CN102119195B - 水性底漆组合物以及使用该组合物的涂覆方法 - Google Patents
水性底漆组合物以及使用该组合物的涂覆方法 Download PDFInfo
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- CN102119195B CN102119195B CN2009801310074A CN200980131007A CN102119195B CN 102119195 B CN102119195 B CN 102119195B CN 2009801310074 A CN2009801310074 A CN 2009801310074A CN 200980131007 A CN200980131007 A CN 200980131007A CN 102119195 B CN102119195 B CN 102119195B
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Classifications
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Abstract
本发明提供水性底漆组合物,该组合物含有改性聚烯烃的水性分散体、水性聚氨酯树脂和/或水性丙烯酸类树脂、特定的二酯化合物以及导电性颜料,其中,以特定量含有该二酯化合物,该水性底漆组合物与塑料基材的附着性优异,如果使用该水性底漆组合物,则涂覆后不预热即进行下一步骤的面漆涂覆,也不会混层,可形成完成性、耐水性优异的多层涂膜。
Description
技术领域
本发明涉及与塑料基材的附着性优异、并且即使在涂覆后不预热即进行下一步骤的面漆涂覆时也不会混层、可形成完成性、耐水性优异的多层涂膜的水性底漆组合物、以及使用该组合物的涂覆方法。
背景技术
汽车外板部、家电制品等的部件大多使用聚烯烃等的塑料成型品。为了提高面漆涂膜与成型品的附着性,这些成型品常常预先涂覆含有氯化聚烯烃等的底漆。从氯化聚烯烃的溶解性考虑,该底漆中使用甲苯、二甲苯等芳族系有机溶剂,从安全卫生、环境保护等考虑,近年来水性化得到进展。
上述成型品通常具有约1010Ω·cm以上的体积固有电阻率,因此,难以采用涂着效率优异的静电涂覆法直接在上述塑料成型品上涂覆面漆涂料,通常是使上述底漆具有导电性,涂覆底漆后,静电涂覆以着色为目的的面漆涂料(例如参照日本特开平6-165966号公报、国际公开WO2007/046532等)。
作为该涂覆方法,例如日本特开平10-296171号公报、日本特开2004-331911号公报中提出了在涂覆水性底漆后依次涂覆着色基底涂料和透明涂料的包含面漆涂覆的三涂一烤方式。在上述湿碰湿方式中使用水性底漆时,从确保面漆涂覆后的完成性考虑,在涂覆水性底漆后、进入下一涂覆步骤之前,即使是几分钟也必须进行预备干燥(预热)。
但是,从节省空间、节约能源考虑,在实际的涂覆生产线中需要去除预热步骤,如果为此来减薄底漆的膜厚、加速干燥,则由于喷漆橱环境(特别是相对湿度65%以下的低湿度条件)导致成膜不良,与此相伴,发生外观不良,还发生由于成膜不良而无法确保导电性的问题。并且在多层涂膜中,不仅由于面漆涂覆后的完成性,从耐水性等涂膜物性考虑,也难以省略预热步骤。
发明内容
本发明的目的在于提供:即使涂覆后不预热即进行下一步骤的面漆涂覆,也可以形成完成性、耐水性等优异的多层涂膜的水性底漆组合物、以及使用该组合物的涂覆方法。
本发明人进行了深入的研究,结果发现,通过使用以特定量含有特定的二酯化合物的水性底漆组合物,可以实现上述目的,从而完成了本发明。
即,本发明提供水性底漆组合物,其特征在于,该组合物含有:
(A)改性聚烯烃的水性分散体、
(B)水性聚氨酯树脂和/或水性丙烯酸类树脂、
(C)通式(1)所示的二酯化合物:
[式中,R1和R2独立地表示碳原子数为4~18的烃基,R3表示碳原子数为2~4的亚烷基,m为3~20的整数,m个R3互相可以相同或不同]、和
(D)导电性颜料,
该二酯化合物(C)的含量相对于成分(A)和成分(B)的固形物合计100质量份,在1~15质量份的范围内。
本发明还提供涂覆方法,其特征在于,在塑料基材面上涂覆上述水性底漆组合物,接着在该涂面上涂覆面漆涂料。
根据本发明,通过使用含有上述式(1)的特定化合物的水性底漆组合物,在低湿度等的涂敷橱环境下,即使涂覆后不预热即进行下一步骤的面漆涂覆,也可形成完成性、耐水性优异的多层涂膜。
具体实施方式
改性聚烯烃的水分散体(A):
本发明的水性底漆组合物含有改性聚烯烃的水性分散体(A)。改性聚烯烃的水分散体(A)是将用不饱和羧酸或酸酐改性的聚烯烃(i)分散于水性介质中而成。
不饱和羧酸或酸酐改性聚烯烃(i)例如可以如下获得:将选自乙烯、丙烯、丁烯、己烯等碳原子数为2~10、特别是2~4的烯烃类的至少 1种烯烃(共)聚合,对于所得的聚烯烃,进一步使用(甲基)丙烯酸、马来酸、富马酸、衣康酸等碳原子数为3~10、特别是4~8的不饱和羧酸(优选不饱和单或二羧酸)或它们的不饱和羧酸的酸酐,按照本身已知的方法进行接枝聚合获得,特别优选用马来酸或其酸酐改性所得的。对该不饱和羧酸或其酸酐的接枝量没有严格限制,可根据形成涂膜所需要的物性等来改变,基于聚烯烃的质量,通常为1~20质量%、优选1.5~15质量%、进一步优选2~10质量%的范围内是适当的。
特别是从得到的聚烯烃的分子量分布窄、无规共聚性等也优异等考虑,上述不饱和羧酸或酸酐改性聚烯烃(i)中使用的聚烯烃优选使用单活性中心催化剂(シングルサイト触媒)作为聚合催化剂制备的。单活性中心催化剂是活性点为同种(单活性中心)的催化剂,该单活性中心催化剂中特别优选金属茂系催化剂,该金属茂系催化剂通常是将具有至少一个共轭五元环配体且含有元素周期表第4~6族或第8族过渡金属化合物、第3族稀土类过渡金属的化合物——金属茂(双(环戊二烯)金属络合物及其衍生物)、与可将其活化的铝氧烷等的助催化剂、进一步与三甲基铝等的有机铝化合物组合得到的。
该聚烯烃可按照本身已知的方法制备,例如可一边将丙烯、乙烯等的烯烃和氢供给反应容器,一边连续地添加烷基铝和金属茂系催化剂来制备。
上述不饱和羧酸或酸酐改性聚烯烃(i)可进一步根据需要进行丙烯酸改性(アクリル変性)。可在该丙烯酸改性中使用的聚合性不饱和单体例如可举出:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸己酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸月桂基酯、(甲基)丙烯酸硬脂基酯等(甲基)丙烯酸的烷基酯;(甲基)丙烯酸、(甲基)丙烯酸缩水甘油基酯、(甲基)丙烯酸2-羟基乙基酯、(甲基)丙烯酰胺、(甲基)丙烯腈等的丙烯酸系单体;进一步可举出苯乙烯等,它们可分别单独使用或将2种以上组合使用。
本说明书中,“(甲基)丙烯某”是指丙烯某或甲基丙烯某,“(甲基)丙烯酸酯”是指丙烯酸酯或甲基丙烯酸酯。
上述丙烯酸改性的方法例如可举出以下的方法:首先,使不饱和羧酸或酸酐改性聚烯烃与和该改性聚烯烃中的羧基具有反应性的例如(甲 基)丙烯酸缩水甘油基酯等反应,导入聚合性不饱和基团,接着,将至少1种其它的单体与导入了聚合性不饱和基团的不饱和羧酸或酸酐改性聚烯烃共聚等的方法。丙烯酸改性时,从与其它成分的相容性、形成涂膜的附着性等考虑,上述聚合性不饱和单体的使用量是基于所得的改性聚烯烃(i)的固形物质量,优选为30质量%以下、特别是0.1~20质量%、更特别优选0.15~15质量%的范围内。
从形成涂膜的耐水性、耐湿性、耐乙醇汽油性等考虑,上述不饱和羧酸或酸酐改性聚烯烃(i)可根据需要用具有聚氧化烯链的化合物改性。具有聚氧化烯链的化合物中的聚氧化烯链例如可举出聚氧乙烯链、聚氧丙烯链、聚氧乙烯与聚氧丙烯的嵌段链等。
具有聚氧化烯链的化合物通常具有400~3,000、优选500~2,000范围内的数均分子量。如果该数均分子量比400小,则无法充分发挥亲水基团的效果,可能对涂膜性能(特别是耐水性)产生不良影响,而如果比3,000大,则在室温下形成固体,溶解性变差,难以处理。
上述用具有聚氧化烯链的化合物进行的改性例如可如下进行:使一个末端具有羟基且具有聚氧化烯链的化合物(a)与不饱和羧酸或酸酐改性聚烯烃反应;或者如上所述,当不饱和羧酸或酸酐改性聚烯烃是用丙烯酸改性了的时,可使一个末端具有聚合性不饱和基团且具有聚氧化烯链的化合物(b)与其反应来进行。
上述一个末端具有羟基且具有聚氧化烯链的化合物(a)例如可举出:聚氧乙烯硬脂基醚等的聚氧化烯烷基醚;聚氧乙烯壬基苯基醚、聚氧乙烯十二烷基苯基醚等的聚氧化烯烷基苯基醚;聚氧乙烯脂肪酸酯等聚氧化烯二醇脂肪酸酯;聚氧乙烯烷基胺、烷基烷醇胺的氧化乙烯氧化丙烯聚合物加成物等的聚氧化烯烷基胺等,它们可分别单独使用或将2种以上组合使用。
不饱和羧酸或酸酐改性聚烯烃与一个末端具有羟基且具有聚氧化烯链的化合物(a)的反应例如如下进行:将不饱和羧酸或酸酐改性聚烯烃在80~200℃的温度下加热熔融,向其中添加化合物(a),根据需要添加碱性物质等,并加热。此时的化合物(a)的使用比例相对于不饱和羧酸或酸酐改性聚烯烃的固形物100质量份,通常为0.5~50质量份,特别优选0.5~25质量份的范围内。
上述一个末端具有聚合性不饱和基团且具有聚氧化烯链的化合物 (b)例如可举出(甲基)丙烯酸聚乙二醇酯(ポリエリレングリコ一ル(メタ)アクリレ一ト)、(甲基)丙烯酸聚丙二醇酯、聚氧乙烯甲基醚(甲基)丙烯酸酯、聚氧丙烯甲基醚(甲基)丙烯酸酯、聚氧乙烯月桂基醚(甲基)丙烯酸酯、聚氧乙烯壬基苯基醚(甲基)丙烯酸酯、聚氧乙烯月桂基醚马来酸酯、含烯丙基的聚氧乙烯壬基苯基醚等,它们可分别单独使用或将2种以上组合使用。
不饱和羧酸或酸酐改性聚烯烃与一个末端具有聚合性不饱和基团且具有聚氧化烯链的化合物(b)的反应例如可如下进行:将不饱和羧酸或酸酐改性聚烯烃在80~200℃的温度下加热熔融,与对上述丙烯酸改性所述的同样,添加与不饱和羧酸或酸酐改性聚烯烃中的羧基具有反应性的例如(甲基)丙烯酸缩水甘油基酯、(甲基)丙烯酸2-羟基乙酯等,且根据需要添加聚合抑制剂、碱性物质等,并加热,首先向改性聚烯烃中导入聚合性不饱和基团,接着向其中添加化合物(b),根据需要添加聚合引发剂等并加热。化合物(b)的使用比例是相对于不饱和羧酸或酸酐改性聚烯烃的固形物100质量份,通常为0.5~50质量份,特别优选0.5~25质量份的范围内。
上述不饱和羧酸或酸酐改性聚烯烃(i)可根据需要进一步进行氯化。聚烯烃的氯化例如可通过向聚烯烃或其改性物的有机溶剂溶液或分散体中吹入氯气来进行,反应温度可以是50~120℃的范围内。聚烯烃的氯化物(固形物)中的氯含有率可根据聚烯烃氯化物所需的物性等改变,从所形成涂膜的附着性等考虑,基于聚烯烃氯化物的质量,通常为35质量%以下、特别优选10~30质量%,进一步优选12~25质量%的范围内。
上述不饱和羧酸或酸酐改性聚烯烃(i)中使用的聚烯烃特别优选含有丙烯作为聚合单元,从与其它成分的相容性、所形成涂膜的附着性考虑,该不饱和羧酸或酸酐改性聚烯烃(i)中的丙烯的质量分数通常为0.5~0.99,特别优选0.6~0.97,进一步优选0.7~0.95的范围内。
如上所述得到的不饱和羧酸或酸酐改性聚烯烃(i)通常具有120℃以下、优选50~100℃、进一步优选60~90℃范围内的熔点,以及通常具有30,000~180,000、优选50,000~150,000、进一步优选70,000~120,000范围内的质均分子量(Mw)。如果该改性聚烯烃的熔点和质均分子量脱离这些范围,则与其它成分的相容性、与形成涂膜的基材、面 漆涂膜层的层间附着性等降低,因此不优选。另外,从上述附着性考虑,不饱和羧酸或酸酐改性聚烯烃(i)通常具有1~50mJ/mg、特别优选2~50mJ/mg范围内的熔解热。
这里,熔点和熔解热通过使用差示扫描热容量测定装置“DSC-5200”(セイコ一电子工业社制造,商品名),将20mg改性聚烯烃以10℃/分钟的升温速度由-100℃加热至150℃、测定其热量来获得。难以求出熔解热时,可将测定试样加热至120℃,然后以10℃/分钟冷却,然后静置2天以上,按照上述方法测定热量。
改性聚烯烃(i)熔点的调节例如可通过改变聚烯烃的组成、特别是α-烯烃单体量来进行。
上述改性聚烯烃(i)的质均分子量是对通过凝胶渗透色谱测定的质均分子量以聚苯乙烯的质均分子量为基准进行换算所得的值,通过“HLC/GPC150C”(Water制造,商品名60cm×1)、柱温135℃、溶剂使用邻二氯苯、以流量1.0ml/分钟测定。注入样品是以3.4ml邻二氯苯中5mg改性聚烯烃的溶液浓度,在140℃下溶解1~3小时来制备。凝胶渗透色谱中使用的柱可举出“GMHHR-H(S)HT”(东ソ一(株)制备,商品名)。
并且,从与其它成分的相容性、所形成涂膜的附着性考虑,上述不饱和羧酸或酸酐改性聚烯烃(i)的质均分子量与数均分子量之比(Mw/Mn)通常为1.5~4.0,特别优选2.0~3.5,更特别优选2.0~3.0的范围内。
本发明中使用的改性聚烯烃的水分散体(A)可通过将上述不饱和羧酸或酸酐改性聚烯烃(i)分散于水性介质中、例如去离子水中获得,此时可根据需要,将不饱和羧酸或酸酐改性聚烯烃(i)中的羧基的一部分或全部用胺化合物中和、和/或用乳化剂进行水分散。上述改性聚烯烃(i)具有聚氧化烯链时,不使用该胺化合物、乳化剂或只使用少量的它们,即可以将改性聚烯烃(i)分散于水性介质中。
上述胺化合物例如可举出:三乙胺、三丁基胺、二甲基乙醇胺、三乙醇胺等叔胺;二乙胺、二丁基胺、二乙醇胺、吗啉等仲胺;丙胺、乙醇胺等伯胺等。
使用上述胺化合物时,其使用量优选相对于上述不饱和羧酸或酸酐改性聚烯烃(i)中的羧基通常为0.1~1.0摩尔当量的范围内。
上述乳化剂例如可举出:聚氧乙烯单油基醚、聚氧乙烯单硬脂基醚、聚氧乙烯单月桂基醚、聚氧乙烯十三烷基醚、聚氧乙烯苯基醚、聚氧乙烯壬基苯基醚、聚氧乙烯辛基苯基醚、聚氧乙烯单月桂酸酯、聚氧乙烯单硬脂酸酯、聚氧乙烯单油酸酯、失水山梨糖醇单月桂酸酯、失水山梨糖醇单硬脂酸酯、失水山梨糖醇三油酸酯、聚氧乙烯失水山梨糖醇单月桂酸酯等非离子系乳化剂;烷基磺酸、烷基苯磺酸、烷基磷酸等的钠盐或铵盐等阴离子系乳化剂等,进一步可使用1分子中具有阴离子性基团和聚氧乙烯基、聚氧丙烯基等的聚氧化烯基的含聚氧化烯基的阴离子性乳化剂、1分子中具有该阴离子性基团和聚合性不饱和基团的反应性阴离子性乳化剂等。它们可分别单独使用或将2种以上组合使用。
上述乳化剂的使用量是相对于上述不饱和羧酸或酸酐改性聚烯烃(i)的固形物100质量份,通常为30质量份以下,特别优选0.5~25质量份的范围内。
水性聚氨酯树脂和/或水性丙烯酸类树脂(B):
本发明的水性底漆组合物含有水性聚氨酯树脂(B-1)和/或水性丙烯酸类树脂(B-2)。
水性聚氨酯树脂(B-1)是分子中具有氨酯键的水溶性或水分散性的树脂,可举出:具有酸值的自乳化型乳液、并用乳化剂的乳液、水溶性树脂等,特别优选分散体的形态。聚氨酯分散体是通常在乳化剂的存在下预先使二醇和二异氰酸酯、进一步根据需要使二羟甲基烷酸等反应,一边将得到的聚氨酯预聚物分散于水中,一边通过强制乳化或自乳化获得的分散体。
水性聚氨酯树脂(B-1)的骨架例如可举出醚系、碳酸酯系、酯系等,其中,从所形成膜的耐水性考虑,优选醚系、碳酸酯系。水性聚氨酯树脂(B-1)还可以含有羟基。
水性丙烯酸类树脂(B-2)通常可以使用将单体混合物(该单体混合物包含:含羧基的聚合性不饱和单体等的含亲水性基团的聚合性不饱和单体以及其它的聚合性不饱和单体)共聚获得的质均分子量通常为5,000~100,000、优选5,000~50,000范围内的水溶性丙烯酸类树脂、或质均分子量为50,000以上、优选100,000以上的丙烯酸类树脂乳液。 上述质均分子量是将使用四氢呋喃作为溶剂、通过凝胶渗透色谱测定的质均分子量以聚苯乙烯的质均分子量为基准进行换算时的值。凝胶渗透色谱装置可以使用“HLC8120GPC”(东ソ一(株)制造,商品名),凝胶渗透色谱中使用的柱可以使用“TSKgel G-4000H×L」、「TSKgel G-3000H×L」、「TSKgel G-2500H×L」、「TSKgel G-2000H×L」(均为东ソ一(株)制造,商品名)4根。
上述含有羧基的聚合性不饱和单体例如可举出:(甲基)丙烯酸、巴豆酸、马来酸、富马酸、衣康酸、以及它们中的二羧酸的半单烷基酯化物等,除此以外的含亲水性基团的聚合性不饱和单体例如可举出:(甲基)丙烯酸聚乙二醇酯、(甲基)丙烯酸聚丙二醇酯等含聚亚烷基链的聚合性不饱和单体;2-丙烯酰胺-2-甲基丙磺酸、(甲基)丙烯酸2-磺基乙酯等的(甲基)丙烯酸磺基烷基酯等含磺酸基的聚合性不饱和单体;(甲基)丙烯酸N,N-二甲基氨基乙酯、(甲基)丙烯酸N,N-二乙基氨基乙酯等含叔氨基的聚合性不饱和单体;2-(甲基丙烯酰氧基)乙基三甲基氯化铵、2-(甲基丙烯酰氧基)乙基三甲基溴化铵等含季铵盐基的聚合性不饱和单体;季铵盐化含羧基的聚合性不饱和单体等。
上述其它的聚合性不饱和单体例如可举出:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正或异丙酯、(甲基)丙烯酸正、异或叔丁基酯、(甲基)丙烯酸2-乙基己基酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸月桂基酯、(甲基)丙烯酸异冰片基酯等丙烯酸或甲基丙烯酸的碳原子数为1~24烷基酯或环烷基酯;(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸2-或3-羟基丙酯、(甲基)丙烯酸4-羟基丁酯等丙烯酸或甲基丙烯酸的羟基烷基酯;(甲基)丙烯酸缩水甘油基酯、丙烯腈、丙烯酰胺、苯乙烯、乙烯基甲苯、乙酸乙烯基酯、氯乙烯、二丙烯酸1,6-己二醇酯等,它们可以分别单独使用或将2种以上组合使用。
对上述单体混合物的共聚没有特别限定,可按照本身已知的方法进行,例如,水溶性丙烯酸类树脂可通过溶液聚合法等进行,丙烯酸类树脂乳液可通过乳液聚合法等进行。
水性丙烯酸类树脂(B-2)特别是为通过乳液聚合得到的丙烯酸类树脂乳液时,可以是在水和乳化剂的存在下使用单体混合物、分多步进行乳液聚合得到的多层结构颗粒状的乳液。
水性丙烯酸类树脂(B-2)中的来自含亲水性基团的聚合性不饱和单 体的羧基等的酸性基团可以根据需要使用碱性物质中和。此时可使用的碱性物质优选水溶性的,例如可举出:氨、甲基胺、乙基胺、丙基胺、丁基胺、二甲基胺、三甲基胺、三乙基胺、乙二胺、吗啉、甲基乙醇胺、二甲基乙醇胺、二乙醇胺、三乙醇胺、二异丙醇胺、2-氨基-2-甲基丙醇等,它们可分别单独使用或将2种以上组合使用。
水性丙烯酸类树脂(B-2)优选含有羟基,从水分散性、与其它成分的相容性、所形成涂膜的固化性等考虑,通常具有20~200mgKOH/g、特别优选20~150mgKOH/g范围内的羟值、以及通常具有1~100mgKOH/g、特别优选10~70mgKOH/g范围内的酸值。
本发明中,上述水性分散体(A)与上述树脂(B)的使用比按照成分(A)/成分(B)的固形物质量比计,通常为10/90~70/30,特别优选15/85~65/35,进一步优选20/80~60/40的范围内。如果脱离该范围,则所形成涂膜与材料的附着性、耐水性、耐乙醇汽油性等降低,因此不优选。
二酯化合物(C):
本发明的水性底漆组合物含有通式(1)所示的二酯化合物:
[式中,R1和R2独立地表示碳原子数为4~18的烃基,R3表示碳原子数为2~4的亚烷基,m为3~20的整数,m个R3互相可以相同也可以不同],
由此,即使减薄底漆的膜厚,成膜性也优异,可以确保导电性,不依赖喷漆橱环境,即使涂覆底漆后不预热即进行下一步骤的面漆涂覆,也可以形成完成性、耐水性优异的多层涂膜。
上述式(1)中,R1或R2所示的烃基优选碳原子数为5~11的烷基,更优选碳原子数为5~9的烷基,进一步优选碳原子数为6~8的烷基。特别是上述R1和R2为碳原子数为6~8的支链状的烷基时,即使将涂料储藏较长期间后涂覆,也可以使所形成的涂膜具有优异的成膜性。另外,R3优选为亚乙基,并且,特别优选m为4~10的整数。
上述二酯化合物(C)例如可使具有2个末端羟基的聚氧亚烷基二醇与具有碳原子数为4~18的烃基的单羧酸进行酯化反应来获得。
上述聚氧亚烷基二醇例如可举出:聚乙二醇、聚丙二醇、聚乙二醇与聚丙二醇的嵌段共聚物、聚丁二醇等,其中特别优选使用聚乙二醇。从耐水性等考虑,这些聚氧亚烷基二醇通常具有约120~约800、特别优选约150~约600、更特别优选约200~约400范围内的重均分子量。
上述具有碳原子数为4~18的烃基的单羧酸例如可举出:戊酸、己酸、2-乙基丁酸、3-甲基戊酸、苯甲酸、环己烷甲酸、庚酸、2-乙基戊酸、3-乙基戊酸、辛酸、2-乙基己酸、4-乙基己酸、壬酸、2-乙基庚酸、癸酸、2-乙基辛酸、4-乙基辛酸、十二烷酸、十六烷酸、十八烷酸等。其中优选己酸、庚酸、2-乙基戊酸、3-乙基戊酸、辛酸、2-乙基己酸、4-乙基己酸、壬酸、2-乙基庚酸、癸酸、2-乙基辛酸、4-乙基辛酸等具有碳原子数为5~9的烷基的单羧酸,更优选庚酸、2-乙基戊酸、3-乙基戊酸、辛酸、2-乙基己酸、4-乙基己酸、壬酸、2-乙基庚酸等具有碳原子数为6~8的烷基的单羧酸,进一步优选2-乙基戊酸、3-乙基戊酸、2-乙基己酸、4-乙基己酸、2-乙基庚酸等具有碳原子数为6~8的支链状烷基的单羧酸。
上述聚氧亚烷基二醇与上述单羧酸的二酯化反应可按照本身已知的方法进行。上述聚氧亚烷基二醇和上述单羧酸可分别单独使用或将2种以上组合使用。
从成膜性、完成性、耐水性等考虑,所得二酯化合物(C)通常具有约320~约1,000、特别优选约400~约800、更特别优选约500~约700范围内的分子量。
本发明的水性底漆组合物中的二酯化合物(C)的含量是相对于成分(A)和成分(B)的固形物合计100质量份,通常为1~15质量份,优选2~13.5质量份,进一步优选3~12质量份的范围内。如果二酯化合物(C)的含量脱离该范围,在减薄底漆的膜厚时,成膜性降低,完成性降低;如果脱离该范围较多,则多层涂膜的耐水性、完成性降低,因此不优选。
导电性颜料(D):
本发明的水性底漆组合物含有导电性颜料(D)。
导电性颜料(D)只要可使所形成的涂膜具有导电性即可,没有特别限定,可以使用颗粒状、薄片(flake)状、纤维(包含晶须)状的任何形 状。具体例如可举出:导电性碳黑、碳纳米管、碳纳米纤维、碳微线圈等导电性碳;银、镍、铜、石墨、铝等金属粉,进一步可举出:掺杂了锑的氧化锡、掺杂了磷的氧化锡、表面被氧化锡/锑覆盖的针状氧化钛、氧化锑、锑酸锌、氧化铟锡、碳或石墨的晶须表面被覆氧化锡等得到的颜料;在薄片状的云母表面被覆选自氧化锡、掺杂锑的氧化锡、掺杂锡的氧化铟(ITO)、掺杂氟的氧化锡(FTO)、掺杂磷的氧化锡和氧化镍的至少1种导电性金属氧化物所得的颜料;二氧化钛颗粒表面含有氧化锡和磷的具有导电性的颜料等,它们可以分别单独使用或将2种以上组合使用。其中,可特别优选使用导电性碳。
从赋予导电性和所形成涂膜的附着性、耐水性等考虑,上述导电性颜料(D)的含量是相对于水性底漆组合物中的成分(A)和成分(B)的固形物合计100质量份,通常为1~300质量份、特别优选3~250质量份、更特别优选5~180质量份的范围内。特别是使用导电性碳时,其使用量是相对于组合物中的成分(A)和成分(B)的固形物合计100质量份,通常为1~30质量份、特别优选3~25质量份、更特别优选5~25质量份的范围内。
本发明的水性底漆组合物可进一步根据需要含有上述导电性颜料以外的颜料,例如可含有氧化钛、氧化铁红、铝糊、偶氮系、酞菁系等的着色颜料;滑石、二氧化硅、碳酸钙、硫酸钡、锌白(氧化锌)等的体质颜料,它们可以分别单独使用或将2种以上组合使用。
水性底漆组合物:
本发明的水性底漆组合物例如可如下制备:将以上所述的改性聚烯烃的水分散体(A)、树脂(B)、二酯化合物(C)和导电性颜料(D)按照常规方法混合,用适当的水性介质、例如去离子水稀释来制备。
本发明的水性底漆组合物中可以根据需要含有交联剂。该交联剂可举出:通常可与上述树脂(B)等中所含的羟基反应的氨基树脂和/或(封端)聚异氰酸酯。还可以使用可以与改性聚烯烃的水分散体(A)中的羧基反应的环氧化合物作为交联剂。
本发明的水性底漆组合物可以进一步根据需要含有固化催化剂、增稠剂、消泡剂、有机溶剂、表面调节剂等的涂料用添加剂等。
本发明的水性底漆组合物可以使涂覆在被涂物上的涂膜中的水分 含有率降低,因此涂覆时的固形物含有率通常为30重量%以上,特别优选35~45重量%的范围内。
如上所述,本发明的水性底漆组合物可以涂覆在塑料成型品上。塑料成型品例如可举出:保险杠、扰流板、格栅、挡泥板等的汽车外板部;家用电器制品的外板部等中使用的塑料成型品等,其材质例如特别优选使乙烯、丙烯、丁烯、己烯等碳原子数为2~10的烯烃类的1种或2种以上(共)聚合而成的聚烯烃,除此之外,聚碳酸酯、ABS树脂、聚氨酯树脂、聚酰胺等上也可采用本发明的水性底漆组合物。
对于这些塑料成型品,在涂覆本发明的水性底漆组合物之前,可按照本身已知的方法适当进行脱脂处理、水洗处理等。
本发明的水性底漆组合物的涂覆优选使用空气喷涂、无空气喷涂、浸涂、刷毛等对塑料成型品进行,使干燥膜厚通常为1~20μm、优选2~10μm、并且,为了确保成膜性、使涂覆后的涂着涂料的固形物尽快提高,优选在3~7μm的范围内。涂覆该组合物后,可以将所得涂膜面根据需要、在室温下定型30秒~60分钟左右,或在约40~约80℃的温度下预备加热(预热)1~60分钟左右,或者在约60~约140℃、优选约70~约120℃的温度下加热20~40分钟左右使其固化,本发明中,特别是涂覆本发明的水性底漆组合物后无需预热即可进行下一步骤的面漆涂覆,涂覆本发明的水性底漆组合物后,优选在室温(约20~约35℃)下定型30秒~3分钟左右。由此可以尽快提高本发明的水性底漆组合物涂覆后的涂着涂料的固形物(例如涂覆1分钟后的涂着涂料的固形物为50质量%以上,优选60%以上),即使不预热也可以防止与上层涂膜的混层。涂着涂料的固形物、例如涂覆1分钟后的涂着涂料的固形物可如下求出。首先,按照与上述相同的条件,在铝箔的一定面积上涂着涂料,1分钟后回收,立即将铝箔折叠,使其在这以后不发生水分的蒸发,迅速测定重量。然后打开铝箔,在与多层涂膜的加热固化条件相同的条件下测定固化后的重量。由该重量和预先测定的铝箔自身的重量计算涂着涂料的固形物浓度。
如上所述形成的底漆涂膜具有导电性,固化涂膜的表面电阻率通常为1×108Ω/□以下,特别优选1×107Ω/□以下。由此作为导电底漆涂膜,可以进行下一步骤的良好的静电涂覆。这里,“表面电阻率”的测定可以将涂覆成干燥膜厚约15μm的涂膜在80℃、10分钟的条件下 干燥,使用TREK公司制造的表面电阻计、商品名“TREK MODEL 150”进行(单位:Ω/□)。
对于涂覆了本发明的水性底漆组合物的塑料成型品,接着可以在其涂面静电涂覆面漆涂料。面漆涂料可以单独使用着色涂料涂覆,也可以使用该着色涂料作为底涂料,依次涂覆底涂料和透明涂料。上述底漆涂膜上可以依次涂覆例如白色底涂料和干涉珠光色底涂料,以此作为着色基底涂膜层,形成多层膜。
上述着色涂料可以使用本身已知的涂料,通常可使用以有机溶剂和/或水为主要的溶剂,含有着色颜料、闪光颜料、染料等着色成分和基体树脂、交联剂等树脂成分的涂料。
上述着色涂料中使用的基体树脂例如可举出:具有羟基、环氧基、羧基、硅烷醇基这样的反应性官能基的丙烯酸类树脂、聚酯树脂、醇酸树脂等的树脂。交联剂可列举:具有可与上述官能团反应的反应性官能团的三聚氰胺树脂、尿素树脂等的氨基树脂、(封端)多异氰酸酯、聚环氧化物、多元羧酸等。
上述着色涂料可根据需要含有体质颜料、固化催化剂、紫外线吸收剂、涂面调节剂、流变性控制剂、抗氧化剂、消泡剂、蜡、防腐剂等的涂料用添加剂。
上述着色涂料可以在上述未固化或固化的底漆涂膜上以干燥膜厚通常为5~50μm、优选5~30μm、进一步优选10~20μμm的范围静电涂覆,可将所得涂膜面根据需要在室温下定型1~60分钟左右,或在约40~约80℃温度下预备加热1~60分钟左右,或者在约60~约140℃、优选约80~约120℃温度下加热20~40分钟左右,使其固化。本发明中,优选在涂覆着色底涂料后不固化,可接着进行透明涂覆。
上述透明涂料例如可使用含有基体树脂、交联剂等树脂成分和有机溶剂、水等,进一步根据需要配合紫外线吸收剂、光稳定剂、固化催化剂、涂面调节剂、流变性控制剂、抗氧化剂、消泡剂、蜡等的涂料用添加剂而成的有机溶剂系或水系热固化性涂料,该涂料具有透过所形成的透明涂膜可以看见下层涂膜的程度的透明性。
上述基体树脂例如可举出含有羟基、羧基、硅烷醇基、环氧基等的至少1种反应性官能基团的丙烯酸类树脂、聚酯树脂、醇酸树脂、氟树脂、聚氨酯树脂、含硅的树脂等的树脂,特别优选含羟基的丙烯酸 类树脂。上述交联剂可举出:具有可与这些官能基团反应的反应性官能基的三聚氰胺树脂、尿素树脂、(封端)多异氰酸酯化合物、环氧化合物、含羧基的化合物、酸酐、含烷氧基硅烷基的化合物等,特别优选多异氰酸酯化合物。
上述透明涂料的涂覆可如下进行:在未固化或固化的着色基底涂膜上以干燥膜厚通常为10~50μm、优选20~40μm范围内进行静电涂覆,将所得涂膜面根据需要在室温下定型1~60分钟左右,或在约40~约80℃温度预备加热1~60分钟左右,然后在约60~约140℃、优选约70~约120℃温度下加热20~40分钟左右,使其固化。
如此,可得到在本发明的底漆涂膜上涂覆有着色基底涂膜和透明涂膜的塑料成型品。
实施例
以下给出实施例,进一步具体说明本发明。如无特别说明,例中的“份”和“%”表示“质量份”和“质量%”。
改性聚烯烃的水性分散体的制备
制备例1
在安装了搅拌器、冷凝管、温度计和滴液漏斗的4颈烧瓶中,将100g马来酸酐接枝聚丙烯(通过对使用金属茂系催化剂得到的聚丙烯加成马来酸(加成量4质量%)进行改性所得,熔点:80℃,Mw:约15万,Mw/Mn:约2.5)在140℃下加热熔融,添加15g聚氧乙烯硬脂基醚(“ニユ一コ一ル1820”,一个末端含羟基的聚氧乙烯化合物,日本乳化剂制备,商品名),边搅拌边在140℃下反应4小时。反应后冷却至90℃,加入去离子水进行过滤,得到固形物为30%的改性聚烯烃的水性分散体(A-1)。
制备例2
在安装了搅拌器、冷凝管、温度计和滴液漏斗的四颈烧瓶中,将200g马来酸酐接枝聚丙烯(通过对使用金属茂系催化剂得到的聚丙烯加成马来酸(加成量4质量%),进行改性所得,熔点:80℃,Mw:约15万,Mw/Mn:约2.5)在120℃下加热熔融,添加10g 2-羟基丙烯酸酯、0.1g聚合抑制剂(二叔丁基羟基甲苯)和2.0g三乙基胺,搅拌1小时。边搅拌边在120℃、用1小时向其中添加30g聚乙二醇单甲基丙烯酸酯(“ブレンマ一PE-350”,日本油脂社制,商品名)和0.3g聚合引发剂(“パ一ブチルO),日本油脂社制备,商品名)进行反应。反应后添加4g三乙基胺,搅拌30分钟后冷却至90℃,加入去离子水进行过滤,得到固形物为30%的改性聚烯烃的水性分散体(A-2)。
含羟基的丙烯酸类树脂溶液的制备
制备例3
在具备搅拌机、回流冷凝器和温度计的反应器中加入40份丙二醇单甲基醚,加热至120℃并保持,用3个小时滴加53份甲基丙烯酸环己基酯、20份丙烯酸正丁基酯、21份丙烯酸2-羟基乙基酯、6份丙烯酸和5份偶氮二异丁腈的混合物。滴加后,在相同温度下熟化1小时,用1小时滴加1份偶氮双二甲基戊腈和10份丙二醇单甲基醚的混合液,进一步熟化1小时,然后边搅拌边添加7.4份二甲基乙醇胺和193份去离子水,得到含羟基的丙烯酸类树脂溶液(B-1)。所得树脂的酸值是47mgKOH/g,羟值为101mgKOH/g,质均分子量为约1万。
水性底漆的制作
实施例1
将固形物质量为30份的改性聚烯烃的水性分散体(A-1)、固形物质量为70份的含羟基的丙烯酸类树脂溶液(B-1)、5份二酯化合物(C-1)(注3)、20份导电性颜料(D-1)(注6)和80份钛白(注8)按照常规方法配合,用去离子水稀释,使固形物为40%,得到水性底漆(1)。
实施例2~8和比较例1~5
实施例1中,使配比组成为表1所示,除此之外与实施例1同样操作,得到各水性底漆(2)~(13)。
表1的配比是以固形物表示,表1中的(注1)~(注9)如下所述。
(注1)改性聚烯烃的水性分散体(A-3):“EH-801”,酸改性氯化聚烯烃的水性分散体,东洋化成公司制备,商品名,氯化度:16%,固 形物:30%。
(注2)水性聚氨酯树脂(B-2):“ユ一コ一トUX-310”,三洋化成公司制备,商品名,水性聚氨酯分散体。
(注3)二酯化合物(C-1):聚氧亚乙基二醇与正己酸的二酯化合物。是上述通式(1)中,R1和R2分别为戊基、R3为亚乙基、m为5的化合物。分子量:434。
(注4)二酯化合物(C-2):聚氧亚乙基二醇与2-乙基己酸的二酯化合物。是上述通式(1)中,R1和R2分别为2-乙基戊基、R3为亚乙基、m为7的化合物。分子量:578。
(注5)二酯化合物(C-3):聚氧亚乙基二醇与2-乙基己酸的二酯化合物。是上述通式(1)中,R1和R2分别为2-乙基戊基、R3为亚乙基、m为25的化合物。分子量:1,370。
(注6)导电性颜料(D-1):“バルカンXC72”,キヤボツトスペシヤリテイ一ケミカルズ制备,商品名,导电性碳黑颜料。
(注7)导电性颜料(D-2):“ケツチエンEC300J”,ケツチエンブラツクインタ一ナシヨナル制备,商品名,导电性碳黑颜料。
(注8)导电性颜料(D-3):“ET-500W”,石原产业社制备,商品名,导电性氧化钛。
(注9)钛白:“JR-806”,テイカ制备,商品名。
试验涂覆物1的制备
在室温25℃、相对湿度60%的喷漆橱内,在成型加工成保险杠的聚丙烯(脱脂处理完毕)上喷气涂覆如上所述制备的水性底漆(1)~(13),分别形成表1所示的干燥膜厚,放置90秒后,在其上静电涂覆“ソフレツクス415”(关西ペイント社制,商品名,溶剂型着色底涂涂料)作为着色底涂涂料,使干燥膜厚为约15μm,接着,静电涂覆“ソフレツクス7500クリヤ一”(关西ペイント社制,商品名,丙烯酸聚氨酯系溶剂型透明涂料)作为透明涂料,使干燥膜厚为约30μm,在80℃下加热干燥30分钟,制备各试验涂覆物。
试验涂覆物2的制备
在室温25℃、相对湿度60%的喷漆橱内,对成型加工成保险杠的聚丙烯(脱脂处理完毕)喷气涂覆如上所述制备的水性底漆(1)~(13),分别形成表1所示的干燥膜厚,放置90秒后,在其上静电涂覆“レタンWBエコベ一ス”(关西ペイント社制,商品名,水性着色底涂涂料)作为着色底涂涂料,使干燥膜厚为约15μm,在80℃下预热3分钟,然后静电涂覆“ソフレツクス7500クリヤ一”(关西ペイント社制,商品名,丙烯酸聚氨酯系溶剂型透明涂料)作为透明涂料,使干燥膜厚为约30μm,在80℃下加热干燥30分钟,制备各试验涂覆物。
试验涂覆物3的制备
在室温25℃、相对湿度60%的喷漆橱内,对成型加工成保险杠的聚丙烯(脱脂处理完毕)喷气涂覆如上所述制备的水性底漆(1)~(13),分别形成表1所示的干燥膜厚,放置90秒后,在其上静电涂覆“ソフレツクス415(白色)”(关西ペイント社制,商品名,溶剂型着色底涂涂料)作为着色底涂涂料,使干燥膜厚为约15μm,接着,静电涂覆“ソフレツクス415(珠光色)”(关西ペイント社制,商品名,溶剂型着色底涂涂料)作为干涉珠光色底涂涂料,使干燥膜厚为约10μm,进一步静电涂覆“ソフレツクス7500クリヤ一”(关西ペイント社制,商品名,丙烯酸聚氨酯系溶剂型透明涂料)作为透明涂料,使干燥膜厚为约30μm,在80℃下加热干燥30分钟,制备各试验涂覆物。
涂覆水性底漆1分钟后的涂着涂料的固形物如下测定:首先,在与 上述相同的喷漆橱内、在相同条件下,在铝箔的一定面积上涂覆涂料,1分钟后回收,立即将铝箔折叠,防止之后的水分的蒸发,迅速测定重量。然后打开铝箔,在80℃下加热干燥30分钟后,测定重量。由这些重量和预先测定的铝箔自身的重量,可计算求出涂着涂料的固形物浓度。
性能试验
如上所述制备的各试验涂覆物用于下述的性能试验。其结果一并表示在表1中。
(*1)底漆导电性:在聚丙烯板(脱脂处理完毕)上喷涂各水性底漆(1)~(13),使各干燥膜厚为约15μm,将由此形成的底漆涂膜在80℃下加热5分钟,然后用“MODEL150”(TREK公司制造,商品名)在20℃下测定各涂膜面的表面电阻率(Ω/□),以以下的基准表示。
◎低于1MΩ、
○为1MΩ以上但低于100MΩ、
△为100MΩ以上但低于10000MΩ、
×为10000MΩ以上。
(*2)完成品外观:涂覆面漆后的涂膜的完成品外观按照以下基准目视评价。
○:完成品纹理、光泽感均良好、
△:完成品纹理稍差,或光泽感稍差,
×:完成品纹理、光泽感均差。
(*3)初期附着性:用切刀在各试验涂覆物的涂膜面引入切线,深度达到基材,制作100个大小为2mm×2mm的方格,在其表面粘贴胶带(粘着セロハンテ一プ(注册商标)),在20℃下将其迅速剥离,之后调查方格的残留涂膜数,按照以下的基准表示。
○为100个(没有剥离)、
△为99~50个、
×为49个以下。
(*4)耐水性和耐水后附着性:切取涂覆了各试验涂覆物的保险杠的一部分,在40℃的温水中浸泡10天,提起,干燥,然后与上述的初期附着性试验同样地进行附着性试验,调查残留涂膜数,与上述同样 地评价(耐水后附着性)。观察涂膜的表面,调查有无鼓泡发生,以以下的基准表示(耐水性)。
○:无鼓泡的发生、
×:有鼓泡的发生。
Claims (14)
2.根据权利要求1的水性底漆组合物,其中,改性聚烯烃的水性分散体(A)是将改性聚烯烃分散于水性介质中所得,所述改性聚烯烃是将不饱和羧酸或酸酐改性聚烯烃(i)进一步用具有聚氧化烯链的化合物改性而成。
3.根据权利要求1或2的水性底漆组合物,其中,不饱和羧酸或酸酐改性聚烯烃(i)是用马来酸或其酸酐改性的聚烯烃。
4.根据权利要求1或2的水性底漆组合物,其中,不饱和羧酸或酸酐改性聚烯烃(i)具有50~100℃范围内的熔点。
5.根据权利要求1或2的水性底漆组合物,其中,不饱和羧酸或酸酐改性聚烯烃(i)具有30,000~180,000范围内的质均分子量。
6.根据权利要求1或2的水性底漆组合物,其中,不饱和羧酸或酸酐改性聚烯烃(i)具有1.5~4.0范围内的质均分子量(Mw)/数均分子量(Mn)之比。
7.根据权利要求1的水性底漆组合物,其中,水性聚氨酯树脂为聚氨酯分散体。
8.根据权利要求1的水性底漆组合物,其中,水性丙烯酸树脂具有20~200mgKOH/g的羟值和1~100mgKOH/g的酸值。
9.根据权利要求1的水性底漆组合物,其中,成分(A)/成分(B)的固形物质量比在10/90~70/30的范围内。
10.根据权利要求1的水性底漆组合物,其中,二酯化合物(C)是R1和R2独立地表示碳原子数为6~8的烷基、R3表示亚乙基、m为4~10的整数的式(1)的化合物。
11.根据权利要求1的水性底漆组合物,其中,导电性颜料(D)是导电性碳。
12.涂覆方法,其特征在于,在塑料基材面上涂覆权利要求1~11中任一项的水性底漆组合物,接着在该涂面上涂覆面漆涂料。
13.根据权利要求12的方法,其中,依次涂覆着色底涂料和透明涂料作为面漆涂料。
14.通过权利要求12或13所述的方法涂覆的物品。
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