CN109476805B - 聚氨酯泡沫形成组合物、使用这种组合物制备低密度泡沫的方法及由此形成的泡沫 - Google Patents
聚氨酯泡沫形成组合物、使用这种组合物制备低密度泡沫的方法及由此形成的泡沫 Download PDFInfo
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- CN109476805B CN109476805B CN201780044421.6A CN201780044421A CN109476805B CN 109476805 B CN109476805 B CN 109476805B CN 201780044421 A CN201780044421 A CN 201780044421A CN 109476805 B CN109476805 B CN 109476805B
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- isocyanate
- polyol
- foam
- reactive
- phthalic anhydride
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Abstract
本文公开了含有相稳定的异氰酸酯‑反应性组合物的聚氨酯泡沫形成组合物,所述异氰酸酯‑反应性组合物包括具有低臭氧消耗潜能或没有臭氧消耗潜能和低全球变暖潜能的卤代烯烃发泡剂。这种聚氨酯泡沫形成组合物适用于喷涂应用,以制备被认为具有良好耐火性能、低烟雾产生和由于放热减少而低焦烧或无焦烧的聚氨酯泡沫,从而使它们特别适合用作例如相对较厚的墙壁和/或屋顶隔热层。
Description
技术领域
本发明涉及含有相稳定的异氰酸酯-反应性组合物的聚氨酯泡沫形成组合物,所述异氰酸酯-反应性组合物包括具有低臭氧消耗潜能或没有臭氧消耗潜能和低全球变暖潜能的卤代烯烃发泡剂。这种聚氨酯泡沫形成组合物适用于喷涂应用,以制备被认为具有良好耐火性能、低烟雾产生和由于放热减少而低焦烧或无焦烧的聚氨酯泡沫,从而使它们特别适合用作例如相对较厚的墙壁和/或屋顶隔热层。
背景技术
喷涂聚氨酯泡沫(SPF)通常通过在水和物理发泡剂的存在下将异氰酸酯-反应性组分和多异氰酸酯结合而形成。芳族聚酯多元醇和/或蔗糖基聚醚多元醇通常用于多元醇组分中。通常选择这些多元醇用于SPF应用,如墙壁或屋顶隔热层应用,因为它们倾向于赋予泡沫耐火性能。
历史上,SPF中使用的物理发泡剂通常为氯氟烃(CFC)和氢氯氟烃(HCFC)。但是,CFC和HCFC因其臭氧消耗潜能和相对较高的全球变暖潜能而变得不受欢迎。因此,正在考虑可替代的物理发泡剂。
具有低臭氧消耗潜能或没有臭氧消耗潜能和低全球变暖潜能的一类可替代的物理发泡剂为包含至少一种卤素(如氟)和至少一个碳-碳双键的某些卤代烯烃,如氟烯烃。这些氟烯烃中的一些还包括氢和至少一个氯原子,因此有时称为氢氯氟烯烃或HFCO。
异氰酸酯-反应性组分的相稳定性对SPF特别重要,因为相不稳定性引起任何的沉淀物或沉积物可导致设备损坏。另外,相不稳定性会在喷涂应用过程中导致计量精度问题,这会影响所得聚氨酯喷涂体系的化学计量,导致反应性差和泡沫性能差。
因此,期望提供含有相稳定的异氰酸酯-反应性组合物的聚氨酯泡沫形成组合物,所述异氰酸酯-反应性组合物包括具有低臭氧消耗潜能或没有臭氧消耗潜能和低全球变暖潜能的卤代烯烃发泡剂,这种聚氨酯泡沫形成组合物适用于喷涂应用,以制备具有良好耐火性、低烟雾产生和由于放热减少而低焦烧或无焦烧的聚氨酯泡沫,从而使它们特别适合用作例如相对较厚的墙壁和/或屋顶隔热层。
鉴于前述要求,提出了本发明。
发明内容
在某些方面,本发明涉及包含多异氰酸酯和异氰酸酯-反应性组合物的聚氨酯泡沫形成组合物。这种泡沫形成组合物中的异氰酸酯-反应性组合物包含:(1)至少50重量%的芳族聚酯多元醇,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计;(2)水;和(3)C2至C6卤代烯烃,其中将异氰酸酯-反应性组合物在50℃下老化7天后,异氰酸酯-反应性组合物未显示出可见的混浊或凝胶。
在其他方面,本发明涉及包含多异氰酸酯和异氰酸酯-反应性组合物的聚氨酯泡沫形成组合物。这种泡沫形成组合物中的异氰酸酯-反应性组合物包含:(1)至少50重量%的邻苯二甲酸酐基聚酯多元醇,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计;(2)水;(3)C2至C6卤代烯烃。
此外,本发明还涉及通过这种泡沫形成组合物的喷涂应用来制备低密度聚氨酯泡沫的方法、通过这种方法形成的低密度聚氨酯泡沫,以及用这种泡沫隔热的器具和/或建筑物等。
具体实施方式
在本说明书中描述了各种实施方案,以提供对所公开的产品和方法的结构、功能、操作、制备和用途的全面理解。应理解,在本说明书中描述和说明的各种实施方案是非限制性的和非穷举性的。因此,本发明不受本说明书中公开的各种非限制性和非穷举性实施方案的描述的限制。相反,本发明仅由权利要求限定。与各种实施方案相关的说明和/或描述的特征和特性可与其他实施方案的特征和特性相组合。这些修改和变化均包括在本说明书的范围内。因此,可以修改权利要求书以引用本说明书中明确地或本身描述的任何特征或特性,或由本说明书明确地或本身支持的任何特征或特性。此外,申请人保留修改权利要求书的权利,以明确地放弃可能存在于现有技术中的特征或特性。因此,任何这种修改均符合美国专利法第112条第一款(35U.S.C.§112,first paragraph)和美国专利法第132(a)条(35U.S.C.§132(a))的要求。在本说明书中公开和描述的各种实施方案可以包括本文中各种描述的特征和特性,由或基本上由本文中各种描述的特征和特性组成。
除非另有说明,否则本文中指定的任何专利、出版物或其他公开材料通过引用整体并入本说明书中,但仅限于所并入的材料与现有定义、陈述或本说明书中明确阐述的其他公开材料不发生抵触的程度。因此,并且在必要的程度上,本说明书中阐述的明确公开内容替代本文通过引用并入的任何相抵触的材料。所述通过引用并入本说明书中但与现有定义、陈述或本文中阐述的其他公开材料相抵触的任何材料或材料的一部分,仅在所并入的材料和现有的公开材料之间不发生抵触的程度上被并入。申请人保留修改本说明书的权利,以明确地列举通过引用并入本文的任何主题或部分主题。
在本说明书通篇引用的“某些实施方案”等意指特定的特征或特性可包括在实施方案中。因此,在本说明书中使用的短语“在某些实施方案中”等不一定是指常见实施方案,还可以指不同的实施方案。此外,在一个或多个实施方案中,特定的特征或特性可以以任何合适的方式组合。因此,结合各种实施方式说明或描述的特定特征或特性可全部地或部分地与一个或多个其他实施方案的特征或特性进行结合,而没有限制。这些修改和变化包括在本说明书的范围内。以此方式,本说明书中描述的各种实施方案是非限制性和非穷举性的。
在本说明书中,除非另有说明,否则所有数值参数应理解为在所有情况下由术语“约”引出和修饰,其中数值参数具有用于测定参数数值的基础测量技术的固有偏差特性。至少,不试图将等同原则的应用限制在权利要求书的范围内,本说明书中描述的各数值参数应至少根据记录的有效数值并应用普通的四舍五入技术来理解。
此外,本说明书中列举的任何数值范围旨在包括所述范围内包含的所有子范围。例如,“1至10”的范围旨在包括所述最小值1和所述最大值10之间(并且包括端值)的所有子范围,即,其具有等于或大于1的最小值和等于或小于10的最大值。本说明书中所述的任何最大数值限度旨在包括其中包含的所有较低数值限度,并且本说明书中所述的任何最小数值限度旨在包括其中包含的所有较高数值限度。因此,申请人保留修改本说明书(包括权利要求书)的权利以明确地叙述包含在本文明确引用的范围内的任何子范围。所有这些范围旨在本身记载于本说明书中,使得对明确引用任何这样的子范围的修改均符合美国专利法第112条第一款(35U.S.C.§112,first paragraph)和美国专利法第132(a)条(35U.S.C.§132(a))的要求。
除非另有说明,否则本说明书中使用的语法冠词“一个/种(one)”、“一个/种(a)”、“一个/种(an)”和“该/所述(the)”旨在包括“至少一个/种”或“一个/种或多个/种”。因此,本说明书中使用的冠词是指冠词语法对象的一个/种或多于一个/种(即,“至少一个/种”)。例如但不限于,“一个/种(a)阻燃剂”意指一种或更多种阻燃剂,因此,可以考虑多于一种阻燃剂,并且可以在所描述的实施方案的实施中应用或使用。此外,单数名词的使用包括复数,并且复数名词的使用包括单数,除非在使用的上下文中另有要求。
如所指出的,本发明的某些实施方案涉及包含多异氰酸酯的聚氨酯泡沫形成组合物。本发明可使用任何已知的有机多异氰酸酯。合适的多异氰酸酯包括芳族、脂族和脂环族多异氰酸酯及其组合。这些类型的代表为二异氰酸酯,如间苯二异氰酸酯、对苯二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、1,6-六亚甲基二异氰酸酯、1,4-六亚甲基二异氰酸酯、1,4-环己烷二异氰酸酯、五亚甲基1,5-二异氰酸酯、六氢甲苯二异氰酸酯的异构体、1,5-亚萘基二异氰酸酯、1-甲基苯基-2,4-苯基二异氰酸酯、4,4'-二苯基甲烷二异氰酸酯、2,4'-二苯基甲烷二异氰酸酯、4,4'-亚联苯基二异氰酸酯、3,3'-二甲氧基-4,4'-亚联苯基二异氰酸酯和3,3'-二甲基二苯基丙烷-4,4'-二异氰酸酯;三异氰酸酯,如2,4,6-甲苯三异氰酸酯;以及多异氰酸酯,如4,4'-二甲基二苯基甲烷-2,2',5,5'-四异氰酸酯和多亚甲基多苯基异氰酸酯。
可使用粗多异氰酸酯,如通过甲苯二胺的混合物的光气化获得的粗甲苯二异氰酸酯。类似地,可使用未蒸馏的多异氰酸酯,如亚甲基桥连的多苯基多异氰酸酯,其可通过芳族胺(如苯胺)与甲醛缩合得到的多苯基多亚甲基多胺的光气化反应而获得。
合适的改性多异氰酸酯可通过多异氰酸酯的化学反应获得,并且可包括但不限于,含有酯基、脲基、缩二脲基、脲基甲酸酯基、碳二亚胺基、异氰脲酸酯基、脲二酮基和/或氨基甲酸酯基的异氰酸酯。
在某些实施方案中,多异氰酸酯包含亚甲基桥连的多苯基多异氰酸酯和/或亚甲基桥连的多苯基多异氰酸酯的预聚物,其中亚甲基桥连的多苯基多异氰酸酯的预聚物的平均官能度为每分子2.0至3.5,如2.1至3.1个异氰酸酯基团,并且游离NCO含量为15至35重量%,如20至35重量%、25至35重量%,或在一些情况下为28至34重量%。在某些实施方案中,这种亚甲基桥连的多苯基多异氰酸酯和/或亚甲基桥连的多苯基多异氰酸酯的预聚物的存在量为至少50重量%,如至少80重量%、至少90重量%或至少99重量%,基于多异氰酸酯的总重量计。
本发明的聚氨酯泡沫形成组合物还包含异氰酸酯-反应性组合物。如本文所用,术语“异氰酸酯-反应性组合物”是指包含特别是具有与异氰酸酯基团反应的官能团的组分的组合物,即下文所定义的异氰酸酯-反应性组分。其中,所述异氰酸酯-反应性组合物包含至少50重量%的芳族聚酯多元醇,基于异氰酸酯-反应性组合物的总重量计。此外,在一些情况下,异氰酸酯-反应性组合物在50℃下老化7天后,未显示出可见的混浊或凝胶。
在某些实施方案中,所述异氰酸酯-反应性组合物包含至少50重量%的邻苯二甲酸酐基聚酯多元醇,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计。如本文所用,术语“邻苯二甲酸酐基聚酯多元醇”是指多元醇与二羧酸和/或其酸酐(包含邻苯二甲酸酐)的缩聚反应产物,在一些情况下,其中二羧酸和/或其酸酐基本上由邻苯二甲酸酐组成,或在其他情况下由邻苯二甲酸酐组成。如本文所用,邻苯二甲酸酐是指以下结构的化合物:
如本文所用,当在前述段落的上下文中使用时,术语“基本上由……组成”意指在缩聚反应中使用的除邻苯二甲酸酐之外的任何二羧酸和/或其酸酐以不足以极大地影响异氰酸酯-反应性组合物的相稳定性的量使用。因此,如果存在任何这样的其他二羧酸和/或其酸酐,则它们的存在量不足以将异氰酸酯-反应性组合物在50℃下在异氰酸酯-反应性组合物老化7天后显示出可见的混浊和/或凝胶。
出于本发明的目的,邻苯二甲酸酐基聚酯多元醇区别于其他芳族聚酯多元醇,如对苯二甲酸酯基聚酯多元醇。因此,在某些实施方案中,在前述缩聚反应中使用的二羧酸和/或其酸酐基本上不含或在一些情况下完全不含对苯二甲酸酯,如聚对苯二甲酸乙二醇酯和/或对苯二甲酸二甲酯。此外,在本发明的某些实施方案中,异氰酸酯-反应性组合物基本上不含,或在一些情况下完全不含非邻苯二甲酸酐基聚酯多元醇的芳族聚酯多元醇。如本文所用,当参照基本上不含非邻苯二甲酸酐基芳族聚酯多元醇时,使用“基本上不含”意指这种芳族聚酯多元醇的存在量不超过10重量%,如不超过2重量%,或在一些情况下不超过1重量%,基于存在的芳族聚酯多元醇的总重量计。
适于在前述缩聚反应中与邻苯二甲酸酐反应的多元醇包括但不限于,分子量为62g/mol至400g/mol的二官能多元醇和更高官能多元醇。这些多元醇的具体实例包括但不限于,1,4-二羟基环己烷、1,2-丙二醇、1,3-丙二醇、2-甲基-1,3-丙二醇、1,5-戊二醇、1,6-己二醇、1,8-辛二醇、新戊二醇、乙二醇、二乙二醇、三乙二醇、四乙二醇、二丙二醇、三丙二醇、二丁二醇、三丙二醇、丙三醇、季戊四醇和/或三羟甲基丙烷,包括两种或更多种任意前述物质的混合物。
如果需要,缩聚反应可在合适的催化剂存在下进行,并且如果需要,可以在减压和升高的温度下进行,同时通过蒸馏除去形成的水或低分子量醇。缩聚反应也可通过共沸方法在作为共沸剂的有机溶剂的存在下进行或通过载气法进行。在某些实施方案中,缩聚反应期间的反应温度为150℃至250℃,如180℃至230℃。
在某些实施方案中,邻苯二甲酸酐基聚酯多元醇的酸值小于5mg KOH/克多元醇,如小于4mg KOH/克多元醇。
在某些实施方案中,邻苯二甲酸酐基聚酯多元醇的羟值为至少290mg KOH/克多元醇,如290至500mg KOH/克多元醇、290至400mg KOH/克多元醇或290至360mg KOH/克多元醇。在某些实施方案中,异氰酸酯-反应性组合物可包含两种或更多种邻苯二甲酸酐基聚酯多元醇,其中邻苯二甲酸酐基聚酯多元醇的加权平均羟值为290至350mg KOH/克多元醇,如290至320mg KOH/克多元醇或300至320mg KOH/克多元醇。出于本发明的目的,羟值可通过酯化实验测定,然后根据DIN 53240-2用标准氢氧化钾醇溶液反滴定过量的酯化试剂。
在某些实施方案中,邻苯二甲酸酐基聚酯多元醇的OH官能度为2至6,如2至3,或在一些情况下为2.1至2.4。本文提及的OH官能度为多元醇的理论平均标称官能度,即基于用于制备多元醇的每分子OH官能反应物的羟基平均数计算的官能度。
可以理解,本发明中使用的多元醇的数均分子量(Mn)可根据以下等式由多元醇的OH官能度和羟值计算:
其中f为OH官能度,且OH#为羟值。在某些实施方案中,邻苯二甲酸酐聚酯多元醇的Mn为200至1000克/摩尔,如300至500克/摩尔或350至450克/摩尔。
在本发明的某些实施方案中,邻苯二甲酸酐基聚酯多元醇包含两种或更多种邻苯二甲酸酐基聚酯多元醇的混合物。例如,在一些实施方案中,邻苯二甲酸酐基聚酯多元醇包含(i)第一邻苯二甲酸酐基聚酯多元醇,其羟值为290至310mg KOH/克多元醇,且OH官能度为2.0至2.2,如2.1,和(ii)第二邻苯二甲酸酐基聚酯多元醇,其羟值为340至360mg KOH/克多元醇,且OH官能度为2.3至2.5,如2.4。在这些实施方案的某些中,第一邻苯二甲酸酐基聚酯多元醇(i)的存在量为50重量%至99重量%,如70重量%至90重量%,或在一些情况下为75重量%至85重量%,基于(i)和(ii)的总重量计。在这些实施方案中,第二邻苯二甲酸酐基聚酯多元醇(ii)的存在量为1重量%至50重量%,如10重量%至30重量%,或在一些情况下为15重量%至25重量%,基于(i)和(ii)的总重量计。
在某些实施方案中,前述邻苯二甲酸酐基聚酯多元醇的存在量为至少50重量%,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计。如本文所用,“异氰酸酯-反应性组分”意指含有与异氰酸酯基反应的官能团的任何化合物,所述官能团的实例包括氨基、硫醇基、羧基和羟基。在某些实施方案中,邻苯二甲酸酐基聚酯多元醇的存在量为至少60重量%、至少70重量%,或在一些情况下为至少80重量%,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计。此外,在某些实施方案中,邻苯二甲酸酐基聚酯多元醇的存在量使得邻苯二甲酸酐基聚酯多元醇提供异氰酸酯-反应性组合物中存在的所有异氰酸酯-反应性基团的至少50%,如至少60%,或在一些情况下至少70%,基于组合物中存在的异氰酸酯-反应性基团(如-OH基团)的总摩尔数计。此外,在某些实施方案中,邻苯二甲酸酐基聚酯多元醇的存在量为至少15重量%,如至少20重量%,如20至40重量%或25至35重量%,基于聚氨酯泡沫形成组合物的总重量计。
出乎意料地发现,与不包括这种占主导优势的邻苯二甲酸酐基聚酯多元醇的异氰酸酯-反应性组合物(如主要使用其他类型的芳族聚酯多元醇,如对苯二甲酸酯基聚酯多元醇的那些)相比,使用这种邻苯二甲酸酐基聚酯多元醇作为异氰酸酯-反应性组合物中异氰酸酯-反应性组分的主要来源——即,以前述段落中所述的量,对于本文公开的包括卤代烯烃发泡剂的异氰酸酯-反应性组合物的相稳定性具有相当大的优势。因此,本发明的某些实施方案涉及包含相稳定的异氰酸酯-反应性组合物的聚氨酯泡沫形成组合物,如本文所用,其意指将异氰酸酯-反应性组合物在50℃下老化7天后,异氰酸酯-反应性组合物未显示出可见的混浊和/或凝胶。
相稳定性的这一优势使得将具有使用低臭氧消耗潜能或没有臭氧消耗潜能和低全球变暖潜能的卤代烯烃发泡剂优点的异氰酸酯-反应性组合物有效用于SPF应用被认为是可行的。此外,所得到的聚氨酯泡沫被认为具有良好的耐火性能、低烟雾产生、由于放热减少而低焦烧或无焦烧,从而使它们特别适合用作例如相对较厚的建筑的隔热材料,而不会引起喷涂应用过程中的设备损坏和计量精度问题方面的显著困难。
本发明的聚氨酯泡沫形成组合物的异氰酸酯-反应性组合物还可包含其他异氰酸酯-反应性组分。例如,在某些实施方案中,异氰酸酯-反应性组合物包含蔗糖基多元醇。
如本文所用,“蔗糖”是指含有D-果糖基和D-葡糖基的结晶二糖,其具有以下结构:
在一些情况下,在本发明的聚氨酯泡沫形成组合物的某些实施方案中使用的蔗糖基多元醇为,例如通过在碱性催化剂(如氢氧化钠和/或氢氧化钾)的存在下,使蔗糖和任选地一种或更多种其他多元醇引发剂(如丙二醇(含或不含水))与环氧烷烃(如环氧乙烷和/或环氧丙烷和/或环氧丁烷)反应而制备的聚醚多元醇。当然,该产物可用酸(如羟基羧酸)处理,以中和碱性催化剂。制备这种蔗糖基多元醇的合适方法记载在美国专利号4,430,490第2栏第25行至第3栏第7行,其引用部分通过引用并入本文中。
在某些实施方案中,蔗糖基多元醇的羟值为400至1000mg KOH/克多元醇,如400至800mg KOH/克多元醇、400至600mg KOH/克多元醇,或在一些情况下为400至500mg KOH/克多元醇或450至500mg KOH/克多元醇。在某些实施方案中,蔗糖基多元醇的OH官能度为至少5.0,例如5.0至7.7、5.0至7.0、5.0至6.0,或在一些情况下为5.0至5.5或5.0至5.4。在某些实施方案中,蔗糖基多元醇的Mn为200至1100克/摩尔,如350至1080克/摩尔、470至840克/摩尔、560至770克/摩尔,或在某些情况下为560至660克/摩尔。
在某些实施方案中,前述蔗糖基多元醇的存在量为1至20重量%,如1至10重量%,或在一些情况下为5至10重量%,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计。在某些实施方案中,前述蔗糖基多元醇的存在量使得蔗糖基多元醇提供1至20%,例如5至15%,或在一些情况下8至12%的在异氰酸酯-反应性组合物中存在的所有异氰酸酯-反应性基团,基于组合物中存在的异氰酸酯-反应性基团(如-OH基团)的总摩尔数计。此外,在某些实施方案中,蔗糖基多元醇的存在量为至少1重量%,如至少2重量%,如1至10重量%或2至5重量%,基于聚氨酯泡沫形成组合物的总重量计。
曼尼希多元醇也适于包含在聚氨酯泡沫形成组合物中。可以理解,曼尼希多元醇为曼尼希碱进行烷氧基化而获得的芳族多元醇,所述曼尼希碱是通过苯酚、甲醛和烷醇胺与环氧烷烃(如环氧乙烷和/或环氧丙烷)之间的曼尼希反应得到的。在某些实施方案中,这种曼尼希多元醇的OH官能度为至少3.0。本发明可以使用的常用曼尼希多元醇包括用苯酚或壬基苯酚或其他合适的苯酚衍生物引发的那些。
在本发明的一些实施方案中,曼尼希多元醇的存在量为至多20重量%,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计。在这些实施方案的一些中,曼尼希多元醇(如果存在)的存在量小于10重量%、小于5重量%,或在一些情况下小于2重量%,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计。
如果需要,异氰酸酯-反应性组合物可包含其他聚醚多元醇,例如胺引发的聚醚多元醇。但是,在一些实施方案中,异氰酸酯-反应性组合物基本上不含或在一些情况下完全不含胺引发的聚醚多元醇。如本文所用,当参照异氰酸酯-反应性组合物中不存在胺引发的聚醚多元醇使用时,“基本上不含”意指胺引发的聚醚多元醇(如果有的话)的存在量小于10重量%,如不超过5重量%、不超过2重量%,或在一些情况下不超过1重量%,基于异氰酸酯-反应性组合物的总重量计。
在某些实施方案中,聚氨酯泡沫形成组合物的异氰酸酯-反应性组合物包含具有至少两个异氰酸酯-反应性氢原子且分子量为32至399的化合物、通常为单体化合物,其可起例如扩链剂的作用。这些化合物通常含有2至8个,如2至4个异氰酸酯-反应性氢原子。其具体实例包括但不限于,乙醇胺、二乙醇胺、三乙醇胺、山梨糖醇和/或丙三醇。
在某些实施方案中,前述扩链剂的存在量为1至20重量%,如1至10重量%,或在一些情况下为5至10重量%,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计。在某些实施方案中,前述扩链剂的存在量使得扩链剂提供1至30%,如10至30%,或在一些情况下10至20%的在异氰酸酯-反应性组合物中存在的所有异氰酸酯-反应性基团,基于组合物中存在的异氰酸酯-反应性基团(如-OH基团)的总摩尔数计。此外,在某些实施方案中,扩链剂的存在量为至少1重量%,如至少2重量%,如1至10重量%或1至5重量%,基于聚氨酯泡沫形成组合物的总重量计。
在本发明的某些实施方案中,异氰酸酯-反应性组合物还包含水,其起发泡剂的作用。在这些实施方案的某些中,水的存在量为0.75至10重量%,如1至6重量%,或在一些情况下为2至4重量%,基于异氰酸酯-反应性组合物的总重量计。
本发明的关键特征为在异氰酸酯-反应性组合物中存在C2-C6卤代烯烃,其也起发泡剂的作用。如本文所用,术语“C2-C6卤代烯烃”是指具有2至6个碳原子、至少一个卤原子和至少一个碳-碳双键的化合物。在某些实施方案中,在1大气压下,C2-C6卤代烯烃的沸点为至少10℃,如10℃至40℃或14℃至40℃。
在某些实施方案中,C2-C6卤代烯烃还包含至少一个氢原子,并且因此称为氢卤代烯烃。在这些实施方案的某些中,卤素包括氟,并且在这些情况下,C2-C6卤代烯烃为氢氟烯烃或HFO。在这些实施方案的某些中,卤素还包括氯,并且在这些情况下,C2-C6卤代烯烃为氢氟氯烯烃或HFCO。
在某些实施方案中,C2-C6卤代烯烃为具有以下结构的化合物:
其中各R1可相同或不同,其为氯、氟、溴、碘或氢,R2为(CR1 2)nX,X为CR1F2,且n为0、1、2或3。
在某些实施方案中,C2-C6卤代烯烃包含C3-C4卤代烯烃,如上述结构的化合物,其中n为0,至少一个R1为H,至少一个其他R1为氯,且X为CF3。三氟一氯丙烯为这些化合物的实例。合适的三氟一氯丙烯包括,例如1,1,1-三氟-2-氯-丙烯(HFCO-1233xf)以及顺式-1,1,1-三氟-3-氯丙烯和反式-1,1,1-三氟-3-氯丙烯(HFCO-1233zd)。本文中,术语HFCO-1233zd包括顺式-1,1,1-三氟-3-氯丙烯和反式-1,1,1-三氟-3-氯丙烯,包括其各种混合物。本文中使用的术语“顺式HFCO-1233zd”和“反式HFCO-1233zd”分别描述1,1,1-三氟-3-氯丙烯的顺式形式和反式形式。在某些实施方案中,主要使用(至少90重量%,基于HFCO-1233zd的总重量计)或仅使用反式HFCO-1233zd。另一种合适的C2-C6卤代烯烃为HFO-1336mzz(Z),其也称为顺式-1,1,1,4,4,4-六氟丁-2-烯。
在某些实施方案中,C2-C6卤代烯烃的存在量为1至20重量%,如2至15重量%、5至15重量%,或在一些情况下为5至10重量%,基于异氰酸酯-反应性组合物的总重量计。
应理解,如果需要,可使用其他发泡剂,如二氧化碳、烃(如正戊烷、环戊烷和异戊烷)和/或多氟烷烃。
在某些实施方案中,异氰酸酯-反应性组合物中使用的发泡剂的量使得所得泡沫的密度不超过160kg/m3,如不超过80kg/m3、不超过60kg/m3,或在某些情况下不超过50kg/m3,或在某些情况下不超过22.4kg/m3,根据ASTM D1622-14测定。在一些情况下,这些泡沫的密度为至少5kg/m3,如至少6.4kg/m3,如至少8kg/m3,或在一些情况下为至少10kg/m3。在某些实施方案中,所述泡沫为低密度泡沫。如本文所用,“低密度泡沫”意指密度为6.4kg/m3至50kg/m3的泡沫,所述密度根据ASTM D1622-14测定。
其他成分可包括在用于本发明的聚氨酯泡沫形成组合物的异氰酸酯-反应性组合物中。在某些实施方案中,异氰酸酯-反应性组合物包含阻燃剂。合适的阻燃剂包括但不限于,溴化阻燃剂,如溴化多元醇和(ii)膦酸化阻燃剂,如卤代(如氯代)磷酸酯,包括它们的混合物。
在某些实施方案中,溴化阻燃剂包含以下通式的溴化聚醚多元醇:
其中n为0到7的数,m为2到3的数;X为饱和或不饱和的溴化多元醇残基;并且R为氢或具有1-5个碳原子的烷基。其他合适的溴化阻燃剂包括但不限于,3,4,5,6-四溴邻苯二甲酸、三溴新戊醇、1,3-丙二醇、2,2-双(溴甲基)和五溴苯醚等,其中包括其两种或更多种的混合物。合适的商购可得的溴化阻燃剂还包括可从ICL Industrial Products以(6000系列)溴化阻燃剂获得的那些和从Albermarle Corporation商购可得的四溴邻苯二甲酸酐的含溴二酯/醚二醇。可以使用两种或更多种这些溴化阻燃剂的混合物。在某些实施方案中,溴化阻燃剂不是膦酸化的,而在其他实施方案(如其中阻燃剂包含四溴邻苯二甲酸酐的含溴二酯/醚二醇的那些)中,阻燃剂也可包含磷酸酯。
合适的膦酸酯(如卤代磷酸酯)的具体实例包括但不限于,三-(2-氯乙基)磷酸酯、三-(2-氯异丙基)磷酸酯(TCPP)、三(1,3-二氯异丙基)磷酸酯、三-(2,3-二溴丙基)磷酸酯和四-(2-氯乙基)乙烯二磷酸酯、双-(2-羟乙基)-氨基甲基膦酸二乙酯、三-(1-氯-2-丙基)磷酸酯、磷酸、三乙基酯、具有环氧乙烷和氧化磷(P2O5)的聚合物、磷酸三乙酯,包括其两种或更多种的混合物。
在某些实施方案中,在含阻燃剂的聚醚多元醇组合物中使用的溴化阻燃剂和膦酸化阻燃剂的相对重量比为1:5至5:1,如1:4至4:1或1:2至2:1,如1:1.5至1.5:1,或在某些情况下为1.2:1至1:1.2或1.1:1至1:1.1。在某些实施方案中,异氰酸酯-反应性组合物中阻燃剂的总量为2至20重量%,如5至15重量%,基于异氰酸酯-反应性组合物的总重量计。
此外,在一些实施方案中,异氰酸酯-反应性组合物还包含表面活性剂,以例如稳定发泡反应混合物直至其获得刚性。这些表面活性剂通常包括液体或固体有机硅化合物;长链醇的聚乙二醇醚;叔胺;长链烷基酸硫酸酯、烷基磺酸酯或烷基芳基磺酸的烷醇胺盐;或其混合物。通常,每100份异氰酸酯-反应性组合物使用0.5至10重量份表面活性剂。
在异氰酸酯-反应性组合物中还通常使用一种或更多种氨基甲酸酯催化剂。可使用任何合适的氨基甲酸酯催化剂,包括已知的叔胺化合物和有机金属化合物。合适的叔胺催化剂的实例包括但不限于,三亚乙基二胺、N-甲基吗啉、五甲基二亚乙基三胺、二甲基环己胺、四甲基乙二胺、1-甲基-4-二甲基氨基乙基-哌嗪、3-甲氧基-N-二甲基-丙胺、N-乙基吗啉、二乙基乙醇胺、N-椰油基吗啉、N,N-二甲基-N',N'-二甲基异丙基-丙二胺、N,N-二乙基-3-二乙基氨基丙胺和二甲基-苄胺。合适的有机金属催化剂的实例包括但不限于,有机汞、有机铅、有机铋、有机锌、有机铁和有机锡催化剂。合适的有机锡催化剂包括但不限于,羧酸的锡盐,如二-2-乙基己酸二丁基锡和二月桂酸二丁基锡。金属盐如氯化亚锡也可用作氨基甲酸酯反应的催化剂。在本文中,也可任选地使用多异氰酸酯三聚的催化剂,如碱金属醇盐或羧酸盐,或某些叔胺。这些催化剂以可显著提高多异氰酸酯的反应速率的量使用。通常的用量为每100重量份多元醇0.1至10.0份催化剂。这些催化剂的实例包括羧酸的钾盐如辛酸钾,和叔胺N,N',N”-三(3-二甲基-氨基丙基)六氢-s-三嗪。
如果需要,其他合适的成分包括反应阻滞剂、泡孔调节剂、乳化剂、泡沫稳定剂、着色剂(如颜料和染料)和填料(例如但不限于硫酸钡和碳酸钙)。
如前所述,本文所述的聚氨酯泡沫形成组合物可特别适用于SPF应用。因此,本发明的某些实施方案涉及制备聚氨酯泡沫的方法。在一些实施方案中,这些方法包括:(a)将如上所述的聚氨酯泡沫形成组合物在喷枪中冲击混合;和(b)将混合物喷涂至表面上。在某些实施方案中,所得泡沫为硬质泡沫,其特别适合用作建筑(墙壁和屋顶)、汽车、器具和其他应用中的隔热泡沫。因此,在某些实施方案中,本发明方法中使用的基材体现为建筑构件,如墙壁、地板或天花板。
在本发明方法的某些实施方案中,多异氰酸酯和异氰酸酯-反应性组合物以1.5:1至1:1.5,如1.1:1至1:1.1的相对体积比结合。在本发明方法的某些实施方案中,多异氰酸酯和异氰酸酯-反应性组合物以这样的相对量结合,使得NCO指数(异氰酸酯基与异氰酸酯-反应性基团的比值乘以100)为50至300,如50至200、70至150、90至150、90至135,或在某些情况下为100至135或100至120。
本发明的某些实施方案还涉及所得泡沫具有例如如上所述的密度。在某些实施方案中,所得泡沫为闭孔泡沫,如本文所用,其意指泡沫的闭孔含量为至少80体积%,如至少85体积%或至少90体积%,根据ISO4590:2002测定。
在某些实施方案中,本文所述的聚氨酯泡沫形成组合物形成等级为B级(火焰蔓延指数为26-75)的泡沫,根据ASTM E 84测试测定。但是,在其他实施方案中,本文所述的聚氨酯泡沫形成组合物形成等级为A级(火焰蔓延指数不超过25且烟雾发展指数不超过450)的泡沫,根据ASTM E 84测试测定。
本文所述的聚氨酯泡沫可用于广泛的应用中。在一些情况下,所述泡沫用在建筑基材上,如墙壁、地板或天花板。在其他情况下,所述泡沫可用于器具、板材或层压板。
以下实施例作为本发明的说明而给出。除非另有说明,这些实施例中给出的所有份数和百分比均为重量份和重量百分比。
实施例
实施例1-12
使用下表1中列出的成分和量(重量份)制备多元醇共混物。为了制备多元醇共混物,将除发泡剂之外的所有组分加入合适的容器中并混合。然后将混合物冷却至10℃,然后加入发泡剂。加入发泡剂后,将完整的多元醇共混物转移至350ml玻璃压力容器中。装料重量为每个容器375克多元醇共混物。
然后将容器置于50℃的烘箱中。在预定时间进行杯试验(cup test)之前,将容器和材料冷却至23℃,然后进行杯试验的发泡。肉眼观察容器的任何相分离或可能已存在的小球珠并记录。
使用975ml(夸脱)纸杯进行杯试验。将45.2克多元醇与54.8克MRLight(聚合二苯基甲烷二异氰酸酯(pMDI),其NCO含量至少为31.0%,在25℃下粘度为150至250mPa·s;平均当量重量为132且官能度为2.8,从Covestro LLC商购可得)混合。记录反应时间(凝胶、杯顶、发起结束)。在泡沫冷却后,切掉杯子的顶部以获得泡沫的密度。结果列于表1中。实施例1、3、5、7、9和11为本发明实施例,实施例2、4、6、8、10和12为对比例。
1邻苯二甲酸酐基聚酯多元醇,其羟值为290-310mg KOH/克多元醇,理论官能度为2.1,平均当量重量为187,可从Stepan Company商购获得。
2邻苯二甲酸酐基聚酯多元醇,其羟值为340-360mg KOH/克多元醇,理论官能度为2.4,平均当量重量为160,可从Stepan Company商购获得。
3芳族对苯二甲酸酯基聚酯多元醇,其羟值为285-305mg KOH/克多元醇,理论官能度为2.4,可从Huntsman Cooperation商购获得。
4三乙醇胺(85%水溶液)。
5625分子量的蔗糖基聚醚多元醇,羟值为450-490mg KOH/克多元醇,可从Covestro LLC商购获得。
6购自Albemarle Corporation的阻燃剂。
7购自Siltech Corporation的二甲基硅氧烷和聚氧化烯的不可水解的嵌段共聚物。
8购自Air Products and Chemicals,Inc.的胺催化剂
实施例13-14
以下实施例证实了在喷雾泡沫应用中使用本说明书中所述类型的聚氨酯泡沫形成组合物制备由于较低放热而无焦烧的厚部件的预期优势。
可采用实施例1-12所述的方法,使用下表2中列出的成分和量来制备多元醇共混物。可以1:1的体积混合比将多元醇共混物与MR Light(聚合二苯甲烷二异氰酸酯(pMDI)喷涂至边框为2x4尺寸木材墙桩的定向刨花板(OSB)基材上,所述MR Light的NCO含量为至少31.0%,在25℃下粘度为150-250mPa·s;平均当量重量为132,官能度为2.8,可从Covestro LLC商购获得,所述喷涂使用带有60英尺加热软管、采用配备42/42混合室的Graco Fusion Air Purge喷枪的Graco E-30喷涂机。在喷涂操作中可使用以下参数:树脂和异氰酸酯的温度:85°F;设备中多元醇共混物和异氰酸酯的温度:125°F;设备软管温度:125°F;设备中多元醇共混物合物和异氰酸酯的设定压力:1500psi。预期结果列于表2中。实施例13为本发明实施例,实施例14为对比例。
表2
9四个热电偶等间隔地分布于24英寸区域内
已参照各种非限制性和非穷举性实施方案来撰写本说明书。但是,本领域普通技术人员应理解,任何所公开实施方案(或其部分)的各种替换、修改或组合可包含在本说明书的范围内。因此,可以考虑并理解的是,本说明书支持未在本文中明确阐述的其他实施方案。这种实施方案例如可以通过组合、修改或重组本说明书中描述的各种非限制性实施方案的任何公开的步骤、组成、元素、特征、方面、特性、限制等而获得。由此,申请人保留在审查期间修改权利要求以增加本说明书所述的各种特征的权利,并且这些修改符合美国专利法第112条第一款(35U.S.C.§112,first paragraph)和美国专利法第132(a)条(35U.S.C.§132(a))的要求。
Claims (9)
1.一种聚氨酯泡沫形成组合物,其包含:
(a)异氰酸酯-反应性组合物,其包含:
(1)至少50重量%的邻苯二甲酸酐基聚酯多元醇,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计;
(2)水;和
(3)C2-C6卤代烯烃,
其中将异氰酸酯-反应性组合物在50℃下老化7天后,异氰酸酯-反应性组合物未显示出可见的混浊或凝胶;和
(b)多异氰酸酯,
其中邻苯二甲酸酐基聚酯多元醇包含两种或更多种邻苯二甲酸酐基聚酯多元醇的混合物,所述邻苯二甲酸酐基聚酯多元醇包含:
(i)第一邻苯二甲酸酐基聚酯多元醇,其羟值为290至310mg KOH/克多元醇,OH官能度为2.0至2.2,和
(ii)第二邻苯二甲酸酐基聚酯多元醇,其羟值为340至360mg KOH/克多元醇,OH官能度为2.3至2.5。
2.权利要求1的泡沫形成组合物,其中:
(i)的存在量为50重量%至99重量%,基于(i)和(ii)的总重量计;且
(ii)的存在量为1重量%至50重量%,基于(i)和(ii)的总重量计。
3.权利要求1的泡沫形成组合物,其中邻苯二甲酸酐基聚酯多元醇的存在量为至少60重量%,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计。
4.权利要求1的泡沫形成组合物,其中异氰酸酯-反应性组合物还包含蔗糖基聚醚多元醇,其羟值为400-800mg KOH/克多元醇,OH官能度为5.0至7.0。
5.权利要求4的泡沫形成组合物,其中蔗糖基聚醚多元醇的存在量为1至20重量%,基于异氰酸酯-反应性组合物中异氰酸酯-反应性组分的总重量计。
6.权利要求1的泡沫形成组合物,其中C2-C6卤代烯烃包括氢氟氯烯烃。
7.权利要求6的泡沫形成组合物,其中氢氟氯烯烃包括1,1,1-三氟-3-氯丙烯(HFCO-1233zd)。
8.一种制备低密度聚氨酯泡沫的方法,其包括:
(a)将权利要求1的泡沫形成组合物在喷枪中冲击混合;和
(b)将混合物喷涂至表面上。
9.包含通过权利要求8的方法形成的泡沫的建筑物墙壁或屋顶隔热材料。
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- 2016-07-25 US US15/218,632 patent/US10131758B2/en not_active Expired - Fee Related
-
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- 2017-07-20 CN CN201780044421.6A patent/CN109476805B/zh not_active Expired - Fee Related
- 2017-07-20 JP JP2019503705A patent/JP6935485B2/ja active Active
- 2017-07-20 EP EP17745952.6A patent/EP3487900A1/en not_active Withdrawn
- 2017-07-20 WO PCT/US2017/042991 patent/WO2018022405A1/en unknown
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EP3487900A1 (en) | 2019-05-29 |
WO2018022405A1 (en) | 2018-02-01 |
US20180022885A1 (en) | 2018-01-25 |
CN109476805A (zh) | 2019-03-15 |
JP2019522098A (ja) | 2019-08-08 |
JP6935485B2 (ja) | 2021-09-15 |
US10131758B2 (en) | 2018-11-20 |
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