CN111133018A - 用于促进的粘附性构建的活化剂 - Google Patents

用于促进的粘附性构建的活化剂 Download PDF

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Publication number
CN111133018A
CN111133018A CN201880062336.7A CN201880062336A CN111133018A CN 111133018 A CN111133018 A CN 111133018A CN 201880062336 A CN201880062336 A CN 201880062336A CN 111133018 A CN111133018 A CN 111133018A
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China
Prior art keywords
activator composition
adhesive
acetate
ketone
methyl
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Granted
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CN201880062336.7A
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CN111133018B (zh
Inventor
C·荣格
M·德米格
R·坎纳斯
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Sika Technology AG
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Sika Technology AG
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    • C08G18/16—Catalysts
    • C08G18/22—Catalysts containing metal compounds
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Abstract

本发明涉及一种活化剂组合物，其包含a)0.5‑50wt％的用于交联双组分粘合剂的催化剂K，其在23℃下为液体，b)40‑99.5wt％的有机溶剂L，c)0‑10wt％的至少一种硅烷S，其具有至少一种可水解的硅烷基团和优选至少一种选自巯基、环氧、氨基、甲基丙烯酰基、乙烯基和烷基的官能团，其特征在于所述催化剂K包含金属的1,3‑酮酰胺化物配合物，和溶剂L选自丙酮、甲基乙基酮、甲基正丙基酮、二异丁基酮、甲基异丁基酮、甲基正戊基酮、甲基异戊基酮、乙酰丙酮、异亚丙基丙酮、环己酮、甲基环己酮、乙酸乙酯、乙酸丙酯、乙酸异丙酯、乙酸丁酯、丙酸正丁酯、丙二酸二乙酯、乙酸1‑甲氧基‑2‑丙酯、乙酸3‑甲氧基正丁酯、乙基3‑乙氧基丙酸酯、二异丙醚、二乙醚、二丁醚、二乙二醇二乙醚、乙二醇二乙醚、乙二醇单丙醚、乙二醇单‑2‑乙基己醚、乙苯、甲苯、二甲苯、庚烷、辛烷、石脑油、石油溶剂油、石油醚、汽油、二氯甲烷、甲醇、乙醇、异丙醇和这些溶剂的混合物。根据本发明的活化剂组合物在至少一个月，优选至少2个月，特别是至少4个月或更长的时间内稳定储存，而没有显示出催化剂或硅烷的沉淀。此外，活化剂组合物的活性与所施加的量无关，并且可以以一定厚度的层来施加，使得可以在最多30秒的时间后施加粘合剂。活化剂组合物还可以促进2‑组分聚氨酯粘合剂在粘合基材上的粘附性构建，使得在施用2017‑0055WO 27/27粘合剂后最多一小时后并在室温下固化之后，已经实现在室温下储存24小时后可获得的粘合体拉伸剪切强度的至少10％，其中1小时后的断裂图样与24小时后一样是内聚性的。

Description

用于促进的粘附性构建的活化剂
技术领域
本发明涉及基于溶剂的活化剂组合物领域。
现有技术
基于溶剂的活化剂，尤其是作为增粘剂预涂层，长期以来一直被用来促进粘合剂、密封剂、涂料和覆层在基材上建立粘附性。这种活化剂能够更快地粘合或涂覆基材，并且在基材上非常迅速地开始建立粘合剂的粘附性，并使粘合仅在很短的时间之后即可以承受应力而不会发生粘合失效。这样可以加快工业制造的周期时间。溶剂的快速蒸发也有助于快速的工作和循环时间。
为了制备活化剂，通常将催化密封剂或粘合剂固化的催化剂溶解在溶剂中。涂布时溶剂会基本上蒸发，并且可以将粘合剂涂布到经过预处理的基材表面上。由于粘合表面上高浓度的催化活性中心，这导致了所需的粘附性的快速建立。
然而，迄今为止已知的许多活化剂组合物的缺点是这种催化剂(通常是金属配合物)在许多优选的溶剂中的溶解性很差。亦即在许多应用中，对溶剂的选择受到极大限制，因为存在与方法相关的有关溶剂的挥发性和健康无害性的严格规范。由此引起不希望的效果，即在短时间后观察到催化剂从溶液中沉淀出来。解决该缺点的一种方法是使用乳化剂或其他改善溶解度的添加剂。然而，这样的添加剂使组合物更昂贵并且会不利地影响粘附性。
同样不利的是，在施加活化剂组合物之后，许多催化剂在基材和粘合剂之间形成固体界面。这通常导致在短时间之后，即使在粘合剂具有良好粘附性的情况下，在基材与由活化剂组合物形成的层之间也会发生粘合失效。
此外，还会由于在很多情况下相对高浓度的催化剂必须存在于活化剂组合物中以实现粘附性建立所需的促进，从而加强这两种提及的不希望的效果。
因此，需要一种活化剂组合物，其具有良好的储存稳定性而不会沉淀出催化剂，并且不会引起由于在基材和粘合剂的界面处形成催化剂沉积物而引起的任何粘附问题。还期望的是，无论使用量，该活化剂都将显示令人满意的活化剂作用，并且例如可以以非常薄的层施加，这由于较短的脱气时间而能节省时间并由于较低的材料消耗而节省成本，或在非常高的施涂量下使用厚涂层，这带来更好的活化剂作用。
发明概述
因此，本发明的目的在于提供一种单组分的基于溶剂的活化剂组合物，其在至少一个月，优选至少两个月，尤其是至少四个月或更长的时间储存稳定，并且不显示出催化剂的沉淀。另外，活化剂组合物应是活性的而与施加的量无关，并且具有如此短的通风时间，使得可以在短时间例如30秒之后施加粘合剂。另外，活化剂组合物应能在粘合基材上建立粘附性的方面促进2-组分聚氨酯粘合剂，使得在施加粘合剂并且在室温下固化后最多一小时之后就已经能达到可以在室温下储存24小时之后获得的粘合体拉伸剪切强度的至少15％、优选至少20％，并且断裂图样在1小时后如24小时后一样是内聚断裂的。
现在已经令人惊讶地发现，如权利要求1所述的活化剂组合物能够实现这些目的。
本发明的其他方面是其它独立权利要求的主题。本发明特别优选的实施方案是从属权利要求的主题。
发明详述
本发明提供了一种活化剂组合物，其包含
a)0.5-50wt％的用于交联双组分粘合剂的催化剂K，其在23℃下为液体，
b)40-99.5wt％的有机溶剂L，
c)0-10wt％的至少一种硅烷S，其具有至少一种可水解的硅烷基团和优选至少一种选自巯基、环氧、氨基、甲基丙烯酰基、乙烯基和烷基的官能团，
其特征在于所述催化剂K包含金属的1,3-酮酰胺化物配合物，和所述溶剂L选自丙酮、甲基乙基酮、甲基正丙基酮、二异丁基酮、甲基异丁基酮、甲基正戊基酮、甲基异戊基酮、乙酰丙酮、异亚丙基丙酮、环己酮、甲基环己酮、乙酸乙酯、乙酸丙酯、乙酸异丙酯、乙酸丁酯、丙酸正丁酯、丙二酸二乙酯、乙酸1-甲氧基-2-丙酯、乙酸3-甲氧基正丁酯、乙基-3-乙氧基丙酸酯、二异丙基醚、二乙基醚、二丁基醚、二乙二醇二乙基醚、乙二醇二乙醚、乙二醇单丙醚、乙二醇单-2-乙基己基醚、乙苯、甲苯、二甲苯、庚烷、辛烷、石脑油、石油溶剂油、石油醚、汽油、二氯甲烷、甲醇、乙醇、异丙醇和这些溶剂的混合物。
在本文中，以“多(聚)”起始的物质名称，例如多元醇或多异氰酸酯，是指形式上每分子包含两个或更多个在其名称中出现的官能团的物质。
在本文中，术语“聚合物”一方面包括一类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的集合，其通过聚合反应制备(聚加成，加聚，缩聚)。该术语另一方面还包含由聚合反应获得的这类大分子集合的衍生物，即通过在给定大分子上的官能团的反应，例如加成或取代反应获得的并且可以是化学均一或化学不均一的化合物。该术语进一步还包括所谓的预聚物，即其官能团参与大分子的构建的反应性低聚预加合物。
术语“聚氨酯聚合物”包括根据所谓的二异氰酸酯加聚方法制备的所有聚合物。这还包括几乎或完全不含氨基甲酸酯基团的那些聚合物。聚氨酯聚合物的实例为聚醚-聚氨酯、聚酯-聚氨酯、聚醚-聚脲、聚脲、聚酯-聚脲、聚异氰脲酸酯和聚碳二亚胺。
在本文中，术语“硅烷”是指在一方面具有至少一个，通常两个、三个或四个经由Si-O键直接与硅原子键合的烷氧基或酰氧基的化合物。术语“有机硅烷”是指其额外地包含至少一个，和有时两个或三个经由Si-C键直接与硅原子键合的有机基团的硅烷。这种硅烷也被本领域技术人员称为有机烷氧基硅烷或有机酰氧基硅烷。因此，“四烷氧基硅烷”根据该定义不是有机硅烷但是属于硅烷。相应地,术语“硅烷基团”是指经由Si-C键与硅烷的有机基团连接的含硅基团。该硅烷，或者其烷氧基-或酰氧基硅烷基团，具有与水分接触时发生水解的特性。这形成了有机硅醇，即含有一个或多个硅烷醇基团(Si-OH基团)的有机硅化合物，并且通过随后的缩合反应形成有机硅氧烷，即含有一个或多个硅氧烷基团(Si-O-Si基团)的有机硅化合物。
术语“硅烷官能”是指包含硅烷基团的化合物。“硅烷官能的聚合物”相应地为包含至少一个硅烷基团的聚合物。
含硅烷的聚合物特别是含硅烷的有机聚合物，其通常和特别在本文中同义地也被描述为“硅烷官能的聚合物”、“硅烷改性的聚合物”(SMP)或“硅烷封端的聚合物”(STP)。它们的交联通过硅醇基团的缩合进行以形成硅氧烷键，并且一般是通过有机锡化合物例如羧酸二烷基锡(IV)进行催化。
术语“含硅烷基团的聚醚”还包括含硅烷基团的有机聚合物，其除了聚醚单元还可以含有氨基甲酸酯基团、脲基团或硫代氨基甲酸酯基团。这种含硅烷基团的聚醚也被称作“含硅烷的聚氨酯”。
“氨基硅烷”、“羟基硅烷”或“巯基硅烷”是指其有机基团分别具有氨基、羟基或巯基的有机硅烷。“伯氨基硅烷”是具有伯氨基的氨基硅烷，所述伯氨基即连接一个有机基团的NH2基团。“仲氨基硅烷”是指具有仲氨基的氨基硅烷，所述仲氨基即连接两个有机基团的NH基团。
当物质或组合物可以在室温下长时间(通常至少3个月至最多6个月或更长时间)存储在合适的容器中，同时其不会在其应用或使用性能方面由于存储而在与其使用相关的程度上有所变化，则该物质或组合物被称为“储存稳定”或“可存储的”。为了估计储存稳定性，可以在提高的温度下进行储存，这能模拟在较低温度例如室温下的较长储存。
“室温”是指约23℃的温度。
所有在本文中提及的工业标准均涉及首次申请的提交时刻有效的版本。
术语“质量”和“重量”在本文中同义地使用。因此，“重量百分比”(重量％)是百分比质量分数，除非另有说明，否则其涉及总组合物或根据上下文整个分子的质量(重量)。
“分子量”在本文中应当理解为是指分子或分子的一部分(也称作“基团”)的摩尔质量(以g/mol计)。“平均分子量”被理解为是指分子或基团的低聚或聚合混合物的数均Mn，其通常通过凝胶渗透色谱法(GPC)以聚苯乙烯为标准物进行测定。
本发明的活化剂组合物的第一重要成分是基于整个组合物计0.5-50wt％、优选0.75-25wt％、尤其是1-10wt％的用于交联双组分粘合剂的催化剂K，其在23℃下为液体。该催化剂K包含金属的1,3-酮酰胺化物配合物。
本发明重要的是，催化剂K在23℃下在纯物质的形式下或在溶剂L已经蒸发后残余的形式下为液体。
催化剂的选择主要取决于活化剂与何种粘合剂一起使用。在双组分粘合剂(例如聚氨酯粘合剂或基于硅烷封端的聚合物的粘合剂)领域的本领域技术人员知晓哪些催化剂对于其固化是有效的并且适用。
所述催化剂K包含具有至少一种1,3-酮酰胺化物配体的至少一种金属催化剂。本领域技术人员在聚氨酯化学领域对于羟基与异氰酸酯基的反应或在烷氧基硅烷化学领域对于烷氧基硅烷和/或硅醇的反应熟知的合适的金属催化剂例如为铝、铋、铁、锌、锆或锡的配合物。
合适的催化剂K尤其是有机锡(IV)化合物，铁(III)、铋(III)或锆(IV)的化合物，尤其是铁(III)配合化合物。这些配合物的配体尤其选自醇盐、羧酸盐、1,3-二酮酸盐、肟酸盐、1,3-酮酸酯化物和1,3-酮酰胺化物。然而，必须存在至少一种1,3-酮酰胺化物配体。
特别优选的是式Fe(L)x(Y)3□x的配合物，尤其是铁(III)配合化合物，其中x为1、2或3，Y为带有一价负电荷的配体，和L为下式(I)的配体
Figure BDA0002425096640000061
其中R1和R2彼此独立地为氢基，具有1-10个碳原子的单价饱和或不饱和烃基，或一起为具有3-6个碳原子的二价亚烷基，和R3和R4彼此独立地为氢基，任选含有杂原子和具有1-12个碳原子的单价饱和烃基，或一起为任选含有杂原子并且具有3-6个碳原子的二价亚烷基。这种配合化合物的制备描述于EP2604617中。
优选的是具有三个相同的式(I)的L配体的式Fe(L)3的配合化合物，尤其是铁(III)配合化合物，其中R1表示具有1-4个碳原子的烷基或苯基，R2表示氢基，和R3和R4表示具有1-8个碳原子的烷基或具有1-4个碳原子的烷基醚基团。
非常特别优选的是具有三个相同的式(I)的L配体的式Fe(L)3的配合化合物，尤其是铁(III)配合化合物，其中R1为甲基、R2为氢基和R3和R4各自为乙基，或R1为甲基、R2为氢基和R3和R4为具有3个碳原子的烷基醚基，或R1为苯基、R2为氢基和R3和R4为丁基，或R1为丁基、R2为氢基和R3和R4为丁基。
作为催化剂K的配合化合物的特别优选的配体为1,3-酮酰胺化物，尤其是N,N-二乙基-3-氧代丁酰胺化物,N,N-二丁基-3-氧代丁酰胺化物,N,N-双(2-乙基己基)-3-氧代丁酰胺化物,N,N-双(2-甲氧基乙基)-3-氧代丁酰胺化物,N,N-二丁基-3-氧代庚酰胺化物,N,N-双(2-甲氧基乙基)-3-氧代庚酰胺化物,N,N-双(2-乙基己基)-2-氧代环戊烷羧酰胺,N,N-二丁基-3-氧代-3-苯基丙酰胺化物和N,N-双(2-甲氧基乙基)-3-氧代-3-苯基丙酰胺化物。这些更优选用作Fe(III)配合物。铁(III)酮酰胺化物具有以下优点：特别热稳定和即使在苛刻的温度条件下，例如大于100℃至150℃下也不会失活。
适用作催化剂K的化合物，除了1,3-酮酰胺化物配合物之外为含氮化合物，例如特别是N-乙基二异丙基胺、N,N,N',N'-四甲基亚烷基二胺、聚氧化烯胺、1,4-二氮杂双环[2.2.2]辛烷；氨基硅烷例如特别是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-氨基丙基甲基二甲氧基硅烷、N-(2-氨基乙基)-N'-[3-(三甲氧基甲硅烷基)丙基]亚乙基二胺以及用乙氧基或异丙氧基代替硅上的甲氧基的类似物；脒，例如特别是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；胍类例如特别是四甲基胍,2-胍基苯并咪唑、乙酰丙酮胍、1,3-二-邻-甲苯基胍,2-叔-丁基-1,1,3,3-四甲基胍；和咪唑类，例如特别是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。
尤其合适的还为不同催化剂的组合物，特别是至少一种金属催化剂和至少一种含氮化合物的组合。
在活化剂组合物的一个优选的实施方案中，催化剂K包含选自Fe,Bi,Al,Zn和Zr的金属和任选另外地选自叔胺、胍和脒的有机化合物的配合物。
在活化剂组合物的一个优选的实施方案中，催化剂K包含金属的1,3-酮酰胺化物配合物，尤其是Fe(III)-1,3-酮酰胺化物配合物。
在活化剂组合物的一个优选的实施方案中，活化剂组合物不含锡化合物。这种组合物特别对用户友好并且对环境友好，因为锡化合物在健康方面令人担忧，并且在某些情况下证明具有毒性。
另外，本发明的活化剂组合物包含40-99.5wt％，优选65-99wt％，尤其是85-99wt％的有机溶剂L，基于整个组合物计。
溶剂L选自丙酮、甲基乙基酮、甲基正丙基酮、二异丁基酮、甲基异丁基酮、甲基正戊基酮、甲基异戊基酮、乙酰丙酮、异亚丙基丙酮、环己酮、甲基环己酮、乙酸乙酯、乙酸丙酯、乙酸异丙酯、乙酸丁酯、丙酸正丁酯、丙二酸二乙酯、乙酸1-甲氧基-2-丙酯、乙酸3-甲氧基正丁酯、乙基-3-乙氧基丙酸酯、二异丙基醚、二乙醚、二丁醚、二乙二醇二乙醚、乙二醇二乙醚、乙二醇单丙醚、乙二醇单-2-乙基己醚、乙苯、甲苯、二甲苯、庚烷、辛烷、石脑油、石油溶剂油、石油醚、汽油、尤其是SolvessoTM类(来自Exxon)、二氯甲烷、甲醇、乙醇、异丙醇和这些溶剂的混合物。
根据本发明的活化剂组合物的优选的实施方案包含选自正庚烷、乙醇、异丙醇、乙酸甲酯、乙酸乙酯、乙酸丁酯、乙酸异丙酯、乙酸1-甲氧基-2-丙基酯、乙酸3-甲氧基-正丁基酯、丙酮、甲基乙基酮、甲基异丁酮、甲苯、乙苯及其混合物的溶剂L。非常特别优选的，溶剂L选自正庚烷、乙醇、异丙醇、乙酸乙酯、甲基乙基酮及其混合物，其中溶剂L最优选包含正庚烷和/或乙醇或由正庚烷和/或乙醇组成。正庚烷和乙醇的混合物是特别优选的，因为活化剂组合物由此特别储存稳定并且同时特别快速地挥发。
另外，本发明的活化剂组合物包含基于整个组合物计0-10wt％、优选0.25-10wt％、尤其是0.5-5wt％的至少一种具有至少一个可水解的硅烷基团，尤其是两个硅烷基团，和优选至少一个选自巯基、环氧、氨基、甲基丙烯酰基、乙烯基和烷基的官能团的硅烷S。
添加至少一种硅烷S具有以下优点：在基材表面上形成共价地或通过其他相互作用而粘附的膜，这改善了粘合剂的粘附性。
合适的硅烷S一方面是在硅原子上具有4个可水解的键的硅烷，例如四烷氧基硅烷、例如四甲氧基硅烷、四乙氧基硅烷或其它四烷氧基硅烷，乙基其水解产物、部分水解产物或缩合物。
作为硅烷S合适和优选的还有有机硅烷OS，其除了在硅原子上的可水解的键之外还具有至少一个非可水解的Si-C键，经由该键将有机基团连接到硅原子上。该有机基团尤其是具有羟基、巯基、环氧、氨基、(甲基)丙烯酰基、乙烯基和/或烷基基团的基团。对于有机硅烷OS的情况，也可以使用其水解产物、部分水解产物或缩合物。
优选的有机硅烷OS包括环氧硅烷，例如特别是3-缩水甘油氧基丙基三甲氧基硅烷或3-缩水甘油氧基丙基三乙氧基硅烷、羟基硅烷、(甲基)丙烯酰基硅烷、酸酐基硅烷、氨基甲酸酯基硅烷、乙烯基硅烷、烷基硅烷或亚氨基硅烷，或这些硅烷的低聚物形式。
合适的有机硅烷OS的实例为辛基三甲氧基硅烷、十二烷基三甲氧基硅烷、十六烷基三甲氧基硅烷、甲基辛基二甲氧基硅烷；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；3-甲基丙烯酰氧基丙基三烷氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷,3-甲基丙烯酰氧基丙基三甲氧基硅烷；3-氨基丙基三甲氧基硅烷,3-氨基丙基三乙氧基硅烷,3-氨基丙基二甲氧基甲基硅烷,3-氨基-2-甲基丙基三甲氧基硅烷,N-(2-氨基乙基)-3-氨基丙基三甲氧基硅烷,N-(2-氨基乙基)-3-氨基丙基三乙氧基硅烷,N-(2-氨基乙基)-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-氨基丁基二甲氧基甲基硅烷,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,4-氨基-3,3-二甲基丁基二甲氧基甲基硅烷,[3-(2-氨基乙基氨基)丙基]三甲氧基硅烷(＝4,7,10-三氮杂癸基三甲氧基硅烷),2-氨基乙基三甲氧基硅烷,2-氨基乙基二甲氧基甲基硅烷,氨基甲基三甲氧基硅烷,氨基甲基二甲氧基甲基硅烷,氨基甲基甲氧基二甲基硅烷,7-氨基-4-氧杂庚基二甲氧基甲基硅烷,N-(甲基)-3-氨基丙基三甲氧基硅烷,N-(n-丁基)-3-氨基丙基三甲氧基硅烷,双[3-(三甲氧基甲硅烷基)丙基]胺和双[3-(三乙氧基甲硅烷基)丙基]胺；3-巯基丙基三乙氧基硅烷,3-巯基丙基三甲氧基硅烷,3-巯基丙基甲基二甲氧基硅烷；3-酰基硫代丙基三甲氧基硅烷；乙烯基三甲氧基硅烷和乙烯基三乙氧基硅烷；双(3-三甲氧基甲硅烷基丙基)四硫烷,双(3-甲基二甲氧基甲硅烷基-丙基)四硫烷,双(3-三乙氧基甲硅烷基丙基)四硫烷,双(3-甲基二乙氧基甲硅烷基丙基)四硫烷,双(3-三甲氧基甲硅烷基丙基)二硫化物,双(3-甲基二甲氧基甲硅烷基丙基)二硫化物,双(3-三乙氧基甲硅烷基丙基)二硫化物和双(3-甲基二乙氧基甲硅烷基丙基)二硫化物；异氰尿酸酯基硅烷化合物例如1,3,5-N-三(3-三甲氧基甲硅烷基丙基)异氰尿酸酯基硅烷,1,3,5-N-三(3-甲基二甲氧基甲硅烷基丙基)异氰尿酸酯基硅烷,1,3,5-N-三(3-三乙氧基甲硅烷基丙基)异氰尿酸酯基硅烷,1,3,5-N-三(3-甲基二乙氧基甲硅烷基丙基)异氰尿酸酯基硅烷。
合适的还有其烷氧基已经被乙酰氧基代替的所提及的有机硅化合物，例如辛基三乙酰氧基硅烷(辛基-Si(O(O＝C)CH3)3)。这种有机硅化合物在水解时分解出乙酸。
同样合适的是这些列举的硅烷的部分水解产物，水解产物或缩合物，其也可以作为低聚有机硅氧烷商购获得。
合适的有机硅烷OS还有选自双[3-(三甲氧基甲硅烷基)丙基]胺,双[3-(三乙氧基甲硅烷基)丙基]胺,4,4,15,15-四乙氧基-3,16-二氧杂-8,9,10,11-四硫代-4,15-二硅杂十八烷(双(三乙氧基甲硅烷基丙基)多硫化物或双(三乙氧基甲硅烷基丙基)四硫烷)、双(三乙氧基甲硅烷基丙基)二硫化物的有机硅化合物。
此外适合作为有机硅烷OS的还有选自三[3-(三甲氧基甲硅烷基)丙基]胺,三[3-(三乙氧基甲硅烷基)丙基]胺,1,3,5-三[3-(三甲氧基甲硅烷基)丙基]-1,3,5-三嗪-2,4,6(1H,3H,5H)-三酮脲(＝三(3-(三甲氧基甲硅烷基)丙基)异氰尿酸酯)和1,3,5-三[3-(三乙氧基甲硅烷基)丙基]-1,3,5-三嗪-2,4,6(1H,3H,5H)-三酮脲(＝三(3-(三乙氧基甲硅烷基)丙基)异氰尿酸酯)的有机硅化合物。
优选作为有机硅烷OS的为氨基硅烷。特别优选的是3-氨基丙基三甲氧基硅烷、N-(2-氨基乙基)-3-氨基丙基三甲氧基硅烷、双[3-(三甲氧基甲硅烷基)丙基]胺、3-氨基丙基三乙氧基硅烷、N-(2-氨基乙基)-3-氨基丙基三乙氧基硅烷和双[3-(三乙氧基甲硅烷基)丙基]胺以及其彼此的混合物。
作为有机硅烷OS同样优选的是乙烯基硅烷，尤其是乙烯基三甲氧基硅烷和乙烯基三乙氧基硅烷。这些硅烷特别便宜并且仍然显示出良好的效果。
作为有机硅烷OS同样优选的是甲基丙烯酰基硅烷，尤其是3-甲基丙烯酰氧基丙基三甲氧基硅烷。
在优选的实施方案中，本发明的活化剂组合物包含0.5-10wt％的硅烷S。
当硅烷S用于本发明的活化剂组合物中时，可能有利的是使用干燥剂。其通过结合任何存在的水并且由此抑制容器中不希望的烷氧基硅烷的水解来增加组合物的储存稳定性。
合适的干燥剂包括例如反应性硅烷，例如四甲氧基硅烷、乙烯基三甲氧基硅烷，α-官能的硅烷如N-(甲硅烷基甲基)-O-甲基氨基甲酸酯,尤其是N-(甲基二乙氧基甲硅烷基甲基)-O-甲基氨基甲酸酯,(甲基丙烯酰氧基甲基)硅烷,乙氧基甲基硅烷,N-苯基-,N-环己基-和N-烷基硅烷,原甲酸酯，氧化钙或分子筛以及异氰酸酯。
活化剂组合物中干燥剂的量为0-3wt％，优选0.5-2wt％，基于整个组合物计。
本发明的活化剂组合物的特别优选的实施方案包含
a)0.5-25wt％、优选0.5-10wt％的催化剂K，
b)65-99.5wt％、优选85-99wt％的有机溶剂L，
c)0-10wt％、优选0.5-5wt％的硅烷S。
可以进一步有利的是，活化剂组合物进一步包含其它添加剂。例如，额外地可以使用至少一种有机成膜剂。这例如可以是环氧树脂或聚(甲基)丙烯酸酯。
该组合物还可以额外地包括其它成分。更特别地，这些是染料，颜料，表面活化剂，乳化剂，染料，UV标记物，荧光指示剂，杀生物剂，阻燃剂和稳定剂，以及活化剂领域中技术人员已知的其他添加剂。尤其有利的添加剂可以是UV标记物。这是在UV光下变得可见的物质。使用这种物质的优点在于，在施加非着色的活化剂化合物之后，可以检查精确地在何处施加了组合物和/或在何处施加了粘合剂。
在另一方面，本发明涉及如上所述的活化剂组合物用于促进双组分粘合剂，优选双组分聚氨酯粘合剂的粘附性建立的用途。
原则上，所使用的双组分粘合剂可以是在将两种组分混合后开始固化的任何双组分粘合剂。该选择尤其取决于开放时间和对所形成粘合体的机械要求。已经发现，本发明的活化剂组合物对于聚氨酯粘合剂具有尤其良好的适用性，尤其是对于含有至少一种具有异氰酸酯基团的聚氨酯预聚物的聚氨酯粘合剂。这种双组分聚氨酯粘合剂是广泛可商购获得的，尤其是在
Figure BDA0002425096640000121
名称下获自Sika Automotive GmbH(德国)。该活化剂组合物同样对于双组分硅烷封端的(硅烷官能的)粘合剂和双组分有机硅粘合剂具有特别良好的适用性。
在再一方面，本发明涉及一种组分的套件，其包含
a)如上所述的活化剂组合物，
b)如上所述的双组分粘合剂，优选双组分聚氨酯粘合剂。
在再一方面，本发明涉及在将基材S1与第二基材S2粘合时促进基材S1上的粘附性建立的方法，包含以下步骤：
i)将上述活化剂组合物施加到待粘合的基材S1和S2的至少一个上，优选基材S1和S2二者上；
ii)使所施加的活化剂组合物脱气；
iii)将双组分粘合剂或密封剂施加到第一基材S1上；
iv)使粘合剂或密封剂与第二基材S2接触；或
i)将如权利要求1-8任一项所述的活化剂组合物施加到第一基材S1和/或第二基材S2上；
ii)使所施加的活化剂组合物脱气；
iii)将双组分粘合剂或密封剂施加到第二基材S1上；
iv)使第二基材S2上存在的粘合剂与第一基材S1接触。
步骤ii)的脱气时间优选不超过30秒。该活化剂组合物可以通过布，例如纤维素纤维布施加。这导致特别薄的快速脱气的活化剂组合物层。另一方面，它也可以通过刷子、棉花棒、毛毡或海绵来施加。这会导致施加更多的量，因此在脱气后基材上的催化活性颗粒的浓度更高。本发明的活化剂化合物具有的优点是，基本上无论其施加量如何，活性效果都令人满意的高。
在刚刚描述的方法的优选实施方案中，基材S1和S2包括金属、涂漆表面或塑料。
在刚刚描述的方法的相同或另一优选的实施方案中，双组分粘合剂是聚氨酯粘合剂或基于硅烷官能聚合物的粘合剂或硅酮粘合剂。
在其它方面，本发明涉及一种制品，其制备通过刚刚描述的方法进行。
后者的制品尤其是一种运输工具，尤其是汽车、公共汽车、卡车、轨道车辆、轮船或飞机。
基材S1可以与基材S2相同或不同。合适的基材S1或S2例如为无机基材例如玻璃、玻璃陶瓷、混凝土、砂浆、砖、瓦、石膏和天然石材，例如花岗岩或大理石；金属或合金，例如铝、钢、有色金属、镀锌金属；有机基材，例如木材，塑料如PVC、聚碳酸酯、PMMA、聚酯、环氧树脂；涂覆的基材，例如粉末涂覆的金属或合金；以及色漆和清漆。作为基材S1或S2尤其优选的是玻璃、玻璃陶瓷、铝、电镀层(浸涂表面)和复合材料，例如碳纤维增强的塑料(CFK)、玻璃纤维增强塑料(GFK)和片状模塑复合材料(SMC)。
如果需要，可以在施加粘合剂之前对基材进行预处理。这种预处理尤其包括物理和/或化学清洁工艺，例如打磨、喷砂、刷涂等，或用清洁剂或溶剂处理。
实施例
根据表1的以下活化剂组合物通过将催化剂K添加到溶剂L中并且在氮气下良好搅拌而制备。在所有情况下，使用正庚烷作为溶剂并且添加基于整个得到的组合物计的1wt％的催化剂K。
Figure BDA0002425096640000131
Figure BDA0002425096640000141
表1:制备的活化剂组合物
将表1中的活性组合物放入密封的玻璃瓶中，并且在室温下储存1天后用于粘附性测试。作为基材使用通过阴极浸涂法涂覆的板(得自德国的Rocholl公司)。
增粘剂组合物的粘附性测试
借助于用组合物浸湿的纤维素布(
Figure BDA0002425096640000142
Tela-Kimberly Switzerland GmbH)或借助于棉花棒将化合物施加到基材上。在通过棉花棒施用时，将明显更多的活化剂施加到粘合表面上，使得活化剂溶液的流动可见。在施加增粘剂组合物之前立即借助于已经用异丙醇浸渍的纤维素布
Figure BDA0002425096640000143
擦拭而清洁所有基材基底并且在施加增粘剂组合物之前脱气至少2分钟。
在施加增粘剂组合物之后30秒，通过挤出料盒和喷嘴而施加双组分聚氨酯粘合剂
Figure BDA0002425096640000144
-7666L10BT，从而产生15x 45mm的粘合面积和1.6mm的层厚度。
Figure BDA0002425096640000145
-7666L10BT是可商购自Sika Automotive GmbH(德国)的高模量双组分聚氨酯粘合剂。
在1小时的固化时间之后，在气候控制室储存('1h')(23℃,50％相对空气湿度)之后和在气候控制室储存24小时('24h')之后测试粘合剂。
借助于拉伸剪切强度测试和断裂图样分析来测试粘合剂的粘附性。在本文中根据ISO 4587/DIN EN 1465，在Zwick/Roell Z010拉伸测试仪上确定在上述的相互粘合的阴极电沉积基材上的拉伸剪切强度(粘合面积：15x 45mm；层厚度：1.6mm；测量速度：10mm/min；温度：23℃)。本发明的所有活化剂给出了完全内聚的断裂图样。
经由在用活化剂预处理的基材上的断裂图样来评估粘附性。期望的是纯内聚失效。
所有制备的根据本发明的组合物显示了优异的储存稳定性。即使几个月后也没有观察到沉淀或浑浊。
Figure BDA0002425096640000151
表2:测试粘合体的拉伸剪切强度。
*粘合体的部分或完全的粘附失效
另外，还采用了红外(IR)固化进行测试。在此过程中，使用如上所述用于粘合的活化剂组合物涂覆测试片，将其夹紧在IR装置中并且从下方对其预热。在此期间，将粘合剂施加到相对侧。在限定的加热阶段后，将第二个涂覆的测试片夹入并因此接合。粘合剂和活化剂层的温度为105℃。之后，将粘合体在标准气候条件下储存24小时。所有活化剂A-1至A-10之中，仅A-4,A-5和A-6显示了完全内聚断裂图样和与所施加的活化剂的量无关的预期强度。

Claims (15)

1.活化剂组合物，其包含
a)0.5-50wt％的用于交联双组分粘合剂的催化剂K，其在23℃下为液体，
b)40-99.5wt％的有机溶剂L，
c)0-10wt％的至少一种硅烷S，其具有至少一种可水解的硅烷基团和优选至少一种选自巯基、环氧、氨基、甲基丙烯酰基、乙烯基和烷基的官能团，
其特征在于所述催化剂K包含金属的1,3-酮酰胺化物配合物，和特征在于溶剂L选自丙酮、甲基乙基酮、甲基正丙基酮、二异丁基酮、甲基异丁基酮、甲基正戊基酮、甲基异戊基酮、乙酰丙酮、异亚丙基丙酮、环己酮、甲基环己酮、乙酸乙酯、乙酸丙酯、乙酸异丙酯、乙酸丁酯、丙酸正丁酯、丙二酸二乙酯、乙酸1-甲氧基-2-丙酯、乙酸3-甲氧基正丁酯、乙基-3-乙氧基丙酸酯、二异丙醚、二乙醚、二丁醚、二乙二醇二乙醚、乙二醇二乙醚、乙二醇单丙醚、乙二醇单-2-乙基己醚、乙苯、甲苯、二甲苯、庚烷、辛烷、石脑油、石油溶剂油、石油醚、汽油、二氯甲烷、甲醇、乙醇、异丙醇和这些溶剂的混合物。
2.如权利要求1所述的活化剂组合物，其特征在于溶剂L选自正庚烷、乙醇、异丙醇、乙酸甲酯、乙酸乙酯、乙酸丁酯、乙酸异丙酯、乙酸1-甲氧基-2-丙酯、乙酸3-甲氧基正丁酯、丙酮、甲乙酮、甲基异丁酮、甲苯、乙苯及其混合物。
3.如权利要求2所述的活化剂组合物，其特征在于溶剂L选自正庚烷、乙醇、异丙醇、乙酸乙酯、甲乙酮及其混合物，其中溶剂L优选包含正庚烷和/或乙醇或由正庚烷和/或乙醇组成。
4.如权利要求1-3任一项所述的活化剂组合物，其特征在于催化剂K包含选自Fe、Bi、Al、Zn和Zr的金属的配合物。
5.如权利要求4所述的活化剂组合物，其特征在于催化剂K包含选自叔胺、胍和脒的有机化合物。
6.如前述权利要求任一项所述的活化剂组合物，其特征在于活化剂组合物不含锡化合物。
7.如前述权利要求任一项所述的活化剂组合物，其特征在于活化剂组合物包含0.5-10wt％的硅烷S。
8.如前述权利要求任一项所述的活化剂组合物，包含
a)0.5-25wt％，优选0.5-10wt％的催化剂K，
b)65-99.5wt％，优选85-99wt％的有机溶剂L，
c)0-10wt％，优选0.5-5wt％的硅烷S。
9.如权利要求1-8任一项所述的活化剂组合物用于促进双组分粘合剂，优选双组分聚氨酯粘合剂的粘附性建立的用途。
10.组分套件，包含
c)如权利要求1-8任一项所述的活化剂组合物，
d)双组分粘合剂，优选双组分聚氨酯粘合剂。
11.在将基材S1与第二基材S2粘合时促进基材S1上粘附性建立的方法，包含以下步骤：
i)将如权利要求1-8任一项所述的活化剂组合物施加到两个基材的至少一个上；
ii)使所施加的活化剂组合物脱气；
iii)在第一基材S1上施加双组分粘合剂或密封剂；
iv)使粘合剂或密封剂与第二基材S2接触；
或
i)将如权利要求1-8任一项所述的活化剂组合物施加到两个基材的至少一个上；
ii)使所施加的活化剂组合物脱气；
iii)在第二基材S2上施加双组分粘合剂或密封剂；
iv)使第二基材S2上存在的粘合剂与第一基材S1接触。
12.如权利要求11所述的方法，其特征在于基材S1和S2的至少一个包含金属、涂漆表面或塑料。
13.如权利要求11或12所述的方法，其特征在于双组分的粘合剂或密封剂为聚氨酯粘合剂或基于硅烷官能的聚合物的粘合剂。
14.通过如权利要求11-13任一项所述的方法制备的制品。
15.如权利要求14所述的制品，其特征在于该制品是运输工具，尤其是汽车、公共汽车、卡车、轨道车辆、轮船或飞机。
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