CN1746243A - 高Tg涂料 - Google Patents

高Tg涂料 Download PDF

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Publication number
CN1746243A
CN1746243A CNA2005101098421A CN200510109842A CN1746243A CN 1746243 A CN1746243 A CN 1746243A CN A2005101098421 A CNA2005101098421 A CN A2005101098421A CN 200510109842 A CN200510109842 A CN 200510109842A CN 1746243 A CN1746243 A CN 1746243A
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CN
China
Prior art keywords
coating
phae
phenoxy group
dispersion
class material
Prior art date
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Pending
Application number
CNA2005101098421A
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English (en)
Inventor
赛德·法哈
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Pepsico Inc
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Pepsico Inc
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Publication date
Application filed by Pepsico Inc filed Critical Pepsico Inc
Publication of CN1746243A publication Critical patent/CN1746243A/zh
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    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
    • C09D171/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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    • C08J7/04—Coating
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Abstract

通过把Tg为至少约75℃的高Tg苯氧基－类材料的涂料组合物涂覆于制品表面的至少一部分上而把制品涂覆，并且在制品表面上形成高Tg苯氧基－类材料的干燥/固化涂层，其中涂层含有高Tg苯氧基－类材料和PHAE；或者制品表面包括含有PHAE的涂层；或者涂层含有高Tg苯氧基－类材料和PHAE，并且制品表面包括PHAE的涂层。

Description

高Tg涂料
                            发明背景
发明领域
本发明广泛涉及用于塑料和玻璃制品的涂料。特别地，本发明涉及用于制品例如预成型制品和瓶子的基于苯氧基的涂料，其具有改善的抗化学品、耐磨耗和耐热性能。
相关技术的讨论
层压制品，例如具有至少一层阻气性材料，即具有比基材更小透气性的材料的多层预成型制品和容器是已知的。例如，Farha的美国专利US 5,472,753披露了双层和三层层压制品，例如预成型制品和瓶子。在所披露的三层层压制品中，第一层是苯氧基-类的热塑性塑料，第二层是无定形热塑性共聚酯，并且第三层是聚对苯二甲酸乙二醇酯。在所披露的双层层压制品中，第一层是苯氧基-类的热塑性塑料和无定形热塑性共聚酯的共混物，并且第二层是聚对苯二甲酸乙二醇酯(“PET”)。所披露的苯氧基-类型热塑性塑料包括聚(羟基醚)、聚(羟基酯醚)和聚(羟基氨基醚)，并且优选的无定形热塑性聚酯是聚(1，4-环己基线性亚甲基(cyclohexylinemethylene))对苯二甲酸酯-共聚-间苯二甲酸酯，其通过将PET中的部分乙二醇和对苯二甲酸分别用环己烷二甲醇和间苯二酸代替而形成。同样地，出于所披露的发明的目的，PET指的是PET均聚物以及对苯二甲酸乙二醇酯的共聚物，在该共聚物中，高达约10mol％的乙二醇被其它单体单元例如二甘醇、丙烷-1，3-二醇、丁烷-1，4-二醇、聚丁二醇、聚乙二醇、聚丙二醇、1，4-羟甲基环己烷等代替，并且高达约10mol％的对苯二甲酸被单体单元例如间苯二甲酸、联苯甲酸、萘1，4-或2，6-二羧酸、己二酸、癸二酸、癸烷-1，10-二羧酸等代替。对于预成型品和容器，内层优选PET层。
Hutchinson等人的美国专利US 6,312,641和6,391,408以及美国专利申请No.10/152,318披露了包括一层或多层热塑性材料的塑料制品，例如瓶子和预成型品，其具有优良的气体阻隔性能，以及该制品的制造方法。所披露的塑料制品由热塑性聚酯形成，在该热塑性聚酯上涂覆了阻隔层。优选的热塑性聚酯是PET，但是同样披露了其它热塑性聚酯，即聚2，6-和1，5-萘二甲酸乙二醇酯(“PEN”)，PETG，聚1，2-二氧苯甲酸乙二醇酯以及对苯二甲酸乙二醇酯和间苯二甲酸乙二醇酯的共聚物。对苯二甲酸、间苯二酸和至少一种二醇的共聚酯排除在基体材料之外，因为那些材料被认为是用于本发明目的的阻隔材料。阻隔层由共聚酯阻隔材料，即对苯二甲酸、间苯二甲酸和至少一种二醇的共聚酯，和苯氧基-类热塑性材料，即羟基官能化的聚(酰胺醚)，聚(羟基酰胺醚)，羟基官能化的聚醚，羟基官能化的聚(醚磺酰胺)，聚(羟基酯醚)，羟基-苯氧基醚聚合物和聚(羟基氨基醚)(“PHAE”)形成。除了披露各种注塑技术之外，同样也披露了使用各种浸涂、喷涂和流涂方法涂覆阻隔涂层。
正如本领域技术人员公知的，在制品上形成多个层在一些应用中可能是合乎需要的，但是无论使用什么方法来形成层都增加了复杂性并且，一般地，增加了制造该制品的成本。因此，由于经济的原因，合理限制制品上的层的数目可能是所希望的。因此，特别在为消费商品、材料设计的预成型品和容器内，例如没有经食品及药品管理局(FDA)批准与食品接触的气体阻隔层优选起到作为制品的外层、保护层的双重作用。。
在玻璃和塑料制品的外层上，各种性能是令人希望的。首先，特别是对于容器，例如经受充填输送管外界环境的瓶和罐，容器的外层优选具有优良的抗磨损和耐化学品性，使得制品可以抵抗充填输送管外界环境，其中瓶容易受到物理损耗以及可能是腐蚀性的润滑剂和饮料或者其它的容器内含物的影响。涂覆材料还优选是相容性的，即可与各种着色剂例如颜料和紫外线阻滞剂混溶，使得对于喷涂、浸涂和流涂方法，涂覆材料形成含有颜料或紫外线阻滞剂的稳定分散体。
此外，为吹塑成型热充填容器设计的热塑性预成型品上的涂料的玻璃转化温度(Tg)应该相对地高，因为在吹塑期间预成型品被放入温度约140℃的吹气模具中。结果，具有相对低Tg的外层例如PHAE材料具有粘到吹气模具内表面上的倾向，该PHAE材料具有约50℃-70℃范围的Tg。因此，依靠相对低Tg材料，可能生产具有不可接受的缺陷、损害模具和导致生产线停车时间的最终产品。
人们已经发现将涂覆材料交联改善了它的化学抗性和耐磨性。然而，因为完全交联的热固性材料在吹塑步骤期间不能拉伸，所以我们不能诱发高程度的交联以进行涂覆。其次，低程度的交联不能显著地改善涂料的化学抗性和耐磨性。此外，与将相对低Tg材料吹塑成热充填容器相关的问题仍然持续。
在一些应用中，还希望把紫外线(“UV”)阻滞剂、颜料、或者其它添加剂共混到涂料中。因此，如上所述，添加剂和涂料组合物之间的相容性在此类应用中是关键的。然而，人们已经发现在浸涂、喷涂、和流涂方法，例如由Hutchinson等人披露的那些中，紫外线阻滞剂和颜料与PHAE材料的分散体不相容，由于PHAE材料对添加剂不充足地润湿，其快速地从分散体中沉淀出。
因此，对于涂料组合物存在具有改善的化学品抗性和耐磨性、Tg、以及与颜料和紫外线阻滞剂相容性的低透气性PHAE材料的需要。本发明提供了这样的组合物。
                          本发明的概述
本发明提供了涂覆制品的新方法，用本发明的方法涂覆的制品，本发明方法中使用的涂料组合物，以及克服了现有技术不足的涂覆制品。本发明的方法包括：把包括Tg为至少约75℃，优选约75℃-约110℃的高Tg苯氧基-类材料的涂料组合物涂覆到制品的至少一部分表面，并且在制品表面上形成包括高Tg苯氧基-类材料的干燥/固化的涂层。包括高Tg苯氧基-类材料的涂层进一步包括PHAE，和/或用高Tg苯氧基-类材料涂覆的制品表面包括包含PHAE的涂层。所涂覆的涂料组合物优选是包括高Tg苯氧基-类材料的分散体，其可以进一步包括PHAE。虽然在本发明中苯氧基-类材料分散体是优选的，但也可以使用该材料的溶液。
优选是包括至少一种苯氧基-类材料的分散体的涂料组合物可以进一步包含至少一种添加剂，例如紫外线阻滞剂、颜料、或者金属化的颜料。一些添加剂与PHAE不相容，以致于当分散体没有进一步地包含高Tg苯氧基-类材料时，添加剂从包括添加剂和PHAE的分散体中沉淀出。相反，此类添加剂与包括高Tg苯氧基-类材料的分散体相容，并且从而即使当分散体包括PHAE时也不会发生沉淀。在添加剂与PHAE分散体不相容的情况下，优选的是在把高Tg苯氧基-类材料与PHAE混合形成分散体之前把添加剂与该高Tg苯氧基-类材料混合。
包括高Tg苯氧基-类涂覆材料的涂料组合物可以由浸涂、喷涂和流涂任意一种单独或结合，或者通过优选使用Huthinson披露的注塑-之上-注塑方法(Inject-over-inject)把高Tg苯氧基-类材料重叠注塑到制品上而涂覆。在使用高Tg苯氧基-类材料之前，例如通过重叠注塑、浸涂、喷涂或流涂的任一种方法采用PHAE涂层涂覆将被涂覆的制品，或者在重叠注塑或者浸涂、喷涂或流涂制品之前把高Tg苯氧基-类材料和PHAE例如在挤出机中熔体混合。还可以把这种熔体共混物用来制备树脂分散体，并且通过浸涂、喷涂或者流涂来涂覆。
在其中根据本发明的涂料组合物包括两种树脂的那些应用中，第一种树脂是高Tg苯氧基-类材料，第二种树脂优选是PHAE材料。优选地，在这种树脂共混物中，两种树脂以苯氧基-类材料∶PHAE的重量比为约10∶90-50∶50，更优选约20∶80-40∶60存在，以两种树脂的总重量为基准。组合物可以是适合于浸涂、喷涂或者流涂的两种树脂的分散体，或者是适合于重叠注塑的两种树脂的熔体混合物。
根据本发明的涂覆制品包括具有表面的制品基材，和包括在制品至少一部分表面上的Tg为至少约75℃的高Tg苯氧基-类材料的涂层。包括高Tg苯氧基-类材料的涂层可以进一步地包括PHAE、和/或包括PHAE的涂层可位于在包括高Tg苯氧基-类材料的涂层和制品基材表面之间。
                          附图简述
图1说明了可以用本发明的涂料和方法涂覆的未涂覆的预成型品。
图2说明了图1中所示的预成型品的横截面；
图3说明了本发明的涂覆的预成型品的横截面；
图4说明了本发明的涂覆的预成型品的横截面，其中层的厚度不同于图3中所示的预成型品的层的厚度；
图4A说明了图4的预成型品的一部分壁区段，其中涂层包括多个层；
图5说明了本发明的涂覆的预成型品的横截面，其中全部外表面是被涂覆的；
图6说明了在一类吹塑设备的空腔里预成型品的横截面，此类模塑设备用来制备本发明的涂覆的容器；
图7说明了本发明的涂覆的容器；和
图8说明了图7中所示的涂覆的容器的横截面。
                    优选实施方案的详细说明
本文中使用的术语“苯氧基-类”是指涉及带有末端α二醇基团的聚羟基醚的材料或者树脂。主链醚键和侧羟基促进润湿和结合到极性基材和填料上。一般的苯氧基-类树脂具有大约25,000-超过60,000的重均分子量。平均苯氧基-类树脂分子含有四十或更多个有规则地隔开的适合于交联的侧羟基。
本文中使用的术语“聚羟基氨基醚”(“PHAE”)是指基于环氧的树脂例如双酚A的二缩水甘油醚(“DGEBA”)与伯胺例如乙醇胺的反应产物。据信在PHAE主链上的侧羟基有助于强烈的链间氢键，高的分子间内聚能密度，和优良的气体例如氧气和二氧化碳阻隔性能。文献指出通过将间苯二酚二缩水甘油醚(“RDGE”)与以上提到的组分共聚合可以获得对PHAE阻隔更进一步的改进。出于本披露内容的目的，基于RDGE的PHAE共聚物将同样地被认为是属于PHAE的定义。
本文中使用的术语“高Tg苯氧基-类材料”是指玻璃转化温度为至少约75℃、优选约75℃-约100℃的热塑性苯氧基-类材料。可用于本发明的高Tg苯氧基-类材料具有显著地比PHAE更高的Tg，并且比PHAE显著更好的抗化学品、耐水、和耐磨性。
本发明涉及用于涂覆制品，例如热塑性预成型品和容器以及玻璃制品的组合物，其中涂层具有PHAE细合物的低透气性和由高Tg苯氧基-类材料提供的高Tg、抗化学品性能和耐磨性，以及与添加剂例如紫外线阻滞剂和颜料的相容性。本发明进一步涉及用本发明组合物涂覆的塑料和玻璃制品以及涂覆此类制品的方法。虽然本发明的披露内容特别涉及涂覆的预成型品和容器，但本领域技术人员将知道本发明适用于任何类型的制品，包括但不限于，有涂层的玻璃制品例如瓶子，以及塑料预成型品和容器和其它塑料制品。
已经发现尽管苯氧基-类材料的透气性比PHAE材料的透气性差，但高Tg苯氧基-类材料具有许多优点。特别地，当与PHAE材料相比时，高Tg苯氧基-类材料具有更高的Tg、优良的抗化学品性能和耐磨性、优良的湿润性、提供了与着色颜料的相容性、和与紫外线阻滞剂优良的相容性和混溶性。
如上所述，相对低Tg的PHAE材料可能不适合热吹塑和热充填容器。特别地，当用作预成型品的外层时，Tg为约50℃-70℃的PHAE材料会粘到吹塑之后的模具上。此外，在热充填工序的期间暴露于热液体会损害此类相对低Tg的材料。
此外，尽管可以通过将PHAE材料的分散体浸涂、喷涂或者流涂而使PHAE材料层涂覆到基材上，但PHAE材料的润湿能力是相对差的，并且从而许多添加剂例如颜料和紫外线阻滞剂从PHAE分散体中沉淀出。因此，即使可能，含有某些添加剂例如颜料和紫外线阻滞剂的基于PHAE的涂料仍难以由PHAE材料的分散体形成。
与PHAE材料相反，我们已经发现Tg为约至少75℃的高Tg苯氧基-类材料当暴露于充填管上的热液体和润滑剂时，与基于PHAE材料的涂料相比由于更高的Tg而具有改善的对粘着到吹塑模具上的抗性，并且还具有显著更好的耐化学品性。高Tg苯氧基-类材料上的抗磨损性同样优于不要求交联的PHAE材料。然而，如果需要，只要涂覆材料在拉伸吹塑期间保持膨胀的柔性，则可以使用现有技术中已知的任何可用类型的交联剂，例如基于蜜胺甲醛的交联剂。
还可以通过采用基于水的高Tg苯氧基-类材料的分散体浸涂、喷涂和/或流涂基材的表面而将高Tg苯氧基-类材料涂覆于基材。然而，已经发现：与PHAE材料相比，高Tg苯氧基-类材料优良的湿润性极大地改善了添加剂例如紫外线阻滞剂和颜料与高Tg苯氧基-类材料的相容性。结果，改善抗紫外线性、提供给制品颜色或者提供给制品其它需要的性能的添加剂不会从高Tg苯氧基-类材料分散体中沉淀出。特别地，已经发现在比采用PHAE材料可能的显著更高的荷载下可以把金属化的颜料分散到高Tg苯氧基-类材料中。这允许在基材表面上形成金属化的结构。
虽然基材优选是热塑性材料，例如热塑性聚酯如PET和PEN，但可用于本发明的PHAE和高Tg苯氧基-类材料的分散体也可以用于涂覆玻璃基材。
本发明的方法提供了具有涂层的制品，该涂层提供了PHAE材料和高Tg苯氧基-类材料的优点。换言之，本发明的方法提供了具有PHAE材料的气体阻隔性能和高Tg苯氧基-类材料的相对高的Tg、化学品抗性和耐磨性以及与添加剂的相容性的涂层。
在一个实施方案中，本发明的方法包括：提供PHAE材料的分散体和高Tg苯氧基-类材料的分散体，并且将两种分散体共混。可以添加酸(例如乳酸或磷酸)以稳定分散体。然后通过浸涂、喷涂或者流涂把两种分散体的共混物涂覆于基材表面。由于高Tg苯氧基-类材料与可以提供给最终产品一种或多种需要性能的添加剂，例如紫外线阻滞剂、颜料和金属化的颜料相容，因此本发明的方法可以进一步包括在将两种分散体共混之前把至少一种可用的添加剂共混入高Tg苯氧基-类材料分散体中。
在另一个优选实施方案中，把PHAE和高Tg材料在挤出机里熔融共混。该共混物的分散体可以形成并且涂覆于基材表面，或者熔体共混物可以重叠注塑到基材上，例如通过被Hutchinson披露的注塑-之上-注塑(inject-over-inject)(“IOI”)和注塑-之上-LIM(LIM-over-inject)技术。已经发现添加剂，例如紫外线阻滞剂和颜料可以与熔体共混物混合或者分散在共混物的分散体中。高Tg苯氧基-类材料的存在提供了形成包括一种或多种添加剂的分散体和/或悬浮液所需的相容性。优选地，在加入PHAE材料之前，把任何添加剂加入到分散体中。
在另一个实施方案中，通过将PHAE分散体浸涂、喷涂或者流涂到基材表面上，或者通过直接重叠注塑树脂而在基材上形成单个基于PHAE的层。然后通过浸涂、喷涂或流涂或者通过直接重叠注塑树脂，把包括高Tg苯氧基-类材料、有或者没有一种或多种添加剂的层涂覆于PHAE涂覆的表面上。
作为可以用本发明的方法涂覆以制备本发明的涂覆制品的制品的代表性说明，未涂覆的预成型品示于图1中。本领域技术人员知道本发明不局限于预成型品和由预成型品制造的容器。优选地，预成型品1由FDA批准的材料例如纯的PET形成，并且可以是适合于拉伸-吹塑成容器的任何可用的形状和尺寸。正如本领域技术人员还将知道的那样，用于制造将含有食品或者饮料的容器的预成型品的内表面必须由FDA批准的材料形成。如所说明的那样，预成型品1是用于形成16盎司碳酸饮料瓶的类型，该瓶可以涂有氧气和/或二氧化碳阻隔层。然而，正如本领域技术人员理解的那样，预成型品的尺寸、形状以及厚度将取决于所需的最终制品的尺寸、形状、厚度和用途。优选地，使用本领域已知的注塑技术形成预成型品，但是可以使用将提供所需要的预成型品的可用的模塑法形成。
图2中表示了图1中所示的代表性未涂覆预成型品1的横截面。该未涂覆预成型品1具有颈口部分2和主体部分4。颈口部分确定了到预成型品1内部的开孔18，从开孔18开始并且延伸至支撑圈6并包括支撑圈6。如图1和2中所示，颈口部分2进一步特征在于存在螺纹8，其提供了将用作由预成型品1生产的瓶子的盖子紧固的方式。然而，正如本领域技术人员所知道的那样，可以使用任意已知的用于固定容器例如瓶子的盖子或者顶部的方法。主体部分4是从颈口部分2向下延伸的细长的、圆柱形状结构，具有外表面14并且在圆头盖10中达到顶点。预成型品厚度12将取决于预成型品的全长以及所得容器的壁厚和总尺寸。
图3是根据本发明的非限制性、代表性涂覆预成型品20的横截面的说明，该涂覆预成型品已经根据本发明涂覆；即优选通过采用包括高Tg苯氧基-类材料和PHAE的分散体浸涂、喷涂或者流涂；通过首先采用包括PHAE的分散体，其次采用包括高Tg苯氧基-类材料的分散体浸涂、喷涂或者流涂通过采用PHAE树脂然后高Tg苯氧基-类树脂重叠注塑；或者通过采用PHAE树脂和高Tg苯氧基-类树脂的共混物重叠注塑。该涂覆预成型品20基本上是图1和2中所示的预成型品，但是已经采用了本发明的材料和方法涂覆。正如图1和2中所示的预成型品1那样，涂层预成型品20具有颈口部分2和主体部分4。
把优选是阻隔涂层的涂层22布置于主体部分4全部表面的周围，在支撑圈6底部终止。涂层22没有延伸到颈口部分2，它也不存在于预成型品16的内表面上，如上所述，其优选是由FDA批准的材料例如PET或者PEN制成。涂层22可以包括单一材料或者至少两种材料的几层微层，其中至少一层微层包括高Tg苯氧基-类材料。
整个预成型品26的厚度等于初始预成型品的厚度加上层24的厚度，并且取决于所得容器的总尺寸和所需的涂层厚度。例如，根据本发明的预成型品的预成型品底部的壁厚度可以为3.2毫米；颈口壁的厚度加工为约3毫米；并且阻隔材料层厚度为约0.3毫米。
根据本发明的代表性涂覆制品的另-个实施方案，即涂覆预成型品21，以横截面示于图4中。涂覆预成型品21主要在底部盖子10区域内的两层的相对厚度上不同于图3的涂覆预成型品20。在涂覆预成型品20中，整个预成型品的全部主体部分，涂层通常比初始预成型品的厚度薄。然而在涂覆预成型品21中，涂层22在底部盖子10的点29处比壁部分3的点25处厚；并且相反地，内部热塑性层的厚度在壁部分3里的点23处的厚度比其在底部盖子10的点27处大。当以重叠注塑方法把涂料涂覆于初始预成型品来制造涂覆预成型制品时，该预成型制品设计十分有用，其中存在包括与降低模塑周期时间有关的某些优点。涂层22可以是均质的或者其可以由如上所述并且示于下述图4A中的多个微层组成。
图4A说明了预成型品21的一部分壁区段，其中涂层22包括多个层112。层110是预成型品的内层，并且多个层112形成了预成型品21的外层22。外层112包括多个例如使用由Huthinson披露的多层注塑(“LIM”)技术制得的材料的微层，其中至少一层微层包括高Tg苯氧基-类材料，并且至少一层微层优选包括PHAE，其中，当高Tg苯氧基-类材料和PHAE在单独的层中时，高Tg苯氧基-类材料在PHAE层的外面。正如本领域技术人知道的那样，不是所有示于图4中的类型的预成型品21必须具有包括多个微层的外层，如图4A中所示。
图5以横截面说明了非限定性、代表性涂覆预成型品31的另一个实施方案。涂覆预成型品31主要与分别示于图3和4中的涂覆预成型品20和21不同，因为涂层22布置在颈口部分2以及主体部分4上。
本发明的预成型品和容器的层可以具有因预成型品或者容器而异的相对厚度，以使得在给定的点或者在全部容器上，给定的层的厚度和整个预成型品或容器的厚度可以被选择以适合于涂覆工艺或者容器的特定最终用途。此外，如上所述，在这里所披露的预成型品和容器实施方案中的涂层可以包括单一材料或者两种或多种材料的几个微层。
一般地，涂覆预成型品例如示于图3-5中的那些，经受拉伸吹塑工艺以形成瓶子或者其它容器。如图6中所示，把涂覆预成型品20放入具有与所希望的容器形状相对应的空腔30的吹塑模具28中。把涂覆预成型品20在吹塑模具28中加热和通过垂直地拉伸预成型品并且通过使空气进入预成型品20内部以横向地拉伸预成型品20而在吹塑模具28中膨胀，以使得预成型品20呈现吹塑模具的形状，由此生产涂覆的容器。由于预成型品的外层包括高Tg苯氧基-类材料，因此与PHAE涂覆的容器相比，吹制的容器的粘着量即使没有消除，也显著地降低。吹塑操作通常只限于预成型品的主体部分4，例如包括螺纹、防盗(pilfer)圈和支撑圈的颈口部分2保留原来模塑形成预成型品的形状。
根据本发明的代表性涂覆容器40的一个实施方案示于图7中，其中容器40是由例如示于图3中的涂覆预成型品20模塑的一类。容器40具有对应于图3的涂覆预成型品20的颈口2和主体4部分的颈口部分2和主体部分4。如所说明的那样，颈口部分2进一步特征在于存在螺纹8，其提供了把盖子固定到容器上的方式。
当涂覆容器40以横截面观察时，如图8中所示，可以看出结构。涂层42覆盖了容器40的全部主体部分4的外部，刚好在支撑圈6下面终止。应该由FDA批准的用作消费商品的材料，优选PET制成的容器的内表面50保持无涂覆层，使得仅仅内表面与饮料或者食品接触。在一个实施方案中，为了用于碳酸饮料，容器上涂层的厚度44优选是约0.020-约0.060英寸(约0.51-约1.52mm)，更优选约0.030-约0.040英寸(约0.76-约1.02mm)；内部涂层46的厚度优选约0.080-约0.160英寸(约2.03-约4.064mm)，更优选约0.100-约0.140英寸(约2.540-约3.556mm)；以及涂覆的容器40的整个壁厚48优选约0.140-约0.180英寸(约3.556-约4，572mm)，更优选约0.150-约0.170英寸(约3.810-约4.318mm)。优选地，平均的，容器40的整个壁厚48由内层得到其主要厚度。
如上所述，根据本发明涂覆的预成型品还可以通过以下方式生产：在含有高Tg苯氧基-类和PHAE树脂的分散体的浴液中，或者依次进入含有PHAE分散体的第一种浴液和含有高Tg苯氧基-类材料的分散体的第二种浴液将预成型品浸涂。可以通过使用固定架等人工地把预成型品浸渍到含有树脂的浴液中，或者可以是通过全自动化的方法来完成，该方法可以包括最后的吹塑工艺。
优选地，浴液优选在其中树脂材料分散的水中含有高Tg苯氧基-类材料和PHAE材料的分散体。树脂可以任何形式使用，但是正如大多数材料的情况那样，较小尺寸的颗粒比较大尺寸的颗粒更容易分散。通常，高Tg苯氧基-类材料和PHAE材料形成稳定的基于含水的分散体。如上所述，分散体可以通过加入弱酸例如乳酸或者磷酸而进一步稳定。
本发明的浸涂分散体优选含有约10wt％-约60wt％的树脂，更优选约20wt％-约50wt％的树脂，最优选约30wt％-约40wt％的树脂。浴液中的分散体的温度优选是约0℃-约100℃，更优选约25℃-约50℃。以树脂总重量为基准，高Tg苯氧基-类材料与PHAE的重量比优选为约10∶90-约50∶50；更优选约20∶80-约40∶60，以两种树酯的总重量为基准。
以浸涂制备制品，优选注塑的热塑性预成型品。在制品是注塑的情况下，在注塑工艺的期间，模具在一定的速度下足够快速地冷却以将热塑性树脂保持于非晶态，而不是使得它结晶。通过注塑生产的热塑性制品例如预成型品的方法通常是本领域非常公知的。制品的表面优选不含任何油、表面活性剂、脱模剂等等，以使得涂覆材料可以直接粘着在基材上。
一旦制备所需要的PHAE和高Tg苯氧基-类材料树脂的分散体，则把制品浸渍到浴液中的树脂分散体中以在制品上形成树脂分散体的层。在制品是预成型品的情况下，优选把它浸渍至高达支撑圈6的下面。分散体可以是静止的或者流动的。优选地，将制品在其浸渍到涂料组合物中时旋转。对于1英寸直径的制品，转速优选约30-80rpm，更优选约40rpm-70rpm，并且最优选约50-约60rpm。这使得制品彻底涂覆。正如本领域技术人员知道的那样，按照物体的圆周，对于较大的物体转速优选较慢，并且因此通过分散体的表面的速度与它的直径成正比。例如，在直径翻倍的情况下，转速应该减少1/2。优选把制品浸渍足够的一段时间以允许完全覆盖。尽管取决于应用可以使用较长和较短的周期，但通常仅仅需要约0.25-约5秒。较长的停留时间看起来没有提供任何增加的涂覆效果。因此，优选把预成型品浸入浴液中的树脂分散体中至多约30秒，更优选浸渍约2-约5秒。
然后把制品从浴液中取出，并且干燥直到从分散体中基本上没有液体材料保留在表面涂层上或者表面涂层中。制品可以通过本领域已知的任何方法例如风干、真空干燥、红外线(“IR”)干燥和/或加热而干燥。干燥方法将取决于分散体内的材料和需要的干燥速率。如果需要，可以进行附加的浸渍和干燥步骤以生产附加层。涂层的厚度优选是约0.01-约3mm，并且更优选约0.1-约1mm。优选地，在任何进一步的加工例如吹塑之前将涂覆制品干燥。
在确定浸渍时间并且因此速度中，还应该考虑涂料组合物的混浊度。如果容器浸渍得太快，则涂料组合物会变成波纹状并且溅散而造成涂层缺陷。此外，许多涂料组合物的分散体起泡沫和/或鼓泡，其会妨碍涂覆工艺。为减少或者消除起泡沫和/或鼓泡，优选调节浸渍速度，从而避免涂料组合物的过度搅拌。如果必要，可以把抗起泡沫/鼓泡剂加入涂料分散体。
由浸涂生产的涂覆预成型品优选是图3中所示的类型。把涂层22仅布置于预成型品的主体部分4上，以使得颈口部分2无涂层。在其中由预成型品吹制的容器的内容物将是食品或者饮料的那些应用中，涂覆预成型品16的内部不应该用高Tg苯氧基-类和PHAE树脂涂覆，因为这些材料没有经FDA批准的用于与食品和饮料接触。
根据本发明的涂覆制品也可以通过喷涂获得。根据本发明的方法，用包括高Tg苯氧基-类和PHAE树脂的含水分散体把预成型品或其它制品喷涂，或者用包括PHAE的第一种分散体，然后用包括高Tg苯氧基-类树脂的第二种分散体依次喷涂制品，其中把每一种树脂分散以形成用于浸涂的如上所述类型的含水分散体。制品的喷涂可以人工或通过利用提供用于在一台机器中喷涂和后喷涂处理的装置来完成。
用于喷涂热塑性预成型品的优选装置披露于Kennon等人的美国专利US4,538,542中，其教导内容以描述设备必须的程度在此引入作为参考，并且该装置可从Nordson Corporation，Amherst Ohio商购获得。由Kennon等人披露的装置包括喷涂室，干燥室和用于在这两个室之间移动预成型品的传送带。该装置可以进一步地包括过喷涂回收系统。
优选地，在喷涂工艺中，各制品通过构造的并且适于该目的的装置部分夹紧并被置于传送带上。例如，当预成型品被喷涂时，通过装置把各预成型品的颈口部分夹紧。优选把制品均匀地放置在传送带上，并输送入喷涂室，制品与一系列喷头密切接近而通过喷涂室，该喷涂室优选是不通风的。通过喷嘴喷洒分散体，当各制品预成型品穿过该室时，接触各制品预成型品的外表面，提供湿的涂层。为了促进树脂粘附到制品上，并且为了将分散体中的水性材料蒸发，优选通过本领域已知的任何可用方法在涂覆之前把制品预加热。
正如浸涂那样，优选在用涂料组合物喷涂的期间把制品旋转。同样，1英寸直径的制品优选在约30-80rpm，更优选约40rpm-约70rpm，最优选约50rpm-约60rpm的速度下旋转，其中较大直径的转速按比例减慢。这允许各制品的彻底涂覆。考虑到较大制品的直径，应该调节转速。
优选把制品喷涂足够的一段时间以允许制品的彻底覆盖。尽管取决于制品和涂料组合物而可能需要较长或者较短的时间，但通常约0.25-约5秒是足够的。正如漫涂那样，较长的停留时间没有表现出提供了额外的好处，因此优选在浴液中用树脂分散体把制品喷涂至多约30秒。更优选地把制品喷涂约2-约5秒。
在确定喷涂时间、喷嘴尺寸和结构等等中，应该考虑到涂料组合物的性能。如果喷射速度太高和/或喷嘴尺寸不恰当，涂料组合物可能溅散，造成涂层缺陷。如果速度太缓慢的和/或喷嘴尺寸不恰当，所得的涂层可能比所希望的厚。正如浸涂那样，起泡沫和/或鼓泡还会妨碍涂覆工艺，但是通过选择喷射速度、喷嘴和为避免过度搅拌涂料组合物相关的流体而可以避免起泡沫和/或鼓泡。如果必要，可以把抗起泡沫/鼓泡剂加入到涂料分散体中。
把湿的、喷涂的涂覆制品从喷涂室输送出来进入干燥室，如浸涂那样，干燥室可以包括烘箱、多个加热灯例如红外灯，或者任何其它的热能源，这些将提供蒸发和/或把湿的涂层中的液体排出所必需的温度。正如本领域技术人员所知道的那样，温度不应该足够地高以免涂覆制品的扭曲或者否则破坏涂覆制品。当制品通过干燥室时，把液体蒸发，在预成型品上留下干燥和/或固化的涂层。
在本发明的流涂工艺中，类似于落下的淋浴帘或者瀑布，制品通过PHAE和/或高Tg苯氧基-类材料的流动层(Flowing sheet)。与如上所述的关于喷涂和浸涂方法那样，树脂可以以单个分散体或者依次以单独的分散体一起涂覆。优选地，在涂料组合物的流动中，在短的制品停留时间内发生流涂。制品仅仅需要通过流动层(sheet)足够的时间以涂覆制品的表面。此外，较长的停留时间没有为涂覆带来任何额外的效果。为了提供均匀的涂覆，当制品通过涂料组合物层(sheet)时，优选把制品旋转。同样，1英寸的制品优选在约30-80rpm，更优选约40rpm-约70rpm，最优选约50rpm-约60rpm的速度下旋转，其中较大直径的转速按比例减慢。当制品通过分散体流体时，更优选把制品旋转和置于一定的角度。制品的角度优选与分散体的流动平面成锐角。这有利地允许彻底涂覆制品而不涂覆中空制品的颈口部分或内部。
涂覆材料的分散体优选含于在密闭体系中与生产线流体联通的槽或者其它合适的制品中，并且优选循环以防止浪费任何未使用的涂料组合物。这可以通过把流动的物流返回涂料组合物槽来完成，但是由于起泡沫和鼓泡会妨碍涂覆工艺，优选以避免起泡沫和气泡形成的方式来完成。优选把涂料组合物的分散体从槽底部或者槽中间除去，以防止或者降低起泡沫和鼓泡。另外，为了进一步降低起泡沫和/或鼓泡，在将分散体返回到涂料槽之前优选使分散体的流动减速。这可以通过本领域技术人员公知的方式来完成。如果需要，可以把至少一种消泡剂加入到涂料分散体中。
在选择涂料组合物分散体适当的流速中，为了提供合适的流动层则应该考虑到几个变量，包括流动速率、制品的长度和直径、线速度和制品间距。流动速率确定分散体流动的准确性。如果流动速率太快或者太慢，分散体不能均匀地涂覆制品。当流动速度太快时，材料会溅散和/或冲出生产线，造成制品的涂覆不完全、浪费涂料组合物和增加的起泡沫和/或鼓泡问题。如果流动速度太慢，则涂料组合物仅仅可能部分地涂覆制品。
当选择流速时，也应该考虑到将被涂覆的制品的长度和直径。材料流动层应该彻底覆盖全部制品，因此当制品的长度和直径被改变时，流动速率调节是必须的。本领域技术人员可容易地确定合适的流动速率。
考虑的另一个因素是生产线上的制品的间距。当制品穿过分散体的液流时，可以观察到“尾流影响”。如果一个制品紧跟在另一个制品后面通过分散体液流，则它不能得到合适的涂覆。因此监测制品的速度和轴心线是重要的。制品的速度将取决于所使用的具体设备的产量。
有利地，优选的方法提供了PHAE和/或高Tg苯氧基-类树脂充分有效的沉积，几乎没有过剩的材料需要除去。然而，在某些应用中，在通过浸涂、喷涂、或者流涂方法的任意一种涂覆制品之后必须除去过剩的涂料组合物。优选地，转速和重力将使制品上的流体层归一化，并且除去任何过剩的材料。如果涂料组合物的贮料槽以使得制品在涂覆之后通过槽的方式放置，则制品的旋转和重力应该造成一些过剩的材料从制品滴下回落到涂料组合物槽中。这允许过剩的材料再循环而不需要任何额外的努力。如果槽以其中过剩的材料不能滴落回槽的方式放置，则可以使用任何其它用于收集过剩的材料并且将其回收以重新使用的合适装置。
在以上方法由于生产环境而不实际或者不足够的情况下，可以使用本领域技术人员公知的各种方法和装置以除去过剩的材料。例如，可以单独或者以组合的方式使用擦拭器、刷子、空气刮刀或者气流。另外，这些方法的任何一种可以与上述的旋转和重力法相结合。优选把通过这些方法除去的任何过剩材料再循环以进一步使用。
在制品已经涂覆并且任何的过剩材料除去后，然后把涂覆制品干燥和/或固化。优选地，在干燥和固化过程中使用红外线(“IR”)加热。例如，1000WGeneral Electrics Q1500T3/CL Quartzline钨-卤素石英红外灯是优选的红外源。可以从许多源的任意一种，包括General Electrics和Phillips中商购获得等效的源。为了提供所希望的干燥速度，红外源的强度可以改变，和/或可以使用多个源。
此外，使用红外加热允许涂层干燥而不需要将基材过度加热。也已经发现使用红外加热可以降低泛白并且改善耐化学品性。
虽然在没有额外空气的条件下可以完成固化和/或干燥，但是优选将红外加热同强制空气相结合。所使用的空气可以在任何有效的温度下。红外线和空气固化的结合提供了优选实施方案的优良的耐化学品性、抗泛白性和抗擦痕性能的独特的属性。另外，不希望受任何特别理论的束缚，我们相信涂料的耐化学品性是交联和固化的作用。固化越彻底，耐化学品性和耐擦伤性越好。
在确定彻底干燥和固化涂层所必需的时间长度中，应该考虑几个因素，例如涂覆材料、沉积物厚度和制品基材。不同的涂覆材料在不同的速率下固化。此外，由于固体程度增加，固化速率降低。虽然取决于制品的尺寸、涂层的厚度和固化/干燥法可能需要较长和较短的时间，但是通常，对于有约0.05-约0.75克涂覆材料的制品，固化时间大约为10-120秒。
除红外加热之外使用空气流调节了制品的表面温度，在控制辐射热穿透度中提供了灵活性。如果特定的实施方案需要较慢的固化速率或更深的红外穿透度，则其可以用空气流、红外辐射线的曝光时间、红外灯频率或者它们的组合来控制。
优选地，当将制品干燥时把制品旋转，例如通过暴露于红外加热器的输出能量下。同样，1英寸的制品优选在约30-80rpm，更优选约40rpm-70rpm，并且最优选约50rpm-约60rpm的速度下旋转，其中较大直径的转速按比例减慢。如果转速太高，涂料将飞溅，造成不均匀的制品涂覆。如果转速太低，制品将不均匀地干燥，除非对红外辐射线的暴露均匀分布于制品的涂覆表面上。除了红外线加热之外也可以使用气体加热器，紫外线辐射，燃烧等等或者代替红外线加热。
然后在与固化工艺结合的工艺中把制品冷却，提供了增加的化学品抗性、抗泛白性和耐擦伤性。据信这是由于在单一涂覆之后和在依次涂覆之间除去了挥发物。在一个实施方案中，冷却过程在环境温度下发生。在另一个实施方案中，通过使用加压的大气或者冷空气来加速冷却过程。
冷却时间也受到方法中冷却发生位置的影响。在优选的实施方案中，把多个涂层涂覆于各制品。由于认为提升制品温度加强了涂覆工艺，因此当冷却步骤是在随后的涂覆之前时，可以减少冷却时间。虽然冷却时间改变，但对于24克预成型品、涂层为约0.05-约0.75克的涂层而言，冷却时间通常为约5-约40秒。
尽管已经在上下文的特定实施方案和实施例中披露了本发明，但本领域技术人员将理解本发明在具体披露的实施方案之上扩展到其它选择的实施方案和/或使用明显的改进和其相当方法。因此，本发明并不限于本文中具体披露的优选实施方案。

Claims (17)

1.一种涂覆制品的方法，该方法包括：
把包括Tg为至少约75℃的高Tg苯氧基-类材料的涂料组合物涂覆于制品的至少一部分表面上；和
在制品表面上形成包括高Tg苯氧基-类材料的干燥/固化涂层；其中
包括高Tg苯氧基-类材料的涂料组合物进一步地包括PHAE；或者
制品表面包括含有PHAE的涂层；或者
包括高Tg苯氧基-类材料的涂层进一步地包括PHAE，并且制品表面包括含有PHAE的涂层。
2.根据权利要求1的方法，其中所涂覆的涂料组合物是包括高Tg苯氧基-类材料的分散体。
3.根据权利要求2的方法，其中分散体进一步地包括PHAE。
4.根据权利要求3的方法，其中分散体包括约90wt％-约50wt％的PHAE材料和约10wt％-约50wt％的高Tg苯氧基-类材料，以分散体中的固体总重量为基准。
5.根据权利要求2的方法，其中分散体进一步包括至少一种添加剂。
6.根据权利要求5的方法，其中添加剂包括至少一种紫外线阻滞剂、颜料、交联剂和金属化的颜料。
7.权利要求1的方法，其中制品是热塑性预成型品或者容器。
8.根据权利要求7的方法，其中热塑性制品包括热塑性聚酯。
9.根据权利要求8的方法，其中热塑性聚酯选自于PET、PEN、聚丙烯、及PET和PEN的共混物。
10.根据权利要求1的方法，其中制品包括玻璃。
11.根据权利要求1的方法，其中高Tg苯氧基-类材料的Tg值为约75℃-约110℃。
12.根据权利要求1的方法，进一步包括：
在涂覆步骤之前把PHAE材料的分散体和高Tg苯氧基-类材料的分散体共混以形成PHAE材料和高Tg苯氧基-类材料的分散体。
13.根据权利要求1的方法，进一步包括：
形成PHAE材料和高Tg苯氧基-类材料的熔体共混物；并且分散熔体共混的材料以形成PHAE材料和高Tg苯氧基-类材料的分散体。
14.根据权利要求13的方法，进一步包括通过共挤出高Tg苯氧基-类材料和PHAE材料来形成熔体共混物。
15.根据权利要求1的方法，进一步包括：
形成PHAE材料的分散体，以及使用浸涂、喷涂、或者流涂方法把PHAE分散体涂覆于制品以形成包括PHAE材料的涂层。
16.一种涂料组合物，包括两种树脂，其中：
第一种树脂是高Tg苯氧基-类材料和第二种树脂是PHAE材料；
两种树脂以高Tg苯氧基-类材料：PHAE为约10∶90-约50∶50的重量比存在，以两种树脂的总重量为基准；并且
组合物是适合于浸涂、喷涂或者流涂的两种树脂的分散体的一种，和适合于重叠模塑的两种树脂的熔体共混物。
17.一种涂覆制品，包括：
具有表面的制品基材；和
在制品表面的至少一部分上的包括Tg为至少约75℃的高Tg苯氧基-类材料的涂层；其中
包括高Tg苯氧基-类材料的涂层进一步包括PHAE；或者
包括PHAE的涂层位于包括高Tg苯氧基-类材料的涂层和制品基材表面之间；或者
包括高Tg苯氧基-类材料的涂层进一步包括PHAE，并且包括PHAE的涂层位于包括高Tg苯氧基-类材料的涂层和制品基材表面之间。
CNA2005101098421A 2004-04-07 2005-04-07 高Tg涂料 Pending CN1746243A (zh)

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US20050227083A1 (en) 2005-10-13
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AU2005201453A1 (en) 2005-10-27
AR051164A1 (es) 2006-12-27
CA2502912A1 (en) 2005-10-07
EP1593723A3 (en) 2007-01-10
EP1593723A2 (en) 2005-11-09
RU2005110040A (ru) 2006-10-20
MXPA05003631A (es) 2005-10-11
US7150902B2 (en) 2006-12-19
RU2369624C2 (ru) 2009-10-10
JP2005298821A (ja) 2005-10-27
KR20060046604A (ko) 2006-05-17

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