CN115315493A - 基于硅烷官能聚合物、具有增强的可重叠涂漆性的组合物 - Google Patents
基于硅烷官能聚合物、具有增强的可重叠涂漆性的组合物 Download PDFInfo
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- CN115315493A CN115315493A CN202180022616.7A CN202180022616A CN115315493A CN 115315493 A CN115315493 A CN 115315493A CN 202180022616 A CN202180022616 A CN 202180022616A CN 115315493 A CN115315493 A CN 115315493A
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Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/40—High-molecular-weight compounds
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- C08G18/4866—Polyethers having a low unsaturation value
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- 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
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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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
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- C08G18/242—Catalysts containing metal compounds of tin organometallic compounds containing tin-carbon bonds
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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
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明涉及可湿固化组合物,其包含至少一种含有反应性硅烷基的有机聚合物P,基于总组合物计为1.0wt%‑25.0wt%、优选2.0wt%‑20wt%、特别是2.5wt%至10wt%的脂族C3‑C5二羧酸的二甲酯或二乙酯,和至少一种用于烷氧基硅烷基的固化催化剂。该可湿固化组合物特别适合作为弹性粘合剂、涂料、填料或密封剂,并且显示出优异的可重叠涂漆性,特别是用汽车面漆或类似的涂漆。
Description
技术领域
本发明涉及基于有机硅烷官能聚合物的可固化组合物及其作为粘合剂、密封剂、填料或涂料的用途。
背景技术
基于含有反应性硅烷基团的聚合物的可固化组合物在许多工业或建筑应用中起到重要作用,例如作为粘合剂、密封剂或涂料。含有反应性硅烷基团的聚合物是聚二有机硅氧烷(通常称为“硅酮”或“有机硅橡胶”),或者含有反应性硅烷基团的有机聚合物(也称为“硅烷官能聚合物”、“硅烷改性聚合物”(SMP)或“硅烷封端聚合物”(STP))。含有这些聚合物的组合物通过聚合物上的反应性硅烷基的交联反应而固化,所述硅烷基在水分的影响下水解,彼此缩合为硅烷醇基并因此形成硅氧烷键。
由于其在固化状态下的通用机械性能和在各种基材上的优异粘合性,基于有机硅烷封端聚合物的组合物也广泛用于修复应用。它们的拉伸强度、弹性、肖氏A硬度和许多相关的其它性能可以通过组合物的适当配方在宽范围内调节,并且它们的粘合性能通常在不需要对基材进行广泛预处理的情况下良好地发挥作用。因此,在苛刻的修复操作中,例如在碰撞后的车身修复中,这样的组合物是高度适合的,因为它们在涂漆的金属或原料金属和汽车制造中使用的其它材料上形成耐久的粘合粘结。
基于硅烷官能聚合物的组合物的一个问题是稍微有限的可重叠涂漆性(overpaintability),特别是对于目前用作例如汽车涂漆车间的面漆的硬疏水涂漆(paint)、清漆(varnish)或天然漆(lacquer)。
在修复受损的经涂漆的物品例如受损的车体之后,需要将与已经施加在物品的其余部分上的涂漆相同的涂漆重新施加在物品的修复部分上,使得该修复的损伤变得不可见。
然而,采用目前的耐久性涂漆、清漆和天然漆,可重叠涂漆性对于基于硅烷官能聚合物的组合物而言是个问题。对于基于硅烷官能聚合物的普通组合物,涂漆、清漆或天然漆往往会在一段时间后剥落,尤其是当被刮伤或以其它方式损坏时,留下可见的油漆缺陷,所述缺陷不仅看起来令人不愉快,而且如果涂漆基材是金属的,则还会加速涂漆基材的生锈。此外,观察到基于硅烷官能聚合物的普通组合物的成分,例如增塑剂,经常以某种方式与施涂在其上的干燥涂漆反应或迁移到其中,这导致覆盖基于硅烷官能聚合物的固化组合物的干燥涂漆、清漆或天然漆的部分有可见的变色。
发明概述
因此,本发明的目的是提供一种基于含有反应性硅烷基的有机聚合物的可固化组合物,其可以容易地和持久地被重叠涂漆,使得施加在其上的涂漆、清漆或天然漆不会剥落或显示变色迹象。这也特别适用于目前在汽车涂漆车间中使用的具有高硬度的疏水性和高要求的涂漆、清漆或天然漆。
本发明通过独立权利要求1的特征实现这些目的。
在基于含有反应性硅烷基团的有机聚合物和至少一种用于烷氧基硅烷基的固化催化剂的可湿固化组合物中,基于总组合物计,包含1.0wt%-25.0wt%、优选2.0wt%-20wt%、特别是2.5wt%-10wt%的脂族C3-C5二羧酸二甲酯或二乙酯,令人惊讶地能够显著改进可重叠涂漆性,特别是对于目前在汽车涂漆车间中使用的具有高硬度的疏水性和高要求的涂漆、清漆或清漆而言。
本发明的其它方面是其它独立权利要求的主题。本发明的特别优选的实施方案是从属权利要求的主题。
发明详述
本发明在第一方面涉及可湿固化的组合物,包含
-至少一种含有反应性硅烷基的有机聚合物P;
-基于总组合物计,1.0wt%-25.0wt%、优选2.0wt%-20wt%、特别是2.5wt%-10wt%的脂族C3-C5二羧酸二甲酯或二乙酯;以及-至少一种用于烷氧基硅烷基的固化催化剂。
本文中,术语“反应性硅烷基”是指键合到有机基团或聚有机硅氧烷基团并且在硅原子上具有1-3个、尤其是2个或3个可水解取代基或羟基的甲硅烷基。特别有用的可水解取代基是烷氧基。这些硅烷基也称为“烷氧基硅烷基团”。反应性硅烷基也可以是部分或完全水解的形式,例如作为硅烷醇。
“羟基硅烷”、“异氰酸基硅烷”、“氨基硅烷”和“巯基硅烷”分别是指在有机基团上除了硅烷基之外还具有一个或多个羟基、异氰酸基、氨基或巯基的有机烷氧基硅烷。
“氨基官能化合物”是指含有氨基的化合物。
“伯氨基”是指键合到有机基团上的NH2基团,“仲氨基”是指键合到两个有机基团上的NH基团,所述两个有机基团也可以一起形成环的一部分,和“叔氨基”是指键合到三个有机基团上的N基团,所述三个有机基团中的两个或三个也可以一起形成一个或多个环的一部分。因此,“伯氨基硅烷”是包含伯氨基的氨基硅烷,“仲氨基硅烷”是包含仲氨基的氨基硅烷。后者还包括具有伯氨基和仲氨基的化合物。
“聚氧亚烷基基团”是指含有醚基团并含有连续的两个以上(O-R)型重复单元的直链或支链烃基,其中R为直链或支链亚烷基,例如来自环氧乙烷或1,2-环氧丙烷在具有两个活性氢原子的起始分子上的加聚。
以“聚(多)”开始的物质名称,例如多元醇或多异氰酸酯,是指在形式意义上每分子含有两个或更多个在其名称中出现的官能团的物质。
术语“有机聚合物”包括化学上均一但在聚合度、摩尔质量和链长方面不同的大分子集合,其通过聚合反应(聚加成、加聚、缩聚)制备并且在聚合物骨架中具有占多数的碳原子,以及这种大分子集合的反应产物。具有聚有机硅氧烷主链的聚合物(通常称为“硅酮/有机硅”)在本文的上下文中不是有机聚合物。
术语“含有反应性硅烷基的聚醚”还包括含有硅烷基的有机聚合物,其除了聚醚单元之外,还可含有氨基甲酸酯基、脲基或硫代氨基甲酸酯基。这种含有反应性硅烷基的聚醚也可称为“含有反应性硅烷基的聚氨酯”。
在本文中,“分子量”应理解为是指分子或分子的一部分(也称为“基团”)的摩尔质量(克/摩尔)。术语“基团”在本文献中以形式意义使用,意指通过共价键与原子结合的分子残基,而键在形式上被“切断”以描述与其连接的分子残基。“平均分子量”应理解为表示分子或基团的低聚物或聚合物混合物的数均Mn,其通常通过凝胶渗透色谱法(GPC)相对于聚苯乙烯标样测定。
如果没有另外定义,“重量百分比”或“百分比重量”,以及其缩写“wt%”是指某种化合物在总组合物中的重量百分比。术语“重量”和“质量”在本文中可互换使用,并且是指作为物理物体的性质并且通常以千克(kg)测量的质量。
“储存稳定的”或“可储存的”是指当可在室温下在合适的容器中储存较长的时间,通常至少3个月至6个月或更长时间时,其应用或使用性能(尤其是在粘度和交联速率方面)不会因为储存而在与其使用相关的程度发生任何变化的物质或组合物。
“室温”是指约23℃的温度。
如果没有另外定义,在本文中引用的所有工业标准和规范均参考在提交本发明的首次申请时生效的相应版本。
首先,本发明组合物中需要的是至少一种含有反应性硅烷基的有机聚合物P。
通常,优选组合物中聚合物P的量为10-60wt%、优选10-40wt%、更优选15-30wt%,基于总组合物计。该范围提供良好的机械性能而又不使组合物太昂贵。
含有反应性硅烷基的有机聚合物P尤其是聚氨酯、聚烯烃、聚酯、聚碳酸酯、聚酰胺、聚(甲基)丙烯酸酯或聚醚或这些聚合物的混合形式,它们各自带有一个或优选多于一个硅烷基。硅烷基可以在链中的侧挂位置或在末端位置,并且通过碳原子与有机聚合物键合。
更优选地,含有反应性硅烷基的有机聚合物P是含有反应性硅烷基的聚烯烃或含有反应性硅烷基的聚氨酯或含有反应性硅烷基的聚醚或这些聚合物的混合形式。
最优选地,含有反应性硅烷基的有机聚合物是含有反应性硅烷基的聚醚。
存在于含有反应性硅烷基的有机聚合物中的硅烷基优选为烷氧基硅烷基,尤其是式(VII)的烷氧基硅烷基团,
其中
R14为具有1-5个碳原子的直链或支链一价烃基,尤其是甲基或乙基或异丙基;
R15为具有1-8个碳原子的直链或支链一价烃基,尤其是甲基或乙基;以及
x为值0或1或2,优选0或1,尤其是0。
更优选R14为甲基或乙基。
对于特定的应用,R14基团优选为乙基,因为在这种情况下,在组合物固化过程中释放生态和毒理学上无害的乙醇。
特别优选的是三甲氧基硅烷基团、二甲氧基甲基硅烷基团或三乙氧基硅烷基团。
在本文中,甲氧基硅烷基团具有的优点是它们是特别有反应性的,而乙氧基硅烷基具有的优点是它们是毒理学上有利的并且特别是储存稳定的。
含有反应性硅烷基的有机聚合物每分子平均具有优选1.3-4个,尤其1.5-3个,更优选1.7-2.8个硅烷基团。硅烷基团优选在末端。
含有反应性硅烷基团的有机聚合物优选具有1000-30000g/mol,尤其是2000-20000g/mol的平均分子量,通过GPC相对于聚苯乙烯标样测定。含有反应性硅烷基的有机聚合物优选具有300-25000g/eq,尤其是500-15000g/eq的硅烷当量。
含有反应性硅烷基的有机聚合物在室温下可以是固体或液体。其优选在室温下为液体。
最优选地,含有反应性硅烷基团的有机聚合物是在室温下为液体的含有反应性硅烷基的聚合物,其中硅烷基特别是二烷氧基硅烷基和/或三烷氧基硅烷基,更优选三甲氧基硅烷基或三乙氧基硅烷基。
制备含有反应性硅烷基的有机聚合物的方法是本领域技术人员已知的。
在优选的方法中,含有反应性硅烷基的有机聚合物可由含有烯丙基的有机聚合物与氢硅烷反应获得,任选地使用例如二异氰酸酯进行扩链。
在进一步优选的方法中,含有反应性硅烷基的聚醚可由环氧烷和环氧硅烷的共聚获得,任选地使用例如二异氰酸酯进行扩链。
在进一步优选的方法中,含有反应性硅烷基的有机聚合物可由有机多元醇与异氰酸基硅烷的反应获得,任选地使用二异氰酸酯进行扩链。
在另一优选的方法中,含有反应性硅烷基的聚醚可由含有异氰酸酯基的有机聚合物,尤其是NCO-封端的氨基甲酸酯聚合物与氨基硅烷、羟基硅烷或巯基硅烷的反应获得,所述NCO-封端的氨基甲酸酯聚合物来自多元醇与超化学计量量的多异氰酸酯的反应。特别优选来自该方法的含有反应性硅烷基的聚醚。该方法能够使用大量具有良好商业可获得性的廉价起始材料,通过该方法可以获得不同的聚合物性能,例如高延展性、高强度、低弹性模量、低玻璃化转变点或高耐候性。
更优选地,含有反应性硅烷基的有机聚合物可由NCO-封端的氨基甲酸酯聚醚与氨基硅烷或羟基硅烷的反应获得。合适的NCO-封端的氨基甲酸酯聚合物可由多元醇,尤其是聚醚多元醇,特别是聚氧化亚烷基二醇或聚氧化亚烷基三醇,优选聚氧化亚丙基二醇或聚氧化亚丙基三醇与超化学计量量的多异氰酸酯,尤其是二异氰酸酯的反应获得。其它多元醇,例如聚(甲基)丙烯酸酯多元醇、聚烃多元醇,特别是聚丁二烯多元醇、多羟基官能脂肪或油、聚碳酸酯多元醇、聚酯多元醇和多羟基官能的丙烯腈/丁二烯共聚物也是合适的。此外,少量低分子量二元或多元醇,例如二醇、乙二醇和糖醇可以用作添加剂。
优选地,多异氰酸酯和多元醇之间的反应在排除水分的情况下在50℃-160℃的温度下,任选地在合适的催化剂存在下,在计量加入多异氰酸酯使得其异氰酸酯基相对于多元醇的羟基以化学计量过量存在的情况下进行。更特别地,选择过量的多异氰酸酯,使得在所有羟基反应之后,基于总聚合物计,在所得氨基甲酸酯聚合物中保留0.1wt%-5wt%、优选0.2wt%-4wt%、更优选0.3wt%-3wt%的游离异氰酸酯基含量。
优选的二异氰酸酯选自六亚甲基1,6-二异氰酸酯(HDI)、1-异氰酸基-3,3,5-三甲基-5-异氰酸基甲基环己烷(=异佛尔酮二异氰酸酯或IPDI)、甲苯2,4-和2,6-二异氰酸酯和这些异构体(TDI)的任何所需混合物和二苯甲烷4,4'-、2,4'-和2,2'-二异氰酸酯和这些异构体(MDI)的任何所需混合物。特别优选MDI、IPDI或TDI。在一些实施方案中最优选IPDI。以这种方式,得到具有特别好的耐光性的含有反应性硅烷基的聚醚。
特别适合作为聚醚多元醇的是不饱和度低于0.02meq/g、尤其是低于0.01meq/g,且平均分子量为400-25000g/mol、尤其是1000-20000g/mol的聚氧化亚烷基二醇或聚氧化亚烷基三醇。
除了聚醚多元醇之外,还可以使用部分其它多元醇,特别是聚丙烯酸酯多元醇,和低分子量二醇或三醇。
用于与NCO-封端的氨基甲酸酯聚醚反应的合适的氨基硅烷为伯氨基硅烷和仲氨基硅烷。优选3-氨基丙基三甲氧基硅烷、3-氨基丙基二甲氧基甲基硅烷、4-氨基丁基三甲氧基硅烷、4-氨基-3-甲基丁基三甲氧基硅烷、4-氨基-3,3-二甲基丁基三甲氧基硅烷、N-丁基-3-氨基丙基三甲氧基硅烷、N-苯基-3-氨基丙基三甲氧基硅烷,由伯氨基硅烷和迈克尔受体形成的加合物,伯氨基硅烷例如3-氨基丙基三甲氧基硅烷、3-氨基丙基二甲氧基甲基硅烷或N-(2-氨基乙基)-3-氨基丙基三甲氧基硅烷,和迈克尔受体例如丙烯腈、(甲基)丙烯酸酯、(甲基)丙烯酰胺、马来酸或富马酸二酯、柠康酸二酯或衣康酸二酯,尤其是N-(3-三甲氧基甲硅烷基丙基)氨基琥珀酸二甲酯或二乙酯。同样合适的是用乙氧基或异丙氧基代替硅上甲氧基的所述氨基硅烷的类似物。
用于与NCO-封端的氨基甲酸酯聚醚反应的合适的羟基硅烷尤其可通过将氨基硅烷加成到内酯上或环状碳酸酯上或交酯上而获得。
适合于此目的的氨基硅烷尤其是3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、4-氨基丁基三甲氧基硅烷、4-氨基丁基三乙氧基硅烷、4-氨基-3-甲基丁基三甲氧基硅烷、4-氨基-3-甲基丁基三乙氧基硅烷、4-氨基-3,3-二甲基丁基三甲氧基硅烷、4-氨基-3,3-二甲基丁基三乙氧基硅烷、2-氨基乙基三甲氧基硅烷或2-氨基乙基三乙氧基硅烷。特别优选的是3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、4-氨基-3,3-二甲基丁基三甲氧基硅烷或4-氨基-3,3-二甲基丁基三乙氧基硅烷。
合适的内酯特别是γ-戊内酯、γ-辛内酯、δ-癸内酯和ε-癸内酯,特别是γ-戊内酯。
合适的环状碳酸酯尤其是4,5-二甲基-1,3-二氧戊环-2-酮、4,4-二甲基-1,3-二氧戊环-2-酮、4-乙基-1,3-二氧戊环-2-酮、4-甲基-1,3-二氧戊环-2-酮或4-(苯氧基甲基)-1,3-二氧戊环-2-酮。
合适的交酯尤其是1,4-二噁烷-2,5-二酮(由2-羟基乙酸形成的交酯,也称为“乙交酯”)、3,6-二甲基-1,4-二噁烷-2,5-二酮(由乳酸形成的交酯,也称为“丙交酯”)和3,6-二苯基-1,4-二噁烷-2,5-二酮(由扁桃酸形成的交酯)。
以这种方式获得的优选羟基硅烷是N-(3-三乙氧基甲硅烷基丙基)-2-羟基丙酰胺、N-(3-三甲氧基甲硅烷基丙基)-2-羟基丙酰胺、N-(3-三乙氧基甲硅烷基丙基)-4-羟基戊酰胺、N-(3-三乙氧基甲硅烷基丙基)-4-羟基辛酰胺、N-(3-三乙氧基甲硅烷基丙基)-5-羟基癸酰胺和N-(3-三乙氧基甲硅烷基丙基)-2-羟基丙基氨基甲酸酯。
此外,合适的羟基硅烷也可通过将氨基硅烷加成到环氧化物上或通过将胺加成到环氧硅烷上而获得。优选的以这种方式获得的羟基硅烷是2-吗啉代-4(5)-(2-三甲氧基甲硅烷基乙基)环己-1-醇、2-吗啉代-4(5)-(2-三乙氧基甲硅烷基乙基)环己-1-醇或1-吗啉代-3-(3-(三乙氧基甲硅烷基)丙氧基)丙-2-醇。
其它合适的含有反应性硅烷基的聚醚是市售产品,特别是下列:MS PolymerTM(购自Kaneka Corp.;特别是S203H、S303H、S227、S810、MA903和S943产品);MS PolymerTM或SilylTM(购自Kaneka Corp.;尤其是SAT010、SAT030、SAT200、SAX350、SAX400、SAX725、MAX450、MAX951产品);(购自Asahi Glass Co.Ltd.;尤其是S2410、S2420、S3430、S3630产品);SPUR+*(购自Momentive Performance Materials;尤其是1010LM、1015LM、1050MM产品);VorasilTM(购自Dow Chemical Co.;尤其是602和604产品);(购自Bayer MaterialScience AG;尤其是S XP 2458、SXP 2636、S XP2749、S XP 2774和S XP 2821产品),(购自Evonik Industries AG;尤其是Seal 100、Bond 150、Bond 250产品),Polymer ST(购自Hanse Chemie AG/EvonikIndustries AG,尤其是47、48、61、61LV、77、80、81产品);STP(购自WackerChemie AG;尤其是E10、E15、E30、E35、WP1和WP2产品)。
特别优选的含有反应性硅烷基的有机聚合物具有式(VIII)的端基
其中
R16为直链或支链的二价烃基,其具有1-12个碳原子并任选具有环状和/或芳族部分和任选一个或多个杂原子,尤其是一个或多个氮原子;
T为选自-O-、-S-、-N(R17)-、-O-CO-N(R17)-、-N(R17)-CO-O-和-N(R17)-CO-N(R17)-的二价基团,
其中R17为氢基团或具有1-20个碳原子和任选具有环状部分的直链或支链烃基,且其任选具有烷氧基硅烷、醚或羧酸酯基;以及
R14、R15和x具有已经给出的定义。
优选地,R16为1,3-亚丙基或1,4-亚丁基,其中亚丁基可被一个或两个甲基取代。
更优选地,R16为1,3-亚丙基。
在本发明可湿固化组合物的一些优选实施方案中,聚合物P包含甲氧基甲硅烷基。甲氧基甲硅烷基的优点是它们特别具有反应性,因此组合物固化快和/或催化剂负载量低。
在其它优选的实施方案中,反应性硅烷基是乙氧基硅烷、丙氧基硅烷或高级烷氧基硅烷基,优选乙氧基硅烷基。这些实施方案导致在组合物固化期间和之后VOC中甲醇含量降低。
在本发明可湿固化组合物的相同或其它优选实施方案中,可湿固化组合物不含任何在水解时解离出甲醇的化合物。相反,优选的是,在组合物中仅包含乙醇分解性化合物(即乙氧基硅烷官能的化合物)。这具有的优点是该组合物特别无害,但仍显示出足够的固化行为。
根据本发明的可湿固化组合物包含1.0wt%-25.0wt%,优选2.0wt%-20wt%,特别是2.5wt%-10wt%的脂族C3-C5二羧酸的二甲酯或二乙酯,基于总组合物计。
令人惊奇地发现,脂族C3-C5二羧酸的二甲酯或二乙酯,特别是戊二酸二甲酯,导致本发明组合物提高的可重叠涂漆性的创造性效果。
脂族C3-C5二羧酸的二甲酯或二乙酯可以以纯形式或者更通常地作为所谓的二元酯混合物形式商购获得。最通常地,它们是二甲酯,但也可以使用其它酯如二乙酯或更高级醇的酯。它们通常含有0.5-30wt%的琥珀酸二甲酯、50-99wt%的戊二酸二甲酯和0.5-25wt%的己二酸二甲酯,基于总混合物计,或其它醇如乙醇而不是甲醇的酯。
对于本发明,仅甲醇或乙醇的二酯是合适的。更高级醇酯如异丁醇酯不适用于本发明的组合物,因为它们导致失活和储存稳定性问题。
最优选的是二甲酯。它们使得组合物具有最高的稳定性和最佳的可重叠涂漆性效果。
最优选的二甲酯是戊二酸二甲酯,也称为戊烷二酸二甲酯。
优选地,用于本发明组合物的脂族C3-C5二羧酸二甲酯或二乙酯的混合物含有至少50wt%,特别是至少75wt%,优选至少90wt%,最优选至少95wt%的戊二酸二甲酯,基于总混合物计。
在优选的实施方案中,可固化组合物含有小于5wt%的其它脂族二羧酸二酯,基于组合物中包含的包括戊二酸二甲酯的脂族二羧酸二酯的总量计。
用于本发明组合物的优选戊二酸二甲酯来源是具有高戊二酸二甲酯含量的二元酯。例如,琥珀酸二甲酯、戊二酸二甲酯和己二酸二甲酯的混合物,含有99wt%戊二酸二甲酯(DMG,购自Chemoxy)Estasol DMG,是非常适合于本发明目的的。
此外,可湿固化组合物优选含有基于总组合物计0.1wt%-5wt%、优选0.25wt%-2.5wt%的式(I)有机硅烷OS,
Ra-Si(OCH3)3 (I)
其中
Ra是脂族、环脂族或芳族C4-C12烷基残基,优选C6-C10烷基残基,它任选含有醚氧或仲氨基。
在本发明的组合物中使用有机硅烷OS的优点是可以获得特别好的可重叠涂漆性,甚至超过其中仅使用脂族C3-C5二羧酸的二甲酯或二乙酯,特别是戊二酸二甲酯的组合物的可重叠涂漆性。
优选的有机硅烷OS包括正丁基三甲氧基硅烷、异丁基三甲氧基硅烷、苯基三甲氧基硅烷、辛基三甲氧基硅烷和N-(正丁基)-3-氨基丙基三甲氧基硅烷。
在特别优选的实施方案中,所述有机硅烷OS为N-(正丁基)-3-氨基丙基三甲氧基硅烷、辛基三甲氧基硅烷、苯基三甲氧基硅烷或这些硅烷的任意混合物。
优选地,组合物包含2.5wt%-10wt%的戊二酸二甲酯和0.25wt%-2.5wt%的所述有机硅烷OS,特别是辛基三甲氧基硅烷和/或N-(正丁基)-3-氨基丙基三甲氧基硅烷。
根据本发明的可湿固化组合物可进一步优选包含基于总组合物计0.5-2.5wt%的非根据上述式(I)的有机硅烷。
本发明的组合物可包含0-2.5wt%的至少一种单体或低聚有机硅烷,基于总组合物计。优选地,本发明的组合物包含基于总组合物计0.5-2wt%的单体或低聚的这种另外的有机硅烷。
使用低聚烷氧基硅烷的一个优点是,与纯单体硅烷相比,当以较大量使用它们时,可以实现较低的VOC水平。
合适的单体氨基官能烷氧基硅烷的实例示于式(II),
其中
R2为具有1-6个碳原子,优选1或2个碳原子的一价烷基,最优选甲基;
R3为具有1-20个碳原子且任选包含选自O、N和S的杂原子的一价直链、环状或支链的烷基或芳烷基;
R4为具有1-12个碳原子,优选1-8个碳原子的一价直链、支链或环状的烷基或芳烷基,最优选为甲基;
R5为具有1-12个碳原子,优选1-6个碳原子的一价直链、支链或环状的烷基或芳烷基;
下标i是值为0或1的整数,优选0;
下标k是值为2或3的整数,前提是如果i=1,则k=2;
下标p是值为1-6的整数。
合适的低聚硅烷示于式(III)和(IV),其中式(III)表示直链低聚物,而式(IV)表示环状低聚物。还可以使用支链低聚物,至少为低聚物混合物的一部分。
用作低聚硅烷的合适的直链低聚物示于式(III),
其中
R1独立地代表
-具有1-6个碳原子、优选1或2个碳原子的烷氧基,更优选甲氧基,
-如上定义的R3,或
-如上定义的R4;以及
下标n是值为1-30的整数。
用作低聚硅烷的合适的环状低聚物示于式(IV),
其中
R1具有与上述相同的含义;以及
下标j是值为3-30的整数。
优选的单体或低聚的氨基官能烷氧基硅烷包括3-氨基丙基三甲氧基硅烷、3-氨基丙基二甲氧基甲基硅烷、N-(2-氨基乙基)-3-氨基丙基三甲氧基硅烷、N-(2-氨基乙基)-3-氨基丙基二甲氧基甲基硅烷、N-(2-氨基乙基)-N'-[3-(三甲氧基甲硅烷基)-丙基]乙二胺和由上述氨基硅烷缩合得到的低聚物,所述氨基硅烷任选与烷基烷氧基硅烷,特别是甲基三甲氧基硅烷、乙基三甲氧基硅烷、丙基三甲氧基硅烷、乙烯基三甲氧基硅烷、正丁基三甲氧基硅烷、异丁基三甲氧基硅烷、苯基三甲氧基硅烷和辛基三甲氧基硅烷一起低聚。
还优选的是用乙氧基代替甲氧基的单体或低聚物或其类似物。
当用于本发明的组合物中时,这些硅烷具有的优点是它们既改进了组合物在各种基材上的粘合性,又改进了组合物的固化速率,而不会损害机械性能。
此外,优选作为非根据式(I)的有机硅烷的是环氧或硫醇官能的有机硅烷。这些硅烷改善了在各种基材上的粘合性。
此外,该组合物可以包含0-40wt%,优选5-25wt%,更优选7-15wt%的至少一种增塑剂,基于总组合物计。
增塑剂可以是通常用于基于硅烷官能聚合物的组合物中的任何增塑剂。这些包括例如羧酸酯,如邻苯二甲酸酯,尤其是邻苯二甲酸二辛酯,邻苯二甲酸二(2-乙基己基)酯,邻苯二甲酸二(3-丙基庚基)酯,邻苯二甲酸二异壬酯或邻苯二甲酸二异癸酯,邻环己烷二羧酸二酯,尤其是1,2-环己烷二羧酸二异壬酯,己二酸酯,尤其是己二酸二辛酯,己二酸二(2-乙基己基)酯,壬二酸酯,尤其是壬二酸二(2-乙基己基)酯,癸二酸酯,尤其是癸二酸二(2-乙基己基)酯或癸二酸二异壬酯,二醇醚,二醇酯,有机磷酸酯或磺酸酯,磺酰胺,聚丁烯,或衍生自天然脂肪或油的脂肪酸甲酯或乙酯,也称为“生物柴油”。
此外合适的是聚合物增塑剂。这些具有向周围区域较低趋势迁移和对VOC水平贡献较低的优点。
术语“聚合物增塑剂”在此是指在室温下为液体并且不含可水解硅烷基的聚合物添加剂。与传统的增塑剂如邻苯二甲酸酯相比,聚合物增塑剂通常具有更高的分子量。
优选地,聚合物增塑剂具有500-12000g/mol,特别是1000-10000g/mol,更优选2500-5000g/mol的平均分子量Mn。
合适的聚合物增塑剂包括多元醇,例如那些适于制备在此提及的有机聚合物P的多元醇,只要它们在室温下为液体。优选的适合作为聚合物增塑剂的多元醇包括聚醚多元醇、聚酯多元醇、聚烃多元醇、聚丁二烯多元醇和聚(甲基)丙烯酸酯多元醇。特别优选的是聚醚多元醇,特别是平均分子量Mn为500-12000g/mol,尤其是1000-10000g/mol,更优选2500-5000g/mol的那些。
这种多元醇特别适合与有机聚合物P组合。
使用聚醚多元醇作为聚合物增塑剂的主要优点是特别快的粘附力建立和特别好的粘附性质。聚合物增塑剂的特别优选的实施方案具有封闭的羟基,例如转化成酯基。
该组合物还包含用于烷氧基硅烷固化,尤其是用于含有硅烷基的聚合物交联反应的固化催化剂。合适的催化剂尤其是有机金属化合物和/或碱性含氮或磷化合物。
合适的金属有机化合物尤其是锡、钛、锆、铝或锌的化合物,尤其是二有机锡(IV)化合物,例如特别是二乙酸二丁基锡(IV)、二月桂酸二丁基锡(IV)、二新癸酸二丁基锡(IV)或双(乙酰丙酮)二丁基锡(IV)和二月桂酸二辛基锡(IV),以及钛(IV)或锆(IV)或铝(III)或锌(II)配合物,尤其是与烷氧基、羧酸根、1,3-二酮酸、1,3-酮酸酯或1,3-酮酰胺配体的配合物。
合适的碱性含氮或磷的化合物尤其是咪唑、吡啶、磷腈碱或优选胺、六氢三嗪、双胍、胍或其它脒。
此外,该组合物可以包含作为助催化剂的酸,尤其是羧酸。优选的是脂族羧酸,例如甲酸、月桂酸、硬脂酸、异硬脂酸、油酸、2-乙基-2,5-二甲基己酸、2-乙基己酸、新癸酸、来自天然脂肪和油的水解的脂肪酸混合物或二和多羧酸,尤其是聚(甲基)丙烯酸。
在优选的实施方案中,组合物基本上不含有机锡化合物。不含有机锡的组合物在保护健康和保护环境方面是有利的。更特别地,在一些优选的实施方案中,可固化组合物的锡含量小于0.1wt%,尤其小于0.05wt%。这些实施方案由于低水平的潜在有害有机锡化合物而对消费者特别有益。
合适的碱性含氮或磷化合物尤其是咪唑、吡啶、磷腈碱、仲胺或叔胺、六氢三嗪、双胍、胍或脒。
适合作为催化剂的含氮化合物特别是胺,尤其是N-乙基二异丙基胺、N,N,N',N'-四甲基亚烷基二胺、1,4-二氮杂双环[2.2.2]辛烷;脒,例如尤其是1,8-二氮杂双环[5.4.0]十一碳-7-烯(DBU)、1,5-二氮杂双环[4.3.0]壬-5-烯(DBN)、6-二丁基氨基1,8-二氮杂双环[5.4.0]十一碳-7-烯;胍,例如尤其是四甲基胍、2-胍基-苯并咪唑、乙酰丙酮-胍、3-二-邻甲苯基胍、2-叔丁基-1,1,3,3-四甲基胍;和咪唑,特别是N-(3-三甲氧基甲硅烷基丙基)-4,5-二氢咪唑和N-(3-三乙氧基甲硅烷基丙基)-4,5-二氢咪唑。
权利要求1-7任一项的可湿固化组合物,特征在于用于烷氧基硅烷基的固化催化剂为金属有机催化剂、胺化合物或其混合物。
该组合物可以包含其它成分,特别是以下助剂和添加剂:
-增粘剂和/或交联剂,尤其是其它氨基硅烷、巯基硅烷、环氧硅烷、(甲基)丙烯酰基硅烷、酸酐基硅烷、氨基甲酸酯基硅烷、烷基硅烷或亚氨基硅烷,这些硅烷的低聚形式,由伯氨基硅烷与环氧硅烷或(甲基)丙烯酰基硅烷或酸酐基硅烷形成的加合物,氨基官能的烷基倍半硅氧烷,3-缩水甘油氧基丙基三甲氧基硅烷,3-缩水甘油氧基丙基三乙氧基硅烷或3-脲基丙基三甲氧基硅烷,或这些硅烷的低聚形式;
-干燥剂(desiccants)或干燥剂(drying agents),尤其是四乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷或在硅烷基的α位具有官能团的有机烷氧基硅烷,尤其是N-(甲基二甲氧基甲硅烷基甲基)-O-甲基氨基甲酸酯、(甲基丙烯酰氧基甲基)硅烷、甲氧基甲基硅烷、原甲酸酯、氧化钙或分子筛,尤其是乙烯基三甲氧基硅烷或乙烯基三乙氧基硅烷;
-另外的增塑剂,尤其是反应性增塑剂,其为单官能聚硅氧烷或单官能有机聚合物的形式,即仅在一端具有硅烷反应性的那些;
-溶剂;
-无机或有机填料,尤其是天然、研磨或沉淀的碳酸钙,其任选地用脂肪酸、特别是硬脂酸涂覆,重晶石(heavy spar),滑石,石英粉,石英砂,白云石,硅灰石,高岭土,煅烧高岭土,云母(硅酸铝钾),分子筛,氧化铝,氢氧化铝,氢氧化镁,二氧化硅,包括来自热解工艺的细碎二氧化硅,工业生产的炭黑,石墨,金属粉末如铝、铜、铁、银或钢,PVC粉末或中空球;
-纤维,尤其是玻璃纤维、碳纤维、金属纤维、陶瓷纤维或聚合物纤维,例如聚酰胺纤维或聚乙烯纤维;
-染料;
-颜料,尤其是二氧化钛或氧化铁;
-流变改性剂,特别是增稠剂或触变添加剂,尤其是层状硅酸盐如膨润土、蓖麻油衍生物、氢化蓖麻油、聚酰胺、聚氨酯、脲化合物、煅制二氧化硅、纤维素醚或疏水改性聚氧乙烯;
-抗氧化、热、光或UV辐射的稳定剂;
-天然树脂、脂肪或油,例如松香、虫胶、亚麻子油、蓖麻油或大豆油;
-非反应性聚合物,其优选在室温下为固体,例如特别是不饱和单体,尤其选自乙烯、丙烯、丁烯、异丁烯、异戊二烯、乙酸乙烯酯或(甲基)丙烯酸烷基酯的均聚物或共聚物,尤其是聚乙烯(PE)、聚丙烯(PP)、聚异丁烯、乙烯-乙酸乙烯酯共聚物(EVA)或无规立构聚-α-烯烃(APAO);
-阻燃物质,尤其是已经提到的填料氢氧化铝和氢氧化镁,或特别是有机磷酸酯,例如特别是磷酸三乙酯、磷酸三甲苯酯、磷酸三苯酯、磷酸二苯基甲苯酯、磷酸异癸基二苯酯、磷酸三(1,3-二氯-2-丙基)酯、磷酸三(2-氯乙基)酯、磷酸三(2-乙基己基)酯、磷酸三(氯异丙基)酯、磷酸三(氯丙基)酯、异丙基化三苯基磷酸酯、不同异丙基化程度的磷酸单-、双-或三(异丙基苯基)酯、间苯二酚双(二苯基磷酸酯)、双酚A双(二苯基磷酸酯)或多磷酸铵;
-表面活性物质,尤其是润湿剂、流平剂、脱气剂或消泡剂;
-杀生物剂,尤其是杀藻剂、杀真菌剂或抑制真菌生长的物质;
和其它常用于可固化组合物的物质。在将某些组分混合到组合物中之前,最好对其进行化学或物理干燥。
在本发明可湿固化组合物的优选实施方案中,该组合物还包含增塑剂、填料、触变添加剂、稳定剂和/或颜料。
该组合物优选包含基于总组合物计0.5-2.5wt%、优选1-2wt%的至少一种干燥剂(desciccant)或干燥剂(drying agent),最优选乙烯基三甲氧基硅烷。该范围具有的优点是,可以获得最佳的储存稳定性和结皮时间,而不会使产品在固化后太刚性和/或易碎。
在优选的实施方案中,组合物包含至少一种干燥剂和至少一种增粘剂。
优选在排除水分的情况下生产和储存组合物。通常,它在合适的包装或装置中在排除了水分的情况下是储存稳定的,所述包装或装置例如更具体地为瓶、罐、袋、桶、筒或料盒。
该组合物可以是单组分或多组分,尤其是双组分组合物的形式。
在本文中,“单组分”是指其中组合物的所有成分以混合物形式储存在同一容器中并且可用水分固化的组合物。
在本文中,“双组分”是指组合物的成分存在于两个不同的组分中的组合物,所述两种不同的组分储存在单独的容器中。仅在施用组合物之前不久或施用期间,将两种组分彼此混合,然后任选地在水分的作用下,混合的组合物固化。
在施用之前或施用时,将任何第二组分或任选的其它组分与第一组分混合,尤其是通过静态混合器或通过动态混合器。
该组合物尤其在环境温度下,优选在0℃-45℃,尤其是5℃-35℃的温度范围内施用,并在这些条件下固化。
在应用时,如果合适的话在水分的影响下开始硅烷基的交联反应。存在的硅烷基可以与存在的硅烷醇基缩合,得到硅氧烷基(Si-O-Si基)。存在的硅烷基也可以在与水分接触时水解,得到硅烷醇基(Si-OH基团)并通过随后的缩合反应形成硅氧烷基(Si-O-Si基)。作为这些反应的结果,组合物最终固化。式(I)的脒或其反应产物加速该固化。
如果固化需要水,这可以来自空气(空气水分),或者组合物可以与含水组分接触,例如通过用例如光滑剂涂漆,或者通过喷雾,或者可以在施用时将水或含水组分加入组合物中,例如以含水或释水液体或糊剂的形式。如果组合物本身是糊剂形式,则糊剂是特别合适的。
在通过空气水分固化的情况下,组合物从外到内固化,首先在组合物的表面上形成结皮。所谓“结皮时间”或“结皮形成时间”是组合物固化速率的量度。固化速度通常由多种因素决定,例如水的可用性(例如,相对空气水分)、温度等。
该组合物适合于多种用途,尤其作为涂漆、清漆或底漆,作为用于生产纤维复合材料的树脂,作为硬质泡沫、软质泡沫、模制品、弹性体、纤维、膜(film)或膜(membrane),作为用于建筑和工业应用的灌注混合料、密封剂、粘合剂、覆盖物、涂料或涂漆,例如作为接缝密封、空腔密封、电绝缘混合料、填平料、接头密封剂、焊接或卷压接缝密封剂、装配粘合剂、车身粘合剂、玻璃安装粘合剂、夹层元件粘合剂、层压粘合剂、窗户和立面膜粘合剂、层压粘合剂、包装粘合剂、木材粘合剂、拼接地板粘合剂、锚固粘合剂、地板覆盖物、地板涂料、阳台涂料、屋顶涂料、混凝土保护涂料、停车库涂料、密封、管道涂料、防腐蚀涂料、织物涂料、阻尼元件、密封元件或填平料。
该组合物特别适合作为粘合剂和/或密封剂,尤其是用于建筑和工业应用中的接缝密封和弹性粘合剂粘结,以及作为具有裂缝桥接性能的弹性涂料,尤其是用于保护和/或密封例如屋顶、地板、阳台、停车平台或混凝土管。
因此,该组合物优选为粘合剂或密封剂或涂料。
该组合物最适用于修补或修复经上涂漆、清漆和/或天然漆的基材,特别是金属、涂覆的金属或经上涂漆、天然漆和/或清漆的金属。
这种组合物通常包含增塑剂、填料、粘合促进剂和/或交联剂和干燥剂,以及任选的其它助剂和添加剂。
对于作为粘合剂或密封剂的应用,组合物优选具有结构粘性的糊状稠度。这种糊状密封剂或粘合剂尤其从标准料盒,或从筒或提桶,任选通过涂装机器人施加到基材上,所述标准料盒借助于压缩空气或用电池手动操作,所述筒或提桶借助于输送泵或挤出机操作。
对于作为涂料的应用,组合物优选在室温下具有液体稠度和自流平性质。它可以是略微触变的,使得涂料可应用于倾斜至垂直表面而不会立即流走。尤其是通过辊或刷或通过倾倒和通过例如辊、刮刀或切口抹刀分布来施涂。
在可湿固化组合物的优选实施方案中,可湿固化组合物是可喷涂的。这意味着粘度如此低,以致于组合物是可喷涂的。令人惊奇的是,戊二酸二甲酯的使用有助于实现如此低的粘度。
在施用时,优选将组合物施用到至少一个基材上。
合适的基材尤其是
-玻璃、玻璃陶瓷、混凝土、砂浆、砖、瓦、石膏和天然石材,例如石灰石、花岗岩或大理石;
-皮革、织物、纸、木材、用树脂例如酚醛树脂、三聚氰胺树脂或环氧树脂粘合的木基材料、树脂-织物复合材料和其它聚合物复合材料;
-塑料,例如聚氯乙烯(硬质和软质PVC)、丙烯腈-丁二烯-苯乙烯共聚物(ABS)、聚碳酸酯(PC)、聚酰胺(PA)、聚酯、聚甲基丙烯酸甲酯(PMMA)、环氧树脂、聚氨酯(PUR)、聚甲醛(POM)、聚烯烃(PO)、聚乙烯(PE)或聚丙烯(PP)、乙烯/丙烯共聚物(EPM)和乙烯/丙烯/二烯三元共聚物(EPDM),以及纤维增强塑料,例如碳纤维增强塑料(CFP)、玻璃纤维增强塑料(GFP)和片状模塑料(SMC),其中所述塑料可以已经通过等离子体、电晕或火焰进行表面处理;
-涂覆的基材,例如粉末涂覆的金属或合金;
-涂漆、天然漆或清漆,特别是汽车面漆。
如果需要,可以在施用组合物之前预处理基材,特别是通过化学和/或物理清洁方法或通过施用增粘剂、增粘剂溶液或底漆。
通常,在施用组合物之前不需要预处理表面。该组合物在各种未涂底漆的、未预处理的、甚至未清洁的材料上显示出优异的粘合性。
因此,本发明的另一方面是一种用于修复损坏的经上涂漆、清漆和/或天然漆的物品的方法,包括步骤:
a)任选地除去物品受损部分的涂漆、清漆和/或天然漆;
b)通过使用如上所述的可湿固化组合物粘合粘结、密封、填充或涂覆所述的受损部分而机械地修复或恢复所述的物品受损部分;
c)通过空气水分或添加的水使所施加的可湿固化组合物固化;
d)将涂漆、清漆和/或天然漆重新施加到物品的修复或复原部分上和固化的组合物上。
优选地,所述涂漆、清漆和/或天然漆在步骤d)中通过喷涂重新施加。
在上述方法的优选实施方案中,所述受损的经上涂漆、清漆和/或天然漆的物品是车辆的车身,特别是机动车辆的车身。
本文公开的组合物通常具有优异的机械性能,特别是在高拉伸强度、高断裂伸长率和高抗撕裂扩展性方面,以及中到高的肖氏A硬度、低挤出力并因此容易施用,以及当搁置时优异的储存稳定性和尤其高的可重叠涂漆性。这使得它们尤其适合作为通用的弹性粘合剂、密封剂、填料和涂料,特别是在经上涂漆、天然漆或清漆的物品上的修复和恢复工艺中。
可以粘结或密封两个相同或两个不同的基材,尤其是上述基材。
在用水,特别是空气湿气形式的水和/或用至少一种合适的交联剂固化组合物之后,获得固化的组合物。
本发明的组合物在其固化或已固化状态下具有特别高的可重叠涂漆性,尤其是对于用作汽车面漆的涂漆、天然漆和/或清漆。此外,它通常在未打开容器中具有至少12个月的储存稳定性。
本发明的另一方面是本文所述的粘合剂组合物用于粘合粘结、涂覆或密封基材的用途。
使用该组合物得到的制品尤其是已经粘结、密封或涂布了该组合物的制品。所述制品尤其是建筑结构,尤其是通过结构工程或土木工程、工业建造的结构或消费品,尤其是窗户、家用电器或运输方式,例如更特别地是汽车、巴士、卡车、轨道车辆、船、飞机或直升机;或者该制品可以是其可安装组件。
因此,本发明的另一方面是通过本文所述的粘合剂组合物粘合密封、涂布、填充或粘结的基材。
实施例
下面引入的是工作实施例,其旨在详细阐明所描述的本发明。应当理解,本发明不限于这些描述的工作实施例。
术语“标准气候条件”是指23±1℃的温度和50±5%的相对空气湿度。
测试方法:
拉伸强度和断裂伸长率根据DIN EN 53504(拉伸速度:200mm/min)在标准气候条件下固化7天后在厚度为2mm的固化膜上进行测定。
抗撕裂扩展性根据DIN 53515在标准气候条件下固化7天后在层厚度为2mm的膜上测定。
为了测定挤出力,将组合物分配到内部涂覆的铝料盒(外径46.9mm,内径46.2mm,长度215mm,公制ISO线M15x1.5 mm)中,并用Novelis Germany GmbH的聚乙烯塞子(直径46.1mm)进行气密密封。在23℃下调理24小时(或14天60℃热老化和在23℃下调理4小时)后,打开料盒,使用挤出装置挤出内容物。为此,将具有2mm内径开口的喷嘴拧到料盒螺纹上。使用挤出装置(Zwick/Roell Z005),确定以60mm/min的挤出速率挤出组合物所需的力。报告的数字是在22mm、24mm、26mm和28mm的挤出距离之后测量的力的平均值。在挤出距离为30mm之后,停止测量。
肖氏A硬度根据DIN 53505在标准气候条件下使用固化7天后层厚度为6mm的试样测定。
为了测定结皮时间(直至不粘表面的时间,“无粘时间”),将一小部分待测试的粘合剂组合物(在23℃下测试之前储存24小时或在60℃下在密闭容器中储存7天以模拟老化,并且随后在23℃下适应4小时),以3mm的层厚度施加在纸板上,并且在23℃和50%相对湿度下测定时间,该时间是通过由LDPE制成的移液管在固化粘合剂的表面上轻微敲击所花费的时间。无粘时间是首次在移液管上没有残留粘合剂的时间。
使用网格测试的可涂漆性使用以下程序进行:用庚烷彻底清洗铝板,并用Aktivator-205(Sika Schweiz)预处理,以确保在测试方案期间所有组合物在其上的适当粘附。将木质隔板(厚度3.5mm)放置在铝板上,在这些隔板之间,将组合物施加到铝表面上。使用刮刀除去过量的组合物,从而在铝板上产生3.5mm的新鲜组合物的平坦和光滑的层。在23℃和50%r.h.下固化24h之后,根据各涂漆的应用规格将各汽车涂漆喷涂到固化的组合物上。在油漆干燥后,通过喷涂在其上施加透明涂层(根据涂漆制造商的说明书)。然后将包括透明涂层的整个分层涂料在60℃的烘箱中彻底干燥40分钟。
此后,在覆盖固化组合物的涂漆上开始交叉切割工序。这通过使用薄刀以1mm的切口之间的线距离穿过涂漆水平切割6个切口和垂直切割6个切口来进行。这产生了具有90°交叉角的6×6线的网格。该过程根据ISO 2409(2007)对61-120微米厚的涂漆层进行。然后,用力将压敏胶带按压到切割区域上。在施加胶带的5分钟内,通过抓住自由端并以约45-60°的角度将其快速拉离而将其移除。
涂漆对密封剂胶条的粘附性完全按照ISO 2409(2007)所述进行评价:
GT0:切口边缘完全光滑;没有网格的正方形被分离。
GT1:在切口交叉处的涂层小片分离。不大于5%的交叉切割面积受到影响。
GT2:涂层沿着边缘和/或在切口的交叉处剥落。大于5%,但不大于15%的交叉切割面积受到影响。
GT3:涂层已经沿切口边缘部分或全部以大条带的形式剥落,和/或其已经部分或全部在正方形的不同部分上剥落。大于15%,但不大于35%的交叉切割面积受到影响。
GT4:涂层沿切口边缘剥落成大条带和/或一些方形部分或全部分离。大于35%,但不大于65%的交叉切割面积受到影响。
GT5:甚至不能通过GT4分级进行分级的任何程度的剥落。
该测量结果以%粘附力示于表4和5中,意味着GT0分类以100%示出。例如,表4或5中85%的数值对应于GT2分类。
表1:用于实施例组合物的化合物。
制备含有反应性硅烷基的聚合物P:
聚合物STP:在排除水分的情况下,将1000g12200多元醇(具有低不饱和度的聚氧化亚丙基二醇,得自Covestro;OH值11.0mg KOH/g)、43.6g异佛尔酮二异氰酸酯(IPDI;IPDI,得自Evonik)、126.4g邻苯二甲酸二异癸酯(DIDP)和0.12g二月桂酸二丁基锡(DBTDL)加热至90℃,同时不断搅拌,并在该温度下静置,直到通过滴定分析测定的游离异氰酸酯基团的含量达到0.63wt%的稳定值。随后,将63.0g N-(3-三甲氧基甲硅烷基丙基)-氨基琥珀酸二乙酯(由3-氨基丙基三甲氧基硅烷与马来酸二乙酯形成的加合物;根据US 5,364,955中的详细描述制备)混入,并将混合物在90℃下搅拌,直至通过FT-IR光谱不再能检测到任何游离异氰酸酯。将如此获得的具有硅烷当量为约6880g/eq(由所用的量计算)的含三甲氧基硅烷基的聚醚冷却至室温,并在排除水分的情况下储存。
触变添加剂的制备:
在真空混合器中首先加入1000g邻苯二甲酸二异癸酯(Z,BASF SE,德国)和160g二苯基甲烷4,4'-二异氰酸酯(44MC L,Bayer MaterialScienceAG,德国),并温和加热。然后在剧烈搅拌下逐滴加入90g单丁胺。在减压下继续搅拌所得白色糊状物,同时再冷却一小时。这样得到的触变添加剂包含在80wt%邻苯二甲酸二异癸酯中的20wt%触变剂,并在不进一步加工情况下用于配制。
基于含有反应性硅烷基的聚合物的组合物:
比较例(非根据本发明)在表2-9中由“(Ref)”来标记。所用化合物在表1中详细说明。
组合物C1-C17:
通过在真空混合器中在氮气气氛下混合表2、3、8和8中所示的成分制备一系列实施例组合物。首先,将聚合物P、增塑剂和二烷基酯(例如DMG,如果适用的话)、触变添加剂和VTMO(如果适用的话)充分混合5分钟。随后,在60℃下在15分钟内捏合加入干燥的填料。在关闭加热器的情况下,加入硅烷OS(如果适用的话)和其它硅烷和催化剂,随后在10分钟内将组合物在真空下加工成均匀的糊状物。随后将所述糊状物填充到内部涂覆的铝涂布活塞料盒中,所述活塞料盒是气密封闭的并且在标准气候条件下储存至少24小时,直到采用测试方案。
组合物 | C1(Ref.) | C2 | C3 | C4 |
聚合物STP(聚合物P) | 25 | 25 | 25 | 25 |
DIDP(增塑剂) | 8.5 | 3.5 | 3.5 | 7.5 |
Solusolv(增塑剂) | 4 | 4 | 4 | - |
DMG | - | 5 | 5 | 5 |
VTMO | 1.5 | 1.5 | 1.5 | 1.5 |
触变添加剂 | 6 | 6 | 6 | 6 |
GCC(填料) | 52 | 52 | 52 | 52 |
有机硅烷1 | 1 | 1 | 1 | 1 |
有机硅烷2 | 0.5 | 0.5 | - | - |
有机硅烷OS1 | - | - | 0.5 | 0.5 |
Sn催化剂 | 1.5 | 1.5 | 1.5 | 1.5 |
表2:实施例组合物(所有数值以基于总的各个组合物的wt%计)。
表3:实施例组合物(所有数值以基于总的各个组合物的wt%计)。
结果清楚地显示,本发明组合物显示出显著改善的用所有测试的汽车涂漆的可重叠涂漆性。本发明组合物的机械性能不受本发明组成调节的影响。此外,本发明实施例的挤出力显著低于参考实施例,这对于组合物的容易施用和可喷涂性是有利的。
测试结果示于表4和5中:
表4:所研究样品的测试结果。“n/m”表示“未测量”。
表5:所研究样品的测试结果。
进行另外的实验以研究羧酸的不同酯的影响。这些组合物C9-C12示于表6中。
这些实施例组合物的一些测量结果示于表7中。
表7显示,脂族C3-C5二羧酸的二异丁酯(实验C10)显示在密闭容器中热贮存(老化模拟)后,固化机理严重失活。这在热存储后的大大延长的不粘时间中可观察到。非根据本发明的不同酯(实验C11)显示了太高的挤出力,在热贮存后这甚至更突出。
表6:实施例组合物(所有数值以基于总的各个组合物的wt%计)。
表7:研究样品的测试结果。
表8和9显示了进一步研究不同的二羧酸二甲酯及其混合物的影响的其他实验。这些组合物C13-C17示于表8中。
这些实施例组合物的一些测量结果示于表9中。
表9显示随着戊二酸二甲酯(相对于己二酸二甲酯)量的增加,拉伸强度以及断裂伸长率增加,而挤出力降低。不粘时间、肖氏A和可重叠涂漆性不受显著影响。与含有显著量戊二酸二甲酯的样品相比,使用琥珀酸二甲酯的实验C17显示较低的伸长率和稍高的挤出力。
组合物 | C13 | C14 | C15 | C16 | C17 |
聚合物STP(聚合物P) | 25 | 25 | 25 | 25 | 25 |
DINCH(增塑剂) | 3.5 | 3.5 | 3.5 | 3.5 | 3.5 |
Solusolv(增塑剂) | 4 | 4 | 4 | 4 | 4 |
DMG | 1 | 2.5 | 4 | 5 | - |
DMA | 4 | 2.5 | 1 | - | - |
DMS | - | - | - | - | 5 |
VTMO | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 |
触变添加剂 | 6.0 | 6.0 | 6.0 | 6.0 | 6.0 |
GCC(填料) | 52.0 | 52.0 | 52.0 | 52.0 | 52.0 |
有机硅烷1 | 1 | 1 | 1 | 1 | 1 |
有机硅烷2 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
Sn催化剂 | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 |
表8:实施例组合物(所有数值以基于总的各个组合物的wt%计)。
表9:研究样品的测试结果。
Claims (15)
1.一种可湿固化组合物,包含
-至少一种含有反应性硅烷基的有机聚合物P;
-基于总组合物计,1.0wt%-25.0wt%、优选2.0wt%-20wt%、特别是2.5wt%-10wt%的脂族C3-C5二羧酸的二甲酯或二乙酯;以及
-至少一种用于烷氧基硅烷基团的固化催化剂。
2.权利要求1所述的可湿固化组合物,特征在于含有反应性硅烷基的有机聚合物P为聚氨酯、聚烯烃、聚酯、聚碳酸酯、聚酰胺、聚(甲基)丙烯酸酯或聚醚或这些聚合物的混合形式。
3.权利要求1或2中任一项所述的可湿固化组合物,特征在于所述组合物还含有基于总组合物计0.1wt%-5wt%、优选0.25wt%-2.5wt%的式(I)的有机硅烷OS,
Ra-Si(OCH3)3 (I)
其中
Ra为脂族、环脂族或芳族C4-C12烷基残基,其任选含有醚氧或仲氨基。
4.权利要求3所述的可湿固化组合物,特征在于所述有机硅烷OS为N-(正丁基)-3-氨基丙基三甲氧基硅烷、辛基三甲氧基硅烷、苯基三甲氧基硅烷或这些硅烷的任意混合物。
5.权利要求3或4中任一项所述的可湿固化组合物,特征在于所述组合物包含2.5wt%-10wt%的脂族C3-C5二羧酸的二甲酯或二乙酯,特别是戊二酸二甲酯,和0.25wt%-2.5wt%的所述有机硅烷OS。
6.权利要求1-5中任一项所述的可湿固化组合物,特征在于所述组合物还包含基于总组合物计0.5-2.5wt%的非权利要求3中式(I)的有机硅烷。
7.权利要求1-6中任一项所述的可湿固化组合物,特征在于所述组合物还包含至少一种另外的添加剂,所述添加剂选自增塑剂和稀释剂、填料、触变添加剂、稳定剂、干燥剂和颜料。
8.权利要求1-7中任一项所述的可湿固化组合物,特征在于用于烷氧基硅烷基的固化催化剂为金属有机催化剂、胺化合物或其混合物。
9.权利要求1-8中任一项所述的可湿固化组合物,特征在于所述脂族C3-C5二羧酸的二甲酯或二乙酯包含至少50wt%,优选至少75wt%,特别是至少90wt%的戊二酸二甲酯,基于所述组合物中含有的脂族C3-C5二羧酸酯的总量计。
10.权利要求1-9中任一项所述的可湿固化组合物,特征在于所述有机聚合物P以基于总组合物计10wt%-60wt%的量包含在所述组合物中。
11.权利要求1-10中任一项所述的可湿固化组合物,特征在于可湿固化组合物为可喷涂的。
12.用于修复损坏的经上涂漆、清漆和/或天然漆的物品的方法,包括步骤:
a)任选地除去物品受损部分的油漆、清漆和/或天然漆;
b)通过使用如权利要求1-11中任一项所述的可湿固化组合物粘合粘结、密封、填充或涂覆所述物品的受损部分,机械地修复或恢复所述物品的受损部分;
c)通过空气水分或添加的水使所施加的可湿固化组合物固化;
d)将涂漆、清漆和/或天然漆重新施加到物品的被修复或复原的部分上和固化的组合物上。
13.如权利要求12所述的方法,特征在于所述涂漆、清漆和/或天然漆在步骤d)中通过喷涂而被重新施加。
14.如权利要求12或13所述的方法,特征在于所述损坏的经上涂漆、清漆和/或天然漆的物品是车辆的车身,特别是机动车辆的车身。
15.根据权利要求1-11中任一项的可湿固化组合物用于粘合粘结、涂覆、填充或密封基材的用途。
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