CN100357040C - 用于涂布非极性基材的方法和底漆组合物 - Google Patents

用于涂布非极性基材的方法和底漆组合物 Download PDF

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CN100357040C
CN100357040C CNB2004800062411A CN200480006241A CN100357040C CN 100357040 C CN100357040 C CN 100357040C CN B2004800062411 A CNB2004800062411 A CN B2004800062411A CN 200480006241 A CN200480006241 A CN 200480006241A CN 100357040 C CN100357040 C CN 100357040C
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A·L·亚金德
D·V·帕雷克
邱学婷
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Abstract

本发明涉及一种涂布非极性基材的方法，包括在非极性基材上涂敷包含一种或多种硅烷官能化非极性聚合物的底漆，并随后在底漆层上涂敷一层或多层着色涂料的步骤。另一方面，本发明涉及用于非极性基材的底漆。

Description

用于涂布非极性基材的方法和底漆组合物
技术领域
本发明涉及用于处理非极性基材的方法和底漆。非极性基材是不允许电子自由运动的材料基材，例如热塑性聚烯烃基材。由于例如聚丙烯的热塑性烯烃的低成本及其可模塑和反复利用的性能，对这种材料的使用持续增长，特别在汽车工业中。但是，由于这种材料非常低的表面张力，所以给这种基材上漆要求特殊的预处理技术。
背景技术
经常使用的预处理技术例如是火焰处理或电晕放电。这些技术主要存在安全缺陷。另一种预处理技术是涂敷增粘剂，例如氯化聚烯烃。基于氯化聚烯烃的涂料一般以低固体含量涂敷，并且通常制成导电的以易于随后涂层的静电涂敷。但是，氯化聚烯烃昂贵，且发现它负面地影响耐化学性。
此外，已尝试过未经氯化的聚烯烃，但如使用氯化聚烯烃一样，这些增粘剂降低了耐化学性。而且，据发现对其它涂敷于这种底漆上的涂膜的粘附根据面漆而呈选择性。
发明内容
本发明的目的是提供一种对非极性基材以及涂敷于底漆层上的其它涂层表现出良好粘附且不会降低耐化学性的底漆。本发明的另一目的是提供一种涂布非极性基材，从而形成良好的底漆/基材粘附以及在底漆与涂敷于该底漆上的其它涂层之间形成良好粘附的方法。
发明详述
本发明的目的通过一种涂布非极性基材的方法来实现，该方法包括在基材上涂敷包含一种或多种硅烷官能化非极性聚合物的底漆，并在该底漆层上涂敷着色涂料层的步骤。非极性聚合物是具有除了硅烷官能基以外，基本不含离子或其它极性基团的主链的聚合物。在此方面，“基本不含”表示低于聚合物的约5重量％，优选地低于约1重量％。
已发现根据本发明的方法在使用高温或低温烘烤底涂层/透明涂层体系进行涂布时，也产生优异的底漆-基材粘附。意外地，该底漆不仅对非极性基材，而且对涂敷于其上的极性通常更强的其它着色涂层表现出优异的粘附。利用根据本发明方法所涂布的基材表现出良好的耐化学性，特别是耐汽油性，并且在热冲击和水喷射测试中表现出良好的结果。该底漆似乎特别适用于热塑性聚烯烃基材，例如橡胶改性的聚丙烯基材。
可用在根据本发明底漆的实施方案中的合适硅烷改性聚合物是硅烷改性的聚烯烃，特别是α-聚烯烃，烯烃均聚物或共聚物，例如聚乙烯、聚丙烯、聚丁烯、乙烯-丙烯共聚物、乙烯-己烯共聚物、乙烯-丁烯-苯乙烯共聚物、乙烯-乙烯基酯(例如乙烯-乙酸乙烯基酯)共聚物、乙烯-(甲基)丙烯酸酯(例如乙烯-丙烯酸乙酯、乙烯-丙烯酸甲酯和乙烯-丙烯酸丁酯)共聚物。特别合适的可商购硅烷改性聚烯烃的实例是Degussa的Vestoplast206。
该底漆中所用的聚合物可以包含至多为聚合物的20重量％，例如0.1-10重量％或0.5-6重量％的硅烷官能基。
该底漆通常包含一种或多种溶剂以获得所要求的粘度。为此，可以使用例如芳族烃(例如二甲苯和/或甲苯)或脂族烃、酯、醚、醇、酮、醚乙酸酯或其混合物的溶剂。特别合适的溶剂例如是可从Exxon-Mobil商购的Aromatic100，它是比二甲苯或甲苯呈现出更好的溶液外观并具有更低的有害空气污染物含量的芳烃混合物。合适的非芳族溶剂例如是可从Ashland Chemical Company购得的VMP石脑油。也可以使用两种或更多种这些溶剂的混合物。例如，甲苯、二甲苯和/或VMP石脑油可以单独使用或与Aromatic100联合使用来实现所期望的干燥特性和溶解性。固体含量例如可以为约15重量％-约35重量％，但是如果希望，可以使用更低或更高的固体含量。
在水分的影响下，硅烷基水解形成硅烷醇基团。该聚合物例如可以通过硅烷醇缩合或通过与羟基官能化聚合物反应而随后发生交联。硅烷醇缩合反应可以由例如金属羧酸盐(例如二丁基二月桂酸锡)、有机金属化合物(例如钛酸四丁酯)、有机碱(例如乙胺)、无机酸和脂肪酸的硅烷醇缩合催化剂来催化。其它合适的催化剂在US-A-3,646,155中有公开。催化剂的用量可任选为底漆组合物的0.004-0.2重量％，例如0.01-0.1重量％。
该底漆组合物还可以包含其它组分，例如填料或颜料。合适的填料例如是滑石和碳酸钙。可以使用有机或无机颜料，例如二氧化钛。也可以使用例如导电炭黑的导电颜料。
本发明的底漆组合物还可以包含其它添加剂。典型添加剂的非限制性实例是分散剂，例如大豆卵磷脂；活性稀释剂；增塑剂；均化剂，例如丙烯酸酯低聚物；防沫剂，例如硅油；有机酸的金属盐，例如乙基己酸钴；螯合剂；流变控制剂，例如膨润土、热解硅石、氢化蓖麻油衍生物以及单胺与二或三异氰酸酯的加合物；抗氧化剂，例如取代的酚；以及UV稳定剂，例如二苯甲酮、三唑、苯甲酸酯和受阻联吡啶胺。
据观察，向该底漆组合物中添加一种或多种烷基化芳烃树脂明显地改善该底漆的罐装(in-can)稳定性。合适树脂的可商购实例是可从NevilleChemical Company购得的Nevchem140。
该底漆特别适用于非极性基材，例如热塑性聚烯烃基材，例如由聚丙烯或聚乙烯制得的基材。
如通常例如在汽车工业中那样，涂敷在该底漆上的涂料组合物可以是又涂有透明涂层的底涂层。任选地，这种底涂层/透明涂层体系可以通过湿碰湿工艺来涂敷。在这种工艺中，将底漆涂敷在非极性基材上，快速干燥例如约5分钟，再涂布底涂层。在快速干燥该底涂层例如约5分钟之后，将透明涂层涂敷在该底涂层上。随后，例如通过烘烤或UV固化或任意其它合适的固化方法来一起固化底漆、底涂层和透明涂层。
如果需要，可以不使用底涂层/透明涂层体系而使用单涂层体系。在单涂层体系中，在底漆层上只涂敷着色涂料，而不使用透明涂层。
底涂层、单涂层和/或透明涂层例如可以是水性或溶剂型涂料。溶剂型底涂层可以与水性透明涂层组合，并且如果希望，可以以相反的方式组合。
底涂层、透明涂层或单涂层可以基于任意合适的交联或固化机理。涂料可以是使用封闭型交联剂或潜交联剂的1K或单组分体系。或者，可以使用2K或多组分涂料，其中单独存放交联剂和共反应性粘结剂，并仅在涂敷之前或期间将其混合。
合适的底涂层与透明涂层体系的交联机理例如是一般体现为多异氰酸酯交联剂与羟基官能树脂的NCO-OH交联，或者如果希望，以相反的方式交联。
合适的多异氰酸酯实例包括1，6-己烷二异氰酸酯、1，6-六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、四甲基苯二亚甲基二异氰酸酯、2-甲基-1，5-戊烷二异氰酸酯、2，2，4-三甲基-1，6-六亚甲基二异氰酸酯、1，12-十二烷二异氰酸酯、亚甲基二(4-环己基异氰酸酯)或二(异氰酸酯环己基)甲烷及其加合物，例如缩二脲或异氰脲酸酯。合适的缩二脲例如是可从Bayer以DesmodurN商购的1，6-六亚甲基二异氰酸酯的缩二脲。合适的异氰脲酸酯实例是均可从Bayer分别以DesmodurN-3390和DesmodurZ-4370商购的1，6-六亚甲基二异氰酸酯的异氰脲酸酯和异佛尔酮二异氰酸酯的异氰脲酸酯。一般而言，NCO∶OH的比为0.5-3∶1，例如1-2∶1。
为防止过早交联，交联剂和共反应性化合物单独包装，并仅在涂敷之前或期间混合(一般称之为2K或双组分体系)。或者，可以将其中一种交联官能基封闭，从而允许所有组分的混合物存放在单个包装或容器中(1K或单组分体系)。在例如升温、水分、光等的影响下，被封闭的组分可以解封闭。合适的用于异氰酸酯的封闭剂例如是酮肟、丙二酸酯或乙酰乙酸酯。合适的单官能封闭剂例如是丙二酸二乙基酯、乙酰乙酸乙酯、ε-己内酰胺、丁酮肟、环己酮肟、1，2，4-三唑、二甲基-1，2，4-三唑、3，5-二甲基吡唑或咪唑。优选地，所用的封闭剂在至多160℃、更优选至多150℃的温度范围内断裂。
异氰酸酯交联剂不仅可用在NCO/OH固化体系中，而且可以与包含具有活泼氢的官能基的树脂，例如多硫醇或聚胺联合使用。
其它合适的用于羟基官能化合物的交联剂例如是蜜胺交联剂。合适的蜜胺实例是部分和完全烷基化的蜜胺甲醛缩合物，例如甲基化蜜胺甲醛树脂。具体的实例是六甲氧基甲基蜜胺(例如Cymel303)、混合的醚甲氧基/丁氧基甲基蜜胺(例如Cymel1135)、高亚氨基聚合甲氧基甲基蜜胺(例如Cymel325)，所有提及的Cymel产品都可从Cytec Industries Inc商购。
底漆可以以任意合适的方式涂敷到基材上，例如通过辊涂、喷涂、刷涂、浇涂或浸涂。所涂敷的底漆干膜层厚通常为约5-10微米，例如6-8微米。所涂敷的底涂层或单涂层的干膜层厚一般为20-50微米，例如30-40微米。如果涂敷透明涂层，则干膜层厚通常为约40-50微米。
通过下面的实施例来进一步描述和说明本发明。在实施例中，所有物质的量都以重量份pbw给出，除非另有说明。
实施例1
将可从Degussa得到的Vestoplast206硅烷改性聚烯烃熔化并溶解在Aromatic100中，形成20％溶液。将100 pbw的该溶液与2.4pbw导电炭黑和0.93pbw滑石混合，并在水平分散磨机中精磨(dynomill)以得到最小为4的研磨细度(Hegman Gage)。随后，加入112pbw甲苯和1.91pbw的二丁基二月桂酸锡在Aromatic100中的1％溶液。
将所得的底漆组合物以约5-10μm的干膜厚度涂敷在一系列热塑性材料板(反应器级TPO，Basell的CA 186 AC)上。随后，以约38μm的干膜厚度涂敷双组分溶剂型聚氨酯底涂层。该底涂层基于被异氰酸酯交联剂交联的羟基官能聚酯。在室温下将底漆和底涂层快速干燥5分钟。随后，涂敷基于羟基官能丙烯酸树脂和异氰酸酯交联剂的双组分聚氨酯透明涂层。在快速干燥10分钟之后，将整个体系在80℃下烘烤30分钟。
实施例2
重复实施例1，但使用不同的底涂层/透明涂层体系。底涂层是基于聚酯多醇和蜜胺交联剂的单组分溶剂型组合物。透明涂层是基于聚氨酯多醇和蜜胺交联剂的单组分溶剂型组合物。在涂敷之后，将整个体系在120℃的温度下烘烤30分钟。
使用表1中所指明的测试方法，根据General Motor规范测试各板。
表1
测试 测试方法 实施例1和2的测试结果
240小时的湿度粘附 GM 4465 P，GM 9071P 粘附通过
热冲击 GM 9525P 粘附通过
水喷射 GM 9531P 粘附通过
5品脱冷冻机砾石，45° SAE J400 满足各种OEM规范
汽油浸没 GM 9501 p，方法B 30分钟的浸没时间通过
对比实施例A
将非硅烷化品级的Vestoplast708熔化并溶解在Aromatic100中，形成20％溶液。由每一品级制得类似实施例1的底漆组合物，但不加入二丁基二月桂酸锡在Aromatic100中的1％溶液。将所得的底漆组合物以约5-10μm的干膜厚度涂敷在一系列热塑性材料板(反应器级TPO，Basell的CA 186 AC)上。随后，如实施例1所述涂敷底涂层/透明涂层并烘烤。
经GM测试方法GM9071P的粘附测试，观察到底涂层对底漆层不粘附。对比实施例B
使用Vestoplast828，而不是Vestoplast708来重复对比实施例A。Vestoplast828是不含硅烷官能基的聚烯烃。测试结果与对比实施例A中的相同。
对比实施例C和D
在这两种情况下，使用以Rohm and Haas HP 21054-481商购的氯化聚烯烃底漆，重复实施例1和2。测试结果类似于实施例1和2的结果。
实施例3
将Vestoplast206熔化并溶解在Aromatic100中，形成20％溶液。将71.04pbw的该溶液与4.3pbw的Aromatic150、3.72pbw的Aromatic100和25pbw的VMP石脑油混合。随后，向混合物中加入0.69pbw的二丁基二月桂酸锡在Aromatic100中的1％溶液。
将所得的透明底漆组合物以约5-10μm的干膜厚度喷涂在模塑色(MIC)TPO基材(Sequel 1140 YBTA)上。随后，在室温下将底漆快速干燥5分钟。
随后，以约38μm的干膜厚度涂敷双组分溶剂型聚氨酯底涂层。该底涂层基于被异氰酸酯交联剂交联的羟基官能化聚酯。在室温下将该底涂层快速干燥5分钟。随后，涂敷基于羟基官能化丙烯酸树脂和异氰酸酯交联剂的双组分聚氨酯透明涂层。在快速干燥10分钟之后，将整个体系在80℃下烘烤30分钟。
根据General Motor测试程序GM4465P和GM9071P，测试各板的240小时湿度粘附。测试结果满足湿度暴露后没有粘附损失或形成气泡的程序标准。
使用挤出级的TPO基材(Sequel E3000和Indure 1500 HG)重复实验，得到相同的结果。
实施例4
如在实施例3中制得透明底漆，并将其以约5-10μm的干膜厚度涂敷在模塑色(MIC)TPO基材(Sequel 1140 YBTA)上。在室温下将该底漆快速干燥5分钟。
在上有底漆的基材上涂敷基于聚酯多醇和蜜胺交联剂的单组分底涂层。随后，涂敷基于聚氨酯多醇和蜜胺交联剂的单组分溶剂型透明涂层。在涂敷之后，将整个体系在120℃的温度下烘烤30分钟。
如实施例3中进行相同的测试。没有出现粘附损失或气泡形成。使用挤出级的TPO基材(Sequel E3000和Indure 1500 HG)重复实验，得到相同的结果。
实施例5
将Vestoplast206熔化并溶解在Aromatic100中，形成20％溶液。将35.63pbw的该溶液与3.63pbw的Aromatic100、1.66pbw的导电炭黑和0.65pbw沉淀硫酸钡(Blanc Fixe)混合。在水平分散磨机中精磨该混合物以得到最小为4的研磨细度(Hegman Gage)。随后，加入4.2pbw的Aromatic150、19.91pbw的20％Vestoplast 206溶液、19.80pbw的VMP石脑油、8.47 Aromatic100和0.55pbw的二丁基二月桂酸锡在Aromatic100中的1％溶液。向该混合物中加入5.49pbw的烷基化芳烃树脂(可从Neville Chemical Company得到的Nevchem140)的20％二甲苯溶液。据观察这种树脂的加入明显改善了底漆的罐装稳定性。
将所得的底漆组合物以约5-10μm的干膜厚度涂敷在一系列热塑性材料板(反应器级TPO，Basell的CA 186 AC)上。随后，如实施例1所述以约38μm的干膜厚度涂敷双组分溶剂型聚氨酯底涂层。该底涂层基于被异氰酸酯交联剂交联的羟基官能化聚酯。在室温下将底漆和底涂层快速干燥5分钟。随后，涂敷基于羟基官能化丙烯酸树脂和异氰酸酯交联剂的双组分聚氨酯透明涂层。在快速干燥10分钟之后，将整个体系在80℃下烘烤30分钟。以如实施例1中的相同方式测试各板。测试结果类似(见表1)。

Claims (14)

1.一种涂布非极性基材的方法，包括在所述非极性基材上涂敷包含一种或多种硅烷官能化非极性聚合物的底漆，并随后在所述底漆层上涂敷一层或多层着色涂料的步骤，其中所述非极性聚合物为具有除了硅烷官能基以外具有低于5重量％离子或其它极性基团的主链的聚合物。
2.根据权利要求1的方法，其中涂敷在所述底漆上的着色涂料是底涂层，并且随后在所述底涂层上涂敷一层或多层透明涂层。
3.根据权利要求2的方法，其中湿碰湿地涂敷底涂层和透明涂层，并在随后的步骤中一起固化。
4.一种包含烷基化芳烃树脂和非极性聚合物的底漆组合物，其中所述聚合物包含硅烷基并且具有除了硅烷官能基以外具有低于5重量％离子或其它极性基团的主链。
5.根据权利要求4的底漆组合物，其中所述聚合物是聚烯烃。
6.根据权利要求5的底漆组合物，其中所述聚烯烃是聚丙烯。
7.根据权利要求4的底漆组合物，其中它包含一种或多种导电颜料。
8.根据权利要求4的底漆组合物，其中它包含硅烷醇缩合催化剂。
9.根据权利要求8的底漆组合物，其中所述硅烷醇缩合催化剂是有机锡化合物。
10.根据权利要求9的底漆组合物，其中所述有机锡化合物是二丁基二月桂酸锡。
11.根据权利要求4的底漆组合物，其中所述聚合物包含至多为该聚合物的20重量％的硅烷官能基。
12.根据权利要求1的涂布非极性基材的方法，其中所述基材是聚烯烃基材。
13.根据权利要求12的涂布非极性基材的方法，其中所述聚烯烃基材是聚丙烯基材。
14.根据权利要求13的涂布非极性基材的方法，其中所速基树是橡胶改性的聚丙烯。
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JP2006519689A (ja) 2006-08-31
MXPA05009497A (es) 2005-10-18
DE602004001044T2 (de) 2007-01-04
RU2005127867A (ru) 2006-03-10
AU2004216851A1 (en) 2004-09-16
RU2324672C2 (ru) 2008-05-20
ATE327835T1 (de) 2006-06-15
EP1601470A1 (en) 2005-12-07
US20060257671A1 (en) 2006-11-16
CA2518089A1 (en) 2004-09-16
ZA200508091B (en) 2006-12-27
EP1601470B1 (en) 2006-05-31
CN1771097A (zh) 2006-05-10
WO2004078365A1 (en) 2004-09-16

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