至少一层聚酰胺树脂中间层，其中在所述容器体部中，所述聚酰胺树脂中间层具有通过差示扫描量热法测量的由于结晶导致的放热峰开始温度不低于96℃，将粘土分散于所述聚酰胺树脂中。
2.根据权利要求1所述的多层聚酯容器，其中所述聚酰胺树脂中间层具有不高于9J/g的由于结晶导致的放热峰。
3.根据权利要求1所述的多层聚酯容器，其中所述聚酰胺树脂为聚己二酰间苯二甲胺。
4.根据权利要求1所述的多层聚酯容器，其中所述聚酰胺树脂中间层具有厚度小于20μm。
5.权利要求1所述的多层聚酯容器，其中所述聚酯树脂内层具有结晶度不小于23％，其外层具有结晶度不小于18％，所述内层的结晶度和所述外层的结晶度的平均值不小于24％。
6.一种用于生产多层聚酯容器的方法，所述多层聚酯容器通过双轴拉伸吹塑成型多层预制品来生产，所述多层预制品包括聚酯树脂内外层和至少一层分散粘土的聚酰胺树脂中间层，其中，将所述多层预制品在110至120℃的温度加热下双轴拉伸吹塑成型，以将多层聚酯容器成型，其中，所述聚酰胺树脂中间层具有通过差示扫描量热法测量的由于结晶导致的放热峰开始温度不低于96℃。
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2008
- 2008-04-02 KR KR1020097021759A patent/KR101509828B1/ko active IP Right Grant
- 2008-04-02 JP JP2009509279A patent/JP5240189B2/ja active Active
- 2008-04-02 EP EP08739703.0A patent/EP2130783A4/en not_active Withdrawn
- 2008-04-02 US US12/594,171 patent/US20100206762A1/en not_active Abandoned
- 2008-04-02 WO PCT/JP2008/056592 patent/WO2008126745A1/ja active Application Filing
- 2008-04-02 CN CN2008800188831A patent/CN101678935B/zh active Active
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| CN102892835A (zh) * | 2010-05-17 | 2013-01-23 | 三菱瓦斯化学株式会社 | 聚酰胺树脂组合物 |
| CN102906197A (zh) * | 2010-05-17 | 2013-01-30 | 三菱瓦斯化学株式会社 | 聚酰胺树脂组合物 |
| CN102892835B (zh) * | 2010-05-17 | 2015-07-01 | 三菱瓦斯化学株式会社 | 聚酰胺树脂组合物 |
| CN102906197B (zh) * | 2010-05-17 | 2015-07-22 | 三菱瓦斯化学株式会社 | 聚酰胺树脂组合物 |
| CN104893286A (zh) * | 2010-05-17 | 2015-09-09 | 三菱瓦斯化学株式会社 | 聚酰胺树脂组合物 |
| US9657159B2 (en) | 2010-05-17 | 2017-05-23 | Mitsubishi Gas Chemical Company, Inc. | Polyamide resin composition |
| CN104893286B (zh) * | 2010-05-17 | 2017-09-15 | 三菱瓦斯化学株式会社 | 聚酰胺树脂组合物 |
| CN109383004A (zh) * | 2017-08-11 | 2019-02-26 | 赫斯基注塑系统有限公司 | 模塑制品、容器以及在其上印刷的方法 |
| CN109383004B (zh) * | 2017-08-11 | 2022-01-11 | 赫斯基注塑系统有限公司 | 模塑制品、容器以及在其上印刷的方法 |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2130783A1 (en) | 2009-12-09 |
| JPWO2008126745A1 (ja) | 2010-07-22 |
| JP5240189B2 (ja) | 2013-07-17 |
| EP2130783A4 (en) | 2015-10-28 |
| CN101678935B (zh) | 2012-03-28 |
| KR101509828B1 (ko) | 2015-04-06 |
| KR20090125273A (ko) | 2009-12-04 |
| US20100206762A1 (en) | 2010-08-19 |
| WO2008126745A1 (ja) | 2008-10-23 |
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