CN108779208A - 聚合物、组合物、涂膜、层积体、背板和太阳能电池组件 - Google Patents
聚合物、组合物、涂膜、层积体、背板和太阳能电池组件 Download PDFInfo
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- CN108779208A CN108779208A CN201780015850.0A CN201780015850A CN108779208A CN 108779208 A CN108779208 A CN 108779208A CN 201780015850 A CN201780015850 A CN 201780015850A CN 108779208 A CN108779208 A CN 108779208A
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N tetraisopropyl titanate Substances CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
- C08G18/6275—Polymers of halogen containing compounds having carbon-to-carbon double bonds; halogenated polymers of compounds having carbon-to-carbon double bonds
- C08G18/6279—Polymers of halogen containing compounds having carbon-to-carbon double bonds; halogenated polymers of compounds having carbon-to-carbon double bonds containing fluorine atoms
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Abstract
本发明提供一种聚合物,该聚合物能够得到与基材具有良好的初期密合性、在高压蒸煮测试后也具有良好的密合性、由落砂磨耗性试验测定的耐磨耗性优异的涂膜。一种聚合物,其特征在于,其包含全卤烯烃单元、不含羟基和芳香环中的任一种的乙烯基酯单元以及含羟基单体单元,羟值为110mgKOH/g以上。
Description
技术领域
本发明涉及聚合物、组合物、涂膜、层积体、背板和太阳能电池组件。
背景技术
在有机溶剂或水中可溶、在室温可交联的含氟共聚物由于分子内的C-F键的高键能和低极化率,因而耐候性、耐化学药品性、防水防油性、耐污染性等优异,被用于各种用途。
例如,在专利文献1中,作为可得到耐污染性优异的固化涂膜的含氟共聚物,记载了一种含氟共聚物,其含有(A)四氟乙烯和/或六氟丙烯单元30~60摩尔%、(B)苯甲酸乙烯酯和/或对叔丁基苯甲酸乙烯酯单元10~35摩尔%、以及(C)具有官能团的单体的单元10~40摩尔%。
在专利文献2中记载了一种含氟共聚物,其含有(a)四氟乙烯结构单元、(b)不含羟基和羧基的非芳香族系的乙烯基酯单体结构单元、(c)不含芳香族基团和羧基的含羟基乙烯基单体结构单元、以及(f)其他单体结构单元,(a)为20摩尔%以上49摩尔%以下、(b)为25摩尔%以上69.9摩尔%以下、(c)为8摩尔%以上30摩尔%以下、以及(f)为0摩尔%或10摩尔%以下。
在专利文献3中记载了一种含氟共聚物,其为包含氟代烯烃的重复单元(1)、乙烯基单体或烯丙基单体的重复单元(2)、结合有羟基的乙烯基单体或结合有羟基的烯丙基单体的重复单元(3)、结合有羧基盐基的乙烯基单体或烯丙基单体的重复单元(4)的共聚物,单元(4)的比例相对于重复单元总数为0.4摩尔%以上且小于4摩尔%。
另外,还已知有将在有机溶剂或水中可溶、在室温可交联的含氟共聚物用于太阳能电池组件的背板的技术。
例如,在专利文献4中记载了一种太阳能电池组件的背板,其是在不透水性片材的至少一面形成含固化性官能团的含氟聚合物涂料的固化涂膜而成的。
在专利文献5中记载了一种太阳能电池组件用背板,其是在基材片的单侧或两侧形成有包含含氟聚合物(A)的涂料的固化涂膜层,该含氟聚合物(A)具有基于氟代烯烃(a)的重复单元、基于含交联性基团的单体(b)的重复单元、以及基于含烷基单体(c)的重复单元,该含烷基单体(c)是将不含季碳原子的碳原子数为2~20的直链或支链烷基与聚合性不饱和基团通过醚键或酯键连结而成的。
现有技术文献
专利文献
专利文献1:日本特开平6-184243号公报
专利文献2:日本特开2004-204205号公报
专利文献3:国际公开第2008/035779号
专利文献4:日本特开2007-35694号公报
专利文献5:国际公开第2009/157449号
发明内容
发明所要解决的课题
但是,现有的包含聚合物的涂膜容易由于落砂而磨耗,耐磨耗性有改善的余地。
鉴于上述现状,本发明的目的在于提供一种聚合物,该聚合物能够得到与基材具有良好的初期密合性、在高压蒸煮测试后也具有良好的密合性、由落砂磨耗性试验测定的耐磨耗性优异的涂膜。
本发明的目的还在于提供一种组合物,该组合物能够得到与基材具有良好的初期密合性、在高压蒸煮测试后也具有良好的密合性、由落砂磨耗性试验测定的耐磨耗性优异的涂膜。
本发明的目的还在于提供一种涂膜以及具备上述涂膜的背板和太阳能电池组件,该涂膜与基材具有良好的初期密合性、在高压蒸煮测试后也具有良好的密合性、由落砂磨耗性试验测定的耐磨耗性优异。
本发明还在于提供一种层积体以及具备上述层积体的背板和太阳能电池组件,该层积体除了耐磨耗性和初期密合性优异以外,在高压蒸煮测试后也具有良好的密合性,由于高交联密度而使涂膜强度增加,从而使得辊加工时的破裂减轻性也优异。
用于解决课题的手段
本发明涉及一种聚合物,其特征在于,其包含全卤烯烃单元、不含羟基和芳香环中的任一种的乙烯基酯单元以及含羟基单体单元,羟值为110mgKOH/g以上(在本说明书中,有时称为“聚合物(A)”)。
上述全卤烯烃优选为选自由四氟乙烯、三氟氯乙烯以及六氟丙烯组成的组中的至少一种。
上述乙烯基酯优选为选自由乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、异丁酸乙烯酯、新戊酸乙烯酯、己酸乙烯酯、叔碳酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯和环己基甲酸乙烯酯组成的组中的至少一种。
上述含羟基单体优选为羟基烷基乙烯基醚。
本发明涉及一种组合物,其特征在于,该组合物包含聚合物(在本说明书中,有时称为“聚合物(B)”)和多异氰酸酯化合物,上述聚合物包含全卤烯烃单元以及含羟基单体单元、且羟值为90mgKOH/g以上,上述多异氰酸酯化合物所具有的异氰酸酯基与上述聚合物所具有的羟基的当量比小于1.0。
上述全卤烯烃优选为选自由四氟乙烯、三氟氯乙烯以及六氟丙烯组成的组中的至少一种。
上述含羟基单体优选为羟基烷基乙烯基醚。
聚合物(B)优选进一步包含选自由不含羟基和芳香环中的任一种的乙烯基酯单元和不含羟基的烷基乙烯基醚单元组成的组中的至少一种单元(b)。
上述组合物优选进一步包含溶剂。
本发明还涉及一种涂膜,其特征在于,其包含上述的聚合物、或者由上述组合物形成。
本发明涉及一种层积体,其特征在于,该层积体包含基材以及设于上述基材上的涂膜,该涂膜包含氨基甲酸酯键,落砂磨耗性为80L以上;
对上述涂膜根据JIS D0202-1988进行棋盘格胶带剥离试验的情况下,100格中未剥离的方格的数目为30以上。
本发明还涉及一种背板,其特征在于,其具备上述的涂膜或上述的层积体。
本发明还涉及一种太阳能电池组件,其特征在于,其具备上述的层积体或上述的背板。
发明的效果
本发明的聚合物由于具有上述构成,因而能够得到与基材具有良好的初期密合性、在高压蒸煮测试后也具有良好的密合性、由落砂磨耗性试验测定的耐磨耗性优异的涂膜。
本发明的组合物由于具有上述构成,因而能够得到与基材具有良好的初期密合性、在高压蒸煮测试后也具有良好的密合性、由落砂磨耗性试验测定的耐磨耗性优异的涂膜。
本发明的涂膜由于具有上述构成,因而与基材具有良好的初期密合性,在高压蒸煮测试后也具有良好的密合性,由落砂磨耗性试验测定的耐磨耗性优异。本发明的背板和太阳能电池组件由于具有上述构成,因而在具备上述涂膜以外的层的情况下层间牢固地密合,在高压蒸煮测试后层间也牢固地密合,由落砂磨耗性试验测定的耐磨耗性也优异。
本发明的层积体由于具有上述构成,因而除了上述涂膜的耐磨耗性以及上述涂膜与上述基材的初期密合性优异以外,在高压蒸煮测试后也具有良好的密合性,由于高交联密度而使涂膜强度增加,从而使得辊加工时的破裂减轻性也优异。
附图说明
图1是太阳能电池组件的第1结构的示意性截面图。
图2是太阳能电池组件的第2结构的示意性截面图。
图3是太阳能电池组件的第3结构的示意性截面图。
具体实施方式
以下具体说明本发明。
本发明的聚合物(在本说明书中有时称为“聚合物(A)”)的特征之一在于,其羟值为110mgKOH/g以上。作为上述羟值,优选为120mgKOH/g以上、更优选为125mgKOH/g以上、进一步优选为130mgKOH/g以上,优选为180mgKOH/g以下、更优选为170mgKOH/g以下、进一步优选为160mgKOH/g以下、特别优选为150mgKOH/g以下。
上述羟值由聚合物(A)的重量和-OH基的摩尔数通过计算求出。-OH基的摩尔数可以通过NMR测定、IR测定、滴定、元素分析等求出。
聚合物(A)的特征在于,其包含全卤烯烃单元、不含羟基和芳香环中的任一种的乙烯基酯单元以及含羟基单体单元。
构成上述全卤烯烃单元的全卤烯烃是全部氢原子被卤原子取代的烯烃。作为构成上述全卤烯烃单元的全卤烯烃,可以举出四氟乙烯(TFE)、三氟氯乙烯(CTFE)、六氟丙烯(HFP)、全氟(烷基乙烯基醚)等。
其中,作为上述全卤烯烃,优选为选自由TFE、CTFE和HFP组成的组中的至少一种,更优选为选自由TFE和CTFE组成的组中的至少一种。
作为构成上述乙烯基酯单元的乙烯基酯,优选羧酸乙烯酯,更优选为选自由乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、异丁酸乙烯酯、新戊酸乙烯酯、己酸乙烯酯、叔碳酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯和环己基甲酸乙烯酯组成的组中的至少一种,进一步优选为选自由乙酸乙烯酯、叔碳酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯和环己基甲酸乙烯酯组成的组中的至少一种,特别优选为选自由乙酸乙烯酯和叔碳酸乙烯酯组成的组中的至少一种。
另外,作为上述乙烯基酯,出于密合性和耐磨耗性更为优异的原因,优选羧酸的碳原子数为6以上的羧酸乙烯酯,更优选羧酸的碳原子数为9以上的羧酸乙烯酯。羧酸乙烯酯中的羧酸的碳原子数的上限优选为20、更优选为15。处于与密封材层的密合性优异的原因,最优选新壬酸乙烯酯、新癸酸乙烯酯等叔碳酸乙烯酯。
需要说明的是,上述乙烯基酯不含羟基和芳香环中的任一种。另外,上述乙烯基酯优选不含卤原子。
作为构成上述含羟基单体单元的含羟基单体,优选为选自由羟基烷基乙烯基醚、羟基烷基烯丙基醚、羟基羧酸乙烯酯、羟基羧酸烯丙酯和(甲基)丙烯酸羟烷基酯组成的组中的至少一种,更优选为选自由羟基烷基乙烯基醚和羟基烷基烯丙基醚组成的组中的至少一种,进一步优选为羟基烷基乙烯基醚。
作为上述羟基烷基乙烯基醚,可以举出2-羟基乙基乙烯基醚、3-羟基丙基乙烯基醚、2-羟基丙基乙烯基醚、2-羟基-2-甲基丙基乙烯基醚、4-羟基丁基乙烯基醚、4-羟基-2-甲基丁基乙烯基醚、5-羟基戊基乙烯基醚、6-羟基己基乙烯基醚等。
作为上述羟基烷基烯丙基醚,可以举出2-羟基乙基烯丙基醚、4-羟基丁基烯丙基醚、甘油单烯丙基醚等。
作为上述羟基羧酸乙烯酯,可以举出羟基乙酸乙烯酯、羟基丙酸乙烯酯、羟基丁酸乙烯酯、羟基己酸乙烯酯、4-羟基环己基乙酸乙烯酯等。
作为上述羟基羧酸烯丙酯,可以举出羟基乙酸烯丙酯、羟基丙酸烯丙酯、羟基丁酸烯丙酯、羟基己酸烯丙酯、4-羟基环己基乙酸烯丙酯等。
作为上述(甲基)丙烯酸羟烷基酯,可以举出丙烯酸-2-羟基乙酯、甲基丙烯酸-2-羟基乙酯等。
作为上述含羟基单体,其中更优选由下式(A)表示的单体:
式(A):CH2=CH-(CH2)l-O-(CH2)m-OH
(式中,l为0或1,m为2~20的整数),特别优选为选自由4-羟基丁基乙烯基醚、2-羟基乙基乙烯基醚、2-羟基乙基烯丙基醚和4-羟基丁基烯丙基醚组成的组中的至少一种单体。
作为上述全卤烯烃单元的含量,相对于聚合物(A)的全部单体单元,优选为30~60摩尔%、更优选为40~55摩尔%。
作为上述不含羟基和芳香环中的任一种的乙烯基酯单元的含量,相对于聚合物(A)的全部单体单元优选为1~40摩尔%、更优选为10~30摩尔%。
作为上述含羟基单体单元的含量,相对于聚合物(A)的全部单体单元优选为15~40摩尔%、更优选为20~35摩尔%。
在本说明书中,构成聚合物的上述各单体单元的含量可以通过将NMR、FT-IR、元素分析、荧光X射线分析根据单体的种类适宜地组合而计算出。
聚合物(A)优选数均分子量为3000~100000。上述数均分子量更优选为5000以上、进一步优选为8000以上,更优选为50000以下、进一步优选为35000以下。数均分子量若过小,则耐候性、耐溶剂性和耐污染性优异,同时有可能无法形成具有高硬度的涂膜;数均分子量若过大,则在制成涂料的情况下的粘度增大,可能难以处理。上述数均分子量可以通过使用四氢呋喃作为洗脱液的凝胶渗透色谱法(GPC)进行测定。
聚合物(A)通过差示扫描量热计(DSC)求出的玻璃化转变温度(第二轮)优选为10~70℃、更优选为15~60℃。玻璃化转变温度若过小,则耐候性、耐溶剂性和耐污染性差,同时有可能无法形成具有高硬度的涂膜;玻璃化转变温度若过大,则在制成涂料的情况下的粘度增大,可能难以处理。
从与多异氰酸酯化合物或颜料等的相容性良好的方面考虑,聚合物(A)的酸值优选为0.6~28.8mgKOH/g、更优选为2~12mgKOH/g。
聚合物(A)可以进一步包含与全卤烯烃单元、上述不含羟基和芳香环中的任一种的乙烯基酯单元以及含羟基单体单元不同的单体单元。例如,聚合物(A)可以包含含有芳香环且不含羟基的羧酸乙烯酯、含羧基单体、含氨基单体、含水解性甲硅烷基单体、不含羟基的烷基乙烯基醚、不含卤原子和羟基的烯烃等的单元。这些单体单元的含量相对于聚合物(A)的全部单体单元可以为0~10摩尔%、优选为0.1~5摩尔%、更优选为0.5~3摩尔%。
作为上述的含有芳香环且不含羟基的羧酸乙烯酯,可以举出苯甲酸乙烯酯、对叔丁基苯甲酸乙烯酯等。
作为上述含羧基单体,优选由下式(B)表示的单体:
式(B):R1aR2aC=CR3a-(CH2)n-COOH
(式中,R1a、R2a和R3a相同或不同,均是氢原子或碳原子数为1~10的直链或支链状的烷基;n为0以上的整数),可以举出例如丙烯酸、甲基丙烯酸、乙烯基乙酸、丁烯酸、戊烯酸、己烯酸、庚烯酸、辛烯酸、壬烯酸、癸烯酸、十一碳烯酸、十二碳烯酸、十三碳烯酸、十四碳烯酸、十五碳烯酸、十六碳烯酸、十七碳烯酸、十八碳烯酸、十九碳烯酸、二十碳烯酸、22-二十三碳烯酸等。其中优选为选自由丙烯酸、丁烯酸和十一碳烯酸组成的组中的至少一种,更优选为选自由丙烯酸和丁烯酸组成的组中的至少一种。
另外,作为上述含羧基单体,还可以举出肉桂酸、3-烯丙氧基丙酸、衣康酸、衣康酸单酯、马来酸、马来酸单酯、马来酸酐、富马酸、富马酸单酯、邻苯二甲酸乙烯酯、苯均四酸乙烯酯、柠康酸、中康酸、乌头酸等。
作为上述含氨基单体,可以举出例如由CH2=CH-O-(CH2)x-NH2(x=0~10)表示的氨基乙烯基醚类;由CH2=CH-O-CO(CH2)x-NH2(x=1~10)表示的胺类;以及氨基甲基苯乙烯、乙烯胺、丙烯酰胺、乙烯基乙酰胺、乙烯基甲酰胺等。
作为上述含水解性甲硅烷基单体,可示例出例如CH2=CHCO2(CH2)3Si(OCH3)3、CH2=CHCO2(CH2)3Si(OC2H5)3、CH2=C(CH3)CO2(CH2)3Si(OCH3)3、CH2=C(CH3)CO2(CH2)3Si(OC2H5)3、CH2=CHCO2(CH2)3SiCH3(OC2H5)2、CH2=C(CH3)CO2(CH2)3SiC2H5(OCH3)2、CH2=C(CH3)CO2(CH2)3Si(CH3)2(OC2H5)、CH2=C(CH3)CO2(CH2)3Si(CH3)2OH、CH2=CH(CH2)3Si(OCOCH3)3、CH2=C(CH3)CO2(CH2)3SiC2H5(OCOCH3)2、CH2=C(CH3)CO2(CH2)3SiCH3(N(CH3)COCH3)2、CH2=CHCO2(CH2)3SiCH3[ON(CH3)C2H5]2、CH2=C(CH3)CO2(CH2)3SiC6H5[ON(CH3)C2H5]2等(甲基)丙烯酸酯类;CH2=CHSi[ON=C(CH3)(C2H5)]3、CH2=CHSi(OCH3)3、CH2=CHSi(OC2H5)3、CH2=CHSiCH3(OCH3)2、CH2=CHSi(OCOCH3)3、CH2=CHSi(CH3)2(OC2H5)、CH2=CHSi(CH3)2SiCH3(OCH3)2、CH2=CHSiC2H5(OCOCH3)2、CH2=CHSiCH3[ON(CH3)C2H5]2、乙烯基三氯硅烷或它们的部分水解物等乙烯基硅烷类;三甲氧基甲硅烷基乙基乙烯基醚、三乙氧基甲硅烷基乙基乙烯基醚、三甲氧基甲硅烷基丁基乙烯基醚、甲基二甲氧基甲硅烷基乙基乙烯基醚、三甲氧基甲硅烷基丙基乙烯基醚、三乙氧基甲硅烷基丙基乙烯基醚等乙烯基醚类等。
作为上述的不含羟基的烷基乙烯基醚,可以举出甲基乙烯基醚、乙基乙烯基醚、正丙基乙烯基醚、正丁基乙烯基醚、十八烷基乙烯基醚、2-乙基己基乙烯基醚、环己基乙烯基醚、异丙基乙烯基醚、异丁基乙烯基醚等,其中优选为选自由乙基乙烯基醚和环己基乙烯基醚组成的组中的至少一种。
作为上述烯烃,可以举出乙烯、丙烯、正丁烯、异丁烯等非氟系烯烃等。
聚合物(A)可以适当地用于后述的本发明的组合物、本发明的涂膜、本发明的层积体、本发明的背板、本发明的太阳能电池组件等。
聚合物(A)可以利用溶液聚合法、乳液聚合法、悬浮聚合法或本体聚合法制造,其中优选利用溶液聚合法得到的聚合物。
聚合物(A)优选通过使用有机溶剂或聚合引发剂的溶液聚合法对提供上述单元的单体进行聚合而制造。聚合温度通常为0~150℃、优选为5~95℃。聚合压力通常为0.1~10MPaG(1~100kgf/cm2G)。
作为上述有机溶剂,可以举出乙酸甲酯、乙酸乙酯、乙酸丙酯、乙酸正丁酯、乙酸叔丁酯等酯类;丙酮、甲基乙基酮、环己酮等酮类;己烷、环己烷、辛烷、壬烷、癸烷、十一烷、十二烷、矿物精油等脂肪族烃类;苯、甲苯、二甲苯、萘、溶剂石脑油等芳香族烃类;甲醇、乙醇、叔丁醇、异丙醇、乙二醇单烷基醚等醇类;四氢呋喃、四氢吡喃、二氧六环等环状醚类;二甲基亚砜等;或它们的混合物等。
作为上述聚合引发剂,可以使用例如过硫酸铵、过硫酸钾等过硫酸盐类(还可以进一步根据需要合用亚硫酸氢钠、焦亚硫酸钠、环烷酸钴、二甲基苯胺等还原剂);由氧化剂(例如过氧化铵、过氧化钾等)与还原剂(例如亚硫酸钠等)以及过渡金属盐(例如硫酸铁等)构成的氧化还原引发剂类;过氧化乙酰、过氧化苯甲酰等过氧化二酰类;异丙氧基羰基过氧化物、叔丁氧基羰基过氧化物等二烷氧基羰基过氧化物类;过氧化甲基乙基酮、过氧化环己酮等过氧化酮类;过氧化氢、叔丁基过氧化氢、氢过氧化枯烯等氢过氧化物类;二叔丁基过氧化物、二枯基过氧化物等二烷基过氧化物类;叔丁基过氧化乙酸酯、叔丁基过氧化新戊酸酯等烷基过氧化酯类;2,2’-偶氮二异丁腈、2,2’-偶氮二(2,4-二甲基戊腈)、2,2’-偶氮二(2-甲基戊腈)、2,2’-偶氮二(2-环丙基丙腈)、2,2’-偶氮二异丁酸二甲酯、2,2’-偶氮二[2-(羟基甲基)丙腈]、4,4’-偶氮二(4-氰基戊烯酸)等偶氮系化合物等。
本发明的组合物包含聚合物(在本说明书中有时称为“聚合物(B)”)和多异氰酸酯化合物。上述组合物可适当地用作涂料。
聚合物(B)以羟值为90mgKOH/g以上作为其特征之一。作为上述羟值,优选为100mgKOH/g以上、更优选为110mgKOH/g以上,优选为180mgKOH/g以下、更优选为160mgKOH/g以下。
上述羟值由聚合物(B)的重量和-OH基的摩尔数通过计算求出。-OH基的摩尔数可以通过NMR测定、IR测定、滴定、元素分析等求出。
聚合物(B)包含全卤烯烃单元以及含羟基单体单元。
上述全卤烯烃单元与构成聚合物(A)的全卤烯烃单元是同样的。另外,上述含羟基单体单元与构成聚合物(A)的含羟基单体单元是同样的。
作为上述全卤烯烃单元的含量,相对于聚合物(B)的全部单体单元优选为30~90摩尔%、更优选为30~60摩尔%、进一步优选为40~55摩尔%。
作为上述含羟基单体单元的含量,相对于聚合物(B)的全部单体单元优选为10~70摩尔%、更优选为10~40摩尔%、进一步优选为15~35摩尔%。
聚合物(B)优选进一步包含选自由不含羟基和芳香环中的任一种的乙烯基酯单元和不含羟基的烷基乙烯基醚单元组成的组中的至少一种单元(b),更优选包含不含羟基和芳香环中的任一种的乙烯基酯单元。上述乙烯基酯和烷基乙烯基醚优选不含卤原子。
上述不含羟基和芳香环中的任一种的乙烯基酯单元与构成聚合物(A)的不含羟基和芳香环中的任一种的乙烯基酯单元是同样的。上述烷基乙烯基醚单元与构成聚合物(A)的不含羟基的烷基乙烯基醚单元是同样的。
聚合物(B)包含单元(b)的情况下,作为单元(b)的含量,相对于聚合物(B)的全部单体单元优选为1~35摩尔%、更优选为10~30摩尔%。
聚合物(B)也可以进一步包含作为构成聚合物(A)的单体单元而例示出的包含芳香环且不含羟基的羧酸乙烯酯、含羧基单体、含氨基单体、含水解性甲硅烷基单体、不含卤原子和羟基的烯烃等的单元。这些单体单元的含量相对于聚合物(B)的全部单体单元可以为0~10摩尔%,优选为0.1~5摩尔%、更优选为0.5~3摩尔%。
作为聚合物(B),优选为聚合物(A)。
聚合物(B)优选数均分子量为3000~100000。上述数均分子量更优选为5000以上、进一步优选为8000以上,更优选为50000以下、进一步优选为35000以下。数均分子量若过小,则耐候性、耐溶剂性和耐污染性差,同时有可能无法形成具有高硬度的涂膜;数均分子量若过大,则在制成涂料的情况下的粘度增大,可能难以处理。上述数均分子量可以通过使用四氢呋喃作为洗脱液的凝胶渗透色谱法(GPC)进行测定。
聚合物(B)通过差示扫描量热计(DSC)求出的玻璃化转变温度(第二轮)优选为10~70℃、更优选为15~60℃。玻璃化转变温度若过小,则耐候性、耐溶剂性和耐污染性差,同时可能无法形成具有高硬度的涂膜;玻璃化转变温度若过大,则在制成涂料的情况下的粘度增大,可能难以处理。
从与多异氰酸酯化合物或颜料等的相容性良好的方面考虑,聚合物(B)的酸值优选为0.6~28.8mgKOH/g、更优选为2~12mgKOH/g。
本发明的组合物还具有下述特征:其进一步包含多异氰酸酯化合物,上述多异氰酸酯化合物所具有的异氰酸酯基(NCO)与上述聚合物所具有的羟基(OH)的当量比(NCO/OH)小于1.0。
若当量比小于1.0,则即使上述聚合物通过上述多异氰酸酯化合物发生交联,聚合物(B)所具有的羟基的一部分也不会在与异氰酸酯基的反应中被消耗而仍残留。据预测,若有羟基残留,则涂膜中的交联密度不充分,耐磨耗性降低;而与该预测相反,现已判明得到了具有优异的耐磨耗性的涂膜。其理由据推测是由于残留的羟基在涂膜中形成氢键。而且据推测,残留的羟基还有助于与基材的密合性。即,通过使聚合物(B)的羟值高、且上述当量比小于1.0,能够得到与基材具有良好的密合性、由落砂磨耗性试验测定的耐磨耗性优异的涂膜。
出于得到更优异的密合性和耐磨耗性的原因,作为上述当量比优选为0.90以下、更优选为0.85以下,优选为0.20以上、更优选为0.30以上。
作为上述多异氰酸酯化合物,优选为选自由下述化合物组成的组中的至少一种化合物:衍生自选自由苯二亚甲基二异氰酸酯(XDI)和双(异氰酸根合甲基)环己烷(氢化XDI、H6XDI)组成的组中的至少一种异氰酸酯的多异氰酸酯化合物、基于六亚甲基二异氰酸酯(HDI)的封端异氰酸酯化合物、衍生自六亚甲基二异氰酸酯(HDI)的多异氰酸酯化合物、衍生自异佛尔酮二异氰酸酯(IPDI)的多异氰酸酯化合物、以及水分散性多异氰酸酯化合物。
作为上述多异氰酸酯化合物使用衍生自选自由苯二亚甲基二异氰酸酯(XDI)和双(异氰酸根合甲基)环己烷(氢化XDI、H6XDI)组成的组中的至少一种异氰酸酯(以下也称为异氰酸酯(i))的多异氰酸酯化合物(以下也称为多异氰酸酯化合物(I))的情况下,密合性更为优异。
作为上述多异氰酸酯化合物(I),可以举出例如:上述异氰酸酯(i)与3元以上的脂肪族多元醇经加成聚合而得到的加成物、由上述异氰酸酯(i)形成的异氰脲酸酯结构体(三聚氰酸酯结构体(nurate structures))以及由上述异氰酸酯(i)形成的缩二脲(ビウレット)。
作为上述加成物,例如优选具有如下通式(1)所表示的结构:
[化1]
(式中,R1表示碳原子数为3~20的脂肪族烃基。R2表示亚苯基或亚环己基。K为3~20的整数)。
上述通式(1)中的R1为基于上述3元以上的脂肪族多元醇的烃基,更优选碳原子数为3~10的脂肪族烃基,进一步优选碳原子数为3~6的脂肪族烃基。
上述R2为亚苯基的情况下,可以为1,2-亚苯基(邻亚苯基)、1,3-亚苯基(间亚苯基)以及、1,4-亚苯基(对亚苯基)中的任一种。其中优选1,3-亚苯基(间亚苯基)。另外,上述通式(1)中的全部R2可以是相同的亚苯基,也可以混存有2种以上。
上述R2为亚环己基的情况下,可以为1,2-亚环己基、1,3-亚环己基以及1,4-亚环己基中的任一种。其中优选1,3-亚环己基。另外,上述通式(1)中的全部R2可以是相同的亚环己基,也可以混存有2种以上。
上述k为与3元以上的脂肪族多元醇的元数对应的数。作为上述k,更优选为3~10的整数、进一步优选为3~6的整数。
上述异氰脲酸酯结构体在分子中具有1个或2个以上由下述通式(2)表示的异氰脲酸酯环。
[化2]
作为上述异氰脲酸酯结构体,可以举出:通过上述异氰酸酯的三聚化反应得到的三聚体、通过五聚化反应得到的五聚体、通过七聚化反应得到的七聚体等。
其中优选由下述通式(3)所表示的三聚体:
[化3]
(式中,R2与通式(1)中的R2相同)。即,上述异氰脲酸酯结构体优选为选自由苯二亚甲基二异氰酸酯和双(异氰酸根合甲基)环己烷组成的组中的至少一种异氰酸酯的三聚体。
上述缩二脲为具有由下述通式(4)所表示的结构的化合物:
[化4]
(式中,R2与通式(1)中的R2相同),该化合物可以通过在与得到上述异氰脲酸酯结构体的情况不同的条件下将上述异氰酸酯三聚化来得到。
作为上述多异氰酸酯化合物(I),其中优选上述加成物、即、使选自由苯二亚甲基二异氰酸酯和双(异氰酸根合甲基)环己烷组成的组中的至少一种异氰酸酯与3元以上的脂肪族多元醇进行加成聚合而得到的物质。
上述多异氰酸酯化合物(I)为上述异氰酸酯(i)与3元以上的脂肪族多元醇的加成物的情况下,作为该3元以上的脂肪族多元醇,具体地说,可以举出甘油、三羟甲基丙烷(TMP)、1,2,6-己三醇、三羟甲基乙烷、2,4-二羟基-3-羟基甲基戊烷、1,1,1-三(双羟基甲基)丙烷、2,2-双(羟基甲基)-3-丁醇等3元醇;季戊四醇、双甘油等4元醇;阿拉伯糖醇、核醣醇、木糖醇等5元醇(戊五醇);山梨糖醇、甘露醇、半乳糖醇、阿洛醇等6元醇(己糖醇)等。其中特别优选三羟甲基丙烷、季戊四醇。
另外,关于作为上述加成物的构成成分使用的苯二亚甲基二异氰酸酯(XDI),可以举出1,3-苯二亚甲基二异氰酸酯(间苯二亚甲基二异氰酸酯)、1,2-苯二亚甲基二异氰酸酯(邻苯二亚甲基二异氰酸酯)、1,4-苯二亚甲基二异氰酸酯(对苯二亚甲基二异氰酸酯),其中优选1,3-苯二亚甲基二异氰酸酯(间苯二亚甲基二异氰酸酯)。
另外,关于作为上述加成物的构成成分使用的双(异氰酸根合甲基)环己烷(氢化XDI、H6XDI),可以举出1,3-双(异氰酸根合甲基)环己烷、1,2-双(异氰酸根合甲基)环己烷、1,4-双(异氰酸根合甲基)环己烷,其中优选1,3-双(异氰酸根合甲基)环己烷。
通过使选自由苯二亚甲基二异氰酸酯和双(异氰酸根合甲基)环己烷组成的组中的至少一种异氰酸酯与上述的3元以上的脂肪族多元醇进行加成聚合而得到加成物。
作为上述加成物,具体地说,例如可以举出由下述通式(5)表示的化合物:
[化5]
(式中,R3表示亚苯基或亚环己基),即通过使选自由苯二亚甲基二异氰酸酯和双(异氰酸根合甲基)环己烷组成的组中的至少一种异氰酸酯与三羟甲基丙烷(TMP)经加成聚合而得到的多异氰酸酯化合物。
关于上述通式(5)中的由R3表示的亚苯基或亚环己基,如上述通式(1)中的R2中所述。
作为由上述通式(5)表示的多异氰酸酯化合物的市售品,可以举出TakenateD110N(三井化学株式会社制造,XDI与TMP的加成物、NCO含量11.8%)、Takenate D120N(三井化学株式会社制造,H6XDI与TMP的加成物、NCO含量11.0%)等。
作为上述多异氰酸酯化合物(I)为异氰脲酸酯结构体的情况下的具体例,可以举出Takenate D121N(三井化学株式会社制造,H6XDI三聚氰酸酯、NCO含量14.0%)、TakenateD127N(三井化学株式会社制造,H6XDI三聚氰酸酯、H6XDI的三聚体、NCO含量13.5%)等。
通过使用基于六亚甲基二异氰酸酯(HDI)的封端异氰酸酯(以下也简称为封端异氰酸酯)作为上述多异氰酸酯化合物,可使上述组合物具有充分的贮存期(可使用时间)。
作为上述封端异氰酸酯,优选利用封端剂使衍生自六亚甲基二异氰酸酯的多异氰酸酯化合物(以下也称为多异氰酸酯化合物(II))反应而得到。
作为上述多异氰酸酯化合物(II),可以举出例如:六亚甲基二异氰酸酯与3元以上的脂肪族多元醇经加成聚合而得到的加成物、由六亚甲基二异氰酸酯形成的异氰脲酸酯结构体(三聚氰酸酯结构体)、以及由六亚甲基二异氰酸酯形成的缩二脲。
作为上述加成物,例如优选为具有由下述通式(6)所表示的结构的物质:
[化6]
(式中,R4表示碳原子数为3~20的脂肪族烃基。K为3~20的整数)。
上述通式(6)中的R4为基于上述3元以上的脂肪族多元醇的烃基,更优选碳原子数为3~10的脂肪族烃基,进一步优选碳原子数为3~6的脂肪族烃基。
上述k为与3元以上的脂肪族多元醇的元数对应的数。作为上述k,更优选为3~10的整数、进一步优选为3~6的整数。
上述异氰脲酸酯结构体为在分子中具有1个或2个以上由下述通式(2)表示的异氰脲酸酯环。
[化7]
作为上述异氰脲酸酯结构体,可以举出:通过上述异氰酸酯的三聚化反应得到的三聚体、通过五聚化反应得到的五聚体、通过七聚化反应得到的七聚体等。
其中优选由下述通式(7)所表示的三聚体。
[化8]
上述缩二脲为具有由下述通式(8)所表示的结构的化合物:
[化9]
该化合物可以通过在与得到上述异氰脲酸酯结构体的情况不同的条件下将六亚甲基二异氰酸酯三聚化来得到。
作为上述封端剂,优选使用具有活性氢的化合物。作为上述具有活性氢的化合物,优选使用例如选自由醇类、肟类、内酰胺类、活性亚甲基化合物以及吡唑化合物组成的组中的至少一种。
这样,上述封端异氰酸酯为使封端剂与衍生自六亚甲基二异氰酸酯的多异氰酸酯化合物反应而得到的物质,上述封端剂优选为选自由醇类、肟类、内酰胺类、活性亚甲基化合物以及吡唑化合物组成的组中的至少一种。
用于得到上述封端异氰酸酯的多异氰酸酯化合物(II)为六亚甲基二异氰酸酯与3元以上的脂肪族多元醇的加成物的情况下,作为该3元以上的脂肪族多元醇,具体地说,可以举出甘油、三羟甲基丙烷(TMP)、1,2,6-己烷三醇、三羟甲基乙烷、2,4-二羟基-3-羟基甲基戊烷、1,1,1-三(双羟基甲基)丙烷、2,2-双(羟基甲基)-3-丁醇等3元醇;季戊四醇、双甘油等4元醇;阿拉伯糖醇、核醣醇、木糖醇等5元醇(戊五醇);山梨糖醇、甘露醇、半乳糖醇、阿洛醇等6元醇(己糖醇)等。其中特别优选三羟甲基丙烷、季戊四醇。
通过使六亚甲基二异氰酸酯与上述的3元以上的脂肪族多元醇进行加成聚合而得到上述加成物。
作为与上述多异氰酸酯化合物(II)反应的具有活性氢的化合物,具体地说,可以举出甲醇、乙醇、正丙醇、异丙醇、甲氧基丙醇等醇类;丙酮肟、2-丁酮肟、环己酮肟等肟类;ε-己内酰胺等内酰胺类;乙酰乙酸甲酯、丙二酸二乙酯等活性亚甲基化合物;3-甲基吡唑、3,5-二甲基吡唑、3,5-二乙基吡唑等吡唑化合物等,可以使用它们中的1种或2种以上。
其中优选活性亚甲基化合物、肟类,更优选活性亚甲基化合物。
作为上述封端异氰酸酯的市售品,可以举出DURANATE K6000(旭化成化学株式会社制造,HDI的活性亚甲基化合物封端异氰酸酯)、DURANATE TPA-B80E(旭化成化学株式会社制造)、DURANATE MF-B60X(旭化成化学株式会社制造)、DURANATE17B-60PX(旭化成化学株式会社制造)、CORONET2507(日本聚氨酯工业株式会社制造)、CORONET2513(日本聚氨酯工业株式会社制造)、CORONET2515(日本聚氨酯工业株式会社制造)、Sumidur BL-3175(Sumika Bayer Urethane公司制造)、Luxate HC1170(Olin Chemicals公司制造)、LuxateHC2170(Olin Chemicals公司制造)等。
作为上述多异氰酸酯化合物,还可以使用衍生自六亚甲基二异氰酸酯(HDI)的多异氰酸酯化合物(以下也称为多异氰酸酯化合物(III))。作为多异氰酸酯化合物(III),可以举出作为多异氰酸酯化合物(II)的上述物质。
作为多异氰酸酯化合物(III)的具体例,可以举出:CORONET HX(日本聚氨酯工业株式会社制造,六亚甲基二异氰酸酯的异氰脲酸酯结构体、NCO含量21.1%)、SumidurN3300(Sumika Bayer Urethane公司制造,六亚甲基二异氰酸酯的异氰脲酸酯结构体)、Takenate D170N(三井化学株式会社制造,六亚甲基二异氰酸酯的异氰脲酸酯结构体)、Sumidur N3800(Sumika Bayer Urethane公司制造,六亚甲基二异氰酸酯的异氰脲酸酯结构体预聚物型)、D-370N(三井化学株式会社制造,NCO含量25.0%)、AE-700(旭化成株式会社制造,NCO含量11.9%)、D-201(三井化学株式会社制造,NCO含量15.8%)等。
作为上述多异氰酸酯化合物,还可以使用衍生自异佛尔酮二异氰酸酯(IPDI)的多异氰酸酯化合物(以下也称为多异氰酸酯化合物(IV))。
作为上述多异氰酸酯化合物(IV),可以举出例如:异佛尔酮二异氰酸酯与3元以上的脂肪族多元醇经加成聚合而得到的加成物、由异佛尔酮二异氰酸酯形成的异氰脲酸酯结构体(三聚氰酸酯结构体)、以及由异佛尔酮二异氰酸酯形成的缩二脲。
作为上述加成物,例如优选为具有由下述通式(9)所表示的结构的物质:
[化10]
(式中,R5表示碳原子数为3~20的脂肪族烃基。R6为由下述通式(10)表示的基团:
[化11]
k为3~20的整数)。
上述通式(9)中的R5为基于上述3元以上的脂肪族多元醇的烃基,更优选碳原子数为3~10的脂肪族烃基,进一步优选碳原子数为3~6的脂肪族烃基。
上述k为与3元以上的脂肪族多元醇的元数对应的数。作为上述k,更优选为3~10的整数、进一步优选为3~6的整数。
上述异氰脲酸酯结构体为在分子中具有1个或2个以上由如下通式(2)所表示的异氰脲酸酯环的物质。
[化12]
作为上述异氰脲酸酯结构体,可以举出:通过异佛尔酮二异氰酸酯的三聚化反应得到的三聚体、通过五聚化反应得到的五聚体、通过七聚化反应得到的七聚体等。
其中优选由下述通式(11)所表示的三聚体:
[化13]
(式中,R6与通式(9)中的R6相同)。即,上述异氰脲酸酯结构体优选为异佛尔酮二异氰酸酯的三聚体。
上述缩二脲为具有由下述通式(12)所表示的结构的化合物:
[化14]
(式中,R6与通式(9)中的R6相同),该化合物可以通过在与得到上述异氰脲酸酯结构体的情况不同的条件下将异佛尔酮二异氰酸酯三聚化来得到。
作为上述多异氰酸酯化合物(IV),其中优选为选自由上述加成物和上述异氰脲酸酯结构体组成的组中的至少一种。即,上述多异氰酸酯化合物(IV)优选为选自由使异佛尔酮二异氰酸酯与3元以上的脂肪族多元醇经加成聚合得到的加成物以及由异佛尔酮二异氰酸酯形成的异氰脲酸酯结构体组成的组中的至少一种。
上述多异氰酸酯化合物(IV)为异佛尔酮二异氰酸酯与3元以上的脂肪族多元醇的加成物的情况下,作为该3元以上的脂肪族多元醇,具体地说,可以举出甘油、三羟甲基丙烷(TMP)、1,2,6-己三醇、三羟甲基乙烷、2,4-二羟基-3-羟基甲基戊烷、1,1,1-三(双羟基甲基)丙烷、2,2-双(羟基甲基)-3-丁醇等3元醇;季戊四醇、双甘油等4元醇;阿拉伯糖醇、核醣醇、木糖醇等5元醇(戊五醇);山梨糖醇、甘露醇、半乳糖醇、阿洛醇等6元醇(己糖醇)等。其中特别优选三羟甲基丙烷、季戊四醇。
通过进行异佛尔酮二异氰酸酯与上述3元以上的脂肪族多元醇的加成聚合,得到在本发明中适合使用的加成物。
作为本发明中优选使用的加成物,具体地说,可以举出例如由下述通式(13)所表示的化合物:
[化15]
(式中,R7为由下述通式(10)所表示的基团):
[化16]
即可以举出通过进行异佛尔酮二异氰酸酯与三羟甲基丙烷(TMP)的加成聚合而得到的多异氰酸酯化合物。
作为由上述通式(13)所表示的多异氰酸酯化合物(异佛尔酮二异氰酸酯的TMP加成体)的市售品,可以举出Takenate D140N(三井化学株式会社制造,NCO含量11%)等。
作为由异佛尔酮二异氰酸酯形成的异氰脲酸酯结构体的市售品,可以举出Desmodur Z4470(Sumika Bayer Urethane公司制造,NCO含量11%)等。
作为上述多异氰酸酯化合物,还可以使用水分散性多异氰酸酯化合物。上述水分散性多异氰酸酯化合物是指加入到水性介质中并进行搅拌时可形成水分散体的多异氰酸酯化合物。作为这样的水分散性多异氰酸酯化合物,可以举出例如:(1)疏水性多异氰酸酯与具有亲水性基团的多异氰酸酯的混合物;(2)疏水性多异氰酸酯与不具有异氰酸酯基但具有亲水性基团的分散剂的混合物;(3)仅为具有亲水性基团的多异氰酸酯;等等。需要说明的是,本发明中,亲水性基团是指阴离子性基团、阳离子性基团或非离子性基团。作为上述水分散性多异氰酸酯化合物,特别优选为具有亲水性基团的多异氰酸酯。
上述疏水性多异氰酸酯是指不具有亲水性基团的多异氰酸酯,可以举出例如:1,4-四亚甲基二异氰酸酯、乙基(2,6-二异氰酸根合)己酸酯、1,6-六亚甲基二异氰酸酯、1,12-十二亚甲基二异氰酸酯、2,2,4-或2,4,4-三甲基六亚甲基二异氰酸酯等脂肪族二异氰酸酯;1,3,6-六亚甲基三异氰酸酯、1,8-二异氰酸根合-4-异氰酸根合甲基辛烷、2-异氰酸根合乙基(2,6-二异氰酸根合)己酸酯等脂肪族三异氰酸酯;1,3-双(异氰酸根合甲基环己烷)、1,4-双(异氰酸根合甲基环己烷)、1,3-二异氰酸根合环己烷、1,4-二异氰酸根合环己烷、3,5,5-三甲基(3-异氰酸根合甲基)环己基异氰酸酯、二环己基甲烷-4,4’-二异氰酸酯、2,5-二异氰酸根合甲基降莰烷、2,6-二异氰酸根合甲基降莰烷等脂环族二异氰酸酯;2,5-二异氰酸根合甲基-2-异氰酸根合丙基降莰烷、2,6-二异氰酸根合甲基-2-异氰酸根合丙基降莰烷等脂环族三异氰酸酯;间苯二亚甲基二异氰酸酯、α,α,α’α’-四甲基-间苯二亚甲基二异氰酸酯等亚芳烷基二异氰酸酯;间或对苯二异氰酸酯、甲苯-2,4-二异氰酸酯、甲苯-2,6-二异氰酸酯、二苯基甲烷-4,4’-二异氰酸酯、萘-1,5-二异氰酸酯、二苯基-4,4’-二异氰酸酯、4,4’-二异氰酸根合-3,3’-二甲基二苯酯、3-甲基-二苯基甲烷-4,4’-二异氰酸酯、二苯基醚-4,4’-二异氰酸酯等芳香族二异氰酸酯;三苯甲烷三异氰酸酯、三(异氰酸根合苯基)硫代磷酸酯等芳香族三异氰酸酯;上述二异氰酸酯或三异氰酸酯的异氰酸酯基彼此经环化二聚而得到的具有缩脲二酮结构的多异氰酸酯;上述二异氰酸酯或三异氰酸酯的异氰酸酯基彼此经环化三聚而得到的具有异氰脲酸酯结构的多异氰酸酯;通过使上述二异氰酸酯或三异氰酸酯与水反应而得到的具有双缩脲(ビュレット)结构的多异氰酸酯;通过使上述二异氰酸酯或三异氰酸酯与二氧化碳反应而得到的具有噁二嗪三酮结构的多异氰酸酯;具有脲基甲酸酯结构的多异氰酸酯等。它们之中,出于可形成致密的交联涂膜、能够进一步提高固化涂膜的耐醇性的原因,优选具有异氰脲酸酯结构的多异氰酸酯。
作为上述具有亲水性基团的多异氰酸酯,可以举出例如具有亲水性基团和异氰酸酯基的聚醚、聚酯、聚氨酯、乙烯基聚合物、醇酸树脂、氟树脂、硅树脂等。它们之中,出于水分散性良好的原因,优选具有亲水性基团和异氰酸酯基的聚醚或乙烯基聚合物,更优选具有亲水性基团和异氰酸酯基的聚醚。这些具有亲水性基团的多异氰酸酯可以单独使用、也可以将2种以上合用。
作为水分散性多异氰酸酯化合物的市售品,可以举出Bayhydur XP 2700(SumikaBayer Urethane公司制造)、Bayhydur 3100(Sumika Bayer Urethane公司制造)等。
作为上述多异氰酸酯化合物,其中更优选Takenate D120N(三井化学株式会社制造,NCO含量11%)、Sumidur N3300(Sumika Bayer Urethane公司制造,六亚甲基二异氰酸酯的异氰脲酸酯结构体)。
本发明的组合物优选进一步包含溶剂。作为上述溶剂,优选水或有机溶剂。作为上述有机溶剂,可以举出:乙酸乙酯、乙酸正丁酯、乙酸叔丁酯、乙酸异丙酯、乙酸异丁酯、乙酸溶纤剂、丙二醇甲基醚乙酸酯等酯类;丙酮、甲基乙基酮、甲基异丁基酮、环己酮等酮类;四氢呋喃、二氧六环等环状醚类;N,N-二甲基甲酰胺、N,N-二甲基乙酰胺等酰胺类;甲苯、二甲苯等芳香族烃类;丙二醇甲醚等醇类;己烷、庚烷等烃类;这些的混合溶剂等。另外还可以举出被称为弱溶剂的劳动安全卫生法的第三种有机溶剂以及与其相当的溶剂。在制成有机溶剂溶液的情况下,使聚合物(B)的浓度为5~95质量%、优选为10~80质量%即可。
上述组合物还优选进一步包含聚合物(B)以外的树脂。作为其他树脂,可以举出聚苯乙烯、(甲基)丙烯酸系树脂、聚酯系树脂、醇酸树脂、三聚氰胺-甲醛树脂、多异氰酸酯系树脂、环氧系树脂、氯乙烯系树脂(例如氯乙烯-乙酸乙烯酯共聚物等)、酮树脂、石油树脂;以及聚乙烯、聚丙烯等聚烯烃类的氯化物等有机系树脂;硅胶或硅酸等无机系树脂;聚合物(B)以外的各种氟树脂(例如四氟乙烯、三氟氯乙烯的均聚物或它们与其他单体的共聚物等)等。相对于聚合物(B)100质量份,其他树脂的比例为900质量份以下、优选为500质量份以下。下限为得到目的特性所需要的量,根据树脂的种类决定。在(甲基)丙烯酸系树脂的情况下通常为5质量份以上、优选为10质量份以上。
上述组合物优选包含这些树脂中的特别是相容性优异的(甲基)丙烯酸系树脂,从而对所得到的涂膜提供高光泽、高硬度、良好的成品外观。
作为(甲基)丙烯酸系树脂,可以举出一直以来在涂料用途中使用的(甲基)丙烯酸系聚合物,特别优选采用(i)(甲基)丙烯酸的碳原子数为1~10的烷基酯的均聚物或共聚物、以及(ii)在侧链和/或主链末端具有固化性官能团的(甲基)丙烯酸酯共聚物。
作为上述(i)的(甲基)丙烯酸系聚合物,可以举出例如(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸-2-乙基己基酯等(甲基)丙烯酸的碳原子数为1~10的烷基酯的均聚物和共聚物、或者这些烷基酯与能够共聚的烯键式不饱和单体的共聚物。
作为上述能够共聚的烯键式不饱和单体,可以举出例如具有芳香族基团的(甲基)丙烯酸酯类、在α位具有氟原子或氯原子的(甲基)丙烯酸酯类、烷基被氟原子取代的(甲基)丙烯酸氟代烷基酯类、乙烯基醚类、乙烯酯类、苯乙烯等芳香族乙烯基单体类、乙烯、丙烯、异丁烯、氯乙烯、偏二氯乙烯等烯烃类、富马酸二酯类、马来酸二酯类、(甲基)丙烯腈等。
作为上述(ii)的(甲基)丙烯酸系聚合物,可示例出具有固化性官能团的单体与提供上述(i)中说明的(甲基)丙烯酸系聚合物的单体一起共聚而成的聚合物。作为含固化性官能团的单体,可以举出具有羟基、羧基、环氧基、氨基等的单体。作为上述(ii)的(甲基)丙烯酸系聚合物的具体例,可以举出例如(甲基)丙烯酸羟乙酯、(甲基)丙烯酸-2-羟丙酯、2-羟基乙基乙烯基醚、(甲基)丙烯酸、(甲基)丙烯酸缩水甘油酯、甲基丙烯酸-2-氨基乙酯、(甲基)丙烯酸-2-氨基丙酯等具有固化性官能团的单体与上述(甲基)丙烯酸的碳原子数为1~10的烷基酯的共聚物、或者这些单体与上述能够共聚的烯键式不饱和单体的共聚物,但并不仅限于此。
(甲基)丙烯酸系聚合物的数均分子量利用GPC测定优选为1000~200000、更优选为2000~100000。该数均分子量若增大,则溶剂溶解性倾向于降低;该数均分子量若减小,则耐候性倾向于产生问题。
上述组合物也可以进一步包含添加剂。作为添加剂,可以举出固化促进剂、颜料、分散剂、流动性改善剂、流平剂、消泡剂、凝胶化防止剂、紫外线吸收剂、抗氧化剂、亲水化剂、消光剂、密合改良剂、阻燃剂等。
作为上述颜料,可以举出二氧化钛。作为上述二氧化钛没有特别限定,可以为金红石型、锐钛矿型中的任一种,从耐候性的方面出发,优选金红石型。另外,作为上述二氧化钛,可以为二氧化钛微粒的表面进行了无机处理的二氧化钛或进行了有机处理的二氧化钛、或者为进行了无机和有机这两种处理的二氧化钛。作为进行了无机处理的二氧化钛,可以举出例如将二氧化钛微粒的表面利用氧化铝(Al2O3)或二氧化硅(SiO2)、氧化锆(ZrO2)被覆而成的二氧化钛。作为进行了有机处理的二氧化钛,可以举出利用硅烷偶联剂进行了表面处理的二氧化钛、利用有机硅氧烷进行了表面处理的二氧化钛、利用有机多元醇进行了表面处理的二氧化钛、利用烷基胺进行了表面处理的二氧化钛等。二氧化钛中,进一步优选通过滴定法得到的碱值高于酸值的二氧化钛。
作为上述二氧化钛的市售品,可以举出例如D-918(堺化学工业株式会社制造)、R-960、R-706、R-931(杜邦公司制造)、PFC-105(石原产业株式会社制造)等。
作为上述二氧化钛的含量,相对于聚合物(B)100质量份优选为1~500质量份。若小于1质量份,则可能无法屏蔽紫外线。若高于500质量份,则可能由于紫外线的作用而发生黄变、劣化。作为上述二氧化钛的含量,更优选为5质量份以上、进一步优选为10质量份以上,更优选为300质量份以下、进一步优选为200质量份以下。
作为上述颜料,还可以举出炭黑。作为上述炭黑没有特别限定,可以举出通常公知的炭黑。从紫外线屏蔽效果的方面考虑,上述炭黑的平均粒径优选为10~150nm、更优选为20~100nm。上述平均粒径为通过电子显微镜下的观察得到的值。
上述炭黑在上述组合物中可以发生凝集,从紫外线屏蔽效果的方面出发,这种情况下的平均粒径优选为50~1000nm、更优选为100~700nm、进一步优选为100~500nm。上述平均粒径为通过用激光衍射散射式粒度分布计测定而得到的值。
上述炭黑的含量相对于聚合物(B)100质量份优选为0.5~80质量份。炭黑的含量为上述范围内时,能够在上述组合物中良好地分散。上述炭黑的含量相对于聚合物(B)100质量份更优选为3质量份以上、进一步优选为10质量份以上,更优选为60质量份以下、进一步优选为50质量份以下。
作为上述炭黑的市售品,可以举出例如MA-100(三菱化学株式会社制造)、Raven-420(Columbia Carbon公司制造)等。
上述组合物包含上述颜料的情况下,优选进一步包含后述的分散剂或流动性改善剂。
作为上述分散剂,可以举出具有酸基(其中不包括具有不饱和基团的酸基)的化合物。作为上述酸基,可以举出磷酸基、羧酸基、磺酸基等。其中,从更长期地防止颜料的凝集、上述组合物的储藏稳定性优异的方面出发,优选为选自由磷酸基和羧酸基组成的组中的至少一种,更优选为磷酸基。另外,上述分散剂由不具有不饱和基团的化合物形成。由于不具有不饱和基团,因而不容易发生由于暴露于紫外线中所致的化合物的改性。
上述分散剂的重均分子量优选为300~1000000。该重均分子量若小于300,则吸附树脂层的立体稳定化不充分,可能无法防止二氧化钛的凝集。若高于1000000,则可能招致分色(色別れ)或耐候性的降低。上述重均分子量更优选为1000以上、更优选为100000以下。上述重均分子量可以通过凝胶渗透色谱(GPC)(聚苯乙烯换算)进行测定。
从有效地吸附在二氧化钛表面的方面出发,上述分散剂优选酸值为3~2000mgKOH/g。酸值更优选为5mgKOH/g以上、进一步优选为10mgKOH/g以上,更优选为1000mgKOH/g以下、进一步优选为500mgKOH/g以下。上述酸值可以通过使用碱性物质的酸碱滴定法进行测定。
上述分散剂可以进一步具有碱基。作为上述碱,可以举出例如氨基等。
从分散剂的长期储藏稳定性良好的方面出发,上述分散剂的碱值优选为15mgKOH/g以下、更优选为5mgKOH/g以下。上述分散剂的酸值为15mgKOH/g以下的情况下,碱值优选小于5mgKOH/g。
上述分散剂更优选实质上不含碱基。需要说明的是,实质上不含碱基是指,考虑到沾污、反应残渣、测定误差等,作为测定值的碱值为0.5mgKOH/g以下。上述碱值可以通过使用酸性物质的酸碱滴定法进行测定。
作为上述分散剂,可以使用市售品。可以举出例如Disparlon 2150、DisparlonDA-325、DA-375、DA-1200(商品名,楠本化成株式会社制造)、Flowlen G-700、G-900(商品名,共荣社化学株式会社制造)、SOLSPERSE26000、32000、36000、36600、41000、55000(商品名,日本路博润株式会社制造)、DISPERBYK-102、106、110、111、140、142、145、170、171、174、180(商品名,毕克化学(日本)株式会社制造)等。其中,从长期储藏稳定性良好的方面出发,优选Disparlon DA-375、Flowlen G-700、SOLSPERSE36000,更优选Disparlon DA-375。
上述分散剂优选与上述二氧化钛一起使用。上述分散剂的含量相对于二氧化钛100质量份优选为0.1~100质量份。分散剂若小于0.1质量份,则可能得不到防止颜料沉降的效果。若大于100质量份,则可能招致分色或耐候性的降低。上述分散剂的含量更优选为0.5质量份以上、进一步优选为1.5质量份以上,更优选为50质量份以下、进一步优选为20质量份以下。
作为上述流动性改善剂,可以举出具有酸基和碱基的缔合型丙烯酸系聚合物。上述缔合型丙烯酸系聚合物为具有下述效果的聚合物:丙烯酸系聚合物链中含有的极性基团通过聚合物链内或聚合物链间的氢键或电气相互作用而发生部分吸附等从而形成结构,结果使液体粘度增加。
作为上述丙烯酸系聚合物,可以举出例如含有(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)丙烯酸叔丁酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸-2-乙基己基酯、(甲基)丙烯酸异壬酯、(甲基)丙烯酸环己酯等(甲基)丙烯酸酯作为主要单体成分的共聚物。需要说明的是,“(甲基)丙烯酸酯”包括丙烯酸酯和甲基丙烯酸酯。
作为上述酸基,优选羧酸基、磷酸基、磺酸基。其中,从更长期地防止颜料的凝集、能够维持上述组合物的储藏稳定性的方面出发,优选羧酸基。作为上述碱基,可以举出氨基。
另外,上述流动性改善剂可以为羧酸与羟基胺或羟基亚胺等含氮化合物的反应物。进行反应的羧酸与含氮化合物的比例最优选为1:1。作为羧酸,可以举出二羧酸、酸酐。作为上述羟基胺,可以举出例如单乙醇胺、丙醇胺、二乙醇胺、三乙醇胺、正丁基二乙醇胺等伯、仲、叔烷醇胺或其混合物。作为上述羟基亚胺,可以举出例如具有噁唑啉结构的物质,具体地说,可以举出Alkaterge T(商品名,Angus Chemical公司制造)等。
上述流动性改善剂优选重均分子量为1000~1000000。该重均分子量若小于1000,则基于缔合的结构形成不充分,可能无法防止二氧化钛的沉降。该重均分子量若超过1000000,则液体粘度过度增加,涂布性可能受损。上述重均分子量更优选为5000以上、更优选为100000以下。上述重均分子量可以通过凝胶渗透色谱(GPC)(聚苯乙烯换算)进行测定。
作为上述流动性改善剂,可以使用市售品。可以举出例如SOLTHIX250(商品名,日本路博润株式会社制造)等。
上述流动性改善剂的含量在上述组合物中优选为0.05~20质量%。若小于0.05质量%,则可能无法防止二氧化钛的沉降。若大于20质量%,则可能发生分离或分色。上述流动性改善剂的含量更优选为0.1质量%以上、进一步优选为0.3质量%以上,更优选为10质量%以下、进一步优选为5质量%以下。
作为上述阻燃剂,优选为在燃烧初期产生非燃烧性的气体、对燃烧性气体进行稀释和/或氧隔绝从而发挥出阻燃性的物质。
作为上述阻燃剂,优选为选自由包含元素周期表5B族的化合物、包含元素周期表7B族的卤化物的化合物组成的组中的至少一种。
作为包含元素周期表7B族的卤化物的化合物,可以举出脂肪族、脂环族、芳香族有机卤化物,例如溴系的四溴双酚A(TBA)、十溴二苯醚(DBDPE)、八溴二苯醚(OBDPE)、TBA环氧/苯氧基低聚物、溴化交联聚苯乙烯、氯系的氯化石蜡、全氯环十五烷等。
作为包含元素周期表5B族的化合物,对于磷化合物可以举出例如磷酸酯、多磷酸盐系等。另外,锑化合物优选与卤化物组合使用,可以举出例如三氧化锑、五氧化锑等。此外还可以使用氢氧化铝、氢氧化镁、三氧化钼。
这些阻燃剂可以根据聚合物(B)的种类任意选择至少一种及混合量,但并不限于这些。
作为上述阻燃剂,具体地说,更优选含有磷氮的组合物(A)、或者含溴化合物与含锑化合物的混合物(B)。通过在聚合物(B)中组合这些阻燃剂,可发挥出高阻燃性。
作为上述含有磷氮的组合物(A),优选为焦磷酸哌嗪与三聚氰胺氰尿酸盐的混合物。作为焦磷酸哌嗪,可以举出例如日本特开昭48-088791号公报、美国专利第4599375号中公开的物质。作为三聚氰胺氰尿酸盐,可以举出将三聚氰胺与氰尿酸的反应生成物进行粉末化而得到的物质等。上述三聚氰胺与氰尿酸的反应生成物在其结构内具有大量的氮原子,在暴露于约350℃以上的高温时会产生氮气,显示出阻碍燃烧的作用。
上述含有磷氮的组合物(A)中,三聚氰胺氰尿酸盐相对于上述焦磷酸哌嗪的质量比优选为0.014~3.000的范围。三聚氰胺氰尿酸盐为上述范围时,阻燃性提高,涂膜的粘连性也良好。三聚氰胺氰尿酸盐相对于上述焦磷酸哌嗪的质量比在混合物中更优选为0.04以上、进一步优选为0.1以上,更优选为1.4以下、进一步优选为0.5以下。
关于能够作为上述含有磷氮的组合物(A)使用的市售品,可以举出例如SCFR-200(堺化学工业株式会社制造)、SCFR-110(堺化学工业株式会社制造)等。
作为上述含溴化合物,优选溴含量为65%以上、熔点为200℃以上、且5%分解温度为340℃以上的芳香族系化合物。
具体地说,上述含溴化合物优选为选自由十溴二苯醚、1,2-双(2,3,4,5,6-五溴苯基)乙烷、三(三溴苯氧基)三嗪、乙撑双四溴邻苯二甲酰亚胺、聚溴苯基茚满、溴化亚苯醚以及聚丙烯酸五溴苄酯组成的组中的至少一种。
其中,从熔点高、在将涂膜加热固化的情况下也不会发生熔解、渗出的方面出发,更优选由式(a)所表示的1,2-双(2,3,4,5,6-五溴苯基)乙烷。
[化17]
作为上述含溴化合物,可以使用市售品,可以举出例如SAYTEX8010(Albemarle公司制造)等。
作为上述含锑化合物,可以举出例如,三氧化锑、五氧化锑等氧化锑。其中,从能够低成本地获得的方面考虑,优选三氧化锑。
上述阻燃剂的含量相对于聚合物(B)100质量份优选为1~45质量份。上述阻燃剂的含量为上述范围时,能够期待在上述组合物中的良好的分散性以及提高由上述组合物得到的涂膜的阻燃性。上述阻燃剂的含量若小于1质量份,则可能无法期待阻燃性的提高;若超过45质量份,则可能难以维持组合物或涂膜的物性。上述阻燃剂的含量相对于聚合物(B)100质量份更优选为30质量份以下、进一步优选为20质量份以下、特别优选为15质量份以下。另外,更优选为3质量份以上、进一步优选为5质量份以上。
上述阻燃剂为上述含有磷氮的组合物(A)的情况下,其含量相对于聚合物(B)100质量份优选为8~19质量份。上述含有磷氮的组合物(A)的含量相对于聚合物(B)100质量份更优选为9质量份以上、进一步优选为10质量份以上,更优选为17质量份以下、进一步优选为15质量份以下。
上述阻燃剂为上述含溴化合物与含锑化合物的混合物(B)的情况下,关于其含量,相对于聚合物(B)100质量份,含溴化合物的含量优选为1~30质量份、含锑化合物的含量优选为0.5~15质量份。上述含溴化合物的含量相对于聚合物(B)100质量份更优选为3质量份以上、进一步优选为5质量份以上,更优选为20质量份以下、进一步优选为15质量份以下。上述锑化合物的含量相对于聚合物(B)100质量份更优选为1.5质量份以上、进一步优选为2.5质量份以上,更优选为10质量份以下、进一步优选为7.5质量份以下。
作为上述固化促进剂,可以举出例如有机锡化合物、酸性磷酸酯、酸性磷酸酯与胺的反应物、饱和或不饱和的多元羧酸或其酸酐、有机钛酸酯化合物、胺系化合物、辛酸铅等。
作为上述有机锡化合物的具体例,可以举出二月桂酸二丁基锡、马来酸二丁基锡、马来酸二辛基锡、二乙酸二丁基锡、邻苯二甲酸二丁基锡、辛酸锡、环烷酸锡、甲氧基二丁基锡等。
另外,上述酸性磷酸酯是包含
[化18]
部分的磷酸酯,可以举出例如由
(R9-O)b-P(=O)-(OH)3-b
(式中,b表示1或2,R9表示有机残基)表示的有机酸性磷酸酯等。
具体地说,可以举出下述物质等。
[化19]
作为上述有机钛酸酯化合物,可以举出例如钛酸四丁酯、钛酸四异丙酯、三乙醇胺钛酸酯等钛酸酯。作为市售品,可以举出例如Matsumoto Fine Chemicals公司制造的Orgatix TC-100、TC-750、TC-760、TA-30等。
此外,作为上述胺系化合物的具体例,可以举出例如丁胺、辛胺、二丁胺、单乙醇胺、二乙醇胺、三乙醇胺、二亚乙基三胺、三亚乙基四胺、油胺、环己胺、苄基胺、二乙基氨基丙胺、苯二甲胺、三乙二胺、胍、二苯基胍、2,4,6-三(二甲氨基甲基)苯酚、吗啉、N-甲基吗啉、1,8-二氮杂双环(5.4.0)十一碳烯-7(DBU)等胺系化合物、以及它们的羧酸等的盐、由过量的多元胺与多元酸得到的低分子量聚酰胺树脂、过量的多元胺与环氧化合物的反应生成物等。
上述固化促进剂可以使用1种,也可以合用2种以上。上述固化促进剂的混合比例相对于聚合物(B)100质量份优选为1.0×10-6~1.0×10-2质量份左右,更优选为5.0×10-5~1.0×10-3质量份左右。
作为颜料的具体例,可以举出例如二氧化钛、碳酸钙或炭黑等无机颜料;酞菁系、喹吖啶酮系或偶氮系等有机颜料等,但并不仅限于这些。相对于聚合物(B)100质量份,颜料的添加量的上限通常最高为约200质量份。
作为上述亲水化剂,可以使用硅酸甲酯、硅酸乙酯、氟代烷基硅酸酯、它们的缩合物。作为市售品,可以举出例如COLCOAT公司制造的ET40、ET48等;三菱化学株式会社制造的MS56、MS56S、MS57等;大金工业株式会社制造的GH700、GH701等。
作为上述消光剂,可以举出氧化硅、氧化硅-氧化铝、氧化铝、滑石、碳酸钙、二氧化钛等。上述消光剂的添加量相对于聚合物(B)优选为1~100质量%。作为市售品,可以举出例如Fuji Silysia公司制造的Sylysia 350、Sylysia 436、Sylysia 446、Sylophobic 100、Sylophobic 200;Grace公司制造的Syloid ED2、Syloid ED30、Syloid ED50等。
作为上述密合改良剂,可以举出聚酯多元醇、聚碳酸酯多元醇、聚醚多元醇、聚丁二烯多元醇等各种多元醇系添加剂、硅烷偶联剂等。上述密合改良剂的添加量相对于聚合物(B)优选为0.1~50质量%。作为市售品,可以举出例如楠本化成株式会社制造的FLEXOREZ 148、FLEXOREZ 188、FLEXOREZ A308;宇部兴产株式会社制造的ETERNACOLL UH-50、ETERNACOLL UM-90;ADEKA公司制造的ADEKA Polyether P-400、ADEKA Polyol BPX-21;日本曹达株式会社制造的NISSO-PB GI-1000、GI-2000、GI-3000;宇部兴产株式会社制造的PH-50、PH-100;Croda Japan株式会社制造的Priplast-1838、Priplast-3192等。
本发明还涉及一种涂膜,其特征在于,其包含聚合物(A)。上述涂膜由于该特征而与基材具有良好的密合性,在高压蒸煮测试后也具有良好的密合性,由落砂磨耗性试验测定的耐磨耗性优异。上述涂膜优选为固化涂膜。
另外,本发明还涉及一种涂膜,其特征在于,其由上述组合物形成。上述涂膜由于该特征而与基材具有良好的密合性,在高压蒸煮测试后也具有良好的密合性,由落砂磨耗性试验测定的耐磨耗性优异。从密合性和耐磨耗性的方面出发,形成上述涂膜的上述组合物中包含的聚合物(B)优选为聚合物(A)。
上述涂膜可以通过将上述组合物涂布至基材等,根据希望进行干燥和固化来得到。上述干燥和固化可以在10~300℃、通常在100~200℃进行30秒至3天。在上述干燥和固化后可以进行养护,上述养护通常在20~300℃利用1分钟~3天完成。
上述涂膜的特征还在于,其包含氨基甲酸酯键,落砂磨耗性为80L以上。上述涂膜由于这些特征因而耐磨耗性优异,此外与基材具有良好的初期密合性,高压蒸煮测试后也具有良好的密合性,由于高交联密度而使涂膜强度增加,从而使得辊加工时的破裂减轻性也优异。具备这些特征的涂膜能够由上述组合物适宜地制造。特别是上述氨基甲酸酯键通过上述组合物中包含的多异氰酸酯化合物所具有的异氰酸酯基与聚合物(B)所具有的羟基发生反应而形成。上述涂膜包含氨基甲酸酯键这一点可通过红外分光法(IR)来确认。
对上述落砂磨耗性的上限没有特别限定,可以为250L。上述落砂磨耗性可以通过JIS A 1452:1972建筑物材料及建筑物结构部件的磨耗试验方法(落砂法)进行测定。
从隐蔽性、耐候性、耐化学药品性、耐湿性良好的方面出发,上述涂膜的膜厚优选为5μm以上。该膜厚更优选为7μm以上、进一步优选为10μm以上。由于若膜厚过厚则得不到轻量化效果,因而上限优选为1000μm左右、更优选为100μm左右。作为膜厚,特别优选为10~40μm。
上述涂膜可以设置在各种基材上。在上述基材与上述涂膜之间也可以设置底涂层,但由于上述涂膜的密合性优异,因而上述基材与上述涂膜能够以充分的粘接强度进行直接粘接。具备上述涂膜和上述基材的层积体也是本发明的适宜方式之一。
作为上述基材的材料,可以举出金属、陶瓷、树脂、玻璃等。作为上述基材,还可以举出后述的不透水性片材。
作为上述金属,可以举出铁;SUS304、SUS316L、SUS403等不锈钢;铝;实施了镀锌、镀铝等的镀覆钢鈑等。作为上述陶瓷,可以举出陶器、磁器、氧化铝材、氧化锆材、氧化硅材等。作为上述树脂,可以举出聚对苯二甲酸乙二醇酯树脂、聚碳酸酯树脂、有机硅树脂、氟硅树脂、聚酰胺树脂、聚酰胺酰亚胺树脂、聚酰亚胺树脂、聚酯树脂、环氧树脂、聚苯硫醚树脂、酚树脂、丙烯酸类树脂、聚醚砜树脂等。包含本发明的聚合物的涂膜、由本发明的组合物得到的涂膜、以及本发明的涂膜与由有机硅树脂形成的基材也具有良好的初期密合性,在高压蒸煮测试后也具有良好的密合性。
本发明还涉及一种层积体,其特征在于,该层积体包含基材以及设于上述基材上的涂膜,该涂膜包含氨基甲酸酯键,落砂磨耗性为80L以上;对上述涂膜根据JIS D0202-1988进行棋盘格胶带剥离试验的情况下,100格中未剥离的方格的数目为30以上。
本发明的层积体由于这些特征,因而除了耐磨耗性和初期密合性优异以外,在高压蒸煮测试后也具有良好的密合性,由于高交联密度而使涂膜强度增加,从而使得辊加工时的破裂减轻性也优异。上述涂膜能够由上述组合物适宜地制造。特别是上述氨基甲酸酯键通过上述组合物中包含的多异氰酸酯化合物所具有的异氰酸酯基与聚合物(B)所具有的羟基发生反应而形成。上述涂膜包含氨基甲酸酯键这一点可通过红外分光法(IR)来确认。
作为未剥离的方格的数目,优选为50以上、更优选为70以上、进一步优选为90以上、特别优选为100。
上述涂膜优选直接设置在上述基材上。
关于上述层积体,进一步在对上述层积体进行在121℃、湿度100%RH、2个大气压下放置60小时的高压蒸煮测试后进行棋盘格胶带剥离试验的情况下,也优选100格中未剥离的方格的数目为30以上。作为未剥离的方格的数目,优选为50以上、更优选为70以上、进一步优选为90以上、特别优选为100。
作为上述层积体中包含的上述基材的材料,可以举出上述的材料,其中优选聚对苯二甲酸乙二醇酯树脂。
上述层积体能够适当地用作太阳能电池组件的背板。
本发明还涉及一种背板,其特征在于,其具备上述涂膜。上述背板适当地用作用于保护太阳能电池组件的背面的太阳能电池组件的背板。上述太阳能电池组件通常具备表面层、太阳能电池单元、用于密封太阳能电池单元的密封材层、以及背板。已知对上述背板要求机械强度、耐候性、防水·防湿性、电气绝缘性等特性。本发明的背板解决了由落砂磨耗性试验测定的耐磨耗性这一新颖的课题,上述课题是通过具备上述涂膜而得以解决的。
上述背板优选进一步具备不透水性片材。上述不透水性片材是按照使水分不会透过到上述密封材或上述太阳能电池单元的方式进行设置的层,只要为实质上不会透过水的材料就能够使用,从重量、价格、挠性等方面出发,多使用聚对苯二甲酸乙二醇酯(PET)片材、SiOx蒸镀PET片材、铝或不锈钢等金属薄片材等。其中优选使用PET片材。厚度通常为50~250μm左右。其中在特别需要防湿性的情况下,优选使用SiOx蒸镀PET片材。厚度通常为10~20μm左右。
上述涂膜在上述不透水性片材的至少一面形成。上述涂膜可以仅在不透水性片材的单面形成,也可以在双面形成。上述不透水性片材与上述涂膜可以直接粘接,也可以藉由其他层进行粘接,优选直接粘接。作为其他层,可以举出底涂层。
上述底涂层的形成使用现有公知的底层涂料用涂料通过常规方法进行。作为底层涂料用的涂料,可以举出例如环氧树脂、氨基甲酸酯树脂、丙烯酸类树脂、有机硅树脂、聚酯树脂等作为代表例。
从隐蔽性、耐候性、耐化学药品性、耐湿性良好的方面出发,上述涂膜的膜厚优选为5μm以上。该膜厚更优选为7μm以上、进一步优选为10μm以上。由于若膜厚过厚则得不到轻量化效果,因而上限优选为1000μm左右、更优选为100μm左右。作为膜厚,特别优选为10~40μm。
为了提高与上述涂膜的密合性,可以对上述不透水性片材进行现有公知的表面处理。作为表面处理,可示例出例如电晕放电处理、等离子体放电处理、化学处理、金属片材的情况下的喷砂处理等。
上述背板可以与太阳能电池组件的密封材层粘接来使用。在上述背板仅在上述不透水性片材的单面具备上述涂膜的情况下,可以使上述不透水性片材与上述密封材层粘接,也可以使上述涂膜与上述密封材层粘接。由于上述涂膜与上述不透水性片材的密合性优异、而且与上述密封材层的密合性也优异,因而优选使上述涂膜与上述密封材层粘接。另外,由于上述涂膜的耐候性也优异,因而优选使上述涂膜位于太阳能电池组件的最外表面。由于以上原因,上述背板优选在上述不透水性片材的双面具备上述涂膜。
上述密封材层由密封材构成,将上述太阳能电池单元密封在内部。作为上述密封材,可以举出乙烯/乙酸乙烯酯共聚物(EVA)、聚乙烯醇缩丁醛(PVB)、有机硅树脂、环氧树脂、丙烯酸类树脂等,优选EVA。
具备上述层积体或上述背板的太阳能电池组件也是本发明之一。
作为上述太阳能电池组件的优选结构,可以举出例如图1~3所示的结构。
在图1所示的第1结构中,太阳能电池单元1被密封材层2密封,该密封材层2被表面层3与背板4夹在中间。背板4进一步由不透水性片材5与涂膜6构成。在该第1结构中,涂膜6仅设置在密封材层2侧。需要说明的是,在图1~图3中,涂膜6为上述的涂膜。
上述密封材层2由乙烯/乙酸乙烯酯共聚物(EVA)、聚乙烯醇缩丁醛(PVB)、有机硅树脂、环氧树脂、丙烯酸类树脂等构成。
在上述表面层3通常使用玻璃板,但也可以使用树脂片材等柔性材料。
图2所示的第2结构为在不透水性片材5的双面形成涂膜6而成的3层结构。
该第2结构中,虽然背板的膜厚增加,但其兼具由密封材层2侧的涂膜6所带来的密合性、以及由与密封材层2相反侧的涂膜6所带来的耐候性这两方面的优点。
作为3层结构的背板,还可以为如下形成的3层结构的背板:在不透水性片材的一个面上形成上述的涂膜,在另一个面上形成与上述涂膜不同的涂膜、含氟聚合物片材、聚酯片材或聚酯涂料的涂膜(其他片材或涂膜)。
图3所示的第3结构为在不透水性片材5的密封材层2侧形成涂膜6、在与密封材层2相反侧形成其他涂膜7的结构。
构成涂膜7的材料可以为与上述涂膜不同的涂膜、可以为含氟聚合物片材、可以为聚酯片材、也可以为聚酯涂料的涂膜。
另外,为了进一步提高上述涂膜与密封材层密合性,可以对上述涂膜进行现有公知的表面处理。作为表面处理,可示例出例如电晕放电处理、等离子体放电处理、化学处理、喷砂处理等。
作为与上述涂膜不同的涂膜,可以举出例如日本特开2004-214342号公报中记载的在聚偏二氟乙烯(PVdF)中混配四烷氧基硅烷或其部分水解物而成的涂料的涂膜、VdF/TFE/CTFE共聚物与含有烷氧基硅烷单元的丙烯酸类树脂的混合涂料的涂膜、VdF/TFE/HFP共聚物与含羟基丙烯酸类树脂的混合涂料的涂膜、在VdF/HFP共聚物中混配氨基硅烷偶联剂而成的涂料的涂膜等。从隐蔽性、耐候性、耐化学药品性、耐湿性良好的方面出发,膜厚通常优选为5~300μm。该膜厚更优选为10~100μm、进一步优选为10~50μm。这种情况下,也可以夹设底涂层等。
作为上述含氟聚合物片材,可以举出PVdF片材或聚氟乙烯(PVF)片材、PCTFE片材、TFE/HFP/乙烯共聚物片材、TFE/HFP共聚物(FEP)片材、TFE/全氟(烷基乙烯基醚)(PAVE)共聚物(PFA)片材、乙烯/TFE共聚物(ETFE)片材、乙烯/CTFE共聚物(ECTFE)片材等在目前的背板中使用的含氟聚合物片材。从耐候性良好的方面出发,膜厚通常优选为5~300μm。该膜厚更优选为10~100μm、进一步优选为10~50μm。
作为上述聚酯片材,可以直接使用在现有背板中使用的片材,也可以利用丙烯酸系接合剂、氨基甲酸酯系接合剂、环氧系接合剂、聚酯系接合剂等进行其与不透水性片材5的粘接。从耐候性、成本、透明性良好的方面出发,膜厚通常优选为5~300μm。该膜厚更优选为10~100μm、进一步优选为10~50μm。
作为上述聚酯涂料,可以举出:使用了采用多元羧酸与多元醇等而成的饱和聚酯树脂的涂料;使用了采用马来酸酐、富马酸等与二醇类而成的不饱和聚酯树脂的涂料等,可通过辊涂、幕涂、喷涂、模涂等涂布方法形成涂膜。从隐蔽性、耐候性、耐化学药品性、耐湿性良好的方面出发,膜厚优选为5~300μm。该膜厚更优选为10~100μm、进一步优选为10~50μm。这种情况下,也可以夹设底涂层等。
实施例
下面举出参考例对本发明进行说明,但本发明并不仅限于该参考例。
通过以下的方法测定参考例的各数值。
(1)构成聚合物的各单体单元的含量
根据由元素分析测定的含氟量(质量%)和基于1HNMR光谱的组成分析计算出各单体单元的含量(摩尔%)。
(2)羟值
使用聚合时的羟基单体的实际投料量和固体成分浓度通过计算而计算出羟值。
(3)落砂磨耗性
根据JIS A 1452:1972建筑物材料及建筑物结构部件的磨耗试验方法(落砂法)进行测定。
(4)密合性
对于各参考例中得到的背板,依据JIS D0202-1988对初期状态和PCT(高压蒸煮测试、121℃、湿度100%RH、2个大气压)60小时后的涂膜进行棋盘格胶带剥离实验。使用赛璐玢带(“CT24”、米其邦公司制造),利用指肚将其密合在膜上,之后进行剥离。判断以100格中未发生剥离的方格的数目来表示。
(5)耐候性
使用SWOM(SUGA TEST INSTRUMENTS公司制造的耐候性试验机:试验时间6000小时),设初期的60度光泽为100,以6000小时后的光泽保持率来表示耐候性。
参考例1
在容量6000ml的不锈钢制高压釜中投入乙酸丁酯2500g、新壬酸乙烯酯584g、4-羟基丁基乙烯基醚(HBVE)527g,进行减压氮气置换的操作,投入四氟乙烯(TFE)658g。在搅拌下升温至60.0℃,投入过氧化物系聚合引发剂30g引发聚合。在反应器内压从1.0MPaG降低到0.4MPaG的时刻停止反应,得到包含聚合物的溶液。将该聚合物的组成和羟值列于表1。
将由反应得到的包含聚合物的溶液485.0g(聚合物的含量为65质量%)、作为白色颜料的氧化钛(堺化学工业株式会社制造的D918)63.0g、乙酸丁酯208.0g用颜料分散机分散,制备包含颜料的分散液。
在该分散液100质量份中混配异氰酸酯系固化剂(住化拜耳株式会社制造的Sumidur N3300),使得上述异氰酸酯系固化剂所具有的异氰酸酯基(NCO)与上述聚合物所具有的羟基(OH)的当量比(NCO/OH)为表1的当量比,制备组合物。
作为不透水性片材,对聚对苯二甲酸乙二醇酯(PET)片材(东丽株式会社制造的Lumiror S10、厚度250μm)的双面进行电晕放电处理,在该片材的单面涂布上述组合物使干燥涂膜厚为25μm,在150℃干燥3分钟,制作出2层结构的层积体。进一步在相反侧的面涂布上述组合物使干燥涂膜厚为25μm,在150℃干燥3分钟,制作3层结构的背板层积体。对于该背板层积体进行落砂磨耗性、初期密合性、PCT后的密合性和耐候性的研究。将结果列于表1。
参考例2~11和比较参考例1~5
与参考例1同样地制作聚合物、组合物和背板。将结果列于表1。
表中的简写符号的说明
TFE:四氟乙烯
CTFE:三氟氯乙烯
VV9:新壬酸乙烯酯
VV10:新癸酸乙烯酯
VBz:苯甲酸乙烯酯
VAc:乙酸乙烯酯
EVE:乙基乙烯基醚
HBVE:4-羟基丁基乙烯基醚
HEVE:2-羟基乙基乙烯基醚
AA:丙烯酸
CA:丁烯酸
符号的说明
1:太阳能电池单元
2:密封材层
3:表面层
4:背板
5:不透水性片材
6:由本发明的组合物形成的涂膜
7:其他涂膜
Claims (13)
1.一种聚合物,其特征在于,
该聚合物包含:全卤烯烃单元;不含羟基和芳香环中的任一者的乙烯基酯单元;以及含羟基单体单元,
所述聚合物的羟值为110mgKOH/g以上。
2.如权利要求1所述的聚合物,其中,所述全卤烯烃为选自由四氟乙烯、三氟氯乙烯以及六氟丙烯组成的组中的至少一种。
3.如权利要求1或2所述的聚合物,其中,所述乙烯基酯为选自由乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、异丁酸乙烯酯、新戊酸乙烯酯、己酸乙烯酯、叔碳酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯和环己基甲酸乙烯酯组成的组中的至少一种。
4.如权利要求1、2或3所述的聚合物,其中,所述含羟基单体为羟基烷基乙烯基醚。
5.一种组合物,其特征在于,
该组合物包含聚合物和多异氰酸酯化合物,
所述聚合物包含全卤烯烃单元以及含羟基单体单元,且该聚合物的羟值为90mgKOH/g以上,
所述多异氰酸酯化合物所具有的异氰酸酯基与所述聚合物所具有的羟基的当量比小于1.0。
6.如权利要求5所述的组合物,其中,所述全卤烯烃为选自由四氟乙烯、三氟氯乙烯以及六氟丙烯组成的组中的至少一种。
7.如权利要求5或6所述的组合物,其中,所述含羟基单体为羟基烷基乙烯基醚。
8.如权利要求5、6或7所述的组合物,其中,所述聚合物进一步包含:选自由不含羟基和芳香环中的任一者的乙烯基酯单元和不含羟基的烷基乙烯基醚单元组成的组中的至少一种单元(b)。
9.如权利要求5、6、7或8所述的组合物,其中,所述组合物进一步包含溶剂。
10.一种涂膜,其特征在于,其包含权利要求1、2、3或4所述的聚合物、或者由权利要求5、6、7、8或9所述的组合物形成。
11.一种层积体,其特征在于,
该层积体包含基材以及设于所述基材上的涂膜,该涂膜包含氨基甲酸酯键,该涂膜的落砂磨耗性为80L以上;
对所述涂膜根据JIS D0202-1988进行棋盘格胶带剥离试验的情况下,100格中未剥离的方格的数目为30以上。
12.一种背板,其特征在于,其具备权利要求10所述的涂膜或权利要求11所述的层积体。
13.一种太阳能电池组件,其特征在于,其具备权利要求11所述的层积体或权利要求12所述的背板。
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JP2019035080A (ja) | 2019-03-07 |
US11186672B2 (en) | 2021-11-30 |
JP2017190461A (ja) | 2017-10-19 |
US20190016848A1 (en) | 2019-01-17 |
JP6664352B2 (ja) | 2020-03-13 |
WO2017155022A1 (ja) | 2017-09-14 |
JP2017165958A (ja) | 2017-09-21 |
TW201802130A (zh) | 2018-01-16 |
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