CN112375530A - 减少起泡且具有哑光效果的聚氨酯组合物 - Google Patents
减少起泡且具有哑光效果的聚氨酯组合物 Download PDFInfo
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- CN112375530A CN112375530A CN202011344347.XA CN202011344347A CN112375530A CN 112375530 A CN112375530 A CN 112375530A CN 202011344347 A CN202011344347 A CN 202011344347A CN 112375530 A CN112375530 A CN 112375530A
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- polyurethane
- polyether
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Classifications
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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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
本发明涉及聚氨酯组合物,包含基于组合物总重量计:A)20—50重量%的聚氨酯预聚物PU,其是聚醚多元醇与至少两种芳族多异氰酸酯的反应产物或反应产物的混合物,其中所述聚醚多元醇包括聚醚二元醇和聚醚三元醇且所述聚醚三元醇与聚醚二元醇的重量比在4:1到13:1的范围内;和B)基于组合物总重量计12.5%至17.5%的炭黑。此外,本发明还涉及炭黑在聚氨酯组合物中用于减少固化中起泡和增加哑光的用途。
Description
发明领域
本发明涉及聚氨酯粘结剂和密封剂领域,特别涉及一种具有在固化时减少起泡和具有良好哑光效果的低TVOC的聚氨酯耐候组合物,
发明背景
对于用于建筑和工业制造的涂料、粘合剂和密封剂而言,低的总挥发性物质的排放(即低TVOC)越来越成为严苛的要求。因此,在涂料、粘合剂和密封剂组合物中尽可能避免使用挥发性的有机溶剂成为趋势并且也能满足使用者对于环境友好的要求。
通过异氰酸酯基与羟基和/或水分反应而交联的可固化聚氨酯组合物在许多工业应用中被使用,例如在建筑和制造工业中用作粘合剂、密封剂或涂料。当在高空气湿度和/或提高的温度下使用这种组合物时,由于释放出的二氧化碳气体,因此其固化经常形成干扰性的气泡,其不会足够迅速地溶解或导出。为了避免起泡,可以将化学封闭的胺加到组合物中,即所谓的潜在固化剂,其在与水分接触时释放氨基并与异氰酸酯基快速交联而不会形成二氧化碳。作为潜在固化剂通常使用具有醛亚胺、酮亚胺或噁唑烷基团的化合物。然而,已知的潜在固化剂可能是不利的。例如,它们可引发过早的交联反应,并因此降低组合物的储存稳定性和/或将其的固化强烈加速从而导致开放时间太短并因此工作窗口太短。此外,许多已知的潜在固化剂在固化时会导致由易挥发的、强烈气味的醛或酮引起的麻烦的排放,所述醛或酮在潜在固化剂中作为封闭剂并通过水解释放出来。
此外,在一些特别的领域,还要求涂料、粘合剂或密封剂组合物具有哑光的效果,因为哑光的表面可以减少视觉干扰的机会,使得瑕疵与缺陷不像光泽表面那么明显。目前通常可以通过添加有哑光作用的填料如超细二氧化硅、滑石粉等填料使得光泽显著下降,从而增加哑光效果。填料的粒度对光泽有很大影响,粒度越大则光泽越低。但是,增加填料的用量,又会使产品的平整性和机械强度下降。
在CN105733491A中公开了一种低TVOC聚氨酯耐候密封胶。该聚氨酯密封胶中所包含的聚氨酯预聚物由聚醚多元醇和异氰酸酯反应得到。适用的异氰酸酯包括诸如甲苯二异氰酸酯、六亚甲基二异氰酸酯和二环己基甲烷二异氰酸酯等众多脂族或芳族的多异氰酸酯。特别的,在该文献中指出利用芳香族异氰酸酯制备的密封胶的耐候效果会比利用脂肪族异氰酸酯制备的密封胶差很多。该文献没有关注如何在固化时减少起泡,也没有提到哑光效果。
此外,在CN1507479A中提出了一种高耐候性的湿固化单组分聚氨酯组合物。在该组合物中,为了提供组合物足够的固化性并排除固化时的起泡问题,添加了诸如聚醛亚胺的封闭胺化合物添加剂。
发明概述
因此,本发明的一个目的是提供一种聚氨酯组合物,其在固化时能够减少起泡并且能够带来哑光的效果。此外,该组合物还能减少TVOC的排放,在保持和改善机械性能的同时具有优异的耐候性和可加工性。特别的,根据本发明的聚氨酯组合物可以在基本不包含封闭胺化合物如聚醛亚胺的情况下以简单的方式实现在固化时在高温和高湿下减少起泡。
已经令人惊讶地发现,该目的可以通过如权利要求1所述的一种聚氨酯组合物而实现。
根据本发明的聚氨酯组合物中,聚氨酯预聚物特别是通过使包含具有特定比例的聚醚二元醇和聚醚三元醇的聚醚多元醇组分与至少两种芳族多异氰酸酯反应而得到的反应产物或其混合物。包含这样的聚氨酯预聚物的组合物能够特别保证优异的耐候性。
同时,发明人还发现,在该组合物中使用一定量的炭黑还能进一步在固化时减少起泡并有助于提高耐候性和实现哑光效果,同时不损害产品的平整性和机械强度。令人惊讶的是,这尤其是在不使用封闭胺化合物类的潜固化剂的情况下实现的。
另外,在本发明的聚氨酯组合物中也可以不使用溶剂,从而降低总VOC含量。
本发明的其它方面为其它独立权利要求的主题。本发明的特别优选的实施方案为从属权利要求的主题。
发明详述
本发明的主题是一种聚氨酯组合物,包含基于组合物总重量计:
A)20—50重量%、优选25—40重量%的聚氨酯预聚物PU,其是聚醚多元醇与至少两种芳族多异氰酸酯的反应产物或反应产物的混合物,其中所述聚醚多元醇包括聚醚二元醇和聚醚三元醇且所述聚醚三元醇与聚醚二元醇的重量比在4:1到13:1的范围内;和
B)12.5%至17.5%,优选13%至16.5%的炭黑。
以“聚/多”为首的物质名称,如多元醇或多异氰酸酯,在本文中表示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。术语“聚合物”在本文中一方面包括通过聚合反应(聚加成、加聚、缩聚)制得的,在化学上一致但是在聚合度、分子量和链长方面不同的大分子的集合。所述术语另一方面也包括来自聚合反应的所述大分子集合的衍生物,即通过预定大分子上官能团的反应(例如加合或取代)而获得的并且化学上一致或化学上不一致的化合物。所述术语还包括所谓的预聚物,亦即其官能团参与大分子构建的反应性低聚预加合物。
异氰酸酯封端的聚合物是具有至少一个末端异氰酸酯基团,特别是两个末端的异氰酸酯基团的聚合物或预聚物。
术语“预聚物”在此通常是指用作生产具有更高分子量的聚合物的中间产物的低聚物或聚合物。
“分子量”在本文中被理解为分子的摩尔质量(以克/摩尔计)。“平均分子量”表示低聚或聚合形式的分子混合物的数均Mn,其通常通过凝胶渗透色谱法(GPC)相对于聚苯乙烯标样确定。“室温”在本文中表示23℃的温度。
术语“聚氨酯聚合物/预聚物”包括通过所谓的二异氰酸酯-加聚-方法制得的所有聚合物或预聚物。其也包括几乎或完全不含氨基甲酸酯基团的那些聚合物或预聚物。聚氨酯聚合物/预聚物的实例为聚醚-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化二亚胺。
根据本发明的聚氨酯预聚物PU是聚醚多元醇与至少两种芳族多异氰酸酯的反应产物或反应产物的混合物,其中所述聚醚多元醇包括聚醚二元醇和聚醚三元醇且所述聚醚三元醇与聚醚二元醇的重量比在4:1到13:1的范围内、优选5:1或5.1:1到12:1的范围。在本发明中,聚醚二元醇含量过高可能导致产品机械性能降低,而耐热性和耐紫外开裂性也均可能会受影响。聚醚三元醇含量过高,则可能导致韧性不足,耐粉化变差。
适合用于制备根据本发明的组合物的聚氨酯预聚物PU是通过所述聚醚多元醇与至少两种芳族多异氰酸酯(优选二异氰酸酯)的反应可获得的聚合物或聚合物混合物。这种反应可以这样进行:使多元醇和多异氰酸酯通过常见方法,例如在50℃至100℃的温度下,任选伴随使用合适的催化剂进行反应,其中多异氰酸酯这样计量加入,使得其异氰酸酯基团相比于多元醇的羟基以化学计量过量的量存在。
特别地,选择过量的芳族多异氰酸酯,使得基于整个聚合物计,在聚醚多元醇的所有羟基反应之后获得的聚氨酯聚合物中剩余0.1至5重量%,优选0.2至3重量%,特别优选0.3至2.5重量%的量的自由异氰酸酯基团。
任选地,聚氨酯预聚物PU可以在并用增塑剂情况下制得,其中所使用的增塑剂不包含对异氰酸酯有反应性的基团。
优选的是通过所有二异氰酸酯与所有聚醚二元醇以1.3:1至4:1、特别是1.5:1至3:1和特别优选1.7:1至2.5:1的NCO:OH-比例的反应获得的具有所述的自由异氰酸酯基团含量的聚氨酯预聚物。有利的,所述聚氨酯预聚物PU的残余的游离NCO含量为1.0至2.5重量%。
用于制备本发明的聚氨酯预聚物PU的聚醚多元醇包括聚醚二元醇和聚醚三元醇,特别优选由聚醚二元醇和聚醚三元醇组成。
特别适合作为聚醚多元醇(也被称为聚氧亚烷基多元醇或低聚醚醇)的是环氧乙烷、1,2-环氧丙烷、1,2-或2,3-环氧丁烷、氧杂环丁烷、四氢呋喃或其混合物的任选借助于具有两个或更多个活性氢原子的起始剂分子进行聚合得到的聚合产物,所述起始剂分子例如为水、氨或具有多个OH-或NH-基团的化合物,例如1,2-乙二醇、1,2-和1,3-丙二醇、新戊二醇、二乙二醇、三乙二醇、异构的二丙二醇和三丙二醇、异构的丁二醇、戊二醇、己二醇、庚二醇、辛二醇、壬二醇、癸二醇、十一烷二醇、1,3-和1,4-环己烷二甲醇、双酚A、氢化双酚A、1,1,1-三羟甲基乙烷、1,1,1-三羟甲基丙烷、甘油、苯胺,以及上述化合物的混合物。可以使用例如借助于所谓的双金属氰化物络合催化剂(DMC-催化剂)制备的具有低不饱和度(根据ASTM D-2849-69测量并且用毫当量不饱和度/克多元醇(mEq/g)表示)的聚氧亚烷基多元醇,也可以使用例如借助于阴离子型催化剂(例如NaOH、KOH、CsOH或碱金属醇化物)制备的具有较高不饱和度的聚氧亚烷基多元醇。
同样合适的是环氧乙烷-封端(“EO-封端”,ethylene oxide-endcapped)的聚氧亚丙基多元醇。后者特别为聚氧亚丙基聚氧亚乙基多元醇,其例如这样获得:在聚丙氧基化反应结束之后用环氧乙烷进一步烷氧基化纯的聚氧亚丙基多元醇,特别是聚氧亚丙基二元醇和三元醇,并因此使其具有伯羟基。在该情况下优选的是聚氧亚丙基聚氧亚乙基二元醇和聚氧亚丙基聚氧亚乙基三元醇。
在一个优选的实施方式中,所述聚醚二元醇和聚醚三元醇选自聚氧亚乙基二元醇或三元醇、聚氧亚丙基二元醇或三元醇、和聚氧亚丙基聚氧亚乙基二元醇或三元醇;特别是聚氧亚乙基二元醇、聚氧亚丙基二元醇、聚氧亚乙基三元醇和聚氧亚丙基三元醇。
所述多元醇优选具有250至30000g/mol,特别是1000至20000g/mol的平均分子量,和在1.6至3范围内的平均OH-官能度。特别的,所述聚醚二元醇的分子量在3000-5000g/mol的范围内,而所述聚醚三元醇的分子量在4000-6000g/mol的范围内。
在本发明的组合物中还可以任选包含少量如基于组合物总重量计低于2%或1.5%或1%的其他一些多元醇(例如1,2-乙二醇、1,2-和1,3-丙二醇、新戊二醇、二乙二醇、三乙二醇、异构的二丙二醇和三丙二醇、异构的丁二醇、戊二醇、己二醇、庚二醇、辛二醇、壬二醇、癸二醇、十一烷二醇、1,3-和1,4-环己烷二甲醇、氢化双酚A、二聚脂肪醇、1,1,1-三羟甲基乙烷、1,1,1-三羟甲基丙烷、甘油、季戊四醇、糖醇例如木糖醇、山梨醇或甘露醇、糖例如蔗糖、其它更高级的醇、所述二元醇和多元醇的低分子量的烷氧基化产物,聚酯多元醇,以及上述醇的混合物)与多异氰酸酯如上下文所述的多异氰酸酯反应得到的特别是具有末端异氰酸酯基团的聚氨酯预聚物。在本发明的一些有利的实施方式中,也可以仅使用如上所述的聚醚二元醇和三元醇作为与多异氰酸酯反应的多元醇组分,即可以仅包含如上下文所述的聚氨酯预聚物PU作为组合物中的聚氨酯预聚物。
在根据本发明的聚氨酯预聚物PU中,必须使用至少两种芳族多异氰酸酯。与现有技术中的一些教导不同,发明人发现,在根据本发明的聚氨酯组合物中采用至少两种芳族多异氰酸酯是关键的。在本发明范畴内,例如可以采用两种或更多种不同的芳族多异氰酸酯各自与相应的聚醚多元醇反应得到的预聚物或反应产物的混合物,或者也可以采用两种或更多种不同的芳族多异氰酸酯同时与相应的聚醚多元醇反应得到的反应产物。相比于芳族多异氰酸酯,现有技术中常用的脂肪族多异氰酸酯或其预聚物通常反应速度过慢,不能及时形成交联,易在后期老化过程中出现开裂的情况。另外,脂肪族多异氰酸酯或其预聚物还可能导致产品的TVOC含量升高。此外,从产品耐候性角度而言,发明人发现在本发明的聚氨酯预聚物PU中采用两种或更多种芳族多异氰酸酯相比于采用单一一种芳族多异氰酸酯有可能带来耐候性更好的产品。
适用的芳族多异氰酸酯优选是二异氰酸酯,优选选自间-和对-苯二甲基二异氰酸酯(间-和对-XDI)、间-和对-四甲基-1,3-亚二甲苯基二异氰酸酯、间-和对-四甲基-1,4-亚二甲苯基二异氰酸酯、双-(1-异氰酸基-1-甲基乙基)-萘、2,4-和2,6-甲苯二异氰酸酯(TDI)、4.4'-、2,4'-和2,2'-二苯甲烷二异氰酸酯(MDI)、1,3-和1,4-苯二异氰酸酯、2,3,5,6-四甲基-1,4-二异氰酸基苯、萘-1,5-二异氰酸酯(NDI)、3,3'-二甲基-4,4'-二异氰酸基联苯(TODI)及其混合物和低聚物;特别优选所述芳族多异氰酸酯选自4.4'-、2,4'-和2,2'-二苯甲烷二异氰酸酯(MDI)和2,4-和2,6-甲苯二异氰酸酯(TDI)的组合。
原则上,本发明的聚氨酯预聚物PU可以任何形式的反应产物制得。例如,聚氨酯预聚物PU可以是通过将聚醚三元醇、聚醚二元醇和两种芳族多异氰酸酯如MDI和TDI一起加入进行反应而制得的反应产物。其也可以通过首先将聚醚三元醇和/或二元醇与两种芳族多异氰酸酯之一分别反应,然后将形成的反应产物混合而得到。在一个特别优选的实施方式中,所述聚氨酯预聚物PU是如上所述的聚醚三元醇与MDI的反应产物和聚醚三元醇和聚醚二元醇与TDI的反应产物的混合物。
在根据本发明的聚氨酯组合物中,所述聚氨酯预聚物PU以20—50重量%、优选25—40重量%的量存在,基于组合物的总重量计。如果聚氨酯预聚物含量过低,则可能影响产品后期储存稳定性;而含量过高,则可能影响产品耐候性。
此外,在本发明的聚氨酯组合物中,特别地需要包含基于组合物总重量计12.5至17.5重量%,优选13至16.5重量%的炭黑。
适用于本发明的炭黑是工业上常用的产品,是一类疏松而极细的比表面积较大的黑色粉末。通常,炭黑是含碳物质如煤和天然气等在空气不足的条件下经不完全燃烧或受热分解而得的产物,能够以例如卡博特M570市购获得。
发明人发现,在根据本发明的组合物体系中加入如上所述的特定量的炭黑能够意外地实现固化时减少起泡,特别是在无需封闭胺化合物一类的潜固化剂存在的情况下。因此,有利的,根据本发明的组合物可以包含基于组合物总重计小于1重量%、优选小于0.5重量%、更优选小于0.1重量%和特别优选0重量%的封闭胺化合物类潜固化剂,如聚醛亚胺。所述的封闭胺化合物是基本上不与异氰酸酯基反应,而与水分形成伯氨基或仲氨基的封闭胺化合物。这种封闭胺化合物包括醛亚胺、酮亚胺、烯胺、噁唑烷和其他醛或酮与具至少一个伯氨基或仲氨基及还具一个活泼氢如伯氨基或仲氨基和羟基的化合物的缩合物。此外,还包括通过N-羟基噁唑烷与有机多异氰酸酯反应制备的在分子中具有两个或更多个噁唑烷基的化合物。同时,根据本发明的聚氨酯组合物包含特定量的炭黑还能有助于实现哑光效果,却不会损害产品的机械性能。但是,对于实现这些效果,如上所要求的炭黑含量是关键的。如果炭黑的含量过低可能导致产品鼓泡,而含量过高则可能影响施工性能,例如可能使得挤出力过高。
所述组合物优选包含其它对于聚氨酯粘合剂常见的成分,特别是除了炭黑之外的其他填料、增塑剂、流变添加剂、增粘剂、干燥剂或抵抗紫外线和氧化的稳定剂,以及其它常见掺加剂。
所述其他填料包含碳酸钙,二氧化钛,粘土,滑石粉,氧化锌,玻璃球,高岭土,硅微粉,云母粉,聚酰胺,PVC糊中的一种或两种以上的混合物。
在本发明的聚氨酯组合物中,可以有利地包含基于组合物总重量计总计10—70重量%、优选20-60重量%、更优选35—55重量%的包括炭黑在内的填料。
组合物特别可以包含至少一种增塑剂。适合作为增塑剂的特别是有机羧酸的酯,特别是邻苯二甲酸酯例如邻苯二甲酸二异壬酯或邻苯二甲酸二异癸酯,氢化邻苯二甲酸酯例如二异壬基-1,2-环己烷-二羧酸酯,己二酸酯例如己二酸二辛酯,壬二酸酯和癸二酸酯,或有机磷酸和磺酸的酯,或烃例如聚丁烯或聚异丁烯。优选作为增塑剂的是邻苯二甲酸酯、氢化邻苯二甲酸酯或己二酸酯。最优选的是邻苯二甲酸二异壬酯、邻苯二甲酸二异癸酯或二异壬基-1,2-环己烷-二羧酸酯。
基于整个组合物,组合物中的增塑剂的含量优选在5重量%至40重量%,特别是10重量%至30重量%,特别优选15重量%至25重量%的范围内。
适合作为增粘剂,特别是硅烷增粘剂的是有机基团上带有一个反应基团的有机烷氧基硅烷(“硅烷”),特别是环氧硅烷、巯基硅烷、(甲基)丙烯酰基硅烷、异氰酸基硅烷、酸酐基硅烷、S-(烷基羰基)-巯基硅烷、醛亚胺基硅烷或这些硅烷的低聚形式,或氨基硅烷或巯基硅烷与多异氰酸酯的加合物。优选的是3-缩水甘油氧丙基三甲氧基硅烷、β-(3,4-环氧环己基)乙基三甲氧基硅烷、3-巯基丙基三甲氧基硅烷或3-甲基丙烯酰氧丙基三甲氧基硅烷。最优选的是3-缩水甘油氧丙基三甲氧基硅烷,例如可以A-187商购获得的。
基于整个组合物计,组合物中的硅烷增粘剂的含量优选在0.01重量%至1.0重量%、特别是0.05重量%至0.5重量%的范围内。
根据本发明的组合物还可以包含至少一种胺催化剂。适合作为胺催化剂的是叔胺,特别是具有低pKa值,优选12和7之间的pKa值的那些。合适的胺催化剂为例如N-乙基-二异丙胺、N,N,N',N'-四甲基-亚烷基二胺、1,4-二氮杂双环[2.2.2]辛烷或三亚乙基二胺,以及优选的2,2'-二吗啉代二***(DMDEE)及其在吗啉环上具有取代基的衍生物。特别优选是DMDEE以及还有三亚乙基二胺。
基于整个组合物计,组合物中的胺催化剂的含量优选在0.05重量%至1.0重量%,特别是0.1重量%至0.8重量%,特别优选0.15重量%至0.6重量%的范围内。
所述组合物优选还可以包含至少一种金属催化剂。金属催化剂可以额外加入,或者已经存在于组合物的原料中,例如得自具有异氰酸酯基团的聚氨酯聚合物的合成。优选作为金属催化剂的是有机锡(IV)化合物、有机钛酸盐或有机锆酸盐。特别优选的是有机锡(IV)化合物。适合作为有机锡(IV)化合物的特别是二烷基氧化锡、二烷基二氯化锡、二烷基二羧酸锡和二烷基二酮酸锡,优选二丁基氧化锡、二丁基二氯化锡、二丁基二乙酸锡、二月桂酸二丁基锡(DBTDL)、二丁基二乙酰基丙酮酸锡、二辛基氧化锡、二辛基二氯化锡、二辛基二乙酸锡、二辛基二月桂酸锡或二辛基二乙酰基丙酮酸锡。
基于整个组合物,组合物中的金属催化剂的含量优选在0.001重量%至1.0重量%,特别是0.005重量%至0.1重量%的范围内。
基于整个组合物,组合物中可能使用的有机锡(IV)化合物的含量优选在0.001重量%至0.2重量%,特别是0.005重量%至0.1重量%的范围内。
基于整个组合物,组合物中的光稳定剂的含量优选在重量0.05%至5.0重量%,特别是0.05重量%至1.5重量%的范围内。所述组合物进一步包含选自不饱和丙烯酸化合物(优选聚酯丙烯酸酯)的光固化材料与位阻胺光稳定剂的组合。
发明人发现,在根据本发明的组合物中连同位阻胺光稳定剂一起使用一种或多种选自不饱和丙烯酸化合物的光固化材料对于改善耐候性是特别有利的。
光固化材料经光线照射很容易在非常短的时间内在其分子结构上发生化学变化,同时伴随物理变化,如固化。在此特别适用的是不饱和的丙烯酸类化合物,其包括具有一个或多个不饱和基团的丙烯酸和/或甲基丙烯酸单体、其低聚物和其混合物,特别优选的是聚酯丙烯酸酯类化合物,例如可以Aronix M8060商购获得的。
位阻胺光稳定剂包括UV吸收剂(其吸收如来自阳光光线和荧光灯的光能并转化成无害热能)、消灭由光能引发的活性中心的猝光剂。大多数这种位阻胺光稳定剂已经商品化,包括例如ADEKASTAB LA-52,LA-57,LA-62,LA-67,LA-63,LA-68,LA-77,LA-82和LA-87(由ASAHI DENKA KOGYO K.K.生产);癸二酸二(2,2,6,6-四甲基-4-哌啶基)酯、癸二酸二(1,2,2,6,6-五甲基-4-哌啶基)酯、癸二酸1-甲基-8-(1,2,2,6,6-五甲基-4-哌啶基)酯、1-[2-(3,5-二叔丁基-4-羟苯基)-丙酰氧基]乙基]-4-[3-(3,5-二叔丁基-4-羟苯基)丙酰氧基]-2,2,6,6-四甲基哌啶基丁二酸酯、二甲基-1-(2-羟乙基)-4-羟基-2,2,6,6-四甲基哌啶缩聚物、聚[[6-1-(1,1,3,3-四甲基丁基)亚胺基-1,3,5-三嗪-2,4-二基][2,2,6,6-四甲基-4-哌啶基]亚胺基]六亚甲基[(2,2,6,6-四甲基-4-哌啶基)亚胺基]]、丙二酸二(1,2,2,6,6-五甲基-4-哌啶基)2-(3,5-二叔丁基-4-羟苄基)-2-正丁基酯等,或其混合物。优选例如商业可得的Tinuvin 292,其是癸二酸二(1,2,2,6,6-五甲基-4-哌啶基)酯和癸二酸1-甲基-8-(1,2,2,6,6-五甲基-4-哌啶基)酯的混合物。
除了上述之外,根据本发明的组合物还可以包含其它对于聚氨酯粘合剂常见的成分。例如如下成分:
-交联剂,例如二异氰酸酯的低聚物或衍生物,例如MDI、TDI、HDI或IPDI,特别是异氰脲酸酯,碳化二亚胺,脲酮酰亚胺,缩二脲,脲基甲酸酯和亚氨基噁二嗪二酮,或MDI和MDI同系物(聚合MDI或PMDI)的混合物;
-干燥剂或脱水剂,例如对甲苯基异氰酸酯如对甲苯磺酰异氰酸酯和其它反应性异氰酸酯、氧化钙或分子筛;
-流变改性剂,例如增稠剂,例如WO 02/48228A2中第9至11页作为触变剂(“触变赋予剂”)描述的那些的改性聚脲、聚酰胺蜡、聚乙烯蜡,纤维性滑石粉,蓖麻油衍生物,膨润土或气相二氧化硅;
-抵抗热、光和紫外线的稳定剂;阻燃物质;
-表面活性物质,例如润湿剂、流动控制剂、脱气剂或消泡剂;
-杀生物剂,例如杀藻剂或杀真菌剂;
以及其它通常用在含异氰酸酯的单组份组合物中的物质,例如纤维,例如聚乙烯纤维;染料、颜料或其它本领域技术人员已知的掺加剂。
在一个有利的实施方案中,所述组合物中包含基于组合物总重计小于1重量%、优选小于0.5重量%、更优选小于0.1重量%的有机溶剂,特别是酮类、芳香烃、二甲基甲酰胺、四氢呋喃等有机溶剂。
本发明还包括上述组合物作为湿固化粘合剂或密封剂的用途。根据本发明的组合物特别适合应用在混凝土、砂浆、砖、瓦、石膏、天然石材例如花岗石或大理石、玻璃、玻璃陶瓷、丝网印刷陶瓷、金属或金属合金、木材、塑料和涂漆材料上。
根据本发明的组合物优选具有带有结构粘性性能的糊剂稠度。所述组合物可以借助于胶枪或者泵***来施涂,或者通过合适的胶嘴而挤出。
因此,本发明的另一方面涉及一种粘合或密封基材的方法,包括:
a)将根据如上所述的本发明组合物施加在第一基材上;
b)提供第二基材,该基材上任选地施加了根据如上所述的本发明组合物;
c)将第一和第二基材彼此接触;
其中所述第一基材和第二基材由相同或不同的材料制成。优选的,所述第一基材和第二基材相同或不同地选自玻璃、陶瓷、混凝土、砂浆、金属型材、木材或塑料。更优选的,将该组合物用于粘合或密封交通工具及其部件,优选汽车及其部件。
在施用之后,在水分的作用下,任选通过加热促进,根据本发明的组合物迅速固化,同时聚氨酯预聚物PU和任选包含的交联剂和/或潜在交联剂发生迅速交联。固化所需的水分可以源自空气(空气水分),其中组合物通过水分从外至内的扩散而固化。但也可以向组合物中添加含水组分,例如以含水糊剂的形式,所述含水糊剂例如通过静态混合器以均匀或不均匀方式与组合物混合。
根据本发明的组合物具有长的耐久性,即在长时间内储存稳定。“储存稳定的”或“可储存的”表示组合物可以在室温下在合适的容器中保存较长时间,通常至少3个月至6个月和更久,而其应用性能或使用性能(特别是粘度、从容器中施用时所需的推出力和交联速度)不会由于储存以与其使用相关的程度变化。这意味着,例如,相比于已经在23℃下储存7天的新鲜制备的组合物的推出力,在60℃(这造成加速老化)下储存14天之后根据下述方法在23℃下测得的本发明组合物的推出力优选增加至多3倍,特别优选至多2.5倍,特别是至多2倍。
最后,本发明还涉及由如上所述的组合物在用水(特别是空气水分的形式)固化之后获得的经固化组合物。
实施例
下文描述实施例,所述实施例更详细地解释本发明。本发明当然不限于所描述的实施例。
原料列表
测试方法
户外开裂性能:采用phenix显微镜放大20倍观察户外暴晒后的胶片是否有裂纹。
户外流黑水性能:肉眼观察户外暴晒后的胶条下方是否流有黑色印记。
TVOC:测试方法可参照汽车内饰中非金属材料挥发性有机物检测标准VDA277进行。
哑光性:将数克组合物以约2mm的层厚度施涂在卡板纸上,肉眼观察表面的光泽度。用“+”的多少表示哑光性的大小,而“-”则表示亮光,不具有哑光性。
发泡性:在两块透明玻璃板上分别施涂两条组合物,一条20mm宽20mm高,另一条10mm宽10mm高,然后分别放置于60℃的烘箱和40℃/80%的环境箱,10天后用刀切割胶条,看是否有鼓泡。
挤出力:将所述组合物装填在内涂漆的铝料筒(外直径46.9mm,内直径46.2mm,长度215mm,公制ISO螺纹M15×1.5mm)中并且用来自Novelis Deutschland GmbH的聚乙烯塞子(直径46.1mm)气密性封闭。在23℃下调温处理24小时之后,打开料筒并且通过推出设备挤出。为此,将具有3mm内直径开口的喷嘴旋拧在料筒螺纹上。使用挤出设备(Zwick/RoellZ005)确定为了以60mm/min的挤出速度挤出组合物所需的力。给出的值为在22mm、24mm、26mm和28mm的推出距离之后测得的力的平均值。在30mm的推出距离之后停止测量。
拉伸强度等机械性能值:根据DIN EN ISO 527(拉伸速度:200mm/min),分别在23℃(室温“RT”)和50%相对空气湿度下固化7天(d)后和在90℃下固化300h之后的层厚度为2mm的薄膜上确定拉伸强度和断裂伸长。
聚氨酯预聚物PU-1的制备
将Desmodur 44C放在70℃烘箱中2小时。将玻璃反应釜置于电加热套上面。在氮气保护下添加300g的330N和88g增塑剂DOA,升温至50℃。按NCO和OH的摩尔比2.1:1添加50g的Desmodur 44C。搅拌5分钟后,添加0.04g的Dabco33LV催化剂,继续升温至80度,开始计时,1小时后测量NCO含量,待测量值接近设定值,停止反应。
聚氨酯预聚物PU-2的制备
将玻璃反应釜置于电加热套上面。在氮气保护下添加39g的Desmodur T80、325g的JH-240、130g的GY-4000和增塑剂DOA,升温至50℃。搅拌5分钟后,添加0.04克Dabco33LV催化剂,继续升温至80度,开始计时,1小时后测量NCO含量,待测量值接近设定值,停止反应。
聚氨酯预聚物PU-3的组分的制备
将玻璃反应釜置于电加热套上面。在氮气保护下添加69g的Desmodur I、360g的JH-240、135g的GY-4000和增塑剂DOA,升温至50℃。搅拌5分钟后,添加0.06克DBTDL催化剂,继续升温至80度,开始计时,1小时后测量NCO含量,待测量值接近设定值,停止反应。
密封胶的制备:
向行星搅拌釜中加入各个聚氨酯预聚物、吸水稳定剂、偶联剂、光稳定剂,搅拌均匀后,加入填料和炭黑在真空状态下搅拌均匀,用干燥氮气解除真空,加入催化剂抽真空搅拌均匀后出料,灌装在密闭容器中以备用。各组合物的组成如下表1所示,其中%指重量百分比。
性能测试结果
针对所制备的组合物,依据如上所述的测试方法测试组合物的各个性能。所测得的性能列于下表2中。
表1.组合物的组成
表2.各组合物的性能测试
Claims (16)
1.聚氨酯组合物,包含基于组合物总重量计:
A)20—50重量%、优选25—40重量%的聚氨酯预聚物PU,其是聚醚多元醇与至少两种芳族多异氰酸酯的反应产物或反应产物的混合物,其中所述聚醚多元醇包括聚醚二元醇和聚醚三元醇且所述聚醚三元醇与聚醚二元醇的重量比在4:1到13:1的范围内;和
B)12.5%至17.5%,优选13%至16.5%的炭黑。
2.根据权利要求1的聚氨酯组合物,其特征在于,所述芳族多异氰酸酯是二异氰酸酯,优选选自间-和对-苯二甲基二异氰酸酯(间-和对-XDI)、间-和对-四甲基-1,3-亚二甲苯基二异氰酸酯、间-和对-四甲基-1,4-亚二甲苯基二异氰酸酯、双-(1-异氰酸基-1-甲基乙基)-萘、2,4-和2,6-甲苯二异氰酸酯(TDI)、4.4'-、2,4'-和2,2'-二苯甲烷二异氰酸酯(MDI)、1,3-和1,4-苯二异氰酸酯、2,3,5,6-四甲基-1,4-二异氰酸基苯、萘-1,5-二异氰酸酯(NDI)、3,3'-二甲基-4,4'-二异氰酸基联苯(TODI)及其混合物和低聚物;
特别优选所述芳族多异氰酸酯是4.4'-、2,4'-和2,2'-二苯甲烷二异氰酸酯(MDI)和2,4-和2,6-甲苯二异氰酸酯(TDI)。
3.根据前述权利要求任一项的聚氨酯组合物,其特征在于,所述聚醚二元醇和聚醚三元醇选自聚氧亚乙基二元醇或三元醇、聚氧亚丙基二元醇或三元醇、和聚氧亚丙基聚氧亚乙基二元醇或三元醇。
4.根据前述权利要求任一项的聚氨酯组合物,其特征在于,所述聚氨酯预聚物PU是聚醚三元醇和/或二元醇与两种芳族多异氰酸酯之一分别反应而形成的反应产物的混合物,优选是聚醚三元醇与MDI的反应产物和聚醚三元醇和聚醚二元醇与TDI的反应产物的混合物。
5.根据前述权利要求任一项的聚氨酯组合物,其特征在于,所述聚氨酯预聚物PU的残余的游离NCO含量为1.0至2.5重量%。
6.根据前述权利要求任一项的聚氨酯组合物,其特征在于,所述组合物包含总计10—70重量%、优选20-60重量%、更优选35—55重量%的包括炭黑在内的填料。
7.根据前述权利要求任一项的聚氨酯粘合剂组合物,其特征在于,所述组合物进一步包含选自不饱和丙烯酸化合物(优选聚酯丙烯酸酯)的光固化材料与位阻胺光稳定剂的组合。
8.根据前述权利要求任一项的聚氨酯粘合剂组合物,其特征在于,所述聚醚二元醇的分子量在3000-5000g/mol的范围内,而所述聚醚三元醇的分子量在4000-6000g/mol的范围内。
9.根据前述权利要求任一项的聚氨酯粘合剂组合物,其特征在于,所述组合物包含至少一种选自如下的其它成分:交联剂、增塑剂、溶剂、催化剂、增粘剂、干燥剂、其他稳定剂、颜料和流变助剂。
10.根据前述权利要求任一项的聚氨酯粘合剂组合物,其特征在于,所述组合物中包含基于组合物总重计小于1重量%、优选0重量%的聚醛亚胺。
11.由根据权利要求1至10任一项所述的组合物在固化之后获得的经固化组合物。
12.粘合或密封基材的方法,包括:
a)将根据权利要求1至10任一项所述的组合物施加在第一基材上;
b)提供第二基材,该基材上任选地施加了根据权利要求1至10任一项所述的组合物;
c)将第一和第二基材彼此接触;
其中所述第一基材和第二基材由相同或不同的材料制成。
13.根据权利要求12的方法,其特征在于,所述第一基材和第二基材相同或不同地选自玻璃、陶瓷、混凝土、砂浆、金属型材、木材和塑料。
14.根据权利要求12的方法,其特征在于,用于粘合或密封交通工具及其部件,优选汽车及其部件。
15.根据权利要求12至14任一项所述的方法得到的产品。
16.基于组合物总重量计12.5%至17.5%的炭黑在聚氨酯组合物中用于减少固化中起泡和增加哑光的用途,其中所述聚氨酯组合物如权利要求1-10任一项中所述。
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