CN105873993A - 适于制备聚氨酯泡沫且含有至少一种hfo发泡剂的组合物 - Google Patents
适于制备聚氨酯泡沫且含有至少一种hfo发泡剂的组合物 Download PDFInfo
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- CN105873993A CN105873993A CN201480069227.XA CN201480069227A CN105873993A CN 105873993 A CN105873993 A CN 105873993A CN 201480069227 A CN201480069227 A CN 201480069227A CN 105873993 A CN105873993 A CN 105873993A
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- Prior art keywords
- acid
- foam
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- surfactant
- hfo
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Abstract
本发明涉及组合物,其适于制备聚氨酯泡沫并且包含至少一种多元醇组分、至少一种发泡剂、催化氨基甲酸酯或异氰脲酸酯键形成的催化剂、含硅泡沫稳定剂以及任选存在的其它添加剂和任选存在的异氰酸酯组分,其特征在于所述组合物含有至少一种不饱和的卤代烃作为发泡剂以及还含有至少一种不具有硅原子且具有的HLB小于10的表面活性剂TD,其中,所述表面活性剂TD在组合物中的总量所占的比例是0.05‑20质量份(以每100质量份多元醇组分计);还涉及这些多元醇组合物为原料来制备聚氨酯和聚异氰脲酸酯泡沫(特别是硬质泡沫)的方法;泡沫的用途,特别是作为绝热材料;以及绝热材料本身。
Description
技术领域
本发明涉及组合物,其适于制备聚氨酯泡沫并且含有至少一种多元醇组分、至少一种发泡剂、催化氨基甲酸酯或异氰脲酸酯键形成的催化剂、含硅的泡沫稳定剂以及任选存在的其它添加剂和任选存在的异氰酸酯组分,其特征在于它们含有至少一种不饱和的氯氟烃或氟代烃以及另外的至少一种表面活性剂TD,其不具有硅原子,并且具有的HLB小于10,优选小于7,特别优选小于6,其中,表面活性剂TD在组合物中的总量所占的比例是0.05-20质量份(以每100质量份多元醇组分计);还涉及以这些多元醇组合物为原料来制备聚氨酯和聚异氰脲酸酯泡沫(特别是硬质泡沫)的方法;泡沫的用途,特别是作为绝热材料;以及绝热材料本身。
背景技术
目前通过发泡基于聚异氰酸酯、具有反应性氢原子的化合物、发泡剂、稳定剂以及任选存在的其它添加剂的可发泡的反应混合物的聚氨酯或聚异氰脲酸酯泡沫的制备在大工业规模下操作。这些泡沫的用途的重要领域是绝缘,特别是热绝缘。为了制备绝缘泡沫,必须制备具有<50kg/m3的相对低泡沫密度以及作为必要标准的非常大量的小闭孔(高孔密度)的硬质泡沫。
发泡气对于能够形成这种泡沫是必要的。在此,常规发泡剂是烃、(部分)卤代的饱和与不饱和烃以及产生CO2的物质。
除了在发泡期间形成许多小的均匀的闭孔的能力之外,优选的发泡剂还具有低的气相导热性以及低的全球变暖趋势(GWP)。在这种背景下,不饱和的卤代烃,其被称为HFO发泡剂,已经能够被鉴定为特别有效的发泡剂。例如,HFO发泡剂在制备聚氨酯泡沫中的用途在文献EP 2154223 A1、EP 2197 935 B1以及US 2009/0305875 A1中被描述。
尽管不饱和的卤代烃作为发泡剂具有所示效力,这些物质的缺点在于它们往往只能不充分地混溶于待发泡的聚氨酯体系或者用于PU泡沫制备的基本原料。这导致这种类型的混合物仅具有低的存储稳定性,并经常趋于经历相分离成两相或更多相,除其它外,这可导致得到的PU泡沫的缺陷。
在冷却装置(冰箱和直立冰柜或冷冻柜)的绝热材料制备中使用预配制聚氨酯体系时,聚氨酯体系或多元醇混合物的分离稳定性特别重要。在此,习惯上,在发泡之前,将发泡剂与由除了上述发泡剂之外的一种或多种多元醇、一种或多种催化剂、泡沫稳定剂、水、任选存在的阻燃剂以及任选存在的其它添加剂和助剂组成的所谓的A组分进行混合。在发泡期间,将其与所谓的B组分混合并发泡,B组分通常由异氰酸酯(通常是聚合MDI)组成,并且向其中不加入任何添加剂。为了使无故障发泡过程成为可能,A组分必须具有足够的分离稳定性,从而没有不良的分层现象,如上所述,其可能在发泡过程中导致泡沫缺陷的发生。
此外,无故障制备过程可以通过在大规模工业发泡过程中预配制的A组分的足够的存储稳定性得到保证。以这种方式,例如在相对长的设备停工期的情况下,例如维修工作过程中或在周末,可以避免在线系统以及存储容器的分离,这种分离可能在设备重启时,不可避免地导致严重的泡沫缺陷。
因此,本发明的目的是提供含有至少一种多元醇组分、特征在于其是不饱和的卤代烃的至少一种发泡剂、催化氨基甲酸酯或异氰脲酸酯键形成的催化剂以及任选存在的其它添加剂的组合物,其中,组合物的特征在于,在至少三天内,它是分离稳定的(separation-stable)。
为了实现多元醇体系与发泡剂之间的增溶作用,过去已经提出利用多种表面活性剂。
WO 2007/094780描述了含有烃作为发泡剂的多元醇混合物,乙氧基化物-丙氧基化物表面活性剂被添加到混合物中,以改善发泡剂在混合物中的溶解度。
US 6472446描述了含有烃作为发泡剂的多元醇混合物,其中丁醇引发的环氧丙烷聚醚表面活性剂被添加到混合物中,以改善发泡剂在混合物中的溶解度。
类似地,WO 98/42764描述了含有烃作为发泡剂的多元醇混合物,其中C12-C15引发的聚醚作为表面活性剂被添加到混合物,以改善发泡剂在混合物中的溶解度。
类似地,WO 96/12759描述了含有烃作为发泡剂的多元醇混合物,其中,含有具有至少5个碳原子的烷基基团的表面活性剂被添加到混合物,以改善发泡剂在混合物中的溶解度。
EP 0767199 A1描述了天然来源的脂肪酸的二乙醇酰胺在具有烃作为发泡剂的多元醇混合物的制备中作为表面活性剂的用途。
EP 1520873 A2描述了卤代烃发泡剂与具有小于500g/mol的分子量的发泡剂增强剂的混合物,其中发泡剂增强剂可以是聚醚或一元醇,例如乙醇、丙醇、丁醇、己醇、壬醇或癸醇。发泡剂与发泡剂增强剂的比例据称是60-95质量%:40-5质量%。然而,所用的卤代烃不是HFO发泡剂。此外,该文献没有公开所用的发泡剂增强剂是否导致发泡剂在多元醇中的增容作用。
WO 2013/026813描述了多元醇与非极性有机化合物的微乳液,其可以通过使用含有选自非离子表面活性剂、聚合物及其混合物的至少一种两亲性化合物的至少一种无卤化合物以及至少一种不同于这种化合物的化合物而获得,以及它们在聚氨酯制备中的用途。所使用的非极性化合物也可以含有氟代化合物的比例。仅含有卤代非极性化合物的多元醇基微乳液在该文献中没有被描述。
由于卤代烃的溶出特性与非氟代烃存在根本不同,所以不能将为烃类发泡剂提出的添加剂应用于本问题。
已经出乎意料地发现,当具有的HLB小于10、优选小于7、特别优选小于6的表面活性剂被额外添加到混合物中的时候,可以提供由多元醇(一种或多种)、添加剂以及HFO发泡剂所组成的分离稳定的组合物。
HLB通常被用于选择制备油-水乳液的乳化剂。因此,不可能预见到这样的值也适用于选择不是基于水的而是多元醇体系的表面活性剂。在此,表面活性剂的HLB可以通过Griffin(W.C.Griffin,J.Cos.Cosmet.Chem.,1950,311:5,249)以及McGowan(J.C.McGowan,Tenside SurfactantsDetergents,1990,27,229)的增量法来计算。根据该方法,分子的HLB由其分子构建单元(molecular building block)的个体增量构成,按照等式1。
HLB=7+∑Hh+∑Hl (等式1)
Hh与Hl是单个的亲水性和亲脂性分子构建单元的HLB基团数。Hh与Hl的典型值被列于表1中。
表1、多种分子构建单元的HLB基团数(参见R.Sowada and J.C.McGowan,TensideSurfactants Detergents,1992,29,109中的表3)
发明内容
因此,本发明提供了组合物,其适于制备聚氨酯泡沫,并且含有至少一种多元醇组分、至少一种发泡剂、催化氨基甲酸酯或异氰脲酸酯键形成的催化剂、含硅的泡沫稳定剂以及任选存在的其它添加剂和任选存在的异氰酸酯组分,其特征在于它们含有至少一种不饱和的氯氟烃或不饱和的氟代烃作为发泡剂,以及额外的至少一种表面活性剂TD,所述表面活性剂TD不具有硅原子,并且具有的HLB小于10,优选小于7,特别优选小于6,其中,基于总组合物,表面活性剂TD在组合物中的浓度是0.05-20重量%。
类似地,本发明提供了以这些多元醇组合物作为原料制备聚氨酯或聚异氰脲酸酯泡沫(特别是硬质泡沫)的方法;泡沫的用途,特别是作为绝热材料;以及绝热材料本身。
本发明还提供了在上述方法基础上制备的聚氨酯泡沫。
本发明的组合物具有较大量的HFO发泡剂可以被引入到组合物中且组合物甚至在72小时的存储时间之后也不显示肉眼可察觉的相分离的优点。
本发明的组合物的其它优点在于,具有高硅酮含量的泡沫稳定剂也可以在它们中被使用而不发生混合物的相分离,尽管这样的泡沫稳定剂对多元醇与发泡剂的相容性具有不利影响。
具体实施方式
通过举例的方式在下文中描述本发明的主题,并无将本发明限制于这些说明性实施方案的任何意图。在下文中,在指定范围、通式或化合物类别时,这些应当不仅包括明确提及的相应的范围或化合物的组,还包括可以通过除去单个值(范围)或者化合物而得到的所有子范围以及化合物的亚组。当文献在本说明书的上下文中被引用时,其内容(特别是关于文献被引用的内容的主题内容)的整体被视为组成本发明公开内容的部分。除非另行说明,百分比都是重量百分数。如果平均值在下文中被给出,涉及的值是重量平均值,除非另行说明。当在下文中给出已经由测量确定的参数的时候,它们已经在25℃的温度和101 325Pa的压力下被确定,除非另行说明。
对于本发明的目的,聚氨酯泡沫(PU泡沫)是作为基于异氰酸酯与多元醇或具有异氰酸酯反应基团的化合物的反应产物而得到的泡沫。除了给出聚氨酯名称的基团之外,还可以形成其它官能团,例如脲基甲酸酯、缩二脲、脲或异氰脲酸酯。因此,对于本发明的目的,术语PU泡沫既指聚氨酯泡沫(PUR泡沫),又指聚异氰脲酸酯泡沫(PIR泡沫)。优选的聚氨酯泡沫是硬质聚氨酯泡沫。
对于本专利申请应用的目的,不饱和的卤代烃也可以被称为HFO。卤代烃可以具有一个或多个相同或不同的卤素。基于不饱和卤代烃的发泡剂相应地被称为HFO发泡剂。
本发明的组合物,其适于制备聚氨酯泡沫并且含有至少一种多元醇组分、至少一种发泡剂、催化氨基甲酸酯或异氰脲酸酯键形成的催化剂、含硅的泡沫稳定剂以及任选存在的其它添加剂和任选存在的异氰酸酯组分,特征在于它含有至少一种不饱和卤代烃作为发泡剂,优选不饱和的氯氟烃和/或不饱和的氟代烃,以及额外的至少一种表面活性剂TD,其不具有硅原子,并且具有的HLB小于10,优选小于7,特别优选小于6,其中,相对于每100质量份多元醇组分,表面活性剂TD在组合物中的总量所占的比例是0.05-20质量份。
相对于每100质量份多元醇组分,本发明的组合物优选包含0.1-15质量份、更优选0.5-10质量份的表面活性剂TD。
作为表面活性剂TD,本发明的组合物优选包含至少一种式(I)的化合物:
R-[C(O)]x-Y (I)
其中,x=0或1,优选0,R是线性、枝化或环状的,饱和或不饱和的(优选饱和的)具有至少4个、优选8-30、更优选9-20、特别优选9-18个碳原子的烃基基团,并且Y=O-R1或NR1R2或O-CH2-CH(OR3)-CH2OH,其中R1和R2在每种情况下是相同或不同的基团(CnH2nO)m-H,其中n=2-4,优选n=2或3,特别优选n=2,并且m=0-15,优选m=0或1-10,特别优选m=0或1-6,非常特别优选m=0,并且R1和R2可以是相同的或不同的,并且R3=H或R'或C(O)R',其中R'是类似于R的定义的烃基基团,并且可以与R基团相同或不同。
特别优选的表面活性剂TD是这些:其具有至少一个烃基基团具有至少4个碳原子、优选至少8个碳原子、尤其优选9-18个碳原子,并且具有的HLB小于10、优选小于7,特别优选小于6。
当本发明的组合物包含其中x=0且Y=O-R1的式(I)的表面活性剂TD时,则组合物优选含有基于辛醇(octanol)、壬醇、异壬醇、辛醇(caprylalcohol)、癸醇、月桂醇、十三烷醇、异十三烷醇、肉豆蔻醇、鲸蜡醇、硬脂醇或异硬脂醇的醇烷氧基化物,特别优选这些物质的乙氧基化物,作为表面活性剂TD。相应的脂肪醇烷氧基化物的制备可以如现有技术中所描述的进行。
当本发明的组合物包含其中x=0且Y=O-R1且m=0的式(I)的表面活性剂TD时,则该组合物优选含有辛醇(octanol)、壬醇,特别是异壬醇、辛醇(capryl alcohol)、月桂醇、十三烷醇、异十三烷醇、肉豆蔻醇、鲸蜡醇、硬脂醇、异硬脂醇、十三烷醇、癸醇、十二烷醇或这些物质的混合物,优选异十三烷醇和/或(优选)异壬醇(3,5,5-三甲基-1-壬醇),作为表面活性剂TD。其中x=0且Y=O-R1的式(I)的表面活性剂TD优选是其中m=0的那些。
当本发明的组合物包含其中x=0且Y=NR1R2且m=0的式(I)的表面活性剂TD时,则该组合物含有脂肪胺,优选辛胺(octylamine)、壬胺、异壬胺、辛胺(capryl amine)、月桂胺、十三胺、异十三胺、肉豆蔻胺、十六胺(cetylamine)、硬脂酰胺或异硬脂酰胺作为表面活性剂TD。在m和n不是0的情况下,表面活性剂TD特别优选是这些胺的乙氧基化物。
当本发明的组合物包含其中x=0且Y=O-CH2-CH(OR3)-CH2OH的式(I)的表面活性剂TD时,则特别优选饱和的或不饱和醇的甘油单醚和二醚,所述醇例如辛醇(octanol)、壬醇、异壬醇、辛醇(capryl alcohol)、月桂醇、十三烷醇、异十三烷醇、肉豆蔻醇、鲸蜡醇、硬脂醇或异硬脂醇。
当本发明的组合物包含其中x=1且Y=O-R1的式(I)的表面活性剂TD时,则该组合物优选含有具有不多于30个碳原子的饱和或不饱和脂肪酸的烷氧基化物,特别优选乙氧基化物,作为表面活性剂TD,所述饱和或不饱和脂肪酸例如丁酸(butyric acid;butanoic acid)、己酸(caproic acid;hexanoicacid)、辛酸(caprylic acid;octanoic acid)、癸酸(capric acid;decanoic acid)、月桂酸(十二烷酸)、肉豆蔻酸(十四烷酸)、棕榈酸(十六烷酸)、硬脂酸(十八烷酸)、花生酸(二十烷酸)、山嵛酸(二十二烷酸)、木蜡酸(二十四烷酸)、棕榈油酸((Z)-9-十六碳烯酸)、油酸((Z)-9-十八碳烯酸)、反油酸((E)-9-十八碳烯酸)、顺-异油酸((Z)-11-十八碳烯酸)、亚油酸((9Z,12Z)-9,12-十八碳二烯酸)、α-亚麻酸((9Z,12Z,15Z)-9,12,15-十八碳三烯酸)、γ-亚麻酸((6Z,9Z,12Z)-6,9,12-十八碳三烯酸)、二-均-γ-亚麻酸((8Z,11Z,14Z)-8,11,14-二十碳三烯酸)、花生四烯酸((5Z,8Z,11Z,14Z)-5,8,11,14-二十碳四烯酸)、芥酸((Z)-13-二十二碳烯酸)、神经酸((Z)-15-二十四碳烯酸)、蓖麻油酸、羟基硬脂酸以及十一碳烯酸(undecenyloic acid)及它们的混合物。
当本发明的组合物包含其中x=1且Y=O-CH2-CH(OR3)-CH2OH的式(I)的表面活性剂TD时,则该组合物优选含有甘油单酯和甘油二酯,尤其是具有不多于30个碳原子的直链饱和或不饱和脂肪酸的甘油单酯或甘油二酯作为表面活性剂TD,所述饱和或不饱和的脂肪酸例如丁酸(butyric acid;butanoic acid)、己酸(caproic acid;hexanoic acid)、辛酸(caprylic acid;octanoicacid)、癸酸(capric acid;decanoic acid)、月桂酸(十二烷酸)、肉豆蔻酸(十四烷酸)、棕榈酸(十六烷酸)、硬脂酸(十八烷酸)、花生酸(二十烷酸)、山嵛酸(二十二烷酸)、木蜡酸(二十四烷酸)、棕榈油酸((Z)-9-十六碳烯酸)、油酸((Z)-9-十八碳烯酸)、反油酸((E)-9-十八碳烯酸)、顺-异油酸((Z)-11-十八碳烯酸)、亚油酸((9Z,12Z)-9,12-十八碳二烯酸)、α-亚麻酸((9Z,12Z,15Z)-9,12,15-十八碳三烯酸)、γ-亚麻酸((6Z,9Z,12Z)-6,9,12-十八碳三烯酸)、二-均-γ-亚麻酸((8Z,11Z,14Z)-8,11,14-二十碳三烯酸)、花生四烯酸((5Z,8Z,11Z,14Z)-5,8,11,14-二十碳四烯酸)、芥酸((Z)-13-二十二碳烯酸)、神经酸((Z)-15-二十四碳烯酸)、蓖麻油酸、羟基硬脂酸以及十一碳烯酸(undecenyloic acid)及它们的混合物。
当本发明的组合物包含其中x=1且其中Y=NR1R2的式(I)的表面活性剂TD时,则该组合物优选包含单烷醇胺或二烷醇胺(特别优选二异丙醇胺或二乙醇胺)的脂肪酸酰胺作为表面活性剂TD。酰胺(acid amide)可以通过例如,现有技术中例如在DE 1802500、DE 1802503、DE 1745443、DE 1745459或US 3578612中的已知的方法获得。在此例如,相应的羧酸可以被用作原料,并且酰胺形成通过脱水发生。羧酸酯,例如甲基酯,可以类似地被使用,在这种情况下,甲醇被分离。特别优选的是使用天然存在的脂肪和油的甘油酯,在酰胺化中形成的甘油能够保留在反应混合物中。类似地,例如在甘油三酯与胺的反应中,当已经适当地选择反应条件时,甘油二酯和甘油单酯可以存在于反应混合物中。当使用羧酸酯时,任选地使用合适的催化剂,例如醇盐,其允许相对于上述脱水更温和的条件下的酰胺化。当更高官能的胺(DETA、AEEA、TRIS)被使用时,在酰胺的制备中也可以发生相应的环状酰胺的形成,例如咪唑啉或噁唑啉。
如果碱性催化剂被用于酰胺化中,事后使用适量的有机或无机酸进行中和可以是有利的。合适的化合物是本领域技术人员已知的。
特别优选的是由碱性催化制得的酰胺用二羧酸的有机酐中和,因为这些可以与可用的OH或NH官能团反应,并由此结合,因此在成品泡沫中不会以游离羧酸的形式作为排放物出现。此外,例如,当碱醇盐在中和中被使用时,然后形成相应的酯,从而使得游离醇不会从系统中释放出来。
优选的有机酐是环状酸酐如琥珀酸酐、马来酸酐,烷基琥珀酸酐如十二烷基琥珀酸酐或聚异丁烯琥珀酸酐,马来酸酐与诸如聚丁二烯的合适的聚烯烃的加成物,马来酸酐与烯烃的共聚物,苯乙烯-马来酸酐共聚物,乙烯基醚-马来酸酐共聚物以及含有马来酸酐作为单体的一般共聚物,邻苯二甲酸酐,二苯甲酮四羧酸二酐,均苯四甲酸二酐,衣康酸酐或类似的结构同样适合。这种类型的可商购的酸酐的实例是Evonik Degussa GmbH的等级或Sartomer的等级。
所有反应步骤可以整体或在合适的溶剂中进行。当使用溶剂时,基于总组合物,“活性物质”的含量可以在10-99质量%、优选20-98质量%、特别优选30-97质量%的范围内。
羧酸:
用于制备其中x=1的式(I)的表面活性剂时,有用的羧酸是:例如基于脂族烃或芳族烃及其衍生物的单羧酸、二羧酸、三羧酸、四羧酸。
单羧酸的烷基基团的实例是,例如:甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基或癸基等,优选2-乙基己酸、壬酸、异壬酸。
烯基基团的实例是,例如乙烯基、丙烯基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基等。
芳族酸的实例是,例如:芳基和烷芳基(对于本目的,烷芳基是芳基取代的烷基或烷芳基基团),例如:苯基、烷基取代的苯基、萘基、烷基取代的萘基、甲苯基、苄基、二甲基苯基、三甲基苯基、苯乙基、苯丙基、苯丁基、丙基-2-苯乙基、水杨酸基等。
芳族二羧酸可以是,例如:间苯二甲酸、对苯二甲酸或邻苯二甲酸。作为脂肪族二羧酸,例如可以使用:琥珀酸、丙二酸、己二酸、十二烷二羧酸、马来酸、富马酸、衣康酸、柠康酸、中康酸、酒石酸、马来酸、丙二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、柠檬酸。
作为更高官能的酸,例如可以使用:均苯三酸、苯均四酸或二苯甲酮四羧酸。
优选的酸是具有不多于40个碳原子的直链饱和或不饱和脂肪酸,例如:丁酸(butyric acid;butanoic acid)、己酸(caproic acid;hexanoic acid)、辛酸(caprylic acid;octanoic acid)、癸酸(capric acid;decanoic acid)、月桂酸(十二烷酸)、肉豆蔻酸(十四烷酸)、棕榈酸(十六烷酸)、硬脂酸(十八烷酸)、花生酸(二十烷酸)、山嵛酸(二十二烷酸)、木蜡酸(二十四烷酸)、棕榈油酸((Z)-9-十六碳烯酸)、油酸((Z)-9-十八碳烯酸)、反油酸((E)-9-十八碳烯酸)、顺-异油酸((Z)-11-十八碳烯酸)、亚油酸((9Z,12Z)-9,12-十八碳二烯酸)、α-亚麻酸((9Z,12Z,15Z)-9,12,15-十八碳三烯酸)、γ-亚麻酸((6Z,9Z,12Z)-6,9,12-十八碳三烯酸)、二-均-γ-亚麻酸((8Z,11Z,14Z)-8,11,14-二十碳三烯酸)、花生四烯酸((5Z,8Z,11Z,14Z)-5,8,11,14-二十碳四烯酸)、芥酸((Z)-13-二十二碳烯酸)、神经酸((Z)-15-二十四碳烯酸)、蓖麻油酸、羟基硬脂酸以及十一碳烯酸(undecenyloic acid)及其混合物,例如菜籽油酸、大豆脂肪酸、向日葵脂肪酸、花生脂肪酸和妥尔油脂肪酸。也可能使用如在不饱和脂肪酸的低聚中形成的二聚和低聚脂肪酸。
合适的脂肪酸或脂肪酸酯(特别是甘油酯)的来源可以是植物或动物脂肪、油或蜡。例如,有可能使用:猪油、牛油、鹅脂、鸭肪、鸡脂、马脂、鲸油、鱼油、棕榈油、橄榄油、鳄梨油、种子油、椰子油、棕榈仁油、可可脂、棉籽油、南瓜子油、玉米油、葵花籽油、小麦胚芽油、葡萄籽油、芝麻油、亚麻籽油、大豆油、花生油、羽扇豆油、菜籽油、芥子油、蓖麻油、麻风果油、核桃油、霍霍巴油、卵磷脂(例如基于大豆、油菜籽或向日葵)、骨油、牛脚油(cattlefoot oil)、羊毛脂、鸸鹋油、鹿脂、旱獭油、貂油、琉璃苣油(borrage oil)、红花油、大麻油、南瓜油、月见草油、妥尔油以及巴西棕榈蜡、蜂蜡、小烛树蜡、小冠椰子蜡(Ouricuri wax)、甘蔗蜡、Retamo蜡、棕榈蜡(Caranday wax)、酒椰蜡、西班牙草蜡、苜蓿蜡、竹蜡、大麻蜡、花旗松蜡、软木蜡、剑麻蜡、亚麻蜡、棉蜡、达玛蜡、茶蜡、咖啡蜡、米糠蜡、夹竹桃蜡、蜂蜡或羊毛蜡。
胺:
具有至少一个OH官能且适于制备x=1的式(I)的化合物的羟胺是例如:二乙醇胺、单乙醇胺、二异丙醇胺、异丙醇胺、二甘醇胺(2-(2-氨基乙氧基)乙醇)、3-氨基-1-丙醇以及聚醚胺,例如来自Huntsman的Polyetheramin D2000(BASF)、Polyetheramin D 230(BASF)、Polyetheramin T 403(BASF)、Polyetheramin T 5000(BASF)或者相应的Jeffamine等级。
x=1的式(I)的根据本发明的化合物也可以是具有OH或NH官能的市售酰胺,例如购自Evonik Goldschmidt的DC 212S、DO280 SE、DU 185 SE、KSM、C 212、IPP 240、SPA、IM AO、IMAN或IM R 40,以及Stepan的154、1301、40-CO、1281、COMF、M-10以及乙氧基化的二乙醇酰胺,例如C-4l、C-5或1301或者购自Sasol的MAL和DC。特别地,优选的酰胺是椰油酰胺DEA(Cocoamid DEA)。
在本发明的优选实施方案中,酰胺化是利用胺的亚化学计量的量来进行的,从而很少或没有游离胺存在于最终产品内。因为由于它们的刺激性或腐蚀作用,胺通常具有不利的毒理学性质,胺含量最小化是期望的且有利的。基于胺和酰胺的总和,根据本发明在混合物中胺使用的比例,特别是带有伯胺与仲胺基团的化合物的比例优选小于5重量%,特别优选小于3重量%,特别小于1重量%。
作为在本发明的组合物中的表面活性剂TD,特别优选的是其中x=0且Y=NR1R2或Y=O-R1且m=0的式(I)的那些,R1和R2如上所述,非常特别优选Cocoamid DEA、异十三烷醇或异壬醇。
本发明的组合物含有一种或多种多元醇。优选地,多元醇组分不同于存在于组合物中的表面活性剂TD。适用于本发明目的的多元醇是具有多个异氰酸酯反应性基团的所有有机物质以及它们的配制物。优选的多元醇是通常用于制备聚氨酯泡沫的所有聚醚多元醇和聚酯多元醇。聚醚多元醇是通过多官能醇或胺与烯烃氧化物反应而获得的。聚酯多元醇是基于多元羧酸(通常是邻苯二甲酸或对苯二甲酸)与多元醇(通常是乙二醇)的酯。泡沫所要求的属性决定了适当的多元醇的使用,正如例如在US 2007/0072951 A1、WO 2007/111828 A2、US 2007/0238800、US 6359022 B1或WO 96 12759 A2中所述。优选的基于植物油的多元醇同样地在多种专利文献中得以描述,例如WO 2006/094227、WO 2004/096882、US 2002/0103091、WO2006/116456以及EP 1 678 232。
本发明的组合物优选含有至少一种物理发泡剂,即基于不饱和的卤代烃(优选不饱和的氟代烃和/或氯氟烃)的挥发性(沸点小于100℃,优选小于70℃)的液体或气体。优选的不饱和的卤代烃是反-1,3,3,3-四氟-1-丙烯(HFO-1234zeE)、2,3,3,3-四氟-1-丙烯(HFO-1234yf)、顺-1,1,1,4,4,4-六氟-2-丁烯(HFO-1336mzzZ)、反-1,1,1,4,4,4-六氟-2-丁烯(HFO-1336mzzE)和反-1-氯-3,3,3-三氟-1-丙烯(HFO-1233zd-E)。HFO发泡剂可以任选地与其它物理共发泡剂组合,其中这些优选不是烃。例如,优选的共发泡剂是饱和或不饱和氟代烃,特别优选1,1,1,2-四氟乙烷(HFC-134a)、1,1,1,3,3-五氟丙烷(HFC-245fa)、1,1,1,3,3-五氟丁烷(HFC-365mfc)、1,1,1,2,3,3,3-七氟丙烷(HFC-227ea)、1,1-二氟乙烷(HFC-152a);饱和氯氟烃,特别优选1,1-二氯-1-氟乙烷(HCFC-141b);含氧化合物,特别优选甲酸甲酯或二甲氧基甲烷或氯代烃,特别优选1,2-二氯乙烷,或这些发泡剂的混合物。
特别优选的本发明的组合物不具有任何例如正戊烷、异戊烷或环戊烷的烃作为物理发泡剂。
物理发泡剂的优选量完全取决于将要制备的泡沫的期望密度,并且,基于100质量份的多元醇,通常在5-40质量份的范围内。
除了物理发泡剂之外,也可以存在与异氰酸酯反应而逐渐形成气体的化学发泡剂,例如水或甲酸。
作为泡沫稳定剂,本发明的组合物含有至少一种含硅的泡沫稳定剂,其不同于表面活性剂TD。优选的含硅的泡沫稳定剂是有机聚醚硅氧烷,例如聚醚-聚二甲基硅氧烷共聚物。使用的含硅的泡沫稳定剂的典型用量是,每100质量份的多元醇,0.5-5质量份,优选每100质量份的多元醇,1-3质量份。合适的含硅的泡沫稳定剂被描述于例如EP 1873209、EP 1544235、DE 10 2004 001 408、EP 0839852、WO 2005/118668、US 20070072951、DE2533074、EP 1537159、EP 533202、US 3933695、EP 0780414、DE 4239054、DE 4229402和EP 867464中,并且被例如Evonik Industries以商品名销售。硅氧烷的制备可以如现有技术中所描述的进行。制备的特别合适的实例例如在US 4,147,847、EP 0493836和US 4,855,379中被描述。
此外,本发明的组合物可以含有其它组分,例如其它泡沫稳定剂、催化剂、交联剂、阻燃剂、填料、染料、抗氧化剂和增稠剂/流变添加剂。这些额外的组分优选不是表面活性TD,并且与这些不同。
作为催化氨基甲酸酯或异氰脲酸酯键形成的催化剂,本发明的组合物优选地包含适于异氰酸酯-多元醇和/或异氰酸酯-水和/或异氰酸酯三聚的反应的一种或多种催化剂。对于本发明目的合适的催化剂优选是催化胶凝反应(异氰酸酯-多元醇)、发泡反应(异氰酸酯-水)和/或异氰酸酯的二聚或三聚的催化剂。合适的催化剂的典型实例是胺:三乙胺、二甲基环己胺、四甲基乙二胺、四甲基己二胺、五甲基二亚乙基三胺、五甲基二亚丙基三胺、三亚乙基二胺、二甲基哌嗪、1,2-二甲基咪唑、N-乙基吗啉、三(二甲氨基丙基)六氢-1,3,5-三嗪、二甲氨基乙醇、二甲基氨基乙氧基乙醇以及双(二甲基氨基乙基)醚;锡化合物,例如二月桂酸二丁基锡;以及钾盐,例如乙酸钾和2-乙基己酸钾。合适的催化剂在例如EP 1985642、EP 1985644、EP1977825、US 2008/0234402、EP 0656382 B1、US 2007/0282026 A1以及其中所引用的专利文献中被提及。
存在于本发明的组合物中的催化剂的优选量取决于催化剂的种类,其通常在0.05-5pphp(=基于100质量份的多元醇的质量份)的范围内,或在钾盐的情况下的0.1-10pphp的范围内。
作为阻燃剂,本发明的组合物可以包含适于制备聚氨酯泡沫的所有已知的阻燃剂。对于本发明目的合适的阻燃剂优选是液体有机磷化合物,例如无卤素有机磷酸盐,例如磷酸三乙酯(TEP);卤代磷酸酯,例如三(1-氯-2-丙基)磷酸酯(TCPP)与三(2-氯乙基)磷酸酯(TCEP);以及有机膦酸盐,例如二甲基膦酸甲酯(DMMP)、二甲基膦酸丙酯(DMPP);或固体,例如多磷酸铵(APP)和红磷。此外,卤代化合物,例如卤代多元醇,以及固体,例如可膨胀石墨与三聚氰胺适合作为阻燃剂。
从现有技术已知的其它组分,例如聚醚、壬基苯酚乙氧基化物或非离子表面活性剂,其均非根据表面活性剂TD定义的表面活性剂,可以任选地作为其它添加剂存在于组合物中。
例如,本发明的组合物可以被用于制备聚氨酯泡沫,特别是硬质聚氨酯泡沫。特别地,本发明的组合物可以被用于根据本发明的制备聚氨酯或聚异氰脲酸酯泡沫(聚氨酯泡沫)的方法中,特别是用于制备硬质聚氨酯泡沫,其特征在于,根据本发明的组合物进行反应。为此目的,根据本发明的含有异氰酸酯组分的组合物或者异氰酸酯组分已经被添加到其中的本发明的组合物之一进行反应,特别是被发泡。
作为异氰酸酯组分,可以使用适于制备聚氨酯泡沫(特别是硬质聚氨酯或聚异氰脲酸酯泡沫)的所有异氰酸酯化合物。异氰酸酯组分优选包含具有两个或更多异氰酸酯官能的一种或多种有机异氰酸酯。对于本发明的目的,合适的异氰酸酯包括例如任何多官能有机异氰酸酯,例如4,4'-二苯基甲烷二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI)、六亚甲基二异氰酸酯(HMDI)以及异佛尔酮二异氰酸酯(IPDI)。MDI与具有2-4的平均官能度的被称为“聚合MDI”(“粗MDI”)的更高度缩合的类似物的混合物是特别合适的。合适的异氰酸酯的实例在EP 1 712 578 A1、EP 1 161 474、WO 058383 A1、US 2007/0072951 A1、EP 1 678 232 A2以及WO 2005/085310中被提及。
异氰酸酯与多元醇的比例,其表示为指数,优选在40-500的范围内,优选100-350。所述指数描述实际使用的异氰酸酯与计算的异氰酸酯的比率(对于与多元醇的化学计量反应)。指数100代表反应性基团的摩尔比是1:1。
本发明的用于制备聚氨酯泡沫、特别是硬质聚氨酯泡沫的方法,可以通过公知的方法来进行,例如通过手工混合或优选地通过发泡机。如果该方法是由发泡机来进行的,可以使用高压或低压的机器。本发明的方法可以分批进行或者连续进行。
现有技术的总结、可以使用的原料或者可以使用的方法可以在“Ullmann's Encyclopedia of Industrial Chemistry"Vol.A21,VCH,Weinheim,第四版,1992,pp.665 to 715”中找到。
本发明的组合物在制备硬质聚氨酯泡沫中的使用使得有可能获得本发明的聚氨酯泡沫。
根据本发明的优选的硬质聚氨酯或聚异氰脲酸酯泡沫配制物将产生20-150kg/m3的泡沫密度,并且优选具有表2中所示的组成。
表2:硬质聚氨酯或聚异氰脲酸酯配制物的组成
根据本发明的聚氨酯泡沫,特别是硬质聚氨酯泡沫,特征还在于它们是可以通过本发明的方法获得的。
根据本发明的优选的聚氨酯泡沫,特别是硬质聚氨酯泡沫,其已经使用本发明的组合物制得,具有的在23℃下的新鲜(即在室温下固化24h)状态下测定的热传导率小于21mW/m·K,优选小于20mW/m·K(由购自Hesto的2-板热传导率测量仪“Lambda Control”确定)。
根据本发明的聚氨酯泡沫(聚氨酯或聚异氰脲酸酯泡沫),特别是硬质聚氨酯泡沫,可以被用作或用于制备绝热材料,优选绝热板、冰箱、绝热泡沫或喷雾泡沫。
根据本发明的冷却装置的特征在于:它们具有根据本发明的聚氨酯泡沫(聚氨酯或聚异氰脲酸酯泡沫),特别是硬质聚氨酯泡沫,作为隔热材料。
下文列出的实施例通过示例的方式说明本发明,而没有将本发明限制于实施例中指定的实施方案的任何意图,其应用的范围通过说明书与权利要求书的整体而显而易见。
实施例:
比较例1:
为了提供可发泡的A组分,72.0重量份(pbw)多元醇A(含有脂肪族聚醚多元醇与MDA引发的聚醚多元醇,2.3重量份水以及胺催化剂DMCHA与PMDETA的混合物)与24.5份HFO发泡剂反-1-氯-3,3,3-三氟-1-丙烯(HFO-1233zd-E)混合,能够以商品名Solsitce LBA(Honeywell)获得。此外,4份不同的聚醚硅氧烷类泡沫稳定剂(可从Evonik Industries AG获得的BXXXX等级)与所述混合物混合。该混合物的精确组成示于表3中。
表3:基于多元醇A与HFO发泡剂1233zd的可发泡的A组分的组成
通过手工搅拌匀浆后,在所有样品中观察到显著混浊。此外,样品的宏观相分离可以在几天后被观察到。
根据本发明的实施例1:
为了使比较例1中描述的A组分相容,异十三烷醇(BASF SE)或EvonikIndustries AG的Cocoamid DEA(二乙醇胺)DC212 S额外地作为表面活性剂被混合到样品中。所得混合物的精确组成示于表4中。均质化之后,在每种情况下获得清澈的、光学各向同性的样品,其即使在长时间存储之后也不显示相分离。
表4:基于多元醇A和HFO发泡剂1233zd-E的含表面活性剂的可发泡的A组分的组成
比较例2:
为了提供可发泡的A组分,将74.0重量份(pbw)多元醇B(含有脂肪族聚醚多元醇与基于邻苯二甲酸酐的聚酯多元醇、2.4重量份水与胺催化剂DMCHA和PMDETA的混合物)与24.0份HFO发泡剂SolsitceLBA(Honeywell)混合。此外,3份基于聚醚硅氧烷的泡沫稳定剂被混入该混合物。该混合物的精确组成示于表5中。
表5:基于多元醇B和HFO发泡剂1233zd的可发泡的A组分的组成
均质化后,在所有样品中发现了显著的浑浊。此外,样品的宏观相分离可以在几天后被观察到。
根据本发明的实施例2:
为了使比较例2中所描述的A组分相容,异十三烷醇或CocoamidDEA(二乙醇胺)作为表面活性剂TD被额外混合进样品。所得混合物的精确组成示于表6中。
表6:基于多元醇A和HFO发泡剂1233zd的含表面活性剂的可发泡的A组分的组成
均质化后,在所有情况下,得到清澈的、光学各向同性的即使在长存储时间之后也不显示相分离的样品。
Claims (11)
1.组合物,其适于制备聚氨酯泡沫,并且包含至少一种多元醇组分、至少一种发泡剂、催化氨基甲酸酯或异氰脲酸酯键形成的催化剂、含硅的泡沫稳定剂以及任选存在的其它添加剂和任选存在的异氰酸酯组分,其特征在于其含有至少一种不饱和的卤代烃作为发泡剂以及至少一种不具有硅原子且具有的HLB小于10的表面活性剂TD,其中,所述表面活性剂TD的总量在组合物中所占的比例是0.05-20质量份,以每100质量份多元醇组分计。
2.如权利要求1所述的组合物,其特征在于它含有至少一种式(I)的化合物作为表面活性剂TD:
R-[C(O)]x-Y (I)
其中,x=0或1,R是线性、枝化或环状的饱和或不饱和的具有至少4个、优选8-30、更优选9-20、特别优选9-18个碳原子的烃基基团,并且Y=O-R1或NR1R2或O-CH2-CH(OR3)-CH2OH,其中R1和R2在每种情况下是相同或不同的基团(CnH2nO)m-H,其中n=2-4,优选n=2-3,特别优选n=2,并且m=0-15,优选m=0或1-10,特别优选m=0或1-6,非常特别优选m=0,并且R3=H或R'或C(O)R',其中R'是如R所定义的烃基基团,并且可以与R基团相同或不同。
3.如权利要求1或2所述的组合物,其特征在于,所述表面活性剂TD具有至少一个含至少4个碳原子的烃基基团,并且具有小于10的HLB。
4.如权利要求1-3中任一项所述的组合物,其特征在于,所述表面活性剂TD具有小于6的HLB。
5.如权利要求1-4中任一项所述的组合物,其特征在于它含有椰油酰胺DEA、异十三烷醇或异壬醇作为表面活性剂TD。
6.如权利要求1-5中任一项所述的组合物,其特征在于选自反-1,3,3,3-四氟-1-丙烯(HFO-1234zeE)、2,3,3,3-四氟-1-丙烯(HFO-1234yf)、顺-1,1,1,4,4,4-六氟-2-丁烯(HFO-1336mzzZ)、反-1,1,1,4,4,4-六氟-2-丁烯(HFO-1336mzzE)和反-1-氯-3,3,3-三氟-1-丙烯(HFO-1233zd-E)的至少一种化合物作为不饱和的卤代烃存在。
7.如权利要求1-6中任一项所述的组合物,其特征在于其包含至少一种异氰酸酯组分。
8.通过如权利要求1-7中任一项所述的组合物的反应来制备聚氨酯或聚异氰脲酸酯泡沫(聚氨酯泡沫)的方法。
9.通过如权利要求8所述的方法可以获得的聚氨酯泡沫。
10.如权利要求9所述的聚氨酯泡沫被用作或用于制备绝热材料的用途,优选绝热板、冰箱、绝热泡沫、车辆座椅,特别是汽车座椅、车顶衬里、床垫、过滤器泡沫、包装泡沫或喷雾泡沫。
11.冷却装置,其包含如权利要求9所述的聚氨酯泡沫作为绝热材料。
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BR112016014329A2 (pt) | 2018-05-22 |
US10023679B2 (en) | 2018-07-17 |
DE102013226575A1 (de) | 2015-06-25 |
US20160311961A1 (en) | 2016-10-27 |
JP6513090B2 (ja) | 2019-05-15 |
CN105873993B (zh) | 2019-07-09 |
KR102254280B1 (ko) | 2021-05-21 |
DE102013226575B4 (de) | 2021-06-24 |
KR20160101963A (ko) | 2016-08-26 |
EP3083786A1 (de) | 2016-10-26 |
WO2015091021A1 (de) | 2015-06-25 |
MX2016008097A (es) | 2016-09-16 |
JP2017504678A (ja) | 2017-02-09 |
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