CN103814108B - 含有1-氯-3,3,3-三氟丙烯(1233zd)的泡沫和由含有1-氯-3,3,3-三氟丙烯(1233zd)的泡沫制成的阻燃制品 - Google Patents
含有1-氯-3,3,3-三氟丙烯(1233zd)的泡沫和由含有1-氯-3,3,3-三氟丙烯(1233zd)的泡沫制成的阻燃制品 Download PDFInfo
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- CN103814108B CN103814108B CN201280046427.4A CN201280046427A CN103814108B CN 103814108 B CN103814108 B CN 103814108B CN 201280046427 A CN201280046427 A CN 201280046427A CN 103814108 B CN103814108 B CN 103814108B
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Abstract
本发明涉及建筑围护结构和形成建筑围护结构的方法,所述建筑围护结构包含具有聚合泡沫结构的泡沫,所述聚合泡沫结构在其中包括许多闭孔和包含在至少一部分所述闭孔中的反式-1-氯-3,3,3-三氟丙烯(1233zd(E))。
Description
对相关申请的交叉引用
本申请要求2011年7月28日提交的美国临时申请序号No. 61/512,742的优先权,其内容全文经此引用并入本文。
发明领域
本发明涉及泡沫和形成具有相对较高的绝热值和安全/阻燃性水平的制品(包括建筑围护结构(building envelope))的方法。
发明背景
被称作低密度硬质至半硬质聚氨酯或聚异氰脲酸酯泡沫的泡沫类型可用于多种绝缘用途,包括屋顶系统、建筑板、建筑围护隔热、喷施泡沫、单组分和双组分泡沫、冰箱和冷冻机的隔热、和用于减震和安全用途的所谓整皮泡沫( integral skin foam ),如方向盘和其它汽车或航空舱部件、鞋底和游乐园安全带( amusement park restraint)等。许多硬质至半硬质聚氨酯泡沫的大规模商业成功中的一个重要因素是这种泡沫的提供良好性质平衡的能力。通常,硬质聚氨酯和聚异氰脲酸酯泡沫应提供优异绝热、优异耐火性和在合理低的密度下的优异结构性质。
如已知,发泡剂用于形成此类泡沫所需的多孔结构。由于它们的易用性等因素,通常使用液体碳氟化合物发泡剂。碳氟化合物不仅凭借它们的挥发性充当发泡剂,还包封或截留在硬质泡沫的闭孔结构中并通常是硬质聚氨酯泡沫的热导率性质的主要成因。在形成泡沫后,与制成的泡沫相关联的k-系数衡量该泡沫抵抗透过该泡沫材料传热的能力。随着k-系数降低,表明该材料更抗传热,因此是用于绝热用途的更好的泡沫。因此,产生较低k-系数泡沫的材料通常合意和有利。
近年来,对气候变化的关心驱使开发符合臭氧消耗和气候变化规章的要求的新一代碳氟化合物。两种这样的碳氟化合物是反式-1,3,3,3-四氟丙烯(1234ze(E))和反式-1-氯-3,3,3-三氟丙烯(1233zd(E)或HBA-2)。这些产品都包含所需环境性质,同时保持预期的高性能特性,这使得碳氟化合物发泡剂作为用于高性能硬质泡沫绝缘用途的主导候选材料脱颖而出。
发明概述
一方面,本发明涉及将泡沫施加到制品上以形成具有相对较高的绝热值水平和安全水平(例如通过改进的耐火性)的绝热制品的方法,还涉及使用这样的制品形成建筑围护结构的方法和涉及这样的制品的建筑方法。本文所用的术语“建筑围护结构”是指居住或要被一人或多人占据的任何类型的结构。此类结构的实例包括住宅、办公楼、体育场、工厂、水运工具(water craft)等。由于此类结构通常使用相对大量的泡沫(通常用于绝热用途)作为该结构的部件,对此类材料对该结构安全性的影响(包括在该结构的消防安全性方面)尤其非常敏感。申请人已经认识到,提高此类制品或结构的安全系数和/或在较低成本下提供相同消防安全水平的制品和/或建筑方法具有实质优点。
因此,本发明的一个方面提供形成优选用在建筑围护结构中或用作建筑围护结构的一部分的制品的方法,其包含基底和在所述基底上和/或附着到所述基底上的绝热泡沫,其中该泡沫是包含闭孔和在所述泡孔中的气体组合物的聚氨酯或聚异氰脲酸酯泡沫,所述气体组合物包含,优选以主要重量比例包含,再更优选包含至少大约70重量%的反式-1-氯-3,3,3-三氟丙烯(1233zd(E))。在某些优选实施方案中,如下形成该泡沫:提供包含一种或多种可发泡组分和发泡剂的聚氨酯或聚异氰脲酸酯泡沫预混组合物,其中该发泡剂包含,优选以主要重量比例包含,再更优选包含至少大约70重量%的反式-1-氯-3,3,3-三氟丙烯(1233zd(E)),并与要安装在所述建筑围护结构中的制品相关联地和/或与已安装在建筑围护结构中的结构件或基底,如墙、天花板或屋顶部件相关联地由所述预混物形成泡沫。在某些优选实施方案中,如下形成该泡沫:将多元醇泡沫预混组合物喷施到要用在建筑围护结构中的制品上或建筑围护结构的表面或空腔上;并使该可发泡组合物发泡以形成其中含有至少一部分发泡剂的闭孔泡沫。在某些方面中,包含在泡孔中的气体材料包括至少50体积%的所述反式-1-氯-3,3,3-三氟丙烯,在另一些方面中,泡孔内的气体包含至少大约70体积%的所述反式-1-氯-3,3,3-三氟丙烯,在更优选的实施方案中,该气体材料基本由反式-1-氯-3,3,3-三氟丙烯构成。
在某些优选方面中,本发明提供通过在所述围护结构上或内安装聚氨酯或聚异氰脲酸酯泡沫结构或制品来构造建筑围护结构的方法。如上所述,安装步骤可包括预成型该泡沫,如通过形成板或绝热板,并在建筑围护结构上或中安装所述预成型泡沫,和/或安装步骤可包括在构建该围护结构时或后将该泡沫形成到建筑围护结构的基底或部件中或上,如通过将可发泡组合物喷到该基底或部件上或中。
申请人已经认识到,本发明的方法可以为此类建筑围护结构提供提高的消防安全特性。例如,根据本发明的某些优选方面,本发明的泡沫在使用Mobil 45º试验测试时表现出小于大约1.0%重量损失,在某些实施方案中在使用Mobil 45º试验测试时再更优选小于大约0.5%重量损失。尽管上文使用Mobil 45º试验测量改进的易燃性,但这种测试衡量不是本发明的改进的消防安全特征的唯一衡量标准。例如,根据本发明用1233zd(包括反式-1233zd)制成的泡沫优选在本领域中已知的其它标准试验中表现出显著改进的不燃性。作为非限制性实例,本发明的优选泡沫在其它小规模测试,如DIN 4102中表现出显著改进,特别是优于使用245fa制成的泡沫。本发明的优选泡沫还优选在满载试验,如ASTM E-84、NFPA286和FM 4880中测试时表现出火焰高度的显著降低和较低的火焰蔓延。相应地,本发明的优选泡沫表现出易燃性的总体降低和/或降低在泡沫中包含某些附加试剂,如阻燃剂的需要并因此避免此类材料的增值成本和其它可能的缺点。
在本文中的多元醇预混组合物的某些方面中,多元醇组分可以以大约60重量%至大约95重量%的量存在,且反式-1-氯-3,3,3-三氟丙烯的量为大约1重量%至大约30重量%。
本发明的发泡剂除反式-1-氯-3,3,3-三氟丙烯外还可包含至少一种助发泡剂。这样的附加发泡剂可选自水、产生CO2和/或CO的有机酸、烃;醚、卤代醚;酯、醇、醛、酮、五氟丁烷;五氟丙烷;六氟丙烷;七氟丙烷;反式-1,2二氯乙烯;甲缩醛、甲酸甲酯;1-氯-1,2,2,2-四氟乙烷(HCFC-124);1,1-二氯-1-氟乙烷(HCFC-141b);1,1,1,2-四氟乙烷(HFC-134a);1,1,2,2-四氟乙烷(HFC-134);1-氯1,1-二氟乙烷(HCFC-142b);1,1,1,3,3-五氟丁烷(HFC-365mfc);1,1,1,2,3,3,3-七氟丙烷(HFC-227ea);三氯氟甲烷(CFC-11);二氯二氟甲烷(CFC-12);二氯氟甲烷(HCFC-22);1,1,1,3,3,3-六氟丙烷(HFC-236fa);1,1,1,2,3,3-六氟丙烷(HFC-236e);1,1,1,2,3,3,3-七氟丙烷(HFC-227ea)、二氟甲烷(HFC-32);1,1-二氟乙烷(HFC-152a);1,1,1,3,3-五氟丙烷(HFC-245fa);1,3,3,3-四氟丙烯(HFO-1234ze);1,1,1,4,4,4-六氟丁-2-烯(HFO-1336mzzm);丁烷;异丁烷;正戊烷;异戊烷;或环戊烷之一或组合。
该多元醇预混物还可包括选自有机硅表面活性剂、非有机硅表面活性剂、金属催化剂、胺催化剂、阻燃剂及其组合的一种或多种附加试剂。在提供有机硅表面活性剂的实施方案中,其可以以大约0.5重量%至大约5.0重量%的量存在。在提供非有机硅表面活性剂的实施方案中,其可以以大约0.05重量%至大约3.0重量%的量存在。在提供胺催化剂的实施方案中,其可以以大约0.05重量%至大约3.0重量%的量存在。在提供金属催化剂的实施方案中,其可以以大约0.5重量%至大约10.0重量%的量存在。
本领域技术人员基于本文中提供的公开内容容易看出本发明的其它实施方案和优点。
发明详述
申请人已经认识到在使用1233zd(优选其反式形式1233zd(E))作为聚氨酯和聚异氰脲酸酯泡沫用途,特别是喷涂面板(panel)和板材(board)泡沫用途中的发泡剂时存在意外和惊人的优点。本文中提供的一个特定优点在于,该泡沫、由其形成的制品和由其形成的建筑制品具有显著和意外改进的耐火品质,特别是优于使用其它已知HFC发泡剂的泡沫。
如本领域技术人员已知,聚氨酯和聚异氰脲酸酯泡沫广泛用作几种类型的制品中的芯绝热材料。之前,聚氨酯和聚异氰脲酸酯泡沫的一些最常用的发泡剂包括HFC-245fa、HFC-134a和烃。在发展中国家在大多数聚氨酯和聚异氰脲酸酯泡沫市场常使用这些化合物。随着在发达国家出现低全球变暖潜势倡议和在发展中国家逐渐淘汰HCFC,全世界越来越需要和想要低全球变暖潜势(LGWP)发泡剂。
申请人在本文中阐明,本发明的一个优点在于,本发明的制品和/或建筑围护结构具有改进的耐火特性。可燃性是许多地方、区域和国家建筑规范的关键部分。如本文中的数据中证实,与由其它常用发泡剂形成的泡沫观察到的相比,本发明的泡沫具有明显更好的燃烧性质,例如明显更好的燃烧后重量损失百分比,尽管本发明的发泡剂的可燃性类似于常用发泡剂。换言之,根据泡沫工业中常用的标准,基于反式-1234ze的可燃性与HFC-245fa的可燃性的比较,原本预料,由各发泡剂形成的泡沫的耐火性类似。但是,申请人已经意外地发现,事实并非如此,因此已经认识到,根据本发明制成的建筑围护结构可实现重要和实质的,但出乎意料的优点。特别地,要指出,在使用以1233zd作为发泡剂的泡沫的Mobil 45º可燃性测试的过程中观察到小于1.0%重量损失。在另一些实施方案中,观察到小于0.5%重量损失。这表明根据本发明使用1233zd作为发泡剂形成的泡沫和根据本发明形成的建筑围护结构具有出乎意料增强的耐火性。
因此,本发明的一个方面涉及1233zd作为多元醇预混物,特别是可用于喷涂泡沫、面板泡沫和板材泡沫的预混物中的发泡剂和/或所得泡沫泡孔结构的主要气体组分的用途。1233zd可以独自或与一种或多种附加发泡剂共混提供。这样的助发泡剂的非排他名单包括,但不限于,水、产生CO2和/或CO的有机酸、烃;醚、卤代醚;酯、醇、醛、酮、五氟丁烷;五氟丙烷;六氟丙烷;七氟丙烷;反式-1,2二氯乙烯;甲缩醛、甲酸甲酯;1-氯-1,2,2,2-四氟乙烷(HCFC-124);1,1-二氯-1-氟乙烷(HCFC-141b);1,1,1,2-四氟乙烷(HFC-134a);1,1,2,2-四氟乙烷(HFC-134);1-氯1,1-二氟乙烷(HCFC-142b);1,1,1,3,3-五氟丁烷(HFC-365mfc);1,1,1,2,3,3,3-七氟丙烷(HFC-227ea);三氯氟甲烷(CFC-11);二氯二氟甲烷(CFC-12);二氯氟甲烷(HCFC-22);1,1,1,3,3,3-六氟丙烷(HFC-236fa);1,1,1,2,3,3-六氟丙烷(HFC-236e);1,1,1,2,3,3,3-七氟丙烷(HFC-227ea)、二氟甲烷(HFC-32);1,1-二氟乙烷(HFC-152a);1,1,1,3,3-五氟丙烷(HFC-245fa);1,3,3,3-四氟丙烯(HFO-1234ze – 包括其反式或“E”异构体);1,1,1,4,4,4-六氟丁-2-烯(HFO-1336mzzm – 包括其顺式或“Z”异构体);丁烷;异丁烷;正戊烷;异戊烷;环戊烷或其组合。
1233zd组分通常以多元醇预混组合物重量的大约1重量%至大约30重量%,优选大约3重量%至大约25重量%,更优选大约5重量%至大约25重量%的量存在于多元醇预混组合物中。这样的量产生含有主要包含1233zd的气体的泡沫泡孔结构。
当1233zd和一种或多种附加发泡剂都存在时,1233zd可以以发泡剂组分重量的大约5重量%至大约99重量%,大约10重量%至大约90重量%,或大约25重量%至大约85重量%的量存在于发泡剂组分中;且所述任选发泡剂通常以发泡剂组分重量的大约95重量%至大约1重量%,大约90重量%至大约10重量%,或大约15重量%至大约75重量%的量存在于发泡剂组分中。所得泡沫泡孔结构中的气体含量取决于该共混物中所用的发泡剂的组分量。
可包括多元醇混合物的多元醇组分可以是在制备聚氨酯或聚异氰脲酸酯泡沫时以已知方式与异氰酸酯反应的任何多元醇。可用的多元醇包含下列一项或多项:含蔗糖的多元醇;酚、含酚醛的多元醇;含葡萄糖的多元醇;含山梨糖醇的多元醇;含甲基葡糖苷的多元醇;芳族聚酯多元醇;甘油;乙二醇;二乙二醇;丙二醇;聚醚多元醇与乙烯基聚合物的接枝共聚物;聚醚多元醇与聚脲的共聚物;与一种或多种(b)缩合的一种或多种(a):(a)甘油、乙二醇、二乙二醇、三羟甲基丙烷、乙二胺、季戊四醇、大豆油、卵磷脂、妥尔油、棕榈油、蓖麻油;(b)环氧乙烷、环氧丙烷、环氧乙烷和环氧丙烷的混合物;或它们的组合。该多元醇组分优选以多元醇预混组合物重量的大约60重量%至大约95重量%,优选大约65重量%至大约95重量%,更优选大约70重量%至大约90重量%的量存在于该多元醇预混组合物中。
在某些实施方案中,该多元醇预混组合物还可含有至少一种含有机硅的表面活性剂。该含有机硅的表面活性剂用于助于由该混合物形成泡沫,以及控制该泡沫的气泡的尺寸以获得具有所需泡孔结构的泡沫。优选需要其中具有尺寸均匀的小气泡或泡孔的泡沫,因为其具有最合意的物理性质,如压缩强度和热导率。提供具有在成形前或在泡沫升起(foam rise)过程中不坍塌的稳定泡孔的泡沫也是至关重要的。
用于制备聚氨酯或聚异氰脲酸酯泡沫的有机硅表面活性剂可以以本领域技术人员已知的许多商品名获得。这些材料可用于多种配方,允许均匀泡孔形成和最大气体夹带以获得极低密度泡沫结构。优选的有机硅表面活性剂包含聚硅氧烷聚氧化烯嵌段共聚物。可用于本发明的一些代表性的有机硅表面活性剂是Momentive's L-5130、L-5180、L-5340、L-5440、L-6100、L-6900、L-6980和L-6988;Air Products DC-193、DC-197、DC-5582和DC-5598;和来自Goldschmidt AG of Essen, Germany的B-8404、B-8407、B-8409和B-8462。在美国专利2,834,748;2,917,480;2,846,458和4,147,847中公开了另一些,它们的内容经此引用并入本文。该有机硅表面活性剂组分通常以多元醇预混组合物重量的大约0.5重量%至大约5.0重量%,优选大约1.0重量%至大约4.0重量%,更优选大约1.5重量%至大约3.0重量%的量存在于该多元醇预混组合物中。
该多元醇预混组合物可任选含有非有机硅表面活性剂,如非有机硅非离子型表面活性剂。这些可包括氧乙基化烷基酚、氧乙基化脂肪醇、石蜡油、蓖麻油酯、蓖麻酸酯、土耳其红油、花生油、石蜡和脂肪醇。优选但非限制性的非有机硅非离子型表面活性剂是可购自Air Products Corporation的LK-443。当使用非有机硅非离子型表面活性剂时,其以多元醇预混组合物重量的大约0.05重量%至大约3.0重量%,优选大约0.05重量%至大约2.5重量%,更优选大约0.1重量%至大约2.0重量%的量存在于该多元醇预混组合物中。
该多元醇预混组合物还可包括一种或多种催化剂,特别是胺催化剂和/或金属催化剂。胺催化剂可包括,但不限于,伯胺、仲胺或叔胺。可用的叔胺催化剂非排他地包括N,N,N',N",N"-五甲基二乙基三胺、N,N-二环己基甲基胺;N,N-乙基二异丙基胺;N,N-二甲基环己基胺;N,N-二甲基异丙基胺;N-甲基-N-异丙基苄基胺;N-甲基-N-环戊基苄基胺;N-异丙基-N-仲丁基-三氟乙基胺;N,N-二乙基-(α-苯基乙基)胺、N,N,N-三-正丙基胺或其组合。可用的仲胺催化剂非排他地包括二环己基胺;叔丁基异丙基胺;二-叔丁基胺;环己基-叔丁基胺;二-仲丁基胺、二环戊基胺;二-(α-三氟甲基乙基)胺;二-(α-苯基乙基)胺;或其组合。
可用的伯胺催化剂非排他地包括:三苯基甲基胺和1,1-二乙基-正丙基胺。
其它可用的胺包括吗啉、咪唑、含醚化合物等。这些包括
二吗啉并二乙基醚
N-乙基吗啉
N-甲基吗啉
双(二甲基氨基乙基)醚
咪唑
正甲基咪唑
1,2-二甲基咪唑
二吗啉并二甲基醚
N,N,N',N',N",N"-五甲基二亚乙基三胺
N,N,N',N',N",N"-五乙基二亚乙基三胺
N,N,N',N',N",N"-五甲基二亚丙基三胺
双(二乙基氨基乙基)醚
双(二甲基氨基丙基)醚。
在使用胺催化剂时,其以多元醇预混组合物重量的大约0.05重量%至大约3.0重量%,优选大约0.05重量%至大约2.5重量%,更优选大约0.1重量%至大约2.0重量%的量存在于该多元醇预混组合物中。
催化剂还可包括一种金属催化剂或金属催化剂的组合,例如但不限于有机金属催化剂。术语有机金属催化剂是指并在其广义中旨在涵盖预形成的有机金属络合物和包含金属羧酸盐和/或脒的组合物(包括物理组合、混合物和/或共混物)。在优选实施方案中,本发明的催化剂包含:(a) 选自锌、锂、钠、镁、钡、钾、钙、铋、镉、铝、锆、锡或铪、钛、镧、钒、铌、钽、碲、钼、钨、铯的一种或多种金属;(b) 与脒化合物的络合物和/或组合物;和/或(c) 与脂族化合物、芳族化合物和/或聚合羧酸酯的络合物和/或组合物。
在用于某些实施方案的脒化合物中优选的是含有催化脒基的那些,特别是具有杂环的那些(连接基优选是—N═C—N—),例如咪唑啉、咪唑、四氢嘧啶、二氢嘧啶或嘧啶环。或者,可以使用无环脒和胍。一种优选的催化剂络合物/组合物包含锌(II)、己酸甲酯、己酸乙酯或己酸丙酯,和咪唑(优选低级烷基咪唑,如甲基咪唑)。这样的催化剂可包括Zn(1-甲基咪唑)2(2-乙基己酸酯)2以及二-乙二醇,优选作为该催化剂的溶剂。为此,一种示例性的催化剂包括,但不限于,King Industries of Norwalk, Connecticut以商品名K-Kat XK-614出售的催化剂。另一些催化剂包括Air Products, Inc以商品名Dabco K 15和/或DabcoMB 20出售的那些。
当使用一种金属催化剂或金属催化剂的组合时,这种催化剂以多元醇预混组合物重量的大约0.5重量%至大约10重量%,或优选大约1.0重量%至大约8.0重量%的量存在于该多元醇预混组合物中。
使用本文所述的组合物制备聚氨酯或聚异氰脲酸酯泡沫可遵循本领域中公知的任何方法,参见Saunders和Frisch, 第I和II卷,Polyurethanes Chemistry andtechnology, 1962, John Wiley and Sons, New York, N. Y.或Gum, Reese, Ulrich,Reaction Polymers, 1992, Oxford University Press, New York, N.Y.或Klempnerand Sendijarevic, Polymeric Foams and Foam Technology, 2004, Hanser GardnerPublications, Cincinnati, OH。通常,通过合并异氰酸酯、多元醇预混组合物和其它材料,如任选阻燃剂、水、着色剂或其它添加剂来制备聚氨酯或聚异氰脲酸酯泡沫。这些泡沫可以是硬质、软质或半硬质的,并可具有闭孔结构、开孔结构或开孔和闭孔的混合物。
在许多应用中在预混制剂中提供聚氨酯或聚异氰脲酸酯泡沫的组分是方便的。最通常,将泡沫制剂预混成两种组分。异氰酸酯和任选其它异氰酸酯相容原材料,包括但不限于发泡剂和某些有机硅表面活性剂,构成第一组分,常称作“A”组分。包括表面活性剂、催化剂、发泡剂和任选其它成分的多元醇混合物组合物构成第二组分,常称作“B”组分。在任何给定用途中,“B”组分并非含有所有上列组分,例如如果阻燃性不是所需泡沫性质,一些配方省略阻燃剂。相应地,通过将A和B方组分合在一起——对小制品而言通过手动混合或优选通过机械混合技术,容易制备聚氨酯或聚异氰脲酸酯泡沫,以形成块、厚块、层合材料、现场浇注板和其它物品、喷施泡沫、泡沫体等。任选地,其它成分,如阻燃剂、着色剂、辅助发泡剂、水和甚至其它多元醇可作为料流添加至混合头或反应位点。但是,最方便地,除水外,它们都合并到如上所述的一个B组分中。
可以通过使有机多异氰酸酯和上述多元醇预混组合物反应来形成适用于形成聚氨酯或聚异氰脲酸酯泡沫的可发泡组合物。在聚氨酯或聚异氰脲酸酯泡沫合成中可以使用任何有机多异氰酸酯,包括脂族和芳族多异氰酸酯。合适的有机多异氰酸酯包括聚氨酯化学领域中公知的脂族、脂环族、芳脂族、芳族和杂环异氰酸酯。例如在美国专利4,868,224;3,401,190;3,454,606;3,277,138;3,492,330;3,001,973;3,394,164;3,124,605;和3,201,372中描述了这些。优选的一类是芳族多异氰酸酯。
代表性的有机多异氰酸酯符合下式:
R(NCO)z
其中R是多价有机基团——脂族基团、芳烷基、芳族基团或其混合物,且z是符合R的化合价的整数并且是至少2。本文考虑的有机多异氰酸酯的代表包括例如芳族二异氰酸酯,如2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、2,4-和2,6-甲苯二异氰酸酯的混合物、粗制甲苯二异氰酸酯、亚甲基二苯基二异氰酸酯、粗制亚甲基二苯基二异氰酸酯等;芳族三异氰酸酯,如4,4',4"-三苯甲烷三异氰酸酯、2,4,6-甲苯三异氰酸酯;芳族四异氰酸酯,如4,4'-二甲基二苯甲烷-2,2'5,5-'四异氰酸酯等;芳烷基多异氰酸酯,如苯二亚甲基二异氰酸酯(xylylene diisocyanate);脂族多异氰酸酯,如六亚甲基-1,6-二异氰酸酯、赖氨酸二异氰酸酯甲酯等;和它们的混合物。其它有机多异氰酸酯包括多亚甲基多苯基异氰酸酯、氢化亚甲基二苯基异氰酸酯、间亚苯基二异氰酸酯、萘-1,5-二异氰酸酯、1-甲氧基亚苯基-2,4-二异氰酸酯、4,4'-联苯二异氰酸酯、3,3'-二甲氧基-4,4'-联苯二异氰酸酯、3,3'-二甲基-4,4'-联苯二异氰酸酯和3,3'-二甲基二苯甲烷-4,4'-二异氰酸酯;典型的脂族多异氰酸酯是亚烷基二异氰酸酯,如三亚甲基二异氰酸酯、四亚甲基二异氰酸酯和六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、4,4'-亚甲基双(环己基异氰酸酯)等;典型的芳族多异氰酸酯包括间和对亚苯基二异氰酸酯、多亚甲基多苯基异氰酸酯、2,4-和2,6-甲苯二异氰酸酯、邻联茴香胺二异氰酸酯(dianisidine diisocyanate)、bitoylene异氰酸酯、萘1,4-二异氰酸酯、双(4-异氰酸根合苯基)亚甲基、双(2-甲基-4-异氰酸根合苯基)甲烷等。优选的多异氰酸酯是多亚甲基多苯基异氰酸酯,特别是含有大约30至大约85重量%亚甲基双(苯基异氰酸酯)的混合物,该混合物的其余部分包含官能度高于2的多亚甲基多苯基多异氰酸酯。通过本领域中已知的常规方法制备这些多异氰酸酯。在本发明中,多异氰酸酯和多元醇以产生大约0.9至大约5.0的NCO/OH化学计量比的量使用。在本发明中,NCO/OH当量比优选为大约1.0或更大和大约3.0或更小,理想范围是大约1.1至大约2.5。尤其合适的有机多异氰酸酯包括多亚甲基多苯基异氰酸酯、亚甲基双(苯基异氰酸酯)、甲苯二异氰酸酯或其组合。
在聚异氰脲酸酯泡沫的制备中,三聚催化剂用于将该共混物与过量A组分一起转化成聚异氰脲酸酯-聚氨酯泡沫。所用三聚催化剂可以是本领域技术人员已知的任何催化剂,包括但不限于,甘氨酸盐、叔胺三聚催化剂、季铵羧酸盐和碱金属羧酸盐和各种类型催化剂的混合物。这些类别内的优选物类是乙酸钾、辛酸钾和N-(2-羟基-5-壬基酚)甲基-N-甲基甘氨酸盐。
也可以优选以反应物的不多于大约20重量%的量并入常规阻燃剂。任选阻燃剂包括三(2-氯乙基)磷酸酯、三(2-氯丙基)磷酸酯、三(2,3-二溴丙基)磷酸酯、三(1,3-二氯丙基)磷酸酯、三(2-氯异丙基)磷酸酯、磷酸三甲苯酯、三(2,2-二氯异丙基)磷酸酯、N,N-双(2-羟乙基)氨基甲基膦酸二乙酯、甲基膦酸二甲酯、三(2,3-二溴丙基)磷酸酯、三(1,3-二氯丙基)磷酸酯和四-(2-氯乙基)亚乙基二磷酸酯、磷酸三乙酯、磷酸二铵、各种卤代芳族化合物、氧化锑、三水合铝、聚氯乙烯、三聚氰胺等。其它任选成分可包括0至大约7%水,其与异氰酸酯化学反应以产生二氧化碳。这种二氧化碳充当辅助发泡剂。在本发明的情况下,水不能添加到多元醇共混物中,但如果使用,可作为独立化学料流添加。甲酸也用于通过与异氰酸酯反应产生二氧化碳并任选添加到“B”组分中。
除之前描述的成分外,在泡沫制备中可包括其它成分,如染料、填料、颜料等。分散剂和泡孔稳定剂可并入本共混物中。本文所用的常规填料包括例如硅酸铝、硅酸钙、硅酸镁、碳酸钙、硫酸钡、硫酸钙、玻璃纤维、炭黑和二氧化硅。如果使用,填料通常以按重量计每100份多元醇大约5份至100份的量存在。本文中可用的颜料可以是任何常规颜料,如二氧化钛、氧化锌、氧化铁、氧化锑、铬绿、铬黄、铁蓝赭石、钼桔红和有机颜料,如对位红(parareds)、联苯胺黄、甲苯胺红、调色剂和酞菁。
制成的聚氨酯或聚异氰脲酸酯泡沫的密度可以为大约0.5磅/立方英尺至大约60磅/立方英尺,优选大约1.0至20.0磅/立方英尺,最优选大约1.5至6.0磅/立方英尺不等。所得密度取决于在A和/或B组分中存在或在制备泡沫时添加多少本发明中公开的发泡剂或发泡剂混合物+辅助发泡剂,如水或其它助发泡剂的量。这些泡沫可以是硬质、软质或半硬质泡沫并可具有闭孔结构、开孔结构或开孔和闭孔的混合物。这些泡沫用于各种公知用途,包括但不限于绝热、缓冲、浮选、包装、粘合剂、孔隙填充、工艺品和装饰、和减震。
在许多用途中,本发明的泡沫可用于建筑物(例如建筑围护结构)或需要能量管理和/或隔绝其外侧上的温度波动的任何构造的隔热。这样的结构包括本领域中已知的任何标准结构,包括但不限于由粘土、木材、石头、金属、塑料、水泥等制成的那些,包括但不限于住宅、办公楼或需要能量效率和隔热的其它住宅结构、商业结构或其它结构。
在本发明的一个非限制性方面中,可提供根据上述实施方案的双组分喷涂泡沫或可发泡组合物。A方(A-side)的组分和B方(B-side)的组分可通过单独的线路传送到喷枪,如冲击( impingement)型喷枪中。将喷枪加热至高于发泡剂1233zd的沸点的温度,并在高压下将这两种组分泵过小孔以形成A方和B方的各组分的料流。第一和第二组分的料流相交并互相混合并在喷枪内加热。由于组分在喷枪内处于压力下,发泡剂不会汽化。但是,随着该混合物离开喷枪并进入大气压,随着发生多元醇和聚氨酯或聚异氰脲酸酯的交联,发泡剂汽化。在由释气生成的气泡聚结并逸出之前,交联捕获这些气泡并形成提供绝热功能的泡孔。
此类泡沫在某些实施方案中可以(包括通过喷涂)在系梁、屋顶板、基墙、内壁和/或任何建筑围护体或结构的任何封闭或开放的墙身空腔上或作为它们的一部分形成。在某些优选实施方案中,本发明的泡沫可用于密封建筑围护结构,如住宅、商业建筑物等的此类绝热腔或表面,以防止空气流入该绝热腔或表面中的通孔(thru gap)并有效密封和隔绝该围护结构。合意地,在安装建筑内墙之前,将该泡沫喷涂到框架构件、空腔等上或中,尽管也可以在使用本领域中已知的方法安装内墙后将泡沫施加到此类区域。在另一些实施方案中,本发明的泡沫可通过填充建筑物的屋顶或墙体中、门、窗户、电箱等周围的裂缝和/或缝隙来充当空气渗透的密封剂。也可以施加该泡沫以密封墙壁和地板中的孔。
下列非限制性实施例用于例证本发明。
实施例
实施例1 – 泡沫配方
所用泡沫配方是较高指数配方。其是能在相同配方中比较发泡剂的通用配方并提供在下表1中。
在30℃和在30%湿度下形成泡沫。为了模拟建筑环境,将该体系喷到122 cm x 244cm x 1.25 cm胶合板(常见建筑材料)片材上。该胶合板表面吸湿并由于其不规则表面而更难覆盖。将该胶合板储存在环境试验室中并使其达到使用前的温度。在开始各试验之前用手持温度计确定基底的温度。
喷涂泡沫加工设备在概念上非常简单。其由4个主要部件构成:回转泵、配料装置、加热输送软管和喷枪。回转泵、配料装置(proportioning unit)和软管在工业上在供应形式和如何运行方面相当一致。此研究中使用的设备和加工参数列在表2中。为了确保施加中的一致性,使用West Development Group Robotics用机器人施加该泡沫。
实施例2 – 可燃性研究 – 喷涂泡沫
根据实施例1制备泡沫。通过Mobil 45°试验测试它们的可燃性。更具体地,提供测得为5.1cm x 21.6cm x 1.3cm (2” x 8.5” x 1/2”)的至少3个试样,泡沫升起平行于1.3cm (½”)的那个维度(dimension)。将各样品称重并精确至0.01克(0.0004 oz),记录为W0。
将各样品以大约45°角置于微焰灯(micro burner)上方以使样品在微焰灯顶部上方大约1.3cm (½”)。打开该微焰灯并将火焰设定为3.8cm (1.5”)高度,调节以使火焰沿平行于火焰的两个表面和形成45º角的两个表面均匀分布。将微焰灯留在样品下方直至泡沫样品上的所有可见的燃烧停止。然后将各烧焦样品称重并精确至0.01克(0.0004 oz),记录为W1。
如下计算损失百分比:
%重量损失 = (W0 – W1)/W0) X 100并记录。
在所有三个单独的样品上进行这些步骤,结果求平均并提供在下表3中。245fa和1233zd(E)都是不可燃发泡剂。碳氟化合物材料是物理发泡剂,意味着它们在发泡反应过程中由于该反应的放热性质而汽化。这些材料在泡沫制造过程中在物理上不变。在泡沫的泡孔气体中没有检测到发泡剂的分解。出乎意料的是,泡沫的可燃性明显不同。因此令人惊讶的是,发现表3中的结果,即1233zd泡沫在该试验中具有明显好于245fa泡沫的燃烧性质。
实施例3 – 泡沫配方
根据实施例1制备泡沫。通过ASTM E-84测试它们的可燃性。
将各样品置于E-84管道(tunnel)中。打开燃烧器并将火焰设定为该ASTM程序中规定的高度。测量火焰蔓延。在比较时,预计245fa泡沫的火焰蔓延小于1233zd泡沫。
245fa和1233zd(E)都是不可燃发泡剂。碳氟化合物材料是物理发泡剂,意味着它们在发泡反应过程中由于该反应的放热性质而汽化。这些材料在泡沫制造过程中不分解。出乎意料的是,泡沫的可燃性明显不同。
实施例4 – 施加到建筑围护结构
使用上述实施例1和表1中提供的成分和量制备两种样品泡沫A-方和B-方预混物,一种以1233zd为发泡剂,另一种具有HFC-245fa。A-方部分包括异氰酸酯组分,B-方部分包括多元醇混合物表面活性剂、催化剂、阻燃剂和发泡剂(1233zd(E)或HFC-245fa)。使用实施例1和表2中提供的设备和方法,将A和B方组分(1233zd预混物和HFC-245fa预混物)分别合在一起并喷涂到建筑围护结构的框架结构、具有螺栓的结构和由胶合板制成的外墙上,并使其固化。在30℃和在30%湿度下形成泡沫。
通过Mobil 45°试验测试这两种泡沫的可燃性。更具体地,提供测得为5.1cm x21.6cm x 1.3cm (2” x 8.5” x 1/2”)的至少3个试样,泡沫升起平行于1.3cm (½”)的那个维度。将各样品称重并精确至0.01克(0.0004 oz),记录为W0。
将各样品以大约45°角置于微焰灯上方以使样品在微焰灯顶部上方大约1.3cm(½”)。打开该微焰灯并将火焰设定为3.8cm (1.5”)高度,调节以使火焰沿平行于火焰的两个表面和形成45º角的两个表面均匀分布。将微焰灯留在样品下方直至泡沫样品上的所有可见的燃烧停止。然后将各烧焦样品称重并精确至0.01克(0.0004 oz),记录为W1。
如下计算损失百分比:
%重量损失 = (W0 – W1)/W0) X 100并记录。
在所有三个单独的样品上进行这些步骤并将结果求平均。与上述结果一致地,令人惊讶的是,1233zd在该试验中具有明显好于245fa泡沫的燃烧性质。
实施例5 – 施加到建筑围护结构 – 板料或面板上(预制)
使用上表4中提供的成分和量制备两种样品泡沫A-方和B-方预混物,一种以1233zd为发泡剂,另一种具有HFC-245fa。A-方部分包括异氰酸酯组分,B-方部分包括多元醇混合物表面活性剂、催化剂、阻燃剂和发泡剂(1233zd(E)或HFC-245fa)。使用EdgeSweets高压泡沫机,将A和B方组分(1233zd预混物和HFC-245fa预混物)分别合在一起并倒入模具中以制造隔热面板或板材,然后使用普通施工实践将这些面板和板材施加到建筑物的墙壁、屋顶或地基上。
通过Mobil 45°试验测试这两种泡沫的可燃性。更具体地,提供测得为5.1cm x21.6cm x 1.3cm (2” x 8.5” x 1/2”)的至少3个试样,泡沫升起平行于1.3cm (½”)的那个维度。将各样品称重并精确至0.01克(0.0004 oz),记录为W0。
将各样品以大约45°角置于微焰灯上方以使样品在微焰灯顶部上方大约1.3cm(½”)。打开该微焰灯并将火焰设定为3.8cm (1.5”)高度,调节以使火焰沿平行于火焰的两个表面和形成45º角的两个表面均匀分布。将微焰灯留在样品下方直至泡沫样品上的所有可见的燃烧停止。然后将各烧焦样品称重并精确至0.01克(0.0004 oz),记录为W1。
如下计算损失百分比:
%重量损失 = (W0 – W1)/W0) X 100并记录。
在所有三个单独的样品上进行这些步骤并将结果求平均。与上述结果一致地,令人惊讶的是,1233zd在该试验中具有明显更好的燃烧性质。
Claims (18)
1.形成建筑围护结构的方法,其包括:
a. 提供要作为建筑围护结构的基底或部件包括的制品;
b. 由所述制品形成至少一部分所述建筑围护结构;
c. 在所述步骤b之前或之后,在所述制品上和/或中施加泡沫,所述泡沫包含闭孔聚合结构及在至少一部分所述泡孔中的气体材料,所述气体材料包含至少50体积%的反式-1-氯-3,3,3-三氟丙烯(1233zd(E))。
2.权利要求1的方法,其中所述施加步骤包括提供包含含有1233zd(E)的发泡剂的多元醇泡沫预混组合物并将所述多元醇泡沫预混组合物喷涂到所述制品上。
3.权利要求2的方法,其中所述施加步骤在所述形成步骤b之后进行。
4.权利要求2的方法,其中所述施加步骤在所述形成步骤b之前进行。
5.权利要求1的方法,其中所述施加步骤包括形成泡沫面板或板材并将所述面板或板材的至少一部分附着到所述制品。
6.权利要求5的方法,其中所述施加步骤在所述形成步骤b之后进行。
7.权利要求5的方法,其中所述施加步骤在所述形成步骤b之前进行。
8.权利要求1的方法,其中所述制品包含所述建筑围护结构的表面或空腔的一部分。
9.权利要求1的方法,其中所述闭孔泡沫在使用Mobil 45º试验测试时表现出小于1.0%重量损失。
10.权利要求1的方法,其中所述闭孔泡沫在使用Mobil 45º试验测试时表现出小于0.5%重量损失。
11.权利要求1的方法,其中大部分所述泡孔含有包含所述反式-1-氯-3,3,3-三氟丙烯的气体。
12.权利要求11的方法,其中所述泡孔中的所述气体是至少70体积%的所述反式-1-氯-3,3,3-三氟丙烯。
13.将聚氨酯或聚异氰脲酸酯泡沫面板或板材施加到建筑围护结构的方法,其包括:
a. 提供包含反式-1-氯-3,3,3-三氟丙烯(1233zd(E))作为发泡剂的可发泡组合物;
b. 将所述可发泡组合物倒入模具中或倒至传送装置上以形成泡沫面板或板材;
c. 固化所述可发泡组合物以形成含有泡孔的闭孔聚氨酯泡沫,所述泡孔中具有气体材料,所述气体材料包含至少50体积%的1233zd(E);和
d. 形成含有所述面板或板材的建筑围护结构。
14.权利要求13的方法,其中所述形成步骤包括将所述面板或板材插入所述建筑围护结构的墙壁、地板或天花板空腔中。
15.权利要求14的方法,其中所述闭孔泡沫在使用Mobil 45º试验测试时表现出小于1.0%重量损失。
16.权利要求14的方法,其中所述闭孔泡沫在使用Mobil 45º试验测试时表现出小于0.5%重量损失。
17.权利要求16的方法,其中所述泡孔中的所述气体是至少70体积%的所述反式-1-氯-3,3,3-三氟丙烯。
18.根据权利要求17的方法制成的住宅、商业建筑、办公楼或水运工具。
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PCT/US2012/048538 WO2013016632A2 (en) | 2011-07-28 | 2012-07-27 | Foams and flame resistant articles made from foams containing 1-chloro-3,3,3-trifluoropropene (1233zd) |
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US20140220333A1 (en) | 2014-08-07 |
KR20140053212A (ko) | 2014-05-07 |
JP2014527553A (ja) | 2014-10-16 |
BR112014002096A2 (pt) | 2017-06-13 |
EP2737006A2 (en) | 2014-06-04 |
AU2012286730A1 (en) | 2014-02-13 |
MX2014000883A (es) | 2014-03-27 |
ES2529170T1 (es) | 2015-02-17 |
MX353653B (es) | 2018-01-23 |
WO2013016632A3 (en) | 2013-04-25 |
JP2017141465A (ja) | 2017-08-17 |
RU2016137830A (ru) | 2018-12-12 |
CN103814108A (zh) | 2014-05-21 |
EP2737006A4 (en) | 2015-11-04 |
CA2843012A1 (en) | 2013-01-31 |
AU2012286730B2 (en) | 2017-04-20 |
WO2013016632A2 (en) | 2013-01-31 |
RU2014106349A (ru) | 2015-09-10 |
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