CN102405245B - 具有改善的固化性能和防火特性的聚氨酯和多异氰脲酸酯泡沫体 - Google Patents
具有改善的固化性能和防火特性的聚氨酯和多异氰脲酸酯泡沫体 Download PDFInfo
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- CN102405245B CN102405245B CN201080017420.0A CN201080017420A CN102405245B CN 102405245 B CN102405245 B CN 102405245B CN 201080017420 A CN201080017420 A CN 201080017420A CN 102405245 B CN102405245 B CN 102405245B
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Abstract
制备低至中等指数(1至2.5)的聚氨酯或多异氰脲酸酯泡沫体的制剂，包括20至60重量％的配制的多元醇，其包含官能度大于或等于2且羟值大于约50mg KOH/g的芳族聚酯多元醇；10至30重量％的线形酚醛清漆型多元醇；和5至40重量％的羟值大于约200mg KOH/g且官能度为至少约4的蔗糖-或山梨醇-引发的聚醚多元醇。该泡沫体可显示改善的加工性，导致，例如，夹层板减少的收缩和变形，和改善的防火特性，根据德国标准DIN4102测试。
Description
背景
技术领域
本发明涉及聚氨酯和多异氰脲酸酯泡沫体。更具体地，其涉及这种从芳族聚酯多元醇制备的泡沫体，其在一系列厚度显示改善的加工性，且显示改善的防火特性(fire behavior)。
背景技术
聚氨酯和多异氰脲酸酯泡沫体在建筑工业中广泛用作绝缘材料。通常这些泡沫体是闭孔的坚硬泡沫体，其在孔中包含低传导性气体，如烃(HC)。该发泡组合物为液体，其可用于原位倒入的应用；喷雾应用；和形成硬质泡沫体板。所述板可通过连续或不连续工艺技术制备，其可包括贴面，如金属箔，泡沫体粘附至该贴面。这些板可称为夹层板(sandwich panels)。
遗憾的是，这些泡沫体通常由聚酯多元醇和亚甲基二苯基二异氰酸酯(MDI)以MDI/多元醇的比例超过150形成，其可能具有缺点。一个常见的问题为该泡沫体可具有差的固化性能，导致缺陷如收缩和变形。随着官方测试需求变得更加严格，另一问题可涉及防火特性。更严格的要求的一个实例为新的Euroclasses规则，如EN13823。
对于许多聚氨酯和多异氰脲酸酯泡沫体，使用的聚酯多元醇为基于芳族的结构。尽管这些泡沫体具有许多用途，已发现掺入至少一些脂族聚酯多元醇可提供益处。例如，US 2006/0047011A1公开了脂族聚酯多元醇制备的多异氰脲酸酯泡沫体可显示改善的耐燃性、较低的导热性、减少的脆性和改善的表面粘着性。低粘度使得具有用于喷雾泡沫体的潜在用途。其中所使用的脂族多元醇基于己二酸、戊二酸、琥珀酸和硝酸与水的组合，用乙二醇酯化。这些多元醇具有的羟基(OH)数大于200且粘度在2,000mpa*s的范围。
在另一实例中，脂族和芳族聚酯多元醇的组合在US 2001/0003758中描述为可用于制备硬质异氰脲酸酯-改性的聚氨酯泡沫体。该泡沫体具有的异氰酸酯指数范围为80至380。
尽管有上述文献，仍然需要在固化和防火特性表现方面有改善的聚氨酯和多异氰脲酸酯泡沫体。这些和其它特征可参见本发明。
发明内容
在一方面本发明提供聚氨酯或多异氰脲酸酯泡沫体制剂，其包含(a)配制的多元醇，其包含(i)约20至约60重量％的羟值大于约50mg KOH/g且官能度等于或大于约2的芳族聚酯多元醇；(ii)约10至约30重量％的线形酚醛清漆型聚醚多元醇；和(iii)约5至约40重量％的羟值大于约200mgKOH/g且官能度为至少约4的蔗糖-或山梨醇-引发的多元醇；所有百分比基于配制的多元醇整体；(b)多异氰酸酯；和(c)发泡剂；以使异氰酸酯相对配制的多元醇的化学计量指数为约100至约250；且其中相比于由除了配制的多元醇之外都相同的泡沫体制剂制备的聚氨酯或多异氰脲酸酯泡沫体，所述泡沫体制剂适用于制备显示改善的加工性和防火特性的聚氨酯或多异氰脲酸酯泡沫体。本发明包括配制的多元醇和由所给出的制剂制备的泡沫体。
在另一方面，本发明提供制备聚氨酯或多异氰脲酸酯泡沫体的方法，其包括在泡沫体形成条件将(a)配制的多元醇，其包含(i)约20至约60重量％的羟值大于约50mg KOH/g且官能度等于或大于约2的芳族聚酯多元醇；(ii)约10至约30重量％的线形酚醛清漆型聚醚多元醇；(iii)约5至约40重量％的羟值大于约200mg KOH/g且官能度为至少约4的蔗糖-或山梨醇-引发的多元醇；所有百分比基于配制的多元醇整体；(b)多异氰酸酯；和(c)发泡剂接触；且异氰酸酯指数范围为约100至约250；以形成硬质聚氨酯或多异氰脲酸酯泡沫体。本发明还包括通过该方法制备的泡沫体。
具体实施方式
本发明提供对聚氨酯和多异氰脲酸酯工业有利的方法和特性改善如本文所述，术语“多异氰脲酸酯”包括多异氰脲酸酯泡沫体和尿烷-改性的多异氰脲酸酯(PU-PIR)泡沫体。
配制的多元醇
1)芳族聚酯多元醇
第一组分为芳族聚酯多元醇。如本文所述，“芳族”是指具有至少一个交替的单键和双键(其赋予化合物以总体稳定性)的共轭环的有机化合物。本文使用的术语“聚酯多元醇”包括制备聚酯多元醇后剩余的任何少量的未反应的多元醇和/或制备聚酯多元醇后添加的未酯化的多元醇(例如，二醇)。尽管芳族聚酯多元醇可从基本上纯的反应物材料制备，更复杂的起始材料，如聚对苯二甲酸乙二醇酯，可为有利的。其它残余物为对苯二甲酸二甲酯(DMT)的加工残余物，其为制备DMT所得的废物或废残余物。
该芳族聚酯多元醇可任选包含，例如，卤素原子和/或可为不饱和的，且可通常从与上述相同的起始材料制备，但多元醇或多羧酸(优选酸)中的至少一种为芳环含量(表示为每分子包含至少一个芳环的基团的重量％)为至少约50重量％，基于化合物总重量，且优选大于约50重量％的芳族化合物，即，其本质上主要为芳族的。具有有利地包含至少约30重量％的邻苯二甲酸残余物或其异构体的残余物的酸组分的聚酯多元醇，是特别有用的。优选芳族聚酯多元醇的芳环含量为约70至约90重量％，基于化合物总重量。优选的芳族聚酯多元醇为粗反应残余物或废聚酯树脂的酯交换作用得到的粗聚酯多元醇。
该芳族聚酯多元醇的特征还在于其羟值为大于约50mg KOH/g，且在某些实施方案中官能度等于或大于约2。在优选的实施方案中，羟值为大于约50至约400mg KOH/g，且在更优选的实施方案中，羟值为约150至约300mgKOH/g。该官能度可为约1.5至约8，但在某些非限制性实施方案中可为约2至约8，在其它非限制性实施方案中可为约2至约6。
2)线形酚醛清漆型聚醚多元醇
第二成分为线形酚醛清漆型聚醚多元醇。线形酚醛清漆型聚醚多元醇为酚醛树脂的烷氧基化产物，其通过在酸催化剂，如冰醋酸，然后是浓盐酸的存在下，酚与甲醛的消除反应而形成。通常将少量一种或多种酸催化剂添加至可混溶的酚，如对甲苯磺酸，然后是甲醛。甲醛将在两种酚之间反应以形成亚甲基桥，通过在酚的邻位和对位和质子化的甲醛之间的亲电芳族取代产生二聚物。该二聚物为双酚F。另一实例为双酚A，其为丙酮与两种酚的缩合产物。随着二聚物的浓度增加，也可形成三聚物、四聚物和更高级的低聚物。然而，因为甲醛与酚的摩尔比被控制为稍微少于1，因此聚合不完全。因此，线形酚醛清漆然后可被烷氧基化以使分子量达到所需水平，理想地约300至约1500，且在某些非限制性实施方案中，约400至约1000。
可用于制备线形酚醛清漆引发剂的酚包括：邻甲苯酚、间甲苯酚或对甲苯酚，乙基苯酚，壬基苯酚，对苯基苯酚，2，2-二(4-羟基苯酚)丙烷，β-萘酚，β-羟基蒽，对氯苯酚，邻溴苯酚，2，6-二氯-苯酚，对硝基苯酚，4-硝基-6-苯基苯酚，2-硝基-4-甲基苯酚，3，5-二甲基苯酚，对异丙基苯酚，2-溴-4-环己基苯酚，4-叔丁基苯酚，2-甲基-4-溴苯酚，2-(2-羟丙基)苯酚，2-(4-羟基苯酚)乙醇，2-乙酯基苯酚，4-氯-甲基苯酚，及其混合物。特别优选用于制备线形酚醛清漆型聚醚多元醇的酚为未被取代的。
合适的线形酚醛清漆型聚醚多元醇可通过，例如，将酚和甲醛的缩合加合物与一种或多种环氧烷烃(包括环氧乙烷，环氧丙烷和环氧丁烷)反应而制备。这些多元醇，有时称为线形酚醛清漆-引发的多元醇，是本领域技术人员已知的，且可通过公开于以下的方法获得，例如，美国专利2,838,473；2,938,884；3,470,118；3,686,101；和4,046,721；其内容以其整体在此引入作为参考。通常，线形酚醛清漆起始材料通过在酸性催化剂的存在下将酚(例如，甲酚)与每摩尔酚约0.8至约1.5摩尔的甲醛反应而制备，以形成每分子包含2.1至12，优选2.2至6，且更优选3至5个酚单元的多核缩合产物。然后将线形酚醛清漆树脂与环氧烷烃如环氧乙烷，环氧丙烷，环氧丁烷，或异环氧丁烷反应以形成包含多个羟基的氧基烷基化产物。出于本发明目的，优选的线形酚醛清漆多元醇为每分子平均具有3至6个羟基部分且平均羟值为约100至约500mg KOH/g，优选约100至约300mg KOH/g的那些。
3)蔗糖-或山梨醇-引发的多元醇
配制的多元醇的第三所需组分为蔗糖-或山梨醇-引发的多元醇。该多元醇为聚醚多元醇，且羟值可为大于约200mg KOH/g且官能度可为至少约4。甚至更高的官能度，约4.5至约6.0，在一些实施方案中可能特别理想。
蔗糖可获自甘蔗或甜菜，蜂蜜，高梁，糖槭，水果，等。蔗糖组分的萃取、分离和制备手段根据来源而改变，但为广泛已知的且通过本领域技术人员在商业规模实践。
山梨醇可用合适的氢化催化剂通过氢化D-葡萄糖获得。固定床和类似类型的设备尤其适用于该反应。合适的催化剂可包括，例如，RaneyTM(Grace-Davison)催化剂，如以下使用的：Wen，Jian-Ping，et.al.，“Preparationof sorbitol from D-glucose hydrogenation in gas-liquid-solid three-phase flowairlift loop reactor，”The Journal of Chemical Technology and Biotechnology，vol.4，pp.403-406(Wiley Interscience，2004)，以其整体在此引入作为参考。镍-铝和钌-碳催化剂仅为许多可能催化剂中的两种。
在一个备选实施方案中，山梨醇的制备可开始于已被氢化的淀粉水解产物。淀粉为衍生自玉米、小麦和其它产生淀粉的植物的天然材料。为形成该水解产物，该淀粉聚合物分子可在葡萄糖环之间的醚键处分解为较小的低聚物，以生成葡萄糖、麦芽糖和更高分子量的寡糖和多糖。所得分子，具有半缩醛葡萄糖环作为末端单元，其然后可被氢化以形成山梨醇、麦芽糖醇和氢化寡糖和多糖。氢化淀粉水解产物可商购且便宜，经常以糖浆形式，且因为是可再生的资源而提供附加的益处。该方法可进一步需要在氢化之前分离葡萄糖，或在氢化之后分离山梨醇，以由此制备合适的山梨醇-引发的多元醇。通常，氢化减少或消除末端单元形成羟基醛形式的葡萄糖的倾向。因此，可遇到山梨醇较少的副反应，如醛醇缩合和Cannizzaro反应。而且，最终多元醇将包括量减少的副产物。
蔗糖-或山梨醇-引发的多元醇可在合适的催化剂的存在下通过将环氧烷烃聚合至特定的引发剂上而制备。在一个实施方案中，各引发剂可单独在单独的反应中烷氧基化，且混合所得多元醇以获得配制的多元醇的所需组分。在另一实施方案中，可将该引发剂在烷氧基化之前混合在一起，从而作为共引发剂，然后制备具有目标羟值和官能度的多元醇组分。
为实现烷氧基化，环氧烷烃或环氧烷烃混合物可以以任何顺序添加至引发剂，且可以任何数量的增量添加或连续添加。同时添加多于一种环氧烷烃至反应器导致具有无规分布的环氧烷烃分子的嵌段，所谓的混嵌。为制备所选环氧烷烃的嵌段聚氧基-亚烷基，在反应容器中将第一批环氧烷烃添加至引发剂分子。在该第一批之后，可添加第二批且该反应可进行至完成。当第一批和第二批具有不同的环氧烷烃相对组成时，结果为嵌段聚氧亚烷基。优选以此方式制备嵌段多元醇，其中由此形成的嵌段都为环氧乙烷，或都为环氧丙烷，或都为环氧丁烷，但中间体组合物也是可能的。该嵌段可以任何顺序添加，且可存在任何数量的嵌段。例如，可添加环氧乙烷的第一嵌段，然后添加环氧丙烷的第二嵌段。或者，可添加环氧丙烷的第一嵌段，然后添加环氧乙烷的嵌段。也可添加第三和随后的嵌段。选择所有嵌段的组合物以给予最终材料其预期应用所需的性质。
发泡剂
在多元醇组合物中也包括化学发泡剂，其可部分基于最终泡沫体所需密度而选择。在某些非限制性实施方案中，可选择烃发泡剂。例如，可使用烃或含氟的氢卤碳化合物(hydrofluorocarbon)发泡剂，且在一些情况下可用来减少，或进一步降低粘度，从而增强喷雾性。例如这些可为丁烷，异丁烷，2，3-二甲基丁烷，正和异戊烷异构体，己烷异构体，庚烷异构体，环烷烃(包括环戊烷，环己烷，环庚烷)，及其组合，HFC-245fa(1，1，1，3，3-五氟丙烷)，HFC-365mfc(1，1，1，3，3-五氟丁烷)，HFC-227ea(1，1，1，2，3，3，3-七氟丙烷)，HFC-134a(1，1，1，2-四氟乙烷)，以上两种或者更多种的组合，等。这些烃和/或不包含氟的氢卤碳化合物优选的使用量为使得总发泡剂，包括氢氟碳化合物，不大于约15份，更理想的不大于约10份，基于100份的总多元醇组合物。
任选化学发泡剂可选为甲酸或另一羧酸。甲酸可使用的量为约0.5至约8份，每100重量份的多元醇组合物。在某些非限制性实施方案中，甲酸的存在量为从约0.5份，且更优选约1份，至约6份，且更优选至约3.5份，按重量计。尽管甲酸为优选的羧酸，但也考虑使用少量的其它脂族单和多羧酸，如公开于美国专利5,143,945的那些(其以其整体在此引入作为参考)，包括异丁酸，乙基丁酸，乙基己酸，及其组合。
除了甲酸或其它羧酸发泡剂，或作为它们的代替，水也可被任选选作化学发泡剂。水在一些非限制性实施方案中，存在的量为约0.5至约10份，且优选约1至约6份，每100重量份的配制的多元醇。当制备聚氨酯或多异氰脲酸酯泡沫体时，为促进和得到所需的加工特征，有利地是不超过4份水，优选不超过2.5份水，且更优选不超过1.5份水，每100份多元醇组合物。在一些非限制性实施方案中不使用水是有利的。
最后，氨基甲酸酯，其在发泡过程中释放二氧化碳，且其加合物有利地用作任选、另外的化学发泡剂。这在例如，美国专利5,789,451和6,316,662，和EP 1097954中更详细讨论，其以其整体在此引入作为参考。
配制的多元醇的比例
配制的多元醇(不包括发泡剂)的至少需要的三种组分，在某些非限制性实施方案中以特定比例范围存在，以改善它们合并之后的储存稳定性。芳族聚酯多元醇的范围可为约20至约60重量％，基于配制的多元醇整体的重量，线形酚醛清漆型聚醚多元醇的范围可为约10至约30重量％，优选约20至约30重量％。理想的是，在一些实施方案中，芳族聚酯多元醇范围被限制为约20至约40重量％。蔗糖-或山梨醇-引发的多元醇理想地存在的量为约5至约40重量％，基于同样的基础。也可选择多于一种的各类型的多元醇的组合，条件是它们在配制的多元醇整体中的总百分比遵循所述范围。所述烃或氢卤碳化合物发泡剂，无论是包含在配制的多元醇中还是在泡沫体制备过程中单独引入，理想的存在量为约2至约15份，基于100份配制的多元醇，更理想的量为约4至约10份，以同样为基础。
多异氰酸酯
为制备多异氰脲酸酯泡沫体，需要在在合适的泡沫体形成条件将多元醇组合物与多异氰酸酯组分反应。该多异氰酸酯组分在美国称为“A-组分”(在欧洲，称为“B-组分”)。A-组分的选择可基于宽范围的多种多异氰酸酯，包括但不限于本领域技术人员公知的那些。例如，可使用基于有机多异氰酸酯、改性多异氰酸酯、异氰酸酯的预聚物，及其混合物。这些可进一步包括脂族和环脂族异氰酸酯，特别是芳族，且更具体地，多官能芳族异氰酸酯。还特别优选的为多苯基多亚甲基多异氰酸酯(PMDI)。
本发明可用的其它多异氰酸酯包括2，4-和2，6-甲苯二异氰酸酯和相应的异构体混合物；4，4’-，2，4’-和2，2’-二苯基-甲烷二异氰酸酯和相应的异构体混合物；4，4’-，2，4’-和2，2’-二苯基-甲烷二异氰酸酯和多苯基多亚甲基多异氰酸酯(PMDI)的混合物；以及PMDI和甲苯二异氰酸酯的混合物。在此还可使用脂族和环脂族异氰酸酯化合物，如1，6-六亚甲基二异氰酸酯；1-异氰酸基-3，5，5-三甲基-1，3-异氰酸根合甲基环己烷；2，4-和2，6-六氢甲苯-二异氰酸酯和它们的相应异构体混合物；和4，4’-，2，2’-和2，4’-二环己基-甲烷二异氰酸酯和它们的相应异构体混合物。本发明其它可用的为1，3-四-亚甲基二甲苯二异氰酸酯。
其它有利地用于A-组分的物质为所谓改性的多官能异氰酸酯，即，通过上述二异氰酸酯和/或多异氰酸酯的化学反应得到的产物。实例为含酯、脲、缩二脲、脲基甲酸酯，且优选地，碳化二亚胺和/或uretonomine的多异氰酸酯，以及含异氰脲酸酯基和/或尿烷基的二异氰酸酯或多异氰酸酯。也可使用含碳化二亚胺基、uretonomine基和/或异氰脲酸酯环，且具有异氰酸酯基(NCO)含量为120至40重量％，更优选20至35重量％的液体多异氰酸酯。这些包括，例如，基于以下物质的多异氰酸酯：4，4’-2，4’-和/或2，2’-二苯基甲烷二异氰酸酯和相应的异构体混合物，2，4-和/或2，6-甲苯二异氰酸酯和相应的异构体混合物；二苯基甲烷二异氰酸酯和PMDI的混合物；以及甲苯二异氰酸酯和PMDI和/或二苯基甲烷二异氰酸酯的混合物。
用作本发明的制剂的多异氰酸酯组分的合适的预聚物为NCO含量为2至40重量％，更优选4至30重量％的预聚物。这些预聚物通过将二和/或多异氰酸酯与包括较低分子量的二醇和三醇的材料反应制备，但也可用多价活性氢化合物如二和三胺以及二和三醇制备。单独的实例包括含尿烷基团的芳族多异氰酸酯，优选其NCO含量为5至40重量％，更优选20至35重量％，其通过将二异氰酸酯和/或多异氰酸酯与，例如，多元醇如较低分子量的二醇、三醇、氧亚烷基二醇、一缩二氧亚烷基二醇或多氧亚烷基二醇(其分子量至多约800)反应而获得。这些多元醇可单独使用或作为二和/或多氧亚烷基二醇的混合物使用。例如，可使用二甘醇，一缩二丙二醇，聚乙二醇，乙二醇，丙二醇，丁二醇，聚丙二醇和聚氧亚丙基聚氧亚乙基二醇。也可使用聚酯多元醇，以及烷基二醇如丁二醇。其它可使用的二醇包括双羟基乙基-或双羟丙基-双酚A，环己烷二甲醇和双羟基乙基氢醌。
可用于本发明的预聚物制剂的多异氰酸酯组分为：(i)多异氰酸酯，其NCO含量为8至40重量％，含碳化二亚胺基团和/或尿烷基团，源自4，4’-二苯基甲烷二异氰酸酯或4，4’-和2，4’-二苯基甲烷二异氰酸酯的混合物；(ii)预聚物，其包含NCO基，NCO含量为2至35重量％，基于预聚物的重量，通过具有优选1.75至4的官能度和800至15,000的分子量的多元醇和4，4’-二苯基甲烷二异氰酸酯、4，4’-和2，4’-二苯基甲烷二异氰酸酯的混合物，或(i)和(ii)的混合物反应制备；和(iii)2，4’和2，6-甲苯-二异氰酸酯和它们的相应异构体混合物。
任意形式的PMDI为本发明使用的最优选的多异氰酸酯。当使用时，其优选具有的当量为125至300，更优选130至175，且平均官能度大于约1.5。更优选平均官能度为1.75至3.5。多异氰酸酯组分的粘度优选为25至5,000厘泊(cP)(0.025至约5Pa*s)，但在25℃时100至1,000cP的值(0.1至1Pa*s)是方便加工所优选的。类似粘度是优选的，其中选择可选的多异氰酸酯组分。而且，优选本发明的制剂的多异氰酸酯组分选自MDI，PMDI，MDI预聚物，PMDI预聚物，改性MDI，及其混合物。
按比例，理想地是A-组分与B-组分(多异氰酸酯与配制的多元醇)的比例范围为约100至约250，也就是说，异氰酸酯指数为约1至约2.5；在一些非限制性实施方案中，该异氰酸酯指数理想地为约1.5至约1.8，即，所谓的“中间指数”泡沫体。
任选的制剂组分
除了上述所需的三种组分外，其它多元醇也可包含在配制的多元醇和/或最终制剂中，且，如果包含的话，被认为是制剂的B-组分的一部分。尽管这些另外的材料通常在配制过程中作为B-组分的一部分添加，但它们在此单独处理，这是因为认为它们是任选的。可包括方法中通常用来制备聚氨酯和/或多异氰脲酸酯泡沫体的一种或多种其它聚醚或聚酯多元醇种类。也可存在具有至少两个异氰酸酯-反应性氢原子的其它化合物，例如，聚硫醚多元醇，聚酯酰胺和含羟基的聚缩醛，含羟基的脂族聚碳酸酯，胺封端的聚氧亚烷基(polyoxyalkylene)聚醚，且优选地，聚酯多元醇，聚氧亚烷基聚醚多元醇，和接枝分散多元醇。也可使用两种或多种上述材料的混合物。在许多实施方案中，该多元醇每分子具有约2至约8个羟基，摩尔平均官能度为至少约3或更多，且羟值大于100mg KOH/g，在某些实施方案中，大于300mg KOH/g。
在一些非限制性实施方案中，所述配制的多元醇还可包含一种或多种扩链剂和/或交联剂。当选择时，扩链剂可为双官能、低分子量醇，特别是分子量至多为400的那些，例如乙二醇，丙二醇，丁二醇，己二醇，及其混合物。交联剂，在许多实施方案中为至少三官能的，且可选自，例如，低分子量醇如甘油，三羟甲基丙烷，季戊四醇，蔗糖，山梨醇，或其混合物。
本发明的制剂可包含其他本领域熟知的添加剂或改性剂。例如，可使用表面活性剂，催化剂，阻燃剂，和/或填料。特别重要的为一种或多种三聚催化剂。该使用的三聚催化剂可为任何本领域技术人员已知将催化有机异氰酸酯化合物的三聚以形成异氰脲酸酯部分的催化剂。对于典型异氰酸酯三聚催化剂，参见The Journal of Cellular Plastics，11月/12月1975，329页：和美国专利3,745,133；3,896,052；3,899,443；3,903,018；3,954,684和4,101,465；其内容以其整体在此引入作为参考。典型三聚催化剂包括甘氨酸盐，叔胺三聚催化剂，碱金属羧酸盐，和这些类型催化剂的混合物。该类型中的优选物质为N-2-羟基-5-壬基苯基-甲基-N-甲基甘氨酸钠，N，N-二甲基环己基-胺，及其混合物。其它包括在优选催化剂组分中的为美国专利3,745,133中公开的环氧化物，其公开以其整体在此引入作为参考。
可包含的另一类的催化剂为胺催化剂，包括任何包含至少一个叔氮原子且能催化A-组分和B-组分之间的羟基/异氰酸酯反应的有机化合物。典型类型的胺包括N-烷基吗啉，N-烷基-链烷醇胺，N，N-二烷基环己基胺，和烷基胺，其中烷基为甲基、乙基、丙基、丁基和其异构体形式，和杂环的胺。其典型但非限制性实例为三乙二胺(triethylenediamine)，四甲基乙二胺(tetramethylethylenediamine)，二(2-二甲基氨基乙基)醚，三乙胺，三丙基胺，三丁基胺，三戊胺，吡啶，喹啉，二甲基哌嗪，哌嗪，N，N-二甲基环己基胺，N-乙基-吗啉，2-甲基丙烷二胺，甲基三乙二胺，2，4，6-三二甲基氨基-甲基)酚，N，N’，N”-三(二甲基氨基丙基)对称-六氢三嗪，及其混合物。可选择的叔胺的优选基团包括二(2-二甲基氨基-乙基)醚，二甲基环己基胺，N，N-二甲基-乙醇胺，三乙二胺，三乙胺，2，4，6-三(二甲基氨基甲基)酚，N，N’，N-乙基吗啉，及其混合物。
非胺催化剂也可用于本发明。典型的这些催化剂为铋，铅，锡，钛，铁，锑，铀，镉，钴，钍，铝，汞，锌，镍，铈，钼，钒，铜，锰，锆，及其组合的有机金属化合物。仅出于解释性目的，可包括的为硝酸铋，2-乙基己酸铅，苯甲酸铅，环烷酸铅，氯化铁，三氯化锑，乙醇酸锑，其组合，等。优选类型包括羧酸的亚锡盐，如乙酸亚锡，辛酸亚锡，2-乙基己酸亚锡，1-甲基咪唑，和月桂酸亚锡，以及羧酸的二烷基锡盐，如双乙酸二丁基锡，双月桂酸二丁基锡，二马来酸二丁基锡(dibutyl tin dimaleate)，二乙酸二辛基锡，其组合，等。催化剂，如NIAXTM A-1，POLYCATTM 9和/或POLYCATTM77，可包含的量为约1至约8份，基于B-组分总量。(NIAXTM A-1可获自General Electric。POLYCATTM 9和POLYCATTM 77可获自Air Products.)。其它催化剂，如TOYOCATTM DM70或其它胶凝催化剂，可以含有0至约2份的量。(TOYOCATTM DM70可获自Tosoh Corporation.)
尽管该基本制剂使得能制备具有改善的防火特性的泡沫体，如下所定义的，在一些实施方案中，其可理想地进一步通过包含一种或多种溴化或非溴化阻燃剂作为添加剂而增强防火性能，该溴化或非溴化阻燃剂如三(2-氯乙基)磷酸酯，三(2-氯丙基)磷酸酯，三(1，3-二氯丙基)磷酸酯，磷酸二铵，各种卤化的芳族化合物，氧化锑，氧化铝三水合物，聚氯乙烯，及其组合。分散剂、泡孔稳定剂和表面活性剂也可掺入制剂。
也可添加表面活性剂，包括有机表面活性剂和基于聚硅氧烷的表面活性剂，以作为泡孔稳定剂。一些代表性材料以名称SF-1109，L-520，L-521和DC-193销售，其通常为聚硅氧烷聚氧亚烷基嵌段共聚物，如公开于美国专利2,834,748；2,917,480；和2,846,458的那些，其内容以其整体在此引入作为参考。其它包括的为包含聚氧乙烯-聚氧丁烯嵌段共聚物的有机表面活性剂，如美国专利5,600,019所述，其公开以其整体在此引入作为参考。特别理想地是使用少量的表面活性剂以稳定发泡反应混合物直到其固化。其它表面活性剂包括长链醇的聚乙二醇醚，长链烯丙基酸硫酸酯的叔胺或链烷醇胺盐，烷基磺酸酯，烷基芳基磺酸，及其组合。
该表面活性剂使用的量足以稳定发泡反应，以对抗破碎和形成大的不均匀的泡孔。通常，每100重量份配制的多元醇约0.2至约3份表面活性剂对该目的是足够的。表面活性剂，如DABCOTM DC-5598，可以含有0至约6份的任何量。(DABCOTM DC-5598可获自Air Products)。
其它添加剂可包括，但不限于炭黑和着色剂、填料和颜料。实例可包括硫酸钡，碳酸钙，石墨，炭黑，二氧化钛，氧化铁，微球体，氧化铝三水合物，硅灰石，制备的玻璃纤维(间歇的(dropped)或连续的)，和聚酯纤维和其它聚合物纤维，以及它们的各种组合。
泡沫体制备
根据本发明的方法制备的聚氨酯或多异氰脲酸酯聚合物在某些非限制性实施方案中为硬质、起泡的、闭孔的聚合物。该聚合物通常通过以下制备：
在室温或稍微升高的温度下短时间匀质混合反应组分，即，多元醇/发泡剂组分(基本上由上文限定的配制的多元醇和发泡剂组成，或包含上文限定的多元醇/发泡剂组合物)，与异氰酸酯组分，即，至少两种物流；或多元醇组分(基本上由上文限定的配制的多元醇组成，或包含上文限定的多元醇组合物)、发泡剂组分、和异氰酸酯组分，即，至少三种物流，其中所述配制的多元醇和发泡剂组分的混合刚好在其与异氰酸酯组分接触之前)。也可按需要包括其他流，用于引入各种催化剂和其它添加剂。流的混合可在喷雾装置、有或没有用于混合多元醇组分和发泡剂的静态混合器的混合头(mixhead)、或容器中进行，然后喷涂或沉积该反应混合物至基板。该基板可为，例如，由箔或另一材料制备的硬质或柔性面板(面板)，包括另一层类似或不同的聚氨酯或多异氰脲酸酯，其连续或不连续地沿着生产线运输，或直接在传送带上运输。
在备选实施方案中，该反应混合物可倒入开口模或通过设置的设备分配至开口模或仅在其目标位置沉积或沉积至其目标位置，即，一种原位倒入应用(pour-in-place application)，如在结构的内壁和外壁之间。在沉积至面板上的情况下，第二板可施加于沉积的混合物之上。在其它实施方案中，该混合物可在有或没有真空辅助的空腔填充的情况下，注射至封闭的模具中。如果使用模具，最典型进行加热。
通常，该应用可使用已知的一次完成的(one-shot)、预聚物或半预聚物技术以及常规混合方法完成。该混合物，当反应时，以模具的形状或粘连至基板以产生具有或多或少预定的结构的聚氨酯或多异氰脲酸酯聚合物，然后将其在适当位置或在模具中部分或完全固化。促进聚合物固化的合适的条件包括温度，通常为20℃至150℃，优选35℃至75℃，且更优选45℃至55℃。该温度通常允许充分固化的聚合物可从模具去除，其中典型地在使用时，在混合反应物后约1至10分钟内且更典型1至5分钟内从模具去除。最佳固化条件将取决于具体组分，包括制备聚合物使用的催化剂和量以及制备的制品的尺寸和形状。
结果可为板型材料、模制件、填充的空腔形式的硬质泡沫体，包括但不限于管或绝缘壁或船体结构、喷雾泡沫体、发泡泡沫体、或连续或不连续制造的层合制品，包括但不限于与其它材料，如硬纸板、石膏板、塑料、纸、金属或其组合形成的叠层或层合制品。有利地，当与从类似的制剂和制备方法制备的泡沫体比较时，本发明制备的聚氨酯和多异氰脲酸酯泡沫体可显示改善的加工性，该类似的制剂和制备方法的不同在于该制剂不包含本发明使用的特定配制的多元醇。如本文所述，术语“改善的加工性”是指泡沫体显示减少的缺陷的能力，其可包括但不限于收缩和变形。当本发明用于制备夹层板时这种改善特别有利。优选该减少的收缩和变形水平少于约0.5％，基于线性变形，根据欧洲标准EN1603在80℃测试，且样本尺寸在20小时后记录。在一些实施方案中，夹层板可限定为包含至少一层硬质泡沫体的相对平面的层(即，具有两个相对大尺寸和一个相对小尺寸的层)，其较大尺寸的侧面各自面向柔性或者硬质材料如箔的至少一个层(经由该侧面)，或金属或其它提供结构的材料的较厚层。这种层在某些实施方案中可在泡沫体形成过程中作为基板。
还有利地是，当与从类似的制剂和制备方法制备的泡沫体比较时，本发明制备的聚氨酯和多异氰脲酸酯泡沫体可显示改善的防火特性，该类似的制剂和制备方法的不同在于该制剂不包含本发明使用的特定配制的多元醇。如本文所述，术语“改善的防火特性”是指泡沫体显示B2防火特性的能力，其定义为当根据德国标准DIN4102测试时火焰高度不高于15厘米。在某些实施方案中，本发明可用于满足基于新的Euroclasses规则(欧洲标准EN12823)的防火需求。
此外，本发明的多异氰脲酸酯和聚氨酯泡沫体可显示改善的固化性质，包括改善的湿压强度和在选择的泡沫体脱模时间减少的后膨胀(postexpansion)。测定这些性质的测试分别描述于表1和表3的脚注。当本发明用于制备绝缘的夹层板时这些特征可特别有利。
上文是总的描述而不意图包含本发明所有可能的实施方案。类似的，以下实施例仅以解释的目的提供，不是用来以任何方式限定或限制本发明。本领域技术人员将完全能理解，权利要求范围内的其它实施方案，在考虑了本申请公开的本发明的说明书和/或实践后将是明显的。这些其它实施方案可包括具体组分和其比例的选择；混合和反应条件，容器，调配装置，和方案；性能和选择性；产物和副产物的鉴定；后续加工和其用途；等；本领域技术人员将认识到这些可在所附权利要求的范围内改变。
实施例
实施例和/或对比例使用的材料包括以下，依字母顺序给出。
CM265为水和VORANOLTM RN490(50/50重量)的加和混合物。
CP1055为VORANOLTM CP1055，其羟值为165mg KOH/g且官能度为3，可获自The Dow Chemistry Company。
CURITHANETM 52为二甘醇中的N-(2-羟基-5-壬基苯基)甲基)-N-甲基甘氨酸钠。
DABCOTM DC5598为专有的聚硅氧烷表面活性剂，可获自AirProducts。
DABCOTM K2097为基于乙酸钾的三聚催化剂。
IP585为多元醇IP585，为芳族树脂-引发的氧基亚丙基-氧基亚乙基多元醇(线形酚醛清漆型多元醇)，且羟值为195mg KOH/g，平均官能度为3.3。
“其它组分”包括碳酸亚丙基酯。
PEG200为平均分子量为约200的聚乙二醇。
PEG400为平均分子量为约400的聚乙二醇。
TERATETM 2541V为芳族聚酯多元醇，具有的羟值为约240mg KOH/g，可获自INVISTA。
TERCAROLTM 5902为甲苯二胺-引发的聚氧亚丙基多元醇，其羟值为385mg KOH/g，可获自INVISTA.
TMR为乙二醇中的75％N-(2-羟丙基)-N-三甲基铵羧酸盐。
VORANATETM M600为高度粗制的二苯基甲烷二异氰酸酯，其官能度为2.9，可获自The Dow Chemistry Company。
VORANOLTM 1010L为聚丙二醇，其羟值为112mg KOH/g。其可获自The Dow Chemistry Company。
VORANOLTM P400，基于聚环氧丙烷的二醇，且分子量为400，可获自The Dow Chemistry Company。
VORANOLTM RA640为通过丙氧基化乙二胺制备的聚醚多元醇，其羟值为640mg KOH/g。其可获自The Dow Chemistry Company。
VORANOLTM RN490为蔗糖-甘油引发的聚氧亚丙基多元醇，其羟值为485mg KOH/g。
实施例1和对比例2-5
制备5种配制的多元醇，各包括蔗糖-引发的多元醇(VORANOLTMRN490)和线形酚醛清漆型多元醇(IP585)。仅实施例1包含脂族聚酯多元醇，其为TERATETM 2541V；对比例用相等官能度的聚醚多元醇代替脂族聚酯多元醇。对于对比例2-5，该配制的多元醇然后与扩链剂混合，而对于实施例1和对比例2-5，配制的多元醇与阻燃剂、聚硅氧烷表面活性剂、催化剂、水和其它组分混合。然后该混合物与异氰酸酯(VORANATETM M600)和正戊烷以1.8的指数进行反应，形成自由上升的泡沫体。各制剂的组成示于表1。通过测量5分钟时的湿压强度(green compressive strength)测试固化性质，结果也示于表1。最后，各泡沫体的防火特性根据德国标准DIN4102测试，结果示于表1。
表1
--表示制剂中不存在
*GCS(湿压强度)：这在在木盒(20x20x20cm)中产生的自由上升的泡沫体上测量，反应开始后2分钟去除，且置于(垂直于上升)保持在10kN Instron仪器的下板上的5x5cm木基上。在5分钟时移动上面的Instron板以于恒定速度(每分钟20mm)挤压泡沫体。所得GCS值以kPa表示。
可见实施例1显示改善的固化(湿压强度，GCS测试)和防火特性(德国标准DIN4102测试，测量火焰高度)。
对比例6-10
出于对比目的，根据表2制备5种制剂，使用实施例1和对比例2-5使用的相同配制方法和手段。对比例6的结果显示，当与对比例7-10比较时，芳族聚酯多元醇与不为线形酚醛清漆型多元醇的芳族聚醚多元醇组合不改善固化性质。
表2
--表示制剂中不存在
对比例11和实施例12-13
使用高压发泡机和与之前实施例和对比例相同的评价方法制备三种泡沫体制剂，且制剂示于表3。在该情况下实施例12-13各包含芳族聚酯多元醇，而对比例11不包含。
表3
(表3下页继续)
(续前页的表3)
--表示制剂中不存在
*后膨胀％为(15x50x50)cm模制的泡沫体(在固定时间脱模和将其从角至角(comer to comer)切削后测量)的最大厚度和初始厚度之间的比值(difference)乘以100。
可见，与对比例11相比，实施例12和13显示改善的固化(减少的后膨胀和增强的湿压强度结果)和改善的防火特性(德国标准DIN4102测试，测量火焰高度)。
Claims (18)
1.聚氨酯或多异氰脲酸酯泡沫体制剂，其包含
(a)配制的多元醇，该配制的多元醇包含
(i)20至60重量%的芳族聚酯多元醇，其羟值为大于50mg KOH/g且官能度为至少2；
(ii)10至30重量%的线形酚醛清漆型聚醚多元醇；和
(iii)5至40重量%的蔗糖或山梨醇引发的多元醇，其羟值为大于200mg KOH/g且官能度为至少4；
所有百分比基于配制的多元醇整体的重量；
(b)多异氰酸酯；和
(c)发泡剂；
以使多异氰酸酯与配制的多元醇的化学计量指数为100至250；且
其中相比于由除了配制的多元醇之外都相同的泡沫体制剂制备的聚氨酯或多异氰脲酸酯泡沫体，所述泡沫体制剂适用于制备显示出改善的加工性和防火特性的聚氨酯或多异氰脲酸酯泡沫体。
2.权利要求1所述的制剂，其中所述芳族聚酯多元醇选自芳族聚酯多元醇，该芳族聚酯多元醇具有包含至少30重量%的邻苯二甲酸残余物，或其异构体的残余物的酸组分。
3.权利要求2所述的制剂，其中芳族聚酯多元醇具有的芳环含量为70至90重量%，基于化合物总重量。
4.权利要求1所述的制剂，其中所述芳族聚酯多元醇通过粗反应残余物或废料的酯交换作用得到。
5.权利要求1所述的制剂，其中芳族聚酯多元醇的羟值范围为大于50mg KOH/g至400mg KOH/g。
6.权利要求5所述的制剂，其中所述羟值范围为150mg KOH/g至300mg KOH/g。
7.权利要求1所述的制剂，其中所述芳族聚酯多元醇的官能度范围为2至8。
8.权利要求1所述的制剂，其中所述线形酚醛清漆型多元醇的分子量为300至1500。
9.聚氨酯或多异氰脲酸酯泡沫体，其由权利要求1的制剂制备。
10.配制的多元醇，其包含
(a)20至60重量%的芳族聚酯多元醇，其羟值为大于50mg KOH/g且官能度为至少2；
(b)10至30重量%的线形酚醛清漆型聚醚多元醇；和
(c)5至40重量%的蔗糖或山梨醇引发的多元醇，其羟值为大于200mgKOH/g且官能度为至少4。
11.制备聚氨酯或多异氰脲酸酯泡沫体的方法，包括在泡沫体形成条件下，在100至250异氰酸酯指数，将以下(a)、(b)和(c)接触：
(a)配制的多元醇，其包含
(i)20至60重量%的芳族聚酯多元醇，其羟值为大于50mgKOH/g且官能度为等于或大于2；
(ii)10至30重量%的线形酚醛清漆型聚醚多元醇；和
(iii)5至40重量%的蔗糖或山梨醇引发的多元醇，其具有的羟值大于200mg KOH/g且官能度为至少4；
所有百分比基于配制的多元醇整体的重量；
(b)多异氰酸酯；和
(c)发泡剂；
从而形成硬质聚氨酯或多异氰脲酸酯泡沫体。
12.权利要求11所述的方法，其中所述配制的多元醇、多异氰酸酯和发泡剂作为两股流、三股流或多于三股流接触从而形成混合流。
13.权利要求12所述的方法，其中将所述混合流喷涂或沉积至基板上。
14.权利要求13所述的方法，其中所述基板选自硬质面板、柔性面板、一层不同的聚氨酯或多异氰脲酸酯、或传送带。
15.权利要求14所述的方法，其中形成夹层板。
16.聚氨酯或多异氰脲酸酯泡沫体，其通过权利要求11所述的方法形成。
17.权利要求16所述的泡沫体，其中所述泡沫体为夹层板中的层。
18.权利要求17所述的泡沫体，进一步包含至少一种硬质面板、至少一种柔性面板、至少一层不同的聚氨酯或多异氰脲酸酯，或其组合。
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| PCT/US2010/027563 WO2010114703A1 (en) | 2009-04-01 | 2010-03-17 | Polyurethane and polyisocyanurate foams having improved curing performance and fire behavior |
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| CN102405245B true CN102405245B (zh) | 2014-06-11 |
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| EP2414423A1 (en) | 2012-02-08 |
| EP2414423B1 (en) | 2018-05-30 |
| CN102405245A (zh) | 2012-04-04 |
| BRPI1006216A2 (pt) | 2016-11-29 |
| ES2681205T3 (es) | 2018-09-12 |
| RU2653540C2 (ru) | 2018-05-11 |
| JP5850824B2 (ja) | 2016-02-03 |
| JP2012522868A (ja) | 2012-09-27 |
| MX355288B (es) | 2018-04-13 |
| WO2010114703A1 (en) | 2010-10-07 |
| BRPI1006216B1 (pt) | 2020-01-28 |
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| MX2011010293A (es) | 2011-10-11 |
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