CN116323013A - 基础涂料组合物和涂装物品 - Google Patents
基础涂料组合物和涂装物品 Download PDFInfo
- Publication number
- CN116323013A CN116323013A CN202180067975.4A CN202180067975A CN116323013A CN 116323013 A CN116323013 A CN 116323013A CN 202180067975 A CN202180067975 A CN 202180067975A CN 116323013 A CN116323013 A CN 116323013A
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- China
- Prior art keywords
- coating film
- hydroxyl
- acrylic resin
- base coating
- coating composition
- 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.)
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- 239000008199 coating composition Substances 0.000 title claims abstract description 82
- 238000000576 coating method Methods 0.000 claims abstract description 160
- 239000011248 coating agent Substances 0.000 claims abstract description 156
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 102
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 82
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 82
- 239000000049 pigment Substances 0.000 claims abstract description 70
- -1 isocyanate compound Chemical class 0.000 claims abstract description 51
- 229920000642 polymer Polymers 0.000 claims abstract description 42
- 239000010419 fine particle Substances 0.000 claims abstract description 29
- 239000012948 isocyanate Substances 0.000 claims abstract description 26
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 239000000178 monomer Substances 0.000 claims description 125
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- 239000000758 substrate Substances 0.000 claims description 19
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 14
- 230000009477 glass transition Effects 0.000 claims description 10
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- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 6
- 238000004040 coloring Methods 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052782 aluminium Inorganic materials 0.000 description 5
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- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 4
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Abstract
本发明提供基础涂料组合物和由其得到的涂装物品,所述基础涂料组合物能够在满足缩短干燥时间等对环境的考虑的同时形成外观设计性(光亮性颜料的不均等)、密合性和耐水性优异的基础涂膜。本发明提供含有颜料(A)、含羟基丙烯酸树脂(B)、封端异氰酸酯化合物(C)、在前述含羟基丙烯酸树脂(B)溶液中为不溶性的且稳定地分散的聚合物交联微粒(D)、具有与含羟基丙烯酸树脂(B)不同的重均分子量的丙烯酸树脂(E),其中,使用特定的含羟基丙烯酸树脂(B),并且调整了粘度恢复率。本发明还提供使用基础涂料组合物形成的涂装物品。
Description
技术领域
本发明涉及基础涂料组合物和涂装制品。
背景技术
例如,在构成汽车的基材等被涂物上,以赋予外观设计及耐性等为目的,通常设置基础涂膜和其上的透明涂膜。形成这样的基础涂膜的基础涂料组合物是左右被涂物的外观设计性的基本涂料,但考虑到环境、涂装作业的容易化等必须满足各种要求。例如专利文献1和专利文献2中公开了基础涂料组合物。
现有技术文献
专利文献
专利文献1:日本特开2008-138179号公报
专利文献2:日本特开2010-82529号公报
发明内容
发明要解决的课题
考虑到环境,研究了不是溶剂型而是水性型的基础涂料组合物,专利文献1中公开了水性型的基础涂料组合物。但是,水性型的基础涂料组合物为了使水在干燥、固化中蒸发,无论如何都需要能量,对设备的负荷大。
专利文献2中,未使用水性型的基础涂料组合物,而是使用溶剂型的基础涂料组合物,但采用将3层(中层、基础和透明)涂装后一次固化的3涂层1烘焙方式,节能、改良了设备负担,满足对环境的考虑。
但是,基础涂料组合物是决定被涂物外观的最重要的涂料,而且基础涂膜的上下也存在涂膜,要求高的控制,而且在其中加入对环境的考虑是非常困难的,现有技术的涂料未必能够完成。
本发明是鉴于上述情况而进行的,在本发明中,使用高固体成分(也称为“highsolid”)的溶剂型涂料,提供满足缩短干燥时间等对环境的考虑的同时,能够形成外观设计性(使光亮性颜料的不均等)、密合性和耐水性优异的基础涂膜的基础涂料组合物以及由其得到的涂装物品。
解决课题的手段
本发明提供以下方式。
[1]基础涂料组合物,其含有颜料(A)、含羟基丙烯酸树脂(B)、封端异氰酸酯化合物(C)、在前述含羟基丙烯酸树脂(B)溶液中为不溶性的且稳定地分散的聚合物交联微粒(D)、具有与含羟基丙烯酸树脂(B)不同的重均分子量的丙烯酸树脂(E),
固体成分为35质量%以上,
使用锥板型粘度计,在23℃下以0.1/sec的剪切测定粘度V1后,从0.1/sec变更为25000/sec剪切30秒,
接着将剪切恢复到0.1/sec,测定剪切1秒后的粘度V2时,作为V2相对于V1的比率的粘度恢复率V2/V1为90%以上,
前述颜料(A)含有选自着色颜料和鳞片状颜料中的1种以上,
前述含羟基丙烯酸树脂(B)是含有含羟基单体(b)的1种以上单体的聚合物,前述含羟基单体(b)是(甲基)丙烯酸与碳原子数为2以上8以下的二元醇的单酯化合物的内酯改性体,前述含羟基丙烯酸树脂(B)的重均分子量为10000以上20000以下,玻璃化转变温度为10℃以上40℃以下,羟值为10mgKOH/g以上50mgKOH/g以下,
前述丙烯酸树脂(E)的重均分子量为3000以上7500以下。
[2][1]所述的基础涂料组合物,其中,前述含羟基丙烯酸树脂(B)是前述含羟基单体(b)与前述含羟基单体(b)以外的其它单体的聚合物,
在前述含羟基单体(b)与前述其它单体的合计中,前述含羟基单体(b)为5质量%以上20质量%以下。
[3]涂装物品,其包含被涂物和由[1]或[2]所述的基础涂料组合物形成的基础涂膜。
[4][3]所述的涂装物品,其包含多层涂膜,所述多层涂膜包含设置在前述被涂物上的基础涂膜和设置在前述基础涂膜上的透明涂膜。
[5][3]所述的涂装物品,其包含多层涂膜,所述多层涂膜包含设置在预先设置有中层涂膜或底层涂膜的前述被涂物上的基础涂膜和设置在前述基础涂膜上的透明涂膜。
发明的效果
本发明可提供基础涂料组合物,其是用封端异氰酸酯化合物交联含羟基丙烯酸树脂的基础涂料组合物,通过配合与上述含羟基丙烯酸树脂不同的重均分子量低的丙烯酸树脂和聚合物交联微粒,且特定得到的组合物的剪切粘度,即使是高固体成分所配合的颜料(特别是光亮性颜料)的取向也优异、且与基础涂膜的上下的涂膜的密合性等优异。由于本发明的基础涂料组合物为高固体成分,因此在涂装时干燥性优异,并且不扰乱配合的光亮性颜料的配合,形成外观优异的涂膜。
本发明的基础涂料组合物向被涂物提供与其上下存在的涂膜的密合性也优异、涂膜剥离等的缺陷少的外观设计性优异的涂膜。
具体实施方式
本发明的基础涂料组合物的特征在于,含有颜料(A)、含羟基丙烯酸树脂(B)、封端异氰酸酯化合物(C)、在前述含羟基丙烯酸树脂(B)中为不溶性的且稳定地分散的聚合物交联微粒(D)、具有与含羟基丙烯酸树脂(B)不同的重均分子量的丙烯酸树脂(E),其固体成分为35质量%以上的高固体成分,且使用锥板型粘度计,在23℃下以0.1/sec的剪切测定粘度V1后,从0.1/sec变更为25000/sec剪切30秒,然后将剪切恢复到0.1/sec,测定剪切1秒后的粘度V2时,V2相对于V1的比率即粘度恢复率V2/V1为90%以上。进而,所述颜料(A)含有选自着色颜料和鳞片状颜料中的1种以上,所述含羟基丙烯酸树脂(B)是含有含羟基单体(b)的1种以上单体的聚合物,所述含羟基单体(b)是(甲基)丙烯酸与碳原子数为2以上8以下的二元醇的单酯化合物的内酯改性体,所述含羟基丙烯酸树脂(B)的重均分子量为10000以上20000以下,玻璃化转变温度为10℃以上40℃以下,羟值为10mgKOH/g以上50mgKOH/g以下,所述丙烯酸树脂(E)的重均分子量需要为3000以上7500以下。
通过使用该要件的基础涂料组合物,可以得到密合性和耐水性优异、且即使基础涂料组合物为高固体成分涂膜的不均也少的高外观设计性的基础涂膜。
以下,对本发明的实施方式的基础涂料组合物和涂装物品进行详细说明。
[基础涂料组合物]
本发明的实施方式的基础涂料组合物含有颜料(A)、含羟基丙烯酸树脂(B)、封端异氰酸酯化合物(C)、在前述含羟基丙烯酸树脂(B)中为不溶性的且稳定地分散的聚合物交联微粒(D)、具有与含羟基丙烯酸树脂(B)不同的重均分子量的丙烯酸树脂(E)。
(1)颜料(A)
颜料(A)含有选自着色颜料和鳞片状颜料中的1种以上。
作为着色颜料,例如可以举出有机系偶氮螯合物系颜料、不溶性偶氮系颜料、缩合偶氮系颜料、二酮吡咯并吡咯系颜料、苯并咪唑酮系颜料、酞菁系颜料、靛蓝颜料、苝酮系颜料、苝系颜料、二噁烷系颜料、喹吖啶酮系颜料、异吲哚啉酮系颜料、金属络合物颜料等,无机系中可以举出铬黄、氧化铁黄、氧化铁红、炭黑、二氧化钛等。
作为鳞片状颜料,例如可以举出金属片、金属氧化物片、珠光颜料、云母等。作为金属片,例如可以举出铝、铬、金、银、铜、黄铜、钛、镍、镍铬、不锈钢等。另外,作为金属氧化物片,可以举出金属片的氧化物,例如氧化铝、氧化铬等。
在基础涂料组合物含有鳞片状颜料的方式中,可以对基础涂膜赋予金属调的光泽,如后所述,色调根据观察基础涂膜的角度而更显著地变化,即可以形成突变性(flip-flop性,以下有时称为“FF性”)高的基础涂膜。
为了容易地防止金属片、金属氧化物片和珠光颜料等与水反应而产生气体,在金属片、金属氧化物片和珠光颜料上可以形成金属被膜,例如钼酸、铬酸、钇和稀土类金属等金属化合物的被膜或有机高分子被膜,例如使用聚合性单体等得到的有机高分子的被膜。例如,金属片、金属氧化物片和珠光颜料可以具有包含二氧化硅、氧化锆、氧化铝、氧化铬、聚合合成树脂、氧化钒、氧化钼和/或过氧化钼、磷酸盐、亚磷酸盐、硼酸盐、铬酸盐或它们的混合物或组合的被膜。要说明的是,例如在使用氧化铬等的情况下,通过使用使其化学惰性化的物质,可以除去毒性。
鳞片状颜料可以含有蒸镀金属颜料。这样的鳞片状颜料通常通过在基础膜上蒸镀金属薄膜(金属氧化物薄膜),剥离基础膜后,粉碎蒸镀金属膜,制成金属片(金属氧化物片)而得到。作为蒸镀的金属材料,例如可以使用针对金属片和金属氧化物片在上面叙述的材料。在该方式中,鳞片状颜料优选为蒸镀铝颜料、蒸镀铬颜料、蒸镀氧化铝颜料或蒸镀氧化铬颜料。对于蒸镀金属颜料,也可以根据需要在其表面形成上述的被膜。
作为市售鳞片状颜料,可以列举例如:ECKART公司制的METALURE(注册商标)系列、SILVERSHINE(注册商标)系列、HYDROSHINE(注册商标)系列、LiquidBlack(注册商标)、PLISMATIC(注册商标)系列、旭化成化学公司制的FD系列、GX系列和BS系列、东洋铝公司制的46系列、63系列等。颜料(A)可以组合使用2种以上。
颜料(A)的含量没有特别限定,例如颜料(A)的颜料浓度、即颜料(A)相对于基础涂料组合物的树脂固体成分的质量比例可以为1质量%以上20质量%以下。基础涂料组合物的树脂固体成分是指树脂成分、封端异氰酸酯化合物(C)和可包含的其它固化剂。
基础涂料组合物可以含有体质颜料。作为体质颜料,例如可以举出碳酸钙、硫酸钡、粘土、滑石等。
使用体质颜料时,可以单独使用1种,也可以组合使用2种以上。在基础涂料组合物含有体质颜料的情况下,对于体质颜料的含量,例如体质颜料相对于基础涂料组合物的树脂固体成分的质量比例可以为0.1质量%以上20质量%以下。
(2)含羟基丙烯酸树脂(B)
含羟基丙烯酸树脂(B)是含有含羟基单体(b)的1种以上单体的聚合物,含羟基单体(b)是(甲基)丙烯酸与碳原子数为2以上8以下的2元醇的单酯化合物的内酯改性体。另外,含羟基丙烯酸树脂(B)的重均分子量为10000以上20000以下,玻璃化转变温度为10℃以上40℃以下,羟值为10mgKOH/g以上50mgKOH/g以下。
通过含有含羟基丙烯酸树脂(B),即使基础涂料组合物的固体成分高达35质量%以上,涂装粘度也不会过高,因此能够降低涂膜的不均。进而,在基础涂料组合物含有鳞片状颜料的情况下,鳞片状颜料的取向变得不易混乱,因此能够得到优异的FF性(突变性:涂膜面的明暗根据观察角度而变化的性质)。基础涂料组合物的固体成分的上限没有特别限定,例如可以为60质量%。
进而,含羟基丙烯酸树脂(B)使用(甲基)丙烯酸与碳原子数为2以上8以下的二元醇的单酯化合物的内酯改性体即含羟基单体(b)聚合,因此在侧链具有长链结构,所述长链结构具有羟基。由此,能够提高与作为固化剂的异氰酸酯化合物(C)的反应性,能够提高被涂物与基础涂膜的密合性、或者设置在被涂物上的中层涂膜或底层涂膜与基础涂膜的密合性。例如,在被涂物为塑料制的情况下,本发明的实施方式的基础涂料组合物即使不在被涂物上设置底层涂膜,也能够形成与被涂物具有良好密合性的基础涂膜。
含羟基丙烯酸树脂(B)通过将含有含羟基单体(b)的1种以上单体按照常法聚合而得到。
作为含羟基单体(b),例如可以举出将(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸2-羟基丙酯、(甲基)丙烯酸3-羟基丙酯、(甲基)丙烯酸4-羟基丁酯等(甲基)丙烯酸与碳原子数为2以上8以下的二元醇的单酯化物与内酯、例如ε-己内酯等进行改性而得到的内酯改性体。
本说明书中的“(甲基)丙烯酸”是指丙烯酸和甲基丙烯酸两者。
含羟基丙烯酸树脂(B)可以是含羟基单体(b)与含羟基单体(b)以外的其它单体的聚合物,在该方式中,含羟基丙烯酸树脂(B)通过使含羟基单体(b)与上述其它单体的单体混合物聚合而得到,在含羟基单体(b)和其它单体的合计中,含羟基单体(b)优选为5质量%以上20质量%以下。
作为含羟基单体(b)以外的其它单体,可以举出例如丙烯酸、甲基丙烯酸、丙烯酸二聚体、巴豆酸、2-丙烯酰氧基乙基邻苯二甲酸酯、2-丙烯酰氧基乙基琥珀酸酯、ω-羧基-聚己内酯单(甲基)丙烯酸酯、异巴豆酸、α-氢-ω-(((1-氧代-2-丙烯基)氧)聚(氧(1-氧代-1,6-己二基))、马来酸、富马酸、衣康酸、3-乙烯基水杨酸、3-乙烯基乙酰水杨酸、2-丙烯酰氧基乙基酸式磷酸酯、2-丙烯酰胺基-2-甲基丙磺酸等含酸基单体。
另外,作为含羟基单体(b)以外的其它单体,例如可以举出(甲基)丙烯酸酯(例如,(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸2-乙基己酯、甲基丙烯酸月桂酯、丙烯酸苯酯、(甲基)丙烯酸异冰片酯、甲基丙烯酸环己酯、(甲基)丙烯酸叔丁基环己酯、(甲基)丙烯酸二环戊二烯基酯、(甲基)丙烯酸二氢二环戊二烯基酯等)、聚合性芳香族化合物(例如苯乙烯、α-甲基苯乙烯、乙烯基酮、叔丁基苯乙烯、对氯苯乙烯和乙烯基萘等)、聚合性腈(例如丙烯腈、甲基丙烯腈等)、α-烯烃(例如乙烯、丙烯等)、乙烯基酯(例如乙酸乙烯酯、丙酸乙烯酯等)、二烯(例如丁二烯、异戊二烯等)等。从提高耐水性的观点出发,优选使用苯乙烯。
进而,作为含羟基单体(b)以外的其它单体,例如可以举出(甲基)丙烯酸羟基乙酯、(甲基)丙烯酸羟基丙酯、(甲基)丙烯酸羟基丁酯、烯丙醇、甲基烯丙醇等。
含羟基单体(b)可以单独使用1种,也可以组合使用2种以上。另外,含羟基单体(b)以外的其它单体可以单独使用1种,也可以组合使用2种以上。
含羟基丙烯酸树脂(B)的重均分子量例如可以为10,000以上,可以为20,000以下。
重均分子量可以通过例如以聚苯乙烯为标准的凝胶渗透色谱(GPC)法确定。
含羟基丙烯酸树脂(B)的玻璃化转变温度例如可以为10℃以上,可以为40℃以下。
玻璃化转变温度可以通过已知方法进行实测或计算。例如,玻璃化转变温度可以根据JIS K 7121使用差示扫描量热计(DSC)测定。
含羟基丙烯酸树脂(B)的羟值例如可以为10mgKOH/g以上,可以为50mgKOH/g以下。另外,含羟基丙烯酸树脂(B)的酸值例如可以为0.2mgKOH/g以上,可以为20mgKOH/g以下。
羟值和酸值可以通过已知的方法进行实测或计算。例如,羟值和酸值可以根据JISK 0070:1992来测定。
含羟基丙烯酸树脂(B)可以组合使用2种以上。含羟基丙烯酸树脂(B)在基础涂料组合物中的含量没有特别限定,例如,在基础涂料组合物的树脂固体成分中,可以为30质量%以上70质量%以下,可以为40质量%以上,可以为60质量%以下。
(3)封端异氰酸酯化合物(C)
通过将封端异氰酸酯化合物(C)与含羟基丙烯酸树脂(B)一起使用,可以提高被涂物与基础涂膜的密合性、或者设置在被涂物上的中层涂膜或底层涂膜与基础涂膜的密合性。另外,通过使基础涂膜交联,涂膜物性提高,耐水性能提高。
封端异氰酸酯化合物(C)可以通过用封端剂封端多异氰酸酯来制备。
作为多异氰酸酯,例如可以举出六亚甲基二异氰酸酯(包括三聚体)、五亚甲基二异氰酸酯、四亚甲基二异氰酸酯、三甲基六亚甲基二异氰酸酯等脂肪族二异氰酸酯;异佛尔酮二异氰酸酯、4,4’-亚甲基双(环己基异氰酸酯)等脂环式多异氰酸酯;4,4’-二苯基甲烷二异氰酸酯、甲苯二异氰酸酯、苯二亚甲基二异氰酸酯等芳香族二异氰酸酯;这些二异氰酸酯的改性物(氨基甲酸酯化物、碳二亚胺、脲二酮、脲酮亚胺、缩二脲和/或异氰脲酸酯改性物等)。
作为封端剂,可以举出例如正丁醇、正己醇、2-乙基己醇、月桂醇、苯酚甲醇、甲基苯基甲醇等一价烷基(或芳香族)醇类;乙二醇单己基醚、乙二醇单2-乙基己基醚等溶纤剂类;聚乙二醇、聚丙二醇、聚四亚甲基醚二醇苯酚等聚醚型两末端二醇类;由乙二醇、丙二醇、1,4-丁二醇等二醇类和草酸、琥珀酸、己二酸、辛二酸、癸二酸等二羧酸类得到的聚酯型两末端多元醇类;对叔丁基苯酚、甲酚等酚类;二甲基酮肟、甲基乙基酮肟、甲基异丁基酮肟、甲基戊基酮肟、环己酮肟等肟类;以及ε-己内酰胺、γ-丁内酰胺所代表的内酰胺类。作为封端剂,可以使用作为活性氢化合物的甲基二酮、甲基酮酯和甲基二酯化合物,例如乙酰丙酮、乙酰乙酸乙酯、丙二酸二乙酯等烷基酯。另外,也可以使用利用咪唑化合物、吡唑化合物形成的封端异氰酸酯。
封端异氰酸酯化合物(C)的封端率优选为100%。由此,具有基础涂料组合物的贮藏稳定性变得更好的优点。
封端异氰酸酯化合物(C)可以组合使用2种以上。
对封端异氰酸酯化合物(C)的含量没有特别限定,从更适当地促进固化反应的观点出发,封端异氰酸酯化合物(C)的异氰酸酯基的摩尔数与含羟基丙烯酸树脂(B)的羟基的摩尔数的比(NCO/OH)可以为0.2/1.0~0.6/1.0,优选为0.3/1.0~0.5/1.0。
基础涂料组合物作为异氰酸酯化合物(C)以外的固化剂,可以含有三聚氰胺树脂、胍胺树脂、尿素树脂等氨基树脂等其它固化剂。当含有异氰酸酯化合物(C)以外的其它固化剂时,相对于基础涂料组合物的树脂固体成分100质量份,该其它固化剂的含量例如为10质量份以上30质量份以下。
(4)聚合物交联微粒(D)
聚合物交联微粒(D)作为粘性调节剂添加,有助于后述粘度的调节。通常,涂料由于涂装时施加的剪切力而减粘,因此刚涂敷后的粘度比涂装前的粘度低。因此,如果涂敷后的粘度低,则涂料向下方下垂,成为涂膜不均的原因。本发明的实施方式的基础涂料组合物通过含有聚合物交联微粒(D),可以早期恢复并提高涂装时减粘的粘度,可以抑制涂敷在被涂物上的基础涂料组合物下垂,可以降低涂膜的不均。
聚合物交联微粒(D)可以通过聚合单体混合物来制备。聚合方法如果可以得到交联微粒则可以是任何聚合方法,也可以是多级聚合。更具体而言,优选使用乳液聚合。
通过乳液聚合得到的聚合物交联微粒(D)
本发明中使用的聚合物交联微粒(D)通过将烯属不饱和单体和交联性共聚单体用公知的方法,在水性介质中进行乳液聚合而制成含有交联聚合物微粒的乳液,将水通过进行溶剂置换、共沸、离心分离、过滤、干燥等除去而得到。乳液聚合可以使用公知的乳化剂和/或分散剂实施,但优选使用具有两性离子基团的乳化剂。聚合物交联微粒(D)在添加到涂料组合物中时,由于其粒径不同,结构粘度也不同,因此得到均匀的粒径是重要的,但通过使用具有两性离子基团的乳化剂,容易得到粒径均匀的聚合物交联微粒。
作为聚合物交联微粒(D)的制备中使用的烯属不饱和单体,有(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸2-乙基己酯等丙烯酸或甲基丙烯酸的烷基酯,或具有可与其共聚的烯属不饱和键的其它单体,例如苯乙烯、α-甲基苯乙烯、乙烯基甲苯、叔丁基苯乙烯、乙烯、丙烯、乙酸乙烯酯、丙酸乙烯酯、丙烯腈、甲基丙烯腈、(甲基)丙烯酸二甲基氨基乙酯等。这些单体可以使用两种以上。
交联性共聚单体包括在分子中具有2个以上可自由基聚合的烯属不饱和键的单体和/或分别负载可相互反应的基团的2种含烯属不饱和基团的单体。
作为分子内具有2个以上可自由基聚合的烯属不饱和基团的单体,可以举出多元醇的聚合性不饱和单羧酸酯、多元酸的聚合性不饱和醇酯、和被2个以上乙烯基取代的芳香族化合物等,它们的例子有以下化合物。
乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、三乙二醇二甲基丙烯酸酯、四乙二醇二甲基丙烯酸酯、1,3-丁二醇二甲基丙烯酸酯、三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、1,4-丁二醇二丙烯酸酯、新戊二醇二丙烯酸酯、1,6-己二醇二丙烯酸酯、季戊四醇二丙烯酸酯、季戊四醇三丙烯酸酯、季戊四醇四丙烯酸酯、季戊四醇二甲基丙烯酸酯、季戊四醇三甲基丙烯酸酯、季戊四醇四甲基丙烯酸酯、甘油二甲基丙烯酸酯、甘油二丙烯酸酯、甘油丙烯酰氧基二甲基丙烯酸酯、1,1,1-三羟基甲基乙烷二丙烯酸酯、1,1,1-三羟基甲基乙烷三丙烯酸酯、1,1,1-三羟基甲基乙烷二甲基丙烯酸酯、1,1,1-三羟基甲基乙烷三甲基丙烯酸酯、1,1,1-三羟基甲基丙烷二丙烯酸酯、1,1,1-三羟基甲基丙烷三丙烯酸酯、1,1,1-三羟基甲基丙烷二甲基丙烯酸酯、1,1,1-三羟基甲基丙烷三甲基丙烯酸酯、氰脲酸三烯丙基酯、异氰脲酸三烯丙基酯、偏苯三酸三烯丙基酯、对苯二甲酸二烯丙基酯、邻苯二甲酸二烯丙基酯和二乙烯基苯。
此外,作为交联目的单体,也可以代替分子内具有2个以上可自由基聚合的烯属不饱和基团的单体,或者根据需要与它们一起使用分别担载可相互反应的基团的2种具有烯属不饱和基团的单体。例如可举出甲基丙烯酸缩水甘油酯、丙烯酸缩水甘油酯等含有缩水甘油基的烯属不饱和单体与丙烯酸、甲基丙烯酸、巴豆酸等含有羧基的烯属不饱和单体;丙烯酸2-羟基乙酯、丙烯酸羟基丙酯、甲基丙烯酸2-羟基乙酯、甲基丙烯酸羟基丙酯、丙烯酸羟基丁酯、甲基丙烯酸羟基丁酯、烯丙醇、甲基烯丙醇等含羟基的烯属不饱和单体与乙烯基异氰酸酯、异丙烯基异氰酸酯等具有异氰酸酯基的烯属不饱和单体等。但是,除此之外,也可以使用分别担载可相互反应的基团的任意组合的2种烯属不饱和单体。
构成聚合物交联微粒(D)的单体可以含有具有能够与交联剂反应的官能团的单体,作为其例子,例如有含羧基的单体,例如丙烯酸、甲基丙烯酸、巴豆酸、衣康酸、马来酸、富马酸等,含羟基的单体例如丙烯酸2-羟基乙酯、丙烯酸羟基丙酯、甲基丙烯酸2-羟基乙酯、甲基丙烯酸羟基丙酯、丙烯酸羟基丁酯、甲基丙烯酸羟基丁酯、烯丙醇、甲基烯丙醇、含氮系的丙烯酰胺、甲基丙烯酰胺等。
通过非水分散聚合得到的聚合性交联颗粒(D)
聚合物交联微粒(D)的制备中使用的单体混合物包含自由基聚合性单体。上述单体混合物可以含有:具有包含高级不饱和脂肪族基团的侧链的自由基聚合性不饱和单体。通过单体混合物含有具有包含高级不饱和脂肪族基团的侧链的自由基聚合性不饱和单体,具有可以适当制备聚合物交联微粒的优点。
作为上述具有包含高级不饱和脂肪族基团的侧链的自由基聚合性不饱和单体,例如可以举出通过高级不饱和脂肪酸与烯属不饱和缩水甘油酯的反应而得到的单体。作为上述高级不饱和脂肪酸,可以使用肉豆蔻烯酸、棕榈油酸、油酸、亚油酸、亚麻酸、蓖麻油酸等。另外,可以使用亚麻仁油脂肪酸、红花油脂肪酸、大豆油脂肪酸、米糠油脂肪酸、芝麻油脂肪酸、蓖麻油脂肪酸、脱水蓖麻油脂肪酸、紫苏子油脂肪酸、大麻籽油脂肪酸、棉籽油脂肪酸、妥尔油脂肪酸等具有非共轭双键的干性油、半干性油脂肪酸等。上述干性油、半干性油脂肪酸等含有油酸、亚油酸、亚麻酸、桐酸或蓖麻油酸等不饱和脂肪酸类。高级不饱和脂肪族基团的平均碳原子数优选为13以上23以下。另外,也可以以相对于全部饱和脂肪酸为30质量%以下的量组合使用桐油脂肪酸等具有共轭双键的脂肪酸。另外,作为上述烯属不饱和缩水甘油酯,可以使用丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、甲基缩水甘油基丙烯酸酯、甲基缩水甘油基甲基丙烯酸酯、烯丙基缩水甘油基醚、甲基烯丙基缩水甘油基醚等。这些中,特别是优选通过选自油酸、亚油酸、亚麻酸、红花油脂肪酸、大豆油脂肪酸、蓖麻油脂肪酸、脱水蓖麻油脂肪酸、妥尔油脂肪酸中的至少一种与丙烯酸缩水甘油酯和/或甲基丙烯酸缩水甘油酯的反应得到的物质。另外,作为上述自由基聚合性不饱和单体,碘值优选为60以上180以下,特别优选为70以上150以下。
作为上述单体混合物中包含的、具有包含高级不饱和脂肪族基团的侧链的自由基聚合性不饱和单体以外的其它自由基聚合性不饱和单体,可以举出例如:
丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丙酯、丙烯酸正丁酯、丙烯酸异丁酯、丙烯酸叔丁酯、丙烯酸正己酯、丙烯酸正辛酯、丙烯酸异辛酯、丙烯酸2-乙基己酯、丙烯酸异壬酯、丙烯酸硬脂基酯、丙烯酸环己酯、丙烯酸苄酯等丙烯酸酯单体;
甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丁酯、甲基丙烯酸异丁酯、甲基丙烯酸叔丁酯、甲基丙烯酸正己酯、甲基丙烯酸正辛酯、甲基丙烯酸异辛酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸异壬酯、甲基丙烯酸正十二烷基酯、甲基丙烯酸异十二烷基酯、甲基丙烯酸硬脂基酯、甲基丙烯酸环己酯、甲基丙烯酸苄基酯等甲基丙烯酸酯单体;
苯乙烯、乙烯基甲苯、乙基乙烯基苯等芳香族乙烯基单体;
丙烯酸、甲基丙烯酸、衣康酸、马来酸、马来酸酐、富马酸、巴豆酸、柠康酸等含羧基单体;
丙烯酰胺、甲基丙烯酰胺、N,N-二甲基丙烯酰胺、N-甲基丙烯酰胺、N-正丁氧基甲基丙烯酰胺等含酰胺基或取代酰胺基的单体;
丙烯酸2-羟基乙基酯、丙烯酸2-羟基丙基酯、甲基丙烯酸2-羟基乙基酯、甲基丙烯酸2-羟基丙基酯、烯丙醇、甲基烯丙醇等含羟基单体;
氨基乙基丙烯酸酯、N,N-二甲基氨基乙基丙烯酸酯、N,N-二乙基氨基乙基丙烯酸酯、N,N-二甲基氨基乙基甲基丙烯酸酯、N,N-二乙基氨基乙基甲基丙烯酸酯等含氨基或取代氨基的单体;
甲基丙烯酸缩水甘油酯、丙烯酸缩水甘油酯、缩水甘油基烯丙基醚、缩水甘油基甲基烯丙基醚、缩水甘油基乙烯基醚等含环氧基的单体;
乙烯基硫醇、烯丙基硫醇等含巯基的单体;
(聚)乙二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、三羟甲基丙烷三(甲基)丙烯酸酯、烯丙基(甲基)丙烯酸酯、氰脲酸三烯丙基酯、异氰脲酸三烯丙基酯、邻苯二甲酸二烯丙基酯、二乙烯基苯等1分子中具有2个以上自由基聚合性不饱和基团的单体;等。
上述其它自由基聚合性不饱和单体中,优选含有选自例如丙烯酸酯单体(优选丙烯酸乙酯、丙烯酸正丁酯等)、甲基丙烯酸酯单体(优选甲基丙烯酸甲酯、甲基丙烯酸正丁酯等)、含羧基单体(优选丙烯酸、甲基丙烯酸、ω-羧基-聚己内酯单丙烯酸酯等)、含取代氨基的单体(优选N,N-二甲基氨基乙基丙烯酸酯、N,N-二乙基氨基乙基甲基丙烯酸酯等N,N-二低级烷基氨基-低级烷基(甲基)丙烯酸酯等)中的1种或其以上。
相对于单体混合物的总量100质量份,上述单体混合物中含有的、具有包含高级不饱和脂肪族基团的侧链的自由基聚合性不饱和单体的量优选在0.5质量份以上30质量份以下的范围内,更优选在5质量份以上15质量份以下的范围内。另外,相对于单体混合物的总量100质量份,上述单体混合物中含有的丙烯酸酯单体和甲基丙烯酸酯单体的合计量优选在50质量份以上90质量份以下的范围内。另外,上述单体混合物中含有的含羧基单体的量优选在10质量份以下的范围内。进而,上述单体混合物中含有的含取代氨基的单体的量优选在10质量份以下的范围内。要说明的是,本发明的聚合物交联微粒(D)的制备通过多级聚合进行时,上述单体混合物中所含的单体的量是在各聚合中使用的单体的总量。
制备聚合物交联微粒(D)的聚合条件可以根据使用的单体的种类和量适当选择本领域技术人员通常使用的聚合条件来进行。例如,优选使用适当的聚合引发剂和根据需要使用的链转移剂,在氮气流中或有机溶剂的回流温度下,一边搅拌一边加热反应数小时,使上述单体混合物聚合以达到后述的重均分子量的范围内。聚合温度一般为30℃以上180℃以下,优选为60℃以上150℃以下。
作为聚合中使用的有机溶剂,可以举出例如:
环己烷、甲基环己烷、环庚烷、甲基环庚烷“ロウス”、“Mineral Spirit EC”、“Shellsol 71”、“VM&P Naphtha”、“Shell TS28 Solvent”[以上由壳牌么司制造],“IsoparC”,“Isopar E”,“Isopar G”,“Isopar H”,“Isopar M”,“Naphtha 3号”,“Naphtha 5号”,“Naphtha6号”,“Solvent 7”(以上由Exxon Chemical公司制造)、“IP Solvent 1016”、“IPSolvent 1620”、“IP Solvent 2028”、“IP Solvent2835”[以上由出光兴产株式会社制造],“White Sol”[Japan Energy(株)制造]、“Mitsubishi Mineral Turpen”、“DiamondSolvent”、“PEGASOL AN-45”、“PEGASOL 3040”[以上由JXTG Energy(株)制造]等脂肪族或脂环式烃系溶剂;
苯、甲苯、乙基苯、丙基苯、叔丁基苯、邻二甲苯、间二甲苯、对二甲苯、四氢化萘、十氢化萘、“SOLVESSO 100”(Exxon Chemical公司制)、“SOLVESSO 150”(Exxon Chemical公司制)等芳香族烃系有机溶剂;
丙酮、乙酰丙酮、甲基乙基酮、甲基异丁基酮、甲基戊基酮、环己酮等酮系有机溶剂;
乙酸甲酯、乙酸乙酯、乙酸正丁酯、乙酸戊基酯等酯系有机溶剂;
甲基溶纤剂、乙基溶纤剂、正丙基溶纤剂、异丙基溶纤剂、正丁基溶纤剂、异丁基溶纤剂、异戊基溶纤剂、苯基溶纤剂、苄基溶纤剂等溶纤剂系有机溶剂;
甲基卡必醇、乙基卡必醇、正丙基卡必醇、异丙基卡必醇、正丁基卡必醇、异丁基卡必醇、异戊基卡必醇、苯基卡必醇、苄基卡必醇等卡必醇系有机溶剂;等。
作为上述聚合引发剂,可以列举例如:过氧化苯甲酰、过氧化月桂酰、过氧化己酰、过氧化二碳酸二异丙基酯、过氧化二碳酸二-2-乙基己酯、过氧化新戊酸叔丁酯等有机过氧化物;2,2’-偶氮双异丁腈、2,2’-偶氮双-2,4-二甲基戊腈、2,2’-偶氮双-4-甲氧基-2,4-二甲基戊腈等偶氮化合物等。它们可以单独使用,也可以将2种或其以上组合使用。上述聚合引发剂的使用量相对于单体总量100质量份,一般优选为0.5质量份以上15质量份以下,更优选为2质量份以上8质量份以下。
另外,本发明的聚合物交联微粒(D)的制备通过多级聚合进行时,上述聚合引发剂的优选使用量的范围可以适用于各聚合。
在聚合物交联微粒(D)的制备中,将单体混合物进行2级聚合时,在最初的聚合阶段,可将含有具有包含高级不饱和脂肪族基团的侧链的自由基聚合性不饱和单体的单体混合物共聚而形成溶解部,接着共聚不含具有包含高级不饱和脂肪族基团的侧链的自由基聚合性不饱和单体的单体混合物或含有具有包含高级不饱和脂肪族基团的侧链的自由基聚合性不饱和单体的单体混合物而形成颗粒部。
在聚合物交联微粒(D)例如具有溶解部和颗粒部的情况下,溶解部的重均分子量可以为15000以上100000以下,优选颗粒部被具有2个以上聚合不饱和基团的单体交联。
重均分子量可以通过例如以聚苯乙烯为标准的凝胶渗透色谱(GPC)法确定。
聚合物交联微粒(D)具有溶解部和颗粒部时的溶解部和颗粒部的质量比率优选在溶解部:颗粒部=20∶80~80∶20的范围内,更优选在30:70~70:30的范围内。
作为聚合物交联微粒(D)的制备的另一例,可以举出使不含具有包含高级不饱和脂肪族基团的侧链的自由基聚合性不饱和单体的单体混合物聚合,在得到的共聚物中导入包含高级不饱和脂肪族基团的侧链的例子。具体而言,例如可通过使含有含亚烷基单体的单体混合物聚合,然后使高级不饱和脂肪酸的羧基与所得共聚物所具有的亚烷基反应,导入含有高级不饱和脂肪族基团的侧链。
相对于含羟基丙烯酸树脂(B)、封端异氰酸酯化合物(C)和丙烯酸树脂(E)的固体成分合计中100质量份,聚合物交联微粒(D)在基础涂料组合物中的配合量通常为5~40质量份,优选为10~30质量份。如果聚合物交联微粒(D)的配合量过少,则在基础涂料组合物的易滴垂性和wet on wet涂装的情况下向下层涂料组合物的渗透大,不能达到初期的目的。另一方面,配合量过多时,涂膜性能降低、损害被膜的平滑性,得不到高成品外观。
作为聚合物交联微粒(D)的市售品,例如可以举出Setalux1 801、1850、SA-50、53(Allnex公司制)。
(5)丙烯酸树脂(E)
基础涂料组合物包含重均分子量为3000以上7500以下的丙烯酸树脂(E)。由此,能够更容易地调整基础涂料组合物的粘性。
丙烯酸树脂(E)可通过使α,β-烯属不饱和单体聚合而得到,例如,关于含羟基丙烯酸树脂(B),可以使用上述α,β-烯属不饱和单体等。
丙烯酸树脂(E)的重均分子量优选为3500以上,更优选为4000以上,优选为6500以下,进一步优选为5500以下。
重均分子量可以通过例如以聚苯乙烯为标准的凝胶渗透色谱(GPC)法确定。
丙烯酸树脂(E)的羟值例如可以为40mgKOH/g以上。另外,丙烯酸树脂(E)的酸值例如可以为0.1mgKOH/g以上,可以为20mgKOH/g以下。
羟值和酸值可以通过已知的方法进行实测或计算。例如,羟值和酸值可以根据JISK0070:1992来测定。
丙烯酸树脂(E)可以组合使用2种以上。
在含有丙烯酸树脂(E)的情况下,丙烯酸树脂(E)的含量没有特别限定,例如在基础涂料组合物的树脂固体成分中,可以为10质量%以上50质量%以下。如果丙烯酸树脂(E)的配合量过少,则涂料的粘度变高,涂装时产生弊病。丙烯酸树脂(E)的量过多时粘度降低,但涂膜物性降低,密合性、耐水性能降低。
(6)基础涂料组合物
基础涂料组合物可以含有有机溶剂。
作为这样的有机溶剂,可以举出例如丙酮、甲基乙基酮、甲基异丁基酮、甲基戊基酮等酮类;乙酸乙酯、乙酸丁酯、乙酸戊酯、苯甲酸甲酯、乙氧基丙酸乙酯、丙酸乙酯、丙酸甲酯等酯类;四氢呋喃、二噁烷、二甲氧基乙烷等醚类;乙二醇单甲基醚、乙二醇单乙基醚、二乙二醇单甲基醚、丙二醇单甲基醚乙酸酯、3-甲氧基丁基乙酸酯等二醇醚类;芳香族烃类、脂肪族烃类等。
本发明的基础涂料组合物可以含有固化催化剂、聚合物交联微粒(D)以外的粘性调节剂、消泡剂、紫外线吸收剂、光稳定剂(例如受阻胺)、抗氧化剂、表面调节剂、成膜助剂、防锈剂等。
对基础涂料组合物的制造方法没有特别限定,可以采用使用分配器、均化器、辊、砂磨机或捏合机等搅拌、混炼或分散上述材料等该技术领域公知的方法。
本发明的基础涂料组合物的特征在于,使用锥板型粘度计,在23℃下,以0.1/sec的剪切测定粘度V1后,从0.1/sec变更为25000/sec剪切30秒,接着恢复到0.1/sec,测定剪切1秒后的粘度V2时,V2相对于V1的比率即粘度恢复率V2/V1为90%以上。粘度恢复率V2/V1越高越好。粘度恢复率表示弱的剪切时刻的粘度与强的剪切时刻的粘度的比率,粘度的恢复高表示即使在刚涂装后粘度也马上恢复。本发明的基础涂料组合物即使在刚涂装后粘度也会急剧恢复。
[涂装物品]
本发明的实施方式的涂装物品包括被涂物和由本发明实施方式的基础涂料组合物形成的基础涂膜。
本发明的实施方式的涂装物品可以包含多层涂膜,该多层涂膜包含设置在被涂物上的中层涂膜或底层涂膜、设置在中层涂膜或底层涂膜上的基础涂膜和设置在基础涂膜上的透明涂膜。
在某实施方式中,本发明的实施方式的涂装物品可以不具有中层涂膜或底层涂膜,在被涂物上设置基础涂膜。即,在该方式中,本发明的实施方式的涂装物品可以包含多层涂膜,该多层涂膜包含设置在被涂物上的基础涂膜和设置在基础涂膜上的透明涂膜。
例如,在被涂物为塑料制的情况下,本发明的实施方式的基础涂料组合物即使不在被涂物上设置底层涂膜,也能够形成与被涂物具有良好密合性的基础涂膜。
(1)被涂物
被涂物没有特别限定,例如可以举出金属基材、塑料基材及其发泡体等。
作为金属基材,例如可以举出铁、钢、铜、铝、锡、锌等金属以及含有这些金属的合金等。作为金属基材,具体而言,可以举出轿车、卡车、摩托车、公共汽车等汽车车身和汽车车身用的部件等。这样的金属基材优选预先形成电沉积涂膜。另外,在形成电沉积涂膜之前,可以根据需要进行化学转化处理(例如磷酸锌化学转化处理、锆化学转化处理等)。
作为塑料基材,例如可以举出聚丙烯树脂、聚碳酸酯树脂、聚氨酯树脂、聚酯树脂、聚苯乙烯树脂、ABS树脂、氯乙烯树脂、聚酰胺树脂等。作为塑料基材,具体而言,可以举出扰流板、保险杠、镜罩、格栅、门把手等汽车部件等。这些塑料基材优选用石油轻馏分油、异丙醇等溶剂脱脂或用纯水和/或中性洗涤剂洗涤。
(2)中层涂膜、底层涂膜
被涂物为金属基材时,可以在形成有电沉积涂装的金属基材上设置中层涂膜。另外,在被涂物为塑料基材的情况下,可以在塑料基材上设置底层涂膜。
中层涂膜和底层涂膜没有特别限定,可以分别使用例如含有涂膜形成树脂和根据需要的固化剂等的中层涂料组合物或底层涂料组合物来形成。
(3)透明涂膜
可以在基础涂膜上设置透明涂膜。透明涂膜没有特别限定,可以使用含有涂膜形成树脂和根据需要的固化剂等的透明涂料组合物形成。另外,透明涂膜可以含有着色成分。透明涂料组合物的形态没有特别限定,优选溶剂型。
作为溶剂型透明涂料组合物的优选例,从透明性或耐酸蚀刻性等方面考虑,可以举出含有丙烯酸树脂和/或聚酯树脂与氨基树脂和/或异氰酸酯的组合,或者具有羧酸/环氧固化系的丙烯酸树脂和/或聚酯树脂等作为涂膜形成树脂的物质。进而,更优选以异氰酸酯为交联剂的双组份型透明涂料。特别是,透明的异氰酸酯浸入着色基础涂膜层并固化,由此形成耐水性优异的多层涂膜。
作为水性型透明涂料组合物的例子,可以举出含有用碱中和所列举的溶剂型透明涂料组合物的例子中含有的涂膜形成树脂而水性化的树脂的水性型透明涂料组合物。该中和可以在聚合之前或之后,通过添加二甲基乙醇胺和三乙胺等叔胺来进行。
透明涂料组合物可以含有粘性控制剂。作为粘性控制剂,例如可以举出交联或非交联树脂颗粒、脂肪酸酰胺的膨润分散体、酰胺系脂肪酸、长链聚氨基酰胺的磷酸盐等聚酰胺系物质、氧化聚乙烯的胶体状膨润分散体等聚乙烯系等的物质、有机酸蒙皂石粘土、蒙脱石等有机膨润土系的物质等。
涂装物品的制造方法没有特别限定,例如可以通过以下说明的本发明的实施方式的涂装物品的制造方法来制造。
[涂装物品的制造方法]
本发明的基础涂料组合物通过与通常的基础涂料同样的涂装方法涂装在被涂物上。基础涂料组合物涂布在设置有中层涂膜或底层涂膜的被涂布物上。另外,在基础涂膜上涂布透明涂料,形成透明涂膜。涂膜形成方法可以是通常使用的方法,也可以使用喷雾涂饰器进行涂装,形成被称为所谓的wet on wet的未固化涂膜后,同时固化2~3层。
对中层涂料组合物、底层涂料组合物、基础水系涂料组合物和透明涂料组合物的涂装方法没有特别限定。根据被涂物的种类,例如,可以使用基于空气喷雾涂装、静电旋杯涂装、空气静电喷雾涂装的多阶段涂装或1阶段涂装、或者组合了空气静电喷雾涂装和被称为自动金属静电旋杯(metallic bell)的旋转雾化式的静电涂装机的涂装方法等的在涂装领域中通常使用的涂装方法。
作为用于将未固化的涂膜加热固化的加热装置,例如可以举出利用热风、电、气体、红外线等加热源的干燥炉等。另外,如果使用组合使用2种以上这些加热源的干燥炉,则干燥时间缩短,因此优选。
本发明的实施方式的涂装物品也可以通过每次涂布各涂料组合物时将涂膜加热固化,依次形成上层的涂膜来制造。另外,本发明的实施方式的涂装物品可以省略形成中层涂膜和底层涂膜的工序,以不包含中层涂膜和底层涂膜的方式制造。
实施例
以下,使用实施例更详细地说明本发明,但本发明不受实施例的任何限制。在实施例中,除非另有说明,“份”和“%”均为质量基准。
(制造例1)含羟基丙烯酸树脂(B-1)的制造
在具有搅拌叶片、温度计、滴加装置、温度控制装置、氮气导入口和冷凝管的反应装置中加入57份乙酸丁酯,在导入氮气的同时在搅拌下升温至120℃。接着,用3小时向反应装置中滴加甲基丙烯酸0.5份、甲基丙烯酸2-乙基己酯53.1份、甲基丙烯酸甲酯18.1份、苯乙烯15.0份、内酯改性的甲基丙烯酸2-羟基乙酯13.3份的混合物和将2.0份叔丁基过氧-2-乙基己酸酯溶解于5份乙酸丁酯中得到的溶液。滴加结束后,使其熟化1小时,再将0.2份叔丁基过氧-2-乙基己酸酯溶解于5份乙酸丁酯中得到的溶液用1小时滴加到反应装置中,在保持120℃的状态下熟化2小时,完成反应。得到的含羟基树脂的不挥发成分为60%,重均分子量为14500。另外,玻璃化转变温度为20℃,羟值为30mgKOH/g。表1中记载了配合单体成分、特性值、聚合引发剂(叔丁基过氧-2-乙基己酸酯)的第一阶段和第二阶段的量、羟基的种类(内酯改性还是没有内酯改性)。
(制造例2~10)含羟基丙烯酸树脂(B-2~B-10)的制造
在与制造例B-1相同的反应装置中,以表1所述的配合通过同样的操作得到制造例B-2~B-10的含羟基丙烯酸树脂。表1中,将得到的含羟基丙烯酸树脂(B-2~B-10)的特性值等一并记载在表1中。
[表1]
(制造例11~13)丙烯酸树脂(E-1~E-3)的制造
在与上述制造例B-1相同的反应装置中,以表2所述的配合通过同样的操作得到丙烯酸树脂(E-1~E-3),将其特性值(重均分子量、加热残分量、第一阶段和第二阶段的聚合引发剂量)一并记载于表2中。
[表2]
参考例1
具有两性离子基团的聚酯树脂的制造方法
在具备搅拌器、氮气导入管、温度控制装置、冷凝器、倾析器的2Q烧瓶中,加入双羟基乙基牛磺酸134份、新戊二醇130份、壬二酸236份、邻苯二甲酸酐186份和二甲苯27份,升温。将反应生成的水与二甲苯共沸除去。从回流开始经过约2小时使温度为190℃,持续搅拌和脱水直至相当于羧酸的酸值为145,然后冷却至140℃。
接着,保持140℃的温度,用30分钟滴加314份“CARDURA E10”(壳牌公司制的叔羧酸缩水甘油酯),然后继续搅拌2小时,结束反应。所得聚酯树脂的酸值59、羟值90、Mn 1054。
(制造例14)聚合物交联微粒D-1的制造例
在具备搅拌器、冷凝器、温度控制装置的1L反应容器中加入281份去离子水、30份上述参考例1中得到的聚酯树脂和3份二甲基乙醇胺,一边将搅拌温度保持在80℃一边溶解,向其中添加将1.0份偶氮双氰基戊酸溶解于45份去离子水和0.9份二甲基乙醇胺中得到的液体。接着,用60分钟滴加丙烯酸正丁酯30份、苯乙烯70份和乙二醇二甲基丙烯酸酯60份的混合溶液。滴加后进一步添加将0.5份偶氮双氰基戊酸溶解于15份去离子水和0.4份二甲基乙醇胺中得到物质,在80℃下继续搅拌2小时,得到不挥发成分40%、粒径0.12μ的乳液。将该乳液喷雾干燥,得到聚合物交联微粒。
将该聚合物交联微粒用超声波分散机分散在将甲基戊基酮和二甲苯以重量比为1:1的方式混合而成的溶剂中,将加热残分量调整为40%,得到稳定的聚合物交联颗粒的分散溶液。
(制造例15)聚合物交联微粒D-2的制造例
除了在与上述制造例相同的装置中使用二(2-乙基己基)琥珀酸酯磺酸钠5份代替参考例1中获得的聚酯树脂以外,通过同样的操作方法得到粒径0.20μ的乳液。同样,将该乳液喷雾干燥,超声波分散到混合溶剂中,将加热残分调整为50%。
<实施例1~5和比较例1~12>
通过以下表3和表4中记载的组成(配合着色基础涂料)配合原料并搅拌,获得实施例1~5和比较例1~12的基础涂料组成物。要说明的是,表中的组成的单位为质量份,并且,是除去有机溶剂的固体成分换算量。聚合物交联微粒(D)的量表示相对于含羟基丙烯酸树脂(B)、封端异氰酸酯化合物(C)和丙烯酸树脂(E)的合计100质量份的量。
(涂装涂料的准备)
实施例1~5和比较例1~12的涂料使用甲基戊基酮/Solvesso100=1/1(重量比)作为稀释剂,调整为在涂料温度20℃的状态下福特杯No.4的粘度为13秒。此时,不挥发成分不足35%的涂料评价为×、35%以上时评价为○,在表3、4设置涂装时的固体成分栏,记载○和×。未对不挥发成分不足35%的涂料实施其它评价项目。
(涂装物品的制作)
在用异丙醇擦拭了的ABS树脂制基材(70mm×150mm×3mm)的表面、在25℃/70%相对湿度(RH)的环境下,通过喷雾枪“ワイダ-71”(アネスト磐田公司制造)喷雾涂装实施例1的基础涂料(干燥膜厚25μm),在室温下放置5分钟。在其上,使用ROBOBEL951将透明涂料组合物(NIPPON PAINT AUTOMOTIVE COATINGS CO.,LTD.生产的R-2550-1和硬化剂H-250的混合物)在涂装(枪距离:200mm,枪速度:700mm/s,转速:2500rpm,整形空气压力:0.07MPa)条件下喷雾涂装(干燥膜厚25μm)。然后,放置10分钟后,在80℃干燥30分钟,制作实施例1的涂装物品。
除了使用表3和表4所示的实施例2~5和比较例1~12的基础涂料组成物之外,与实施例1同样地得到实施例2~5和比较例1~12的涂装物品。
使用得到的基础涂料组合物和涂装物品,按照以下要领评价不均(涂膜的不均)、密合性、耐水性、涂膜硬度、粘度恢复率和突变性(FF性)。结果如表3和表4所示。
(涂膜不均)
通过目视从正面25度和倾斜75度的角度观察在上述条件下得到的测试面板,观察颜料的取向。
评价标准如下,○为合格,×为不合格。
○:在任何角度都能看到均匀的取向。
×:两个或任意一个角度的取向看起来不均匀。
(密合性)
根据JIS K5600-5-6:1999,对从涂装物品得到的试验片的涂膜进行棋盘格Cellotape(注册商标)剥离试验。准备2mm见方的100个棋盘格,进行透明胶带剥离试验,计算未剥离的棋盘格数。
评价标准如下,○为合格,×为不合格。
○:0/100(无剥离)
×:1/100~100/100(有剥离)
[耐水性]
将从涂装物品得到的试验片在40℃的耐水槽中浸渍240小时。浸渍结束后,对于从耐水槽取出的试验片的涂膜,在取出后1小时以内,按照JISK5600-5-6:1999,进行棋盘格Cellotape(注册商标)剥离试验和外观观察。准备2mm见方的100个棋盘格,进行透明胶带剥离试验,数出未剥离的棋盘格数。另外,确认外观是否存在起泡等异常。
评价标准如下,○为合格,×为不合格。
○:0/100(无剥离)、外观无异常
Δ:0/100(无剥离)、外观有异常
×:1/100~100/100(有剥离),与外观异常无关
(涂膜硬度)
将上述得到的涂板在室温下放置5天后,测定铅笔刮擦硬度。铅笔使用三菱UNI铅笔刮擦值试验用。在测定操作中,将涂板放置固定在水平的台上,以使涂板和在圆柱上露出芯的铅笔的角度成45度的角度的方式拿着铅笔,以约1cm/秒的速度以不使芯折断的程度尽可能强地按压涂板的同时向前方推压,从而刮擦涂面。用相同浓度的铅笔进行5次该操作,对于浓度记号相互相邻的两支铅笔,找到伤痕或破损为2次以上且不足2次的组,将不足2次的铅笔的浓度记号作为涂膜的铅笔硬度。
判断标准如下。
HB以上 ○(良好)
B以下 ×(不艮)
(粘度恢复率〔%〕)
使用TA Instruments公司生产的锥板型粘度计“DHR-3”,在23℃下以0.1/sec剪切测定粘度V1后,从0.1/sec剪切变更为25000/sec剪切,剪切30秒,接着,恢复到0.1/sec剪切,测定剪切1秒后的粘度V2。根据得到的V1和V2,算出粘度恢复率V2/V1〔%〕。
评价标准如下,○为合格,×为不合格。
○:粘度恢复率为90%以上
×:粘度恢复率小于90%
(突变性(FF性))
通过“CM-512m3”(KONICA MINOLTA公司制造的变角色彩色差计),以25度和75度的测定角度测定L值后,计算出FF值(25度的L值/75度的L值)。
评价标准如下,○为合格,×为不合格。
○:FF值为2.2以上
×:FF值小于2.2
[表3]
[表4]
对表3和4中的原料(制造例1~17除外)进行说明。
·封端异氰酸酯化合物(C):旭化成化学公司制、商品名:DURANATE MF-K60B
·颜料(A):铝(鳞片状颜料)、东洋铝公司制、商品名:アルぺ一スト07-0674
·有机溶剂:甲基戊基酮、SOLVESSO100(埃克森美孚公司制)
满足本发明实施方式中规定的要件的实施例1~5的涂装物品具备密合性和耐水性优异、且涂膜不均少的基础涂膜。另外,基于鳞片状颜料的突变性(FF性)也优异。比较例1中,含羟基丙烯酸树脂(B)的重均分子量超过20000,调整为规定粘度时的不挥发成分低于35%,因此不是高固体成分型的涂料,不进行其它评价试验。在比较例2中,与比较例1相反,含羟基丙烯酸树脂(B)的重均分子量为10000以下,涂膜的耐水性、涂膜的硬度存在问题。比较例3中,含羟基丙烯酸树脂(B)的玻璃化转变温度Tg低至-10℃,涂膜的硬度不充分。比较例4与比较例3相反,玻璃化转变温度Tg高达45℃,涂膜的耐水性存在问题。比较例5和6的含羟基丙烯酸树脂(B)的羟值小于10mgKOH/g(比较例5),高于50mgKOH/g(比较例6),比较例5的密合性和耐水性存在问题,比较例6的耐水性不足。比较例7不是含羟基丙烯酸树脂(B)的内酯改性的甲基丙烯酸酯,因此耐水性不足。在比较例8和9中,第二丙烯酸树脂(E)的重均分子量在比较例8中低至2000,在比较例9中重均分子量高至9500,在比较例8中涂膜性能在很多项目中不足,在比较例9中,调整为规定粘度时的不挥发成分低于35%,因此不是高固体成分型的涂料,未进行其它的评价试验。比较例10中不含封端异氰酸酯化合物,没有交联,因此涂膜性能的耐水性和涂膜的硬度不足。比较例11中没有添加第2丙烯酸树脂(E),调整为规定粘度时的不挥发成分低于35%,因此不是高固体成分型的涂料,未进行其它评价试验。比较例12不含聚合物交联微粒(D),同样调整为规定粘度时的不挥发成分低于35%,因此不是高固体成分型的涂料,未进行其它评价试验。
Claims (5)
1.基础涂料组合物,其含有颜料(A)、含羟基丙烯酸树脂(B)、封端异氰酸酯化合物(C)、在前述含羟基丙烯酸树脂(B)溶液中为不溶性的且稳定地分散的聚合物交联微粒(D)、具有与含羟基丙烯酸树脂(B)不同的重均分子量的丙烯酸树脂(E),其中,
固体成分为35质量%以上,
使用锥板型粘度计,在23℃下以0.1/sec的剪切测定粘度V1后,从0.1/sec变更为25000/sec剪切30秒,
接着将剪切恢复到0.1/sec,测定剪切1秒后的粘度V2时,作为V2相对于V1的比率的粘度恢复率V2/V1为90%以上,
前述颜料(A)含有选自着色颜料和鳞片状颜料中的1种以上,
前述含羟基丙烯酸树脂(B)是含有含羟基单体(b)的1种以上单体的聚合物,前述含羟基单体(b)是(甲基)丙烯酸与碳原子数为2以上8以下的二元醇的单酯化合物的内酯改性体,前述含羟基丙烯酸树脂(B)的重均分子量为10000以上20000以下,玻璃化转变温度为10℃以上40℃以下,羟值为10mgKOH/g以上50mgKOH/g以下,
前述丙烯酸树脂(E)的重均分子量为3000以上7500以下。
2.根据权利要求1所述的基础涂料组合物,其中,前述含羟基丙烯酸树脂(B)是前述含羟基单体(b)与前述含羟基单体(b)以外的其它单体的聚合物,
在前述含羟基单体(b)与前述其它单体的合计中,前述含羟基单体(b)为5质量%以上20质量%以下。
3.涂装物品,其包含被涂物和由权利要求1或2所述的基础涂料组合物形成的基础涂膜。
4.根据权利要求3所述的涂装物品,其包含多层涂膜,所述多层涂膜包含设置在前述被涂物上的基础涂膜和设置在前述基础涂膜上的透明涂膜。
5.根据权利要求3所述的涂装物品,其包含多层涂膜,所述多层涂膜包含设置在预先设置有中层涂膜或底层涂膜的前述被涂物上的基础涂膜和设置在前述基础涂膜上的透明涂膜。
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