CN107108835A - 用于穿孔开口的b2等级单组分喷涂聚氨酯泡沫调配物 - Google Patents

用于穿孔开口的b2等级单组分喷涂聚氨酯泡沫调配物 Download PDF

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CN107108835A
CN107108835A CN201580057847.6A CN201580057847A CN107108835A CN 107108835 A CN107108835 A CN 107108835A CN 201580057847 A CN201580057847 A CN 201580057847A CN 107108835 A CN107108835 A CN 107108835A
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weight
composite
foam
pack system
spray foam
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CN107108835B (zh
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S·P·克雷恩
L·梅赛格尔
C·波姆
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DDP Specialty Electronic Materials US LLC
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Dow Global Technologies LLC
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Abstract

一种单组分喷涂聚氨酯泡沫调配物实现在DIN 4102测试中的B2等级，该单组分喷涂聚氨酯泡沫调配物含有标称官能度为2.5到3.5的聚合物异氰酸酯、至少85％脂族且具有三个或更多个官能团的多元醇与总多元醇的摩尔比为0.2到0.75的多元醇组分、15wt％到30wt％的塑化剂、1.5wt％到3.5wt％磷、5.5到11.5卤素以及每克的调配物1.5毫摩尔到5毫摩尔的发泡剂并且不含可膨胀石墨。

Description

用于穿孔开口的B2等级单组分喷涂聚氨酯泡沫调配物
技术领域
本发明涉及在DIN 4102测试中实现B2等级并且适合用于密封穿孔开口的单组分喷涂聚氨酯泡沫调配物。
背景技术
在构建结构中的穿孔开口对于绝缘材料提供具有挑战性的位置。穿孔开口通常在穿孔框架和支撑结构之间围绕穿孔开口具有间隙。如果间隙不被密封和隔绝，那么它们为能量泄漏的来源。聚合物喷涂泡沫绝缘材料/密封剂为用于填充这些穿孔间隙常见和方便的选择。具体地说，单组分喷涂聚氨酯泡沫(OCF)为用于隔绝穿孔间隙期望的选择。
穿孔间隙对于绝缘材料/密封剂提供技术挑战。为了密封穿孔间隙，绝缘材料/密封剂必须粘附到限定间隙的结构材料并且在构建结构安定时当那些结构材料随天气改变和结构变化经历热膨胀和收缩时保持粘附到那些结构材料。因此，结构粘合剂必须为粘合剂材料，但还必须为柔性材料。
为方便起见，在申请书中，期望绝缘材料/密封剂为喷涂泡沫材料，更具体地说OCF调配物，以避免与定量多种组分(如在双组分喷涂聚氨酯泡沫调配物中需要的)相关的困难。同时，通过OCF调配物形成的泡沫需要足够柔性，不仅随它粘附到的结构材料移动，而且贴合间隙间距而不使限定间隙的结构部件变形。如果喷涂泡沫调配物强有力地膨胀成硬质泡沫，那么膨胀可移动限定间隙的结构材料并且由此致使旨在适配在穿孔开口内的穿孔不再恰当地适配在开口中。
OCF应形成开孔泡沫结构以使发泡剂从泡沫逸出并且使水分从穿孔间隙逸出，但同时抑制过度的空气流以便无法具有绝缘特性。因此，期望泡沫具有在0.001升/秒(L/s)和0.02L/s之间的空气流速，如通过ASTM D3574测定。
大量研究和开发已进入识别满足适用作穿孔间隙绝缘体/密封剂的这些要求的OCF调配物。参见，例如WO2014/033231A1和WO 02/12367A1，提供对用于穿孔间隙的OCF调配物的提出的解决方案的两个公布的专利申请。
对于OCF穿孔绝缘材料/密封剂材料的一个外加的挑战为现在需要实现某些阻燃性能以满足法则限制。具体来说，在一些国家中需要OCF在DIN 4102测试中实现B2等级。在WO2014/033231A1中的实例示出只有当以泡沫调配物重量计泡沫含有大于12重量％卤素(溴加氯)时才实现B2等级。期望寻找实现B2等级而不需要在泡沫中如此多卤素的方式。WO2010/058036描述了含有可膨胀石墨以提高阻燃特性的OCF。然而，可膨胀石墨为固体颗粒，这可通过在用于施加OCF调配物的分配方法中堵塞开口而使OCF调配物的分配复杂。因此，期望在OCF调配物中避免使用可膨胀石墨。
期望并且应发展OCF技术的领域以发现产生柔性、开孔泡沫并且在DIN 4102测试中实现B2阻燃性等级而不含有可膨胀石墨并且同时以调配物重量计含有少于12重量％卤素的OCF调配物。
发明内容
本发明提供对发现可喷涂OCF调配物的问题的解决方案，其产生柔性、开孔并且在DIN 4102测试中实现B2阻燃性等级而不含有可膨胀石墨并且同时以调配物重量计含有少于12重量％卤素。
本发明为出人意料地发现均衡高级官能多元醇(那些多元醇每分子具有三个或更多个羟基官能团)与总多元醇的特定比率的结果，其中塑化剂提供产生以调配物重量计具有少于12重量％卤素的解决方案泡沫的OCF调配物。多元醇的比率出人意料地影响阻燃性，其中当所陈述的多元醇比率在0.2到0.75的范围中时出现理想阻燃性。
本发明的调配物可用作单组分喷涂聚氨酯泡沫(OCF)调配物，尤其适用作用于穿孔开口间隙的绝缘/密封剂材料。
具体实施方式
除非用测试方法编号指明日期，否则测试方法是指截至本文档的优先权日的最新测试方法。参考测试方法含有参考测试协会与测试方法编号。通过以下缩写中的一个来提及测试方法组织：ASTM是指ASTM国际(原名是美国测试与材料协会(American Society forTesting and Materials))；EN是指欧洲标准(European Norm)；DIN是指德国标准化学会(Deutsches Institut für Normung)；并且ISO是指国际标准化组织(InternationalOrganization for Standards)。
“和/或”意指“和，或作为一个替代方案”。除非另外指明，否则所有范围都包括端点。
本发明的调配物为单组分喷涂聚氨酯泡沫(OCF)调配物。OCF调配物为从单个加压容器分配的自膨胀、自粘性湿固化聚氨酯调配物。OCF调配物膨胀成在水分存在下固化的聚氨酯泡沫。
OCF调配物不同于双组分喷涂聚氨酯泡沫调配物。双组分喷涂聚氨酯泡沫调配物包含两种不同化学组分，多元醇组分和异氰酸酯组分，它们彼此反应以固化成聚氨酯。在双组分喷涂聚氨酯泡沫调配物中，多元醇组分和异氰酸酯组分一起进料到分配装置中，混合并且从分配装置喷涂，其中混合物发泡并且通过与彼此化学反应而固化。OCF调配物和双组分喷涂聚氨酯泡沫调配物的组成实质上不同或OCF调配物将在使用之前固化。
本发明的OCF调配物尤其被设计成具有密封和隔绝穿孔开口周围间隙的期望特性。如此，通过OCF调配物形成的泡沫为柔性泡沫，这意指在压缩泡沫的原始厚度的75％之后它具有大于45％，优选地50％或更多并且可为55％或更多、60％或更多、65％或更多、70％或更多、75％或更多、80％或更多、85％或更多、90％或更多、95％或更多，甚至100％的压缩回复率。在压缩到原始厚度的75％维持三天并且允许24小时回复之后根据ISO 1856评估压缩回复率。厚度对应于泡沫样品的最小尺寸。泡沫具有三个彼此垂直的尺寸：厚度、宽度和长度。厚度对应于具有最小量级的尺寸而长度对应于具有最大量级的尺寸。期望地，使用具有大约20毫米的厚度的泡沫测试通过OCF调配物形成的泡沫的柔性。
本发明的OCF调配物包含聚合物异氰酸酯。合适的聚合物异氰酸酯包括脂族、环脂族、aryliphatic并且优选芳香族多异氰酸酯。合适的聚合物异氰酸酯的实例包括在亚烷基部分中具有4到12个碳原子的亚烷基二异氰酸酯(如1,12十二烷二异氰酸酯；2-甲基五亚甲基1,5-二异氰酸酯；四亚甲基1,4-二异氰酸酯；以及六亚甲基1,6-二异氰酸酯)、环脂族二异氰酸酯(如环己烷1,3-二异氰酸酯和环己烷1,4-二异氰酸酯；1-异氰酰-3,3,5-三甲基-5-异氰酰甲基环己烷；2,4-六氢甲苯二异氰酸酯和2,6-六氢甲苯二异氰酸酯以及对应的异构体混合物；4,4'-二环己基甲烷二异氰酸酯、2,2'-二环己基甲烷二异氰酸酯和2,4'-二环己基甲烷二异氰酸酯以及对应的异构体混合物)和优选芳香族二异氰酸酯和多异氰酸酯(如2,4-甲苯二异氰酸酯和2,6-甲苯二异氰酸酯以及对应的异构体混合物；4,4'-二苯基甲烷二异氰酸酯、2,4'-二苯基甲烷二异氰酸酯和2,2'-二苯基甲烷二异氰酸酯；聚亚甲基聚苯基异氰酸酯；4,4'-二苯基甲烷二异氰酸酯、2,4'-二苯基甲烷二异氰酸酯和2,2'-二苯基甲烷二异氰酸酯的混合物；以及聚亚甲基聚苯基异氰酸酯(PMDI)；经改性以含有低聚物的任何二苯基甲烷二异氰酸酯或PMDI，所述低聚物含有如描述于WO2011/073355中的矿石或更多缩二脲基团；以及PMDI和甲苯二异氰酸酯的混合物)。
聚合物异氰酸酯具有2.5或更多并且同时3.5或更少，优选地3.0或更少的标称官能度。标称官能度是指每分子反应性基团的平均数。对于聚合物异氰酸酯，标称官能度是指每摩尔的异氰酸酯分子的-NCO官能团的摩尔数。当标称官能度低于2.5时，聚合物异氰酸酯往往会难以处理，因为它在25℃下常常为固体并且它往往会形成二聚体。当标称官能度大于3.5时，成本不当地高并且粘度往往会不当地高。
聚合物异氰酸酯以足以提供以在调配物中异氰酸酯和多元醇的总重量计浓度在10重量％(wt％)或更多，优选地12wt％或更多并且同时20wt％或更少，优选地15wt％或更少范围内的-NCO官能团的浓度存在。当-NCO官能团的浓度小于10wt％时，当经发泡以形成泡沫时调配物经历不当过度的塌陷。当-NCO官能团的浓度大于20wt％时，弹性回复率减小并且可往往会不当地低。
本发明的OCF调配物包含多元醇组分。多元醇组分可为单一类型的多元醇或多于一种类型的多元醇的共混物。合适的多元醇包括聚醚多元醇和聚酯多元醇。以总多元醇重量计，多元醇组分为至少85wt％，优选地90wt％或更多步器可为95wt％或更多或100wt％脂族多元醇。如果多元醇为小于85wt％脂族的，那么所得泡沫的弹性回复率往往会不当地低。脂族多元醇不含芳香族官能团。
聚酯多元醇包括使用多元羧酸和具有2到12个碳原子的多官能醇由常规合成方法获得的那些聚酯多元醇。合适的多元羧酸的实例包括戊二酸、丁二酸、己二酸、癸二酸、邻苯二甲酸、间苯二甲酸和对苯二甲酸。可与这些多元羧酸中的任一种结合的合适的多官能醇的实例包括乙二醇、包括丙二醇的丙二醇、丁二醇和己二醇。
聚醚多元醇包括使用常规合成方法使环氧烷(如选自由环氧乙烷、环氧丙烷和环氧丁烷组成的群组的那些)与对于二醇具有两个活性氢原子的引发剂和与对于三醇具有三个活性氢原子的引发剂以及与对于具有多于三个羟基官能团的多元醇具有多于三个活性氢原子的引发剂反应可获得的那些聚醚多元醇。合适的引发剂的实例包括乙二醇、二乙二醇、丙二醇、二丙二醇、三丙二醇、1,4-丁二醇、1,6-己二醇；环脂族二醇如1,4-环己烷二醇、丙三醇、三甲酰基丙烷、三乙醇胺、蔗糖和芳香族类引发剂或其混合物。期望的多元醇为使用环氧丙烷或环氧丙烷和环氧乙烷的组合可获得的那些。
期望地，多元醇组分为或包含聚醚多元醇的共混物。聚醚多元醇的共混物优选地为或包含三醇和二醇的共混物或三醇的共混物。举例来说，期望的三醇和二醇的共混物具有：(a)50％的羟基官能团作为第二羟基官能团；(b)500克/摩尔(g/mol)或更多，优选地600g/mol或更多并且更优选地800g/mol或更多而同时3000g/mol或更少，优选地2500g/mol或更少，更优选地1500g/mol或更少的平均三醇数均分子量；以及(c)4000g/mol或更多，优选地5000g/mol或更多并且更优选地6000g/mol或更多而同时12,000g/mol或更少，优选地10,000g/mol或更少的二醇数均分子量。
期望地，本发明的OCF调配物期望含有少于4wt％，优选地3wt％或更少，更优选地2wt％，甚至更优选地1wt％或更少，又更优选地0.5wt％或更少并且最优选地不含卤代多元醇，其中wt％相对于总OCF调配物重量。以OCF调配物重量计，当卤代多元醇以4wt％或更多的浓度存在时，所得泡沫往往会不当地硬质。
出人意料地，本发明为发现当多元醇组分的每分子具有三个或更多个羟基的多元醇与所有多元醇的总摩尔数的摩尔比(本文比率被称作“rhoB”)为0.75或更少时在DIN4102测试下实现B2等级的出人意料结果的结果。同时，仅当rhoB为0.2或更多时，实现足够的柔性以具有作为“柔性”泡沫的资格。因此，多元醇组分的每分子具有三个或更多个羟基的多元醇与在调配物中所有多元醇的总摩尔数的摩尔比为0.2或更多，优选地0.3或更多，更优选地0.4或更多，再更优选地0.5或更多，又更优选地0.6或更多并且同时为0.75或更少并且可为0.7或更少，0.65或更少或甚至0.6或更少。
本发明的OCF调配物进一步包含磷和卤素两者以便实现在DIN4102测试中的B2性能等级。磷和卤素可在OCF调配物中的同一分子上或在不同分子上。
总的来说，OCF调配物含有浓度为1.5wt％或更多，优选地2wt％或更多并且可为2.5wt％或更多而同时通常为3.5wt％或更少，并且更通常3wt％或更少并且可为2.5wt％或更少并且甚至2wt％或更少的磷，其中wt％相对于不含发泡剂的OCF调配物的总重量。当磷浓度小于1.5wt％时，燃烧性能往往会受损。当磷浓度大于3.5wt％时，所得泡沫往往会收缩。
存在于OCF调配物中的卤素可为任何卤素或卤素的组合，但期望选自氯和溴。优选地，存在氯并且氯可为存在的唯一卤素。OCF调配物可不含溴。总的来说，OCF调配物含有浓度为5.5wt％或更多，优选地6wt％或更多，更优选地6.5wt％或更多并且可为7wt％或更多，7.5wt％或更多并且甚至8wt％或更多而同时通常为11.5wt％或更少，并且可为11wt％或更少，10wt％或更少，9wt％或更少，甚至8wt％或更少的卤素，在wt％的情况下。当卤素的浓度低于5.5wt％时，燃烧性能受损。当卤素的浓度超过11.4wt％时，所得泡沫往往会变得。一般来说，期望使用氯而不是溴，因为溴具有抑制所得泡沫的弹性的倾向。为此，期望溴以1.5wt％或更少，优选地1.0wt％或更少，更优选地0.5wt％或更少的浓度存在并且甚至更优选地OCF调配物不含溴。卤素的wt％相对于不含发泡剂的OCF调配物的总重量。
本发明的OCF调配物进一步包含塑化剂。塑化剂可含有磷、卤素，或磷和卤素两者。实际上，塑化剂可为卤素、磷或磷和卤素两者的唯一来源。塑化剂还可不含卤素、磷或卤素和磷两者。塑化剂用以通过塑化所得的泡沫的聚合物基质而软化由OCF调配物形成泡沫。合适的塑化剂包括：
(a)含有磷和卤素两者的那些塑化剂，如例如三(2-氯乙基)磷酸酯(TCEP)和三(2-氯异丙基磷酸酯(TCPP)；
(b)含有磷但不含有卤素的那些塑化剂，如例如二甲基丙基磷酸酯(DMPP)、三乙基磷酸酯(TEP)、二甲基甲基膦酸酯(DMMP)和二乙基乙基膦酸酯(DEEP)；
(c)含有卤素但不含有磷的那些塑化剂，如例如氯化链烷烃、液体溴化或氯化塑化剂，如以商品名UNIPLEXTMFRP49N-1出售的那些，和液体溴化邻苯二甲酸酯，如以商品名UNIPLEXTMFRP-42出售的那些(UNIPLEX为Unitex化学公司(Unitex ChemicalCorporation)的商标)；以及
(d)既不含有磷也不含有卤素的那些塑化剂，如例如己二酸二甲酯(DMADP)、邻苯二甲酸二丁酯(DBP)、一般来说邻苯二甲酸酯，癸二酸酯、己二酸酯、对苯二甲酸酯、二苯甲酸酯、戊二酸酯、壬二酸酯、环氧化植物油和液体聚丁烯。
尤其期望的塑化剂为三(2-氯异丙基)磷酸酯(TCPP)。塑化剂可完全为TCPP。可仅使用TCPP全部满足塑化剂、卤素和磷浓度。
以总OCF调配物重量计，在OCF调配物中的塑化剂的浓度为15wt％或更多，优选地17wt％或更多并且可为20wt％或更多，甚至25wt％或更多而同时通常为30wt％或更少，优选地25wt％或更少并且可为20wt％或更少并且甚至18wt％或更少。当塑化剂超过25wt％时，所得泡沫往往会收缩。当塑化剂的浓度低于15wt％时，产生差的燃烧性能。
OCF调配物进一步包含发泡剂。当从加压容器喷涂时，发泡剂用以使调配物发泡成为泡沫为了实现期望所得泡沫密度，以不含发泡剂的OCF调配物的克数计，发泡剂通常以1.5毫摩尔或更多，优选地2毫摩尔或更多并且可为2.5毫摩尔或更多，3毫摩尔或更多，甚至4毫摩尔或更多并且同时通常为6毫摩尔或更少，优选地5毫摩尔或更少，更优选地4.5毫摩尔或更少并且可为4毫摩尔或更少，3毫摩尔或更少，甚至2毫摩尔或更少的浓度存在。合适的发泡剂包括选自由以下组成的群组的那些：烷烃如庚烷、己烷、正戊烷、异戊烷、正丁烷、异丁烷、丙烷、环己烷和环戊烷；醚如呋喃、二甲醚、二乙醚、缩甲醛和七氟二甲醚；酮如丙酮和甲基乙基酮；烷基羧酸酯如甲基甲酸酯、二甲基草酸酯和乙酸乙酯；以及卤代烷烃如二氯甲烷、二氟单氯甲烷、二氟甲烷、1,1,1,2-四氟乙烷、二氟乙烷、1-氯-2,2,2,-三氟乙烷、2,2-二氯-2-氟乙烷、氯乙烷、二氯乙烷、五氟丙烷、七氟丙烷；氢卤烯烃和反式-1,3,3,3-四氟丙烯；以及二氧化碳、氩气和氮气。
期望地，发泡剂包含或由以下组成：异丁烷、丙烷和二甲醚。
通常，OCF调配物含有催化剂，如胺催化剂。合适的胺催化剂包括伯胺、仲胺和叔胺，其中叔胺催化剂为尤其期望的。胺催化剂用以引发在羟基或活性氢和异氰酸酯官能团之间的反应。合适的胺催化剂的实例包括二甲基乙醇胺(DMEA)、双(N,N-二甲基-3-氨基-丙基)胺、N,N-二甲基环己胺(CMCHA)、四乙二胺及其混合物。除胺催化剂外的合适的催化剂包括有机金属化合物如二硫醇二丁基锡和羧酸二丁基锡。
尤其期望作为催化剂的为吗啉化合物，如N-乙基吗啉；N,N-二甲基氨基乙基吗啉；以及N,N'-二吗啉二乙醚。
催化剂期望以至少5毫当量重量的氮气/克摩尔的-NCO官能团(meqN/gmol NCO)，优选地10或更多meqN/gmol NCO或更多并且更优选地15或更多meqN/gmol NCO的浓度存在于OCF调配物中，并且同时期望以100meqN/gmol NCO或更少，优选地75meqN/gmol NCO或更少并且最优选地50meqN/gmol NCO或更少的浓度存在。
OCF调配物期望包含至少一种表面活性剂。表面活性剂可用于提供在发泡剂和成分的其余部分之间的乳化稳定性以及在分配和固化期间为所得泡沫泡孔结构提供稳定性。合适的表面活性剂包括聚硅氧烷聚环氧烷表面活性剂。以总OCF调配物重量计，表面活性剂通常以0.5wt％或更多，优选地1.5wt％或更多并且更优选地2.0wt％或更多而同时通常5.0wt％或更少，优选地4.0wt％或更少并且最优选地3.0wt％或更少的浓度存在。
本发明的OCF调配物可进一步包含或不含以下组分的任一种或多于一种的任何组合：开孔剂(如含硅酮的表面活性剂)、交联剂和扩链试剂(如1,4-丁二醇、丙三醇、二乙醇胺、三乙醇胺、乙二胺、二甲苯二胺和亚甲基双(邻氯苯胺))、硅烷封端的醇、抗氧化剂和着色剂以及提供尺寸稳定性的佐剂(如聚丁二烯弹性体)。合适的聚丁二烯弹性体包括粘度为至少500毫帕斯卡，优选地至少2帕斯卡(Pa)并且更优选地至少3Pa(如在20摄氏度(℃)下测量)的那些聚丁二烯弹性体。一种尤其合适的聚丁二烯弹性体包含约75wt％1,4-顺式双键，大约24wt％1,4-反式双键和大约1wt％乙烯基双键并且分子量(蒸气压渗透)为大约3000克/摩尔。以总OCF调配物重量计，聚丁二烯可以在0.03wt％到1.0wt％范围内的浓度存在。以总OCF调配物称重计，聚亚辛烯(polyoctenylene)还可或可替代地以在0.02wt％到0.5wt％范围内的浓度存在。聚丁二烯和聚亚辛烯的数均分子量优选地为约800g/mol到10,000g/mol并且优选地数均分子量的范围为约1,000g/mol到6,000g/mol并且尤其为约1,500g/mol到4,000g/mol。
与WO2010/058036的调配物和泡沫不同，本发明的OCF调配物和所得泡沫不含可膨胀石墨。WO2010/058036使用可膨胀石墨来改进阻燃特性。然而，本发明OCF调配物不需要可膨胀石墨实现在DIN 4012测试中的要求的B2等级。
本发明进一步包括使用本发明的OCF调配物的方法。方法包含分配来自加压器皿的OCF调配物以形成聚氨酯泡沫。通常提供OCF调配物用于加压器皿(即，容器)。当从容器释放时，OCF调配物就膨胀成泡沫并且在它周围的空气中的水分存在下固化以形成柔性泡沫。OCF调配物尤其很好地被设计成充当用于方法的穿孔开口密封剂，所述方法包括将来自加压器皿的OCF调配物分配到穿孔开口周围或与穿孔开口相邻的间隙中。通常，OCF调配物分配在间隙内的条中使得条膨胀成厚度为30毫米(mm)或更少，优选地25mm或更少，更通常20mm或更少，并且可为17mm或更少，15mm或更少，13mm或更少，12mm或更少并且甚至10mm或更少的泡沫。常常，当填充间隙，如穿孔开口周围的间隙时，泡沫厚度对应于间隙的宽度，因为间隙具有大于其宽度的深度。因此本发明的OCF调配物可用于填充具有如上文对于泡沫厚度所描述的宽度的间隙。
OCF调配物膨胀成实现在DIN 4102测试中的B2等级的柔性聚氨酯泡沫。这是满足聚合泡沫的尤其难的标准但变成在世界范围的某些地区中泡沫构建材料的需要。
柔性聚氨酯泡沫期望为开孔泡沫，这意指它具有大于50％，优选地60％或更多，更优选地70％或更多并且可具有80％或更多，90％或更多并且甚至100％开孔含量，如通过ASTM D6226测试测定。泡沫的开孔特性允许发泡剂从泡沫逸出并且还允许一些程度的蒸气渗透。期望地，柔性聚氨酯泡沫展现在0.05升/分钟和1.2升/分钟范围内的空气流速，如通过ASTM D3574测定，以实现发泡剂和蒸气渗透性而不显著牺牲热绝缘特性。
柔性聚氨酯泡沫还期望特征在于密度为25千克/立方米(kg/m3)或更多，并且可为30kg/m3或更多，35kg/m3或更多并且甚至40kg/m3或更多而同时通常为50kg/m3或更少，优选地45kg/m3或更少并且可为40kg/m3或更少。根据ISO 845-95测定泡沫密度。
实例
以下实例用以进一步说明本发明的实施例。用于OCF调配物的组分的说明在表1中。特定调配物和分析如下。
表1
VORANATE、VORANOL为陶氏化学公司的商标。ACCLAIM为拜耳材料科技(BayerMaterialScience)的商标。REACTINT为Mililiken和公司(Mililiken&Company)的商标。NIAX为通用电气公司(General Electric Company)的商标。JEFFCAT为摩根大通银行(JPMorgan Chase Bank)的商标。SAYTEX为雅保公司(Albemarle Corporation)的商标。PHT4为大湖化学公司(Great Lakes Chemical Corporation)的商标。
制备和泡沫表征
对于以下实例(Ex)和比较实例(Comp Ex)中的每个，通过将除发泡剂(BA)组分外的调配物组分引入到镀锡钢罐并且密封罐以便具有提供流体连通到罐的阀门来制备OCF调配物。将适当量的BA1和然后BA2注入到罐中。
通过从罐分配一条OCF调配物并且允许泡沫固化获得每个Ex和Comp Ex的泡沫样品。按照以下方式表征泡沫：
燃烧性能。根据DIN4102测试表征20mm宽泡沫样品，其为20mm厚、50mm宽和190mm长并且以190mm长度向上延伸取向成在竖直方向上。样品位于具有20mm的标称间隙的两个石膏板之间。
密度。在水中使用ISO845-95体积方法表征每个调配物的300mm长和30mm的直径的圆柱形泡沫珠粒样品。
压缩回复率。根据ISO 1856表征19mm厚、50mm宽和50mm长泡沫样品。计算压缩回复率为100％减去以％计的压缩永久变形，如在75％压缩维持72小时接着回复至少24小时(方法B)l之后根据以上标准测定。
开孔含量。根据ASTM D6226对19mm厚、51mm宽和51mm长的样品测定开孔含量。
空气流速。使用19mm厚、51mm宽和51mm长泡沫样品使用来自TEXTEST仪器(TEXTESTInstruments)的TEXTEST FX3300设备使用其标准测试程序测定通过泡沫的空气流速。
多元醇官能度比率的影响
以下实例(Ex)和比较实例(Comp Ex)示出了具有在0.2到0.75范围内的rhoB值的重要性。调配物和表征在表2中。在调配物中的组分以相对于总调配物重量的wt％报告。
在表2中的数据示出如果rhoB小于0.2，那么所得泡沫不能实现在DIN4102测试中的B2等级，并且当rhoB大于0.75时，分配的调配物塌陷并且不能形成泡沫。
表2
*NA-泡沫塌陷，所以不可表征。
溴化多元醇的影响
以下比较实例(Comp Ex)示出了溴化多元醇的影响。调配物和表征在表3中。在调配物中的组分以相对于总调配物重量的wt％报告。
在表3中的结果示出了测试的溴的含量仍然允许泡沫实现B2等级，但泡沫不再为柔性因为它具有小于45％的弹性回复率。
表3
塑化剂的影响
以下实例(Ex)和比较实例(Comp Ex)示出了溴化多元醇的影响。调配物和表征在表4中。在调配物中的组分以相对于总调配物重量的wt％报告。
在表4中的结果示出了过少的塑化剂产生非柔性泡沫并且过多的塑化剂产生泡的塌陷并且不能形成有意义的泡沫。当7.5wt％TCPP用作塑化剂时，所得泡沫不是柔性也不实现B2防火等级(参见Comp Ex F)。当使用15wt％和30wt％TCPP时，泡沫为柔性且期望的(参见Ex 5和Ex 6)。当使用40wt％TCPP时，调配物塌陷(参见Comp Ex G)。
表4
*NM指示此特性未测量，但预期类似于Ex 4。
NA*不可适用，因为未获得有意义的泡沫。
不同多元醇和异氰酸酯的影响。
以下实例(Ex)示出了用脂族或芳香族多元醇和异氰酸酯制备本发明的OCF调配物的能力。调配物和表征在表5中。在调配物中的组分以相对于总调配物重量的wt％报告。
Ex 7使用官能度大于3的芳香族聚醚多元醇。Ex 8使用官能度大于3的脂族聚醚多元醇。Ex 9使用比前述实例高的官能异氰酸酯。Ex 10和Ex 11使用不同NCO含量。
表5

Claims (10)

1.一种单组分喷涂聚氨酯泡沫调配物，所述单组分喷涂聚氨酯泡沫调配物特征在于包含：
(a)聚合物异氰酸酯，其标称官能度在2.5到3.5的范围内并且以足以提供以在所述调配物中异氰酸酯和多元醇的总重量计的10重量％到20重量％NCO官能团的浓度存在；
(b)多元醇组分，以总多元醇组分重量计其为至少85重量％脂族多元醇并且每分子具有三个或更多个羟基的多元醇与所有多元醇的总摩尔数的摩尔比在0.2到0.75的范围内；
(c)塑化剂，以总调配物重量计其浓度在15重量％到30重量％的范围内；
(d)磷，以不含发泡剂的总调配物的重量计浓度在1.5重量％到3.5重量％的范围内；
(e)卤素，以不含发泡剂的总调配物的重量计浓度在5.5重量％到11.5重量％的范围内；
(f)发泡剂，其浓度在每克的不含发泡剂的调配物重量1.5毫摩尔到5毫摩尔的范围内；
其中所述调配物的特征进一步在于为不含可膨胀石墨。
2.根据权利要求1所述的单组分喷涂聚氨酯泡沫调配物，其特征进一步在于所述塑化剂选自由以下组成的群组：三(1-氯-2-丙基)磷酸酯、三乙基磷酸酯和二甲基丙基膦酸酯。
3.根据权利要求1或权利要求2所述的单组分喷涂聚氨酯泡沫调配物，其特征进一步在于所述调配物不含卤代多元醇。
4.根据前述权利要求中任一项所述的单组分喷涂聚氨酯泡沫调配物，其特征进一步在于所述塑化剂提供在所述单组分喷涂聚氨酯泡沫调配物中的所有的卤素和磷。
5.根据前述权利要求中任一项所述的单组分喷涂聚氨酯泡沫调配物，其特征进一步在于所述塑化剂为三(2-氯丙基)磷酸酯。
6.根据前述权利要求中任一项所述的单组分喷涂聚氨酯泡沫调配物，其特征进一步在于不含溴。
7.一种使用前述权利要求中任一项所述的单组分喷涂聚氨酯泡沫调配物的方法，所述方法包含分配来自加压器皿的所述单组分喷涂聚氨酯泡沫调配物以形成聚氨酯泡沫。
8.根据权利要求7所述的方法，其特征进一步在于所述聚氨酯泡沫的厚度小于30毫米。
9.根据权利要求7或权利要求8所述的方法，其特征进一步在于在与穿孔开口相邻的开口中分配所述单组分喷涂聚氨酯泡沫调配物。
10.根据权利要求7至9中任一项所述的方法，其特征进一步在于如根据ISO 1856测定，在压缩所述泡沫原始厚度的75％维持三天之后在24小时中所述泡沫具有大于45％的压缩回复率，如根据ASTM D6226测定，所述泡沫具有70％或更多的开孔含量，如通过ASTM D3574测定空气流速在0.001升/秒和0.02升/秒的范围内并且实现在DIN 4102测试中的B2等级。
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ES2695536T3 (es) 2019-01-08
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