CN101778881B - 用于铝基材之上的电沉积涂层 - Google Patents

用于铝基材之上的电沉积涂层 Download PDF

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CN101778881B
CN101778881B CN2008801029847A CN200880102984A CN101778881B CN 101778881 B CN101778881 B CN 101778881B CN 2008801029847 A CN2008801029847 A CN 2008801029847A CN 200880102984 A CN200880102984 A CN 200880102984A CN 101778881 B CN101778881 B CN 101778881B
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J·T·沃克
R·M·派弗尔
C·A·威尔逊
A·J·开罗
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Abstract

一种通过阴离子电沉积磷酸化环氧树脂而在铝基材上施加涂层的方法，所述磷酸化环氧树脂通过用磷酸与有机膦酸和/或有机次膦酸使得聚合型环氧化物磷酸化而制得。所述涂层具有降低的形成针孔的倾向。

Description

用于铝基材之上的电沉积涂层
技术领域
本发明涉及利用电沉积在铝基材上提供涂层，其中所述涂层具有改善的外观。
发明背景
铝是在航空器装配中最主要使用的金属。航空器的结构接合处是通过粘合剂粘合在一起的。然而，许多粘合剂不能良好地粘附至铝基材。为了改善接合区域内的粘合强度，已知将电沉积涂层施加至铝基材。在这方面一种优选涂层源自磷酸化环氧树脂，其通过使环氧树脂例如多酚的多缩水甘油醚与磷酸反应而制备。通过阴离子电沉积施加所述涂层，并且该涂层很好地粘附至铝基材和粘附至随后施加的粘合剂。电沉积涂层的一个问题是在涂层中形成针孔，这会产生具有不良外观的粗糙涂层。此外，所述针孔可能是涂层中的破损点(pointof failure)。
发明概述
本发明通过使用磷酸化环氧树脂克服了上述问题，其中通过使一种或多种环氧树脂与磷酸和与有机膦酸和/或有机次膦酸反应而得到磷酸化环氧树脂。更具体地说，本发明提供了一种在铝基材上提供涂层的方法，其通过在充当阳极的基材和与电沉积浴电接触的阴极之间通过电流，所述电沉积浴包含碱中和的树脂组合物的水性分散体，该碱中和的树脂组合物含有未胶凝的磷酸化环氧树脂，所述磷酸化环氧树脂包含一种或多种聚合型环氧化合物与磷酸和与有机膦酸和/或有机次膦酸的反应产物的混合物。
发明详述
本文可用的磷酸化环氧树脂是未胶凝的，并且典型地如下制备。将含环氧基的物质例如多环氧化物与含磷的酸(phosphorus acid)例如磷酸(phosphoricacid)或其等效物反应。本文可用的多环氧化物可以是每分子具有超过1.0个环氧基的化合物或化合物的混合物。本领域已知若干多环氧化物。可以在Handbook of Epoxy Resins，Lee和Neville，1967，McGraw-Hill Book Company中找到多环氧化物的实例。
一类优选的多环氧化物是多酚例如双酚A的多缩水甘油醚。这些通过在碱存在下用表氯醇醚化多酚而制得。所述酚类化合物可以是1，1-双(4-羟基苯基)乙烷；2，2-双(4-羟基苯基)丙烷；1，1-双(4-羟基苯基)异丁烷；2，2-双(4-羟基叔丁基苯基)丙烷；双(2-羟基萘基)甲烷；1，5-二羟基萘；和1，1-双(4-羟基-3-烯丙基苯基)乙烷。类似地由聚酚树脂(polyphenol resin)制得另一类可用的多环氧化物。
除了如上所述多环氧化物，还可以使用包含侧挂环氧基的加成聚合物。通过使多种可聚合的烯属不饱和单体共聚而生产这些聚合物，这些单体中的至少一种是含环氧基的单体，例如丙烯酸缩水甘油酯或甲基丙烯酸缩水甘油酯。
本文中可以使用不含对环氧基呈反应性的基团的合适的烯属不饱和单体作为共聚单体。优选的单体包括α，β-烯属不饱和单体，例如含有1至约8个碳原子的饱和醇的不饱和羧酸酯，和单乙烯基芳族单体例如苯乙烯和乙烯基甲苯。
优选的多环氧化物具有约172至5000、优选300至1000的环氧当量。
除了多环氧化物，反应混合物可以包含单体型单环氧化物例如醇和酚的单缩水甘油醚，例如苯基缩水甘油醚，以及单羧酸的缩水甘油酯例如新癸酸缩水甘油酯。
与所述含环氧基的物质反应的磷酸可以是100％正磷酸或磷酸水溶液例如被称为85％磷酸的。本文可以使用其它形式的磷酸例如过磷酸、焦磷酸和三磷酸。此外，可以使用磷酸的聚合型酸酐或部分酸酐(partial anhydride)。典型地，使用具有约70至90％、优选约85％磷酸的含水磷酸。
除了所述磷酸，还将膦酸或次膦酸与含环氧基的物质反应。膦酸的实例是以下结构的有机膦酸：
Figure GPA00001096720300021
其中R是有机基团，例如具有共计1-30个碳、例如6-18个碳的那些。R可以是脂族、芳族或混合的脂族/芳族的，并可以是未取代的烃或取代的烃。
次膦酸的实例是以下结构的有机次膦酸：
Figure GPA00001096720300031
其中优选地，R和R’各自独立地是氢或有机基团。所述基团的实例是具有共计1-30个碳、例如6-18个碳的那些。次膦酸的有机组分(R，R’)可以是脂族、芳族或混合的脂族/芳族的。R和R’可以是未取代的烃或取代的烃。
有机膦酸的代表如下：3-氨基丙基膦酸、4-甲氧苯基膦酸、苄基膦酸、丁基膦酸、羧乙基膦酸、二苯基次膦酸、十二烷基膦酸、亚乙基二膦酸、十七烷基膦酸、甲基苄基次膦酸、萘基甲基次膦酸、十八烷基膦酸、辛基膦酸、戊基膦酸、甲基苯基次膦酸、苯基膦酸、苯乙烯膦酸、十二烷基双-1，12-膦酸、聚(乙二醇)膦酸。
典型地在有机溶剂中，通过混合多环氧化物与磷酸(phosphorus acid)和有机膦酸和/或有机次膦酸的混合物和任选地在催化剂例如鎓盐的存在下于升高的温度下加热达30至90分钟以完成反应，进行多环氧化物与含磷的酸的反应。彼此反应的多环氧化物和含磷的酸的相对量如下：对于每一当量环氧基，存在0.1至0.8摩尔的磷酸和0.01至0.4摩尔的有机膦酸和/或有机次膦酸，其中磷酸与有机膦酸和/或有机次膦酸的摩尔比为1∶0.01至0.5。环氧-含磷的酸反应产物基于树脂固体典型地具有10至60、优选15至50的酸值。
除了将含环氧基的物质与磷酸(phosphoric acid)和有机膦酸和/或有机次膦酸的混合物反应，可以使多环氧化物分别与磷酸和与有机膦酸和有机次膦酸之一或两者反应。然后可以合并各种反应产物。
典型地将磷酸化环氧树脂与固化剂例如氨基塑料或酚醛塑料树脂一起使用。本发明可用的氨基塑料树脂是醛例如甲醛、乙醛、巴豆醛和苯甲醛与含氨基或酰胺基的物质例如脲、三聚氰胺和苯基胍胺的缩合产物。由醇和甲醛与三聚氰胺、脲和苯基胍胺反应得到的产物是本文中优选的。
可用的氨基塑料树脂的说明性非限定实例是可从Cytec Industries以商标CYMEL获得的那些和可从Solutia Inc以商标RESIMENE获得的那些。具体实例是CYMEL 1130和1156以及RESIMENE 750和753。
(a)磷酸化环氧树脂和(b)固化剂的相对量为50至90、优选60至75wt％磷酸化环氧树脂，以及10至50、优选25至40wt％固化剂，基于(a)和(b)的固体重量。
在制备本发明的可低温固化的组合物中，可以在水中以任何方便的方式混合上述成分。本文可以使用典型的涂料添加剂例如颜料、填料、防腐剂、抗氧化剂、流动控制剂、表面活性剂等。优选的防腐剂为唑类，即杂环中包含两个双键、一个或多个碳原子和任选地硫原子的5元N-杂环化合物。优选的唑类为苯并三唑。其它唑类的实例为5-甲基苯并三唑和2-氨基噻唑。典型地，水性分散体中唑类以基于水性分散体的总重量低至0.001wt％、例如0.001至1wt％的量存在。
在将树脂组合物配制为水基和电泳(electrophoretic)组合物中，使用碱将其中和。本文可用的碱可以为有机或无机的。碱的说明性实例为氨、单烷基胺、二烷基胺或三烷基胺例如乙胺、丙胺、二甲胺、二丁胺和环己胺；单烷醇胺、二烷醇胺或三烷醇胺例如乙醇胺、二乙醇胺、三乙醇胺、丙醇胺、异丙醇胺、二异丙醇胺、二甲基乙醇胺和二乙基乙醇胺；吗啉、例如，N-甲基吗啉或N-乙基吗啉。中和百分比为使树脂共混物为水分散性和电泳的。典型地，树脂共混物被至少部分中和，约40至150％、优选60至120％中和。
本发明的可电沉积组合物典型地具有5至25％、优选5至15％的固体含量。通常，电沉积浴具有每厘米200至3000微欧姆、优选每厘米500至1500微欧姆的操作浴导电率。被涂布的铝基材在浴中的停留时间通常为约90至120秒。可以任选地以腐蚀抑制处理预先处理铝基材，只要基材保持其导电性。
电涂后，取出所述基材，然后将其在烘箱中于一定温度下用足以在低温下进行固化的时间烘烤。通常，在约225°F或更低、更优选200°F或更低的温度下烘烤涂布的基材约20-60分钟。典型地可以在180°F下固化所述基材20分钟以产生硬的、耐溶剂的和非粘性的膜。如果需要，可以在更高的温度如350°F下烘烤电涂的基材。
通过下列非限定实施例进一步说明本发明的这些和其它方面。
实施例
实施例I
将824.2份双酚A二缩水甘油醚(EEW 188)、265.1份双酚A、210.7份2-正丁氧基-1-乙醇的混合物加热至115℃。此时，加入0.8份乙基三苯基碘化鏻。加热该混合物并在至少165℃的温度下保持一小时。当使得混合物冷却至88℃时，加入51.6份Ektasolve EEH溶剂(可以从Eastman Chemical Company获得)和23.4份2-正丁氧基-1-乙醇。在88℃，加入39.2份85％o-磷酸和6.9份Ektasolve EEH，随后将反应混合物保持在至少120℃的温度下30分钟。此时，冷却该混合物至100℃，并逐渐加入72.0份去离子水。一旦加入水，保持约100℃温度2小时。然后冷却混合物至90℃，并加入90.6份二异丙醇胺，随后加入415.5份Cymel 1130甲基化/丁基化三聚氰胺甲醛树脂(可以从CytecIndustries，Inc获得)。混合30分钟后，将1800.0份该混合物反向稀释到1497.8份被搅拌的去离子水中。加入另外的347.1份去离子水，以产生均匀的分散体，其被证实在110℃下1小时后具有39.2％的固体含量。
实施例II
将819.2份双酚A二缩水甘油醚(EEW 188)、263.5份双酚A和209.4份2-正丁氧基-1-乙醇加热至115℃。此时，加入0.8份乙基三苯基碘化鏻。加热该混合物，并在至少165℃的温度下保持一小时。当使得该混合物冷却至88℃时，加入51.3份Ektasolve EEH溶剂和23.2份2-正丁氧基-1-乙醇。在88℃，加入由32.1份85％o-磷酸、18.9份苯基膦酸和6.9份Ektasolve EEH构成的浆料。随后将反应混合物保持在至少120℃温度下30分钟。此时，冷却该混合物至100℃，并逐渐加入71.5份去离子水。一旦加入水，保持约100℃温度2小时。然后冷却反应混合物至90℃并加入90.0份二异丙醇胺，之后加入413.0份Cymel 1130和3.0份去离子水。混合30分钟后，将1800.0份该混合物反向稀释到1506.0份被搅拌的去离子水中。加入另外的348.0份去离子水，以产生均匀的分散体，其被证实在110℃下1小时后具有39.5％的固体含量。
如下制备上述磷酸化环氧树脂的树脂共混物：
  成分   重量份
  磷酸化环氧树脂分散体   1432
  颜料糊1   318
  去离子水   2050
1灰色颜料糊，ACPP-1120，可以从PPG Industries，Inc.获得，51.4％固体。
充分共混上述成分，以产生固体含量19％的树脂共混物，其中颜料/粘结剂比例为0.2。制备包含实施例I的该共混物的电沉积浴，以及包含实施例II的该共混物的另一个电沉积浴，并分别用于涂布清洁/脱氧化的铝面板，以及首先用Alodine 1200(可以从Henkel Corporation获得)处理过的铝面板，其在将各个浴50％超滤之前和之后。在24-27℃浴温度和250至300伏特下进行涂布(coatout)90秒。将所述面板均在以煤气为燃料的烘箱中于93℃(200°F)烘烤30分钟，然后在Nikon optiphot显微镜下用10×目镜和10×物镜检查。观察到用包含实施例II的磷酸化环氧树脂的树脂共混物涂布的面板明显更光滑，并且其被证实比用包含实施例I的磷酸化环氧树脂的树脂共混物涂布的那些面板具有更少的类似针孔的缺陷。
尽管为了说明的目的在上文描述了本发明的特定实施方式，但是对于本领域技术人员而言显见是可以在不偏离所附权利要求书中限定的本发明的情况下对本发明的细节作出许多变换。

Claims (9)

1.一种在铝基材上提供涂层的方法，其通过在充当阳极的基材和与电沉积浴电接触的阴极之间通过电流，所述电沉积浴包含碱中和的树脂组合物的水性分散体，所述碱中和的树脂组合物含有固化剂和未胶凝的磷酸化环氧树脂，其中所述磷酸化环氧树脂包含一种或多种聚合型环氧化合物与磷酸和与有机膦酸和/或有机次膦酸的反应产物的混合物，其中所述磷酸化环氧树脂包含每一当量环氧基0.1至0.8摩尔的磷酸，和每一当量环氧基0.01至0.4摩尔的膦酸和/或有机次膦酸；
其中磷酸化环氧树脂的存在量为50至90wt％，固化剂的存在量为10至50wt％，所述百分比基于磷酸化环氧树脂和固化剂的总固体重量。
2.根据权利要求1所述的方法，其中所述聚合型环氧化合物选自多酚的多缩水甘油醚和环氧官能的丙烯酸类树脂。
3.根据权利要求1所述的方法，其中所述混合物另外包含单体型单环氧化物。
4.根据权利要求1所述的方法，其中所述磷酸化环氧树脂基于树脂固体具有15至50的酸值。
5.根据权利要求1所述的方法，其中所述固化剂为氨基塑料。
6.根据权利要求1所述的方法，其中所述有机膦酸为苯基膦酸。
7.根据叔利要求1所述的方法，其中碱中和的树脂组合物进一步含有唑类。
8.根据权利要求7所述的方法，其中所述唑类为苯并三唑。
9.根据权利要求7或8所述的方法，其中所述组合物中唑类的存在量为0.001至1.0wt％，基于树脂水性分散体中固体的总重量。
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ES2423754T3 (es) 2013-09-24
CA2696158A1 (en) 2009-02-19

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