CN116323736A - 柔性聚氨酯泡沫以及其配制物 - Google Patents
柔性聚氨酯泡沫以及其配制物 Download PDFInfo
- Publication number
- CN116323736A CN116323736A CN202180067912.9A CN202180067912A CN116323736A CN 116323736 A CN116323736 A CN 116323736A CN 202180067912 A CN202180067912 A CN 202180067912A CN 116323736 A CN116323736 A CN 116323736A
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- CN
- China
- Prior art keywords
- polyol
- polyurethane foam
- flexible polyurethane
- foam
- silica
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 174
- 229920005862 polyol Polymers 0.000 claims abstract description 128
- 150000003077 polyols Chemical class 0.000 claims abstract description 123
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 6
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- GTEXIOINCJRBIO-UHFFFAOYSA-N 2-[2-(dimethylamino)ethoxy]-n,n-dimethylethanamine Chemical compound CN(C)CCOCCN(C)C GTEXIOINCJRBIO-UHFFFAOYSA-N 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004604 Blowing Agent Substances 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000004971 Cross linker Substances 0.000 description 2
- 229920000538 Poly[(phenyl isocyanate)-co-formaldehyde] Polymers 0.000 description 2
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- 125000001931 aliphatic group Chemical group 0.000 description 2
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- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 2
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Abstract
柔性聚氨酯泡沫,其包含最高达10wt%的具有50至150m2/g的表面积的气相二氧化硅,其中气相二氧化硅在其表面处具有C1‑C3烷基硅烷基,柔性聚氨酯泡沫表现出具有至少40%例如40%至70%的回弹性,不大于15%例如3%至15%的干压缩永久变形,或这两者。替代地或另外,柔性聚氨酯泡沫可具有如下的通过ASTM D3574测量的在50%的压缩力挠度:与具有相同组成但用多元醇代替二氧化硅的柔性聚氨酯泡沫相比大至少30%,例如,至少50%、至少70%、或30%至155%。
Description
技术领域
本发明涉及用于柔性聚氨酯泡沫的配制物和用其制成的聚合物泡沫。
背景技术
术语“聚氨酯”描述了各种各样的聚合物组合物(compositions,组分)。这些聚合物组合物中的每一种都含有其重复单元包括-N-CO-O-键的聚合物。此外,聚氨酯还可包括脲(-N-CO-N-)键。然而,这些聚氨酯和脲键之间的分子链的组成以及制造聚合物的方法也影响最终性质。因此,具有不同组成和/或通过不同方法制造的聚氨酯用于各种应用,范围从胶粘剂到涂料到弹性体到不同类型的泡沫。通常,聚氨酯通过多异氰酸酯与多元醇(或多胺,以生产聚脲)反应而生产。两种不同的多元醇可用于产生嵌段共聚物。例如,低分子量二醇和二胺导致形成短链,所述短链通过氢键缔合形成结晶域。通过使用聚醚或聚酯多元醇可形成第二“较软”嵌段,这导致无定形域。这样的嵌段共聚物组合物典型地用于形成热塑性聚氨酯(TPU)。聚合物的拉伸性质取决于拉伸力如何干扰结晶域中的氢键。
替代地,聚氨酯泡沫典型地通过在发泡剂的存在下二异氰酸酯与多元醇和多胺的反应而形成。机械性质部分地取决于刚性脲键和更柔性聚氨酯键之间的对比,而不是利用结晶域。发泡剂可为辅助剂,例如挥发性有机化合物,或者可原位生成。向反应混合物添加水导致两个竞争反应,缩聚以及通过异氰酸酯和水之间的反应生成二氧化碳。增加多元醇和异氰酸酯的官能度增加聚合期间更早的交联密度,加强孔壁以及在很大程度上防止增加的二氧化碳压力破坏孔壁,从而增加泡沫的刚性。刚性(闭孔)聚氨酯泡沫典型地用于隔热,而柔性(开孔)聚氨酯泡沫用于缓冲和隔音。
在聚氨酯中通常采用各种填料来改变其机械、电和其他性质。可将这些填料与聚合材料结合,例如通过熔融混合,或者在原位方法中缩聚之前并入到预聚物组合物中。在原位方法中采用的填料必须满足两个功能。它们不仅需要为最终产品提供期望的性质,而且还不能干扰聚合和发泡过程以生成该产品。
气相二氧化硅(fumed silica)经常用于控制聚氨酯泡沫的触变性和孔隙尺寸。在JP04850574中,将气相二氧化硅熔融混合到聚合的聚氨酯组合物中,然后注入二氧化碳以产生孔隙。同样,气相二氧化硅在US20080153935中用作泡沫稳定剂。尽管如此,仍然期望在原位方法中将气相二氧化硅并入到柔性聚氨酯泡沫中(其中在缩聚之前将气相二氧化硅与前体材料结合),并且允许二氧化硅有助于最终材料的机械性质。
发明内容
在表面处具有三甲基硅烷基(trimethylsilyl)的低表面积二氧化硅与叔胺催化剂结合使用使得原位聚合方法能够产生具有有益性质的柔性聚氨酯泡沫。
在一个实施方案中,生产柔性聚氨酯泡沫的方法包括:提供包含至少第一多元醇以及最高达10wt%的具有50至150m2/g的表面积的气相二氧化硅的多元醇组合物,所述第一多元醇具有3000至6000的重均分子量和2.5至3.5的官能度,其中气相二氧化硅在其表面处具有C1-C3烷基硅烷基(alkylsilyl),将多元醇组合物、具有1.8至2.5的官能度的多异氰酸酯、水和叔胺催化剂结合以形成预聚物组合物,允许预聚物组合物聚合以形成具有1.8至4pcf的密度以及a)至少40%,例如40%至70%的回弹性、b)不大于15%,例如3%至15%的干压缩永久变形或两者的开孔泡沫结构。柔性聚氨酯泡沫可表现出1.8至3pcf的密度或2至4pcf的密度。
多异氰酸酯可包含六亚甲基二异氰酸酯(HDI),亚苯基二异氰酸酯(PDI),2,4-甲苯二异氰酸酯(2,4-TDI),2,6-甲苯二异氰酸酯(2,6-TDI),4,4’-二苯基甲烷二异氰酸酯(MDI),二苯基甲烷二异氰酸酯的异构体混合物,或这些中的两种或更多种的混合物。第一多元醇可包含聚醚多元醇或聚酯多元醇。所述多元醇组合物可进一步包含第二多元醇,所述第二多元醇具有2000至10000的重均分子量。气相二氧化硅可具有50至150m2/g或50至100m2/g的BET表面积。所述C1-C3烷基硅烷基(alkylsilyl)可为三甲基硅烷基(trimethylsilyl)或二甲基硅烷基(dimethylsilyl)。
允许可包括将预聚物组合物装入到具有对气氛(大气,atmosphere)开放的一侧的模具中,并且所得柔性聚氨酯泡沫可具有1.8至3pcf的密度。替代地,可包括将预聚物组合物装入到模具中并且封闭模具,并且所得柔性聚氨酯泡沫可具有2至4pcf的密度。
柔性聚氨酯泡沫可具有如下的通过ASTM D3574测量的在50%的压缩力挠度(compression force deflection,压缩力偏移):相对于通过相同方法但用相等质量份的第一多元醇代替二氧化硅生产的柔性聚氨酯泡沫,提高至少30%,例如,至少50%,至少70%,或30%至155%。
在另一个实施方案中,柔性聚氨酯泡沫包含最高达10wt%的具有50至150m2/g的表面积的气相二氧化硅,其中气相二氧化硅在其表面处具有C1-C3烷基硅烷基,柔性聚氨酯泡沫表现出至少40%,例如40%至70%的回弹性,不大于15%,例如3%至15%的干压缩永久变形,或两者。气相二氧化硅可具有50至150m2/g或50至100m2/g的BET表面积。所述C1-C3烷基硅烷基可为三甲基硅烷基或二甲基硅烷基。柔性聚氨酯泡沫可为经模塑的泡沫或自由起发泡沫。聚氨酯泡沫可包含聚醚聚氨酯或聚酯聚氨酯。柔性聚氨酯泡沫可具有1.8至4pcf的密度,例如1.8至3pcf的密度或2至4pcf的密度。
柔性聚氨酯泡沫可具有如下的通过ASTM D3574测量的在50%的压缩力挠度:与具有相同组成但用多元醇代替二氧化硅的柔性聚氨酯泡沫相比大至少30%,例如,至少50%,至少70%,或30%至155%。
应理解,前述一般描述和以下详细描述都只是示例性的和解释性的,并且旨在提供本发明的进一步解释,如要求保护的那样。
附图说明
本发明参照附图的几个图进行描述,其中,
图1显示了用具有不同表面化学性质的气相二氧化硅制备的多元醇分散体的粘度。
图2显示了用具有不同表面积的气相二氧化硅制备的多元醇分散体的粘度。
图3显示了用疏水和亲水(未处理)气相二氧化硅制备的多元醇分散体的粘度。
具体实施方式
在一个实施方案中,生产柔性聚氨酯泡沫的方法包括:提供包含至少第一多元醇以及最高达10wt%的具有50至150m2/g的表面积的气相二氧化硅的多元醇组合物,所述第一多元醇具有3000至6000的重均分子量和2.5至3.5的官能度,其中气相二氧化硅在其表面处具有C1-C3烷基硅烷基,将多元醇组合物、具有1.8至2.5(例如1.8至2.25)的官能度的多异氰酸酯、水和叔胺催化剂结合以形成预聚物组合物,以及允许预聚物组合物在形成具有1.8至4pcf的密度的开孔泡沫结构的条件下聚合。
柔性聚氨酯泡沫典型地通过在发泡剂的存在下二异氰酸酯与多元醇和多胺的反应而形成。对于柔性开孔泡沫,多元醇典型地具有2.5-3.5的官能度,但在某些情况下可使用更高官能度的多元醇。这导致与多元醇官能度明显更高(例如4.5至5)的刚性泡沫相比更少的交联。同样,与异氰酸酯官能度典型地为约2.7或更大的刚性泡沫相比,使用具有高达2.5的官能度的多异氰酸酯,例如具有1.8至2.25的官能度的二异氰酸酯或多异氰酸酯,也降低了交联密度。
用于本文提供的配制物和方法的适当的异氰酸酯包括用于聚氨酯泡沫的任何有机异氰酸酯。芳族异氰酸酯是优选的,但也可使用脂族、脂环族和芳脂族(araliphatic)异氰酸酯。示例性异氰酸酯例如间亚苯基二异氰酸酯,2,4-和/或2,6-甲苯二异氰酸酯(TDI),二苯基甲烷二异氰酸酯(MDI)的各种异构体,六亚甲基-1,6-二异氰酸酯,四亚甲基-1,4-二异氰酸酯,环己烷-1,4-二异氰酸酯,六氢甲苯二异氰酸酯,氢化MDI(H12MDI),萘-1,5-二异氰酸酯,甲氧基苯基-2,4-二异氰酸酯,4,4′-联亚苯基二异氰酸酯,3,3′-二甲氧基-4,4′-联苯二异氰酸酯,3,3′-二甲基二苯基甲烷-4,4′-二异氰酸酯,4,4′,4″-三苯基甲烷三异氰酸酯,聚亚甲基多苯基异氰酸酯或其与MDI的混合物,氢化聚亚甲基多苯基异氰酸酯,甲苯-2,4,6-三异氰酸酯,和4,4′-二甲基二苯基甲烷-2,2′,5,5′-四异氰酸酯,或这些的混合物。三异氰酸酯优选地以与足够的二异氰酸酯的混合物的形式使用,以产生2至2.25的总官能度。
用于本文提供的配制物和方法的适当的聚合物多元醇包括聚醚多元醇和聚酯多元醇两者以及本领域技术人员已知的其他聚合物多元醇。合适的多元醇典型地具有3000至6000的分子量,优选重均分子量。用于开孔泡沫的适当的聚合物多元醇具有2.5至3.5,例如为2.5至3的羟基数。也可使用多元醇混合物。例如,可将具有较低或较高分子量的多元醇结合以提供期望的平均多元醇分子量。因此,可将一种或多种具有2000至10000的重均分子量的另外的多元醇与第一多元醇结合。
聚醚多元醇可通过使小分子多元醇与环氧烷反应形成聚醚多元醇而获得。示例性小分子多元醇包括但不限于乙二醇、二乙二醇、三乙二醇、1,2-丙二醇、三亚甲基二醇、四亚甲基二醇、六亚甲基二醇、甘油、二甘油、山梨醇、季戊四醇、蔗糖和双酚A。示例性聚醚包括聚环氧烷例如聚环氧乙烷、聚环氧丙烷和聚四亚甲基氧化物。替代地或另外,聚合物多元醇可通过使乙烯基单体例如苯乙烯或丙烯腈与多元醇共聚来生产。
聚酯多元醇可通过使小分子多元醇(例如以上描述的那些)与聚酯反应而获得。示例性聚酯包括本领域技术人员已知的用于柔性聚氨酯泡沫的任何聚酯,并且可由有机二羧酸(例如用羧酸基团封端的C2-C12未支化脂族链)和二官能或三官能醇(例如C2-C12亚烷基二醇或聚醚醇)生产。
也可采用聚合物多元醇的混合物。示例性聚合物多元醇包括公开于US201800223030、US9034936和US10119002(其全部内容通过引用的方式并入本文)中的那些,条件是多元醇配制物(一种或多种多元醇)应具有2.5至3的总体官能度(即,每个分子的羟基数)。
叔胺催化剂相对于金属和低阶胺催化剂是优选的,以减少气相二氧化硅和多元醇之间对催化剂的竞争。示例性叔胺催化剂包括本领域技术人员已知适合用于生产聚氨酯泡沫的任何叔胺催化剂,包括但不限于二甲基乙醇胺、三亚乙基二胺、四甲基丙二胺、四甲基六甲基二胺和二甲基环己基胺。
也可采用本领域技术人员已知的用于开孔聚氨酯泡沫的另外的组分。实例包括表面活性剂、粘度调节剂、交联剂、扩链剂、颜料、阻燃剂、辅助胶凝催化剂、辅助吹泡催化剂以及这些中任何一种的组合。另外的多元醇也可用于向聚氨酯引入不同的共聚物或官能团,例如促进孔形成或孔开放。另外的填料例如苯乙烯丙烯腈珠、硫酸钡或碳酸钙,可与本文提供的气相二氧化硅结合采用。
气相二氧化硅典型地通过火成方法生产,其中将包含燃料(例如甲烷或氢)、氧和挥发性硅化合物的气态原料进料到燃烧器中。通过燃料在氧中的燃烧形成的水以液体或气态形式与挥发性硅化合物反应,以生产二氧化硅颗粒。这些颗粒聚结和聚集以形成气相二氧化硅。
在聚氨酯泡沫的形成期间,期望平衡配制物的性质,以协调二氧化碳气泡的生长与多元醇组分的交联。如果配制物太粘稠,则通过水与异氰酸酯的反应形成的二氧化碳的扩散将减慢。另外,膨胀气体将不施加足够的压力以置换液体配制物和形成适当尺寸的气泡。分散在液体体系中的二氧化硅通过两种不同的相互作用影响其流变性质。首先是单个二氧化硅颗粒之间的吸引力。气相二氧化硅的聚集的结构允许其形成链状网络,其可在搅动或剪切下中断,使气相二氧化硅成为有效的触变胶。这些网络的形成有利于具有高表面积(小初级颗粒)二氧化硅的体系。因此,在优选的实施方案中,本文中使用的气相二氧化硅具有不大于150m2/g,例如不大于130m2/g或不大于100m2/g的通过氮吸附(ASTM D1993)测量的表面积。第二种相互作用是液体基质和二氧化硅表面之间的相互作用。在亲水多元醇体系中,高度疏水的且对多元醇具有低的亲和力的经过表面处理的二氧化硅预期具有强的颗粒-颗粒相互作用并且促进高屈服应力。相比之下,未经表面处理的二氧化硅良好地分散在液体(例如水或甲醇)中,并且不显著改变粘度。因此,在复杂配制物中,对二氧化硅表面的仔细改性可对体系流变具有巨大影响。
所制备的气相二氧化硅是亲水的,在表面上具有多个Si-OH基团。这些硅醇基团可通过氢键与醇相互作用,以及通过酸-碱相互作用与聚醚的氧亚烷基基团相互作用。因此,未经处理的二氧化硅预期对多元醇粘度具有小的影响。然而,二氧化硅的羟基在聚合中可与多元醇的羟基竞争。二氧化硅的疏水化封盖了一定比例的硅醇基团。然而,疏水化也改变二氧化硅与预聚物配制物和最终聚合物之间的界面相互作用,潜在地改变预聚物配制物的粘度行为和/或柔性聚氨酯泡沫的机械性质。此外,疏水化处理优选不干扰聚合反应。
已经出乎意料地发现,气相二氧化硅用在表面上留下短烷基硅烷基的试剂的疏水化减少了二氧化硅与聚合物多元醇的竞争,而不会不期望地增加粘度。相比之下,在表面上用较大烷基或硅氧烷基链进行的表面处理太疏水,并且将不利地影响泡沫发展。优选的表面处理在表面上留下C1-C3烷基硅烷基,例如三甲基硅烷基、二甲基硅烷基、乙基硅烷基或甲基乙基硅烷基。硅烷基可通过一个、两个或三个硅氧烷键连接至气相二氧化硅的表面,或者可通过硅氧烷键连接至一个或两个相邻的烷基硅烷基团。
因此,气相二氧化硅可用硅氮烷例如六甲基二硅氮烷或烷基硅烷例如二甲基二氯硅烷、甲基三甲氧基硅烷、甲基三氯硅烷、甲基三甲氧基硅烷、甲基三乙氧基硅烷、二甲基二甲氧基硅烷、二甲基二乙氧基硅烷、三甲基氯硅烷、三甲基甲氧基硅烷、三甲基乙氧基硅烷、乙基三乙氧基硅烷、乙基三氯硅烷、乙基三甲氧基硅烷、丙基三氯硅烷、丙基三甲氧基硅烷、丙基三甲氧基硅烷、丙基三乙氧基硅烷、乙基甲基二氯硅烷以及其他C1-C3直链和支链烷基硅烷疏水化。
气相二氧化硅的高表面积和支链结构也增强了其与周围聚合物基质的表面相互作用。这种相互作用允许二氧化硅比溶胶凝胶或沉淀二氧化硅更有效地增强聚合物泡沫。因此,期望二氧化硅具有足够的表面积,例如,至少50或60m2/g,以提供增强。
聚氨酯的组分可使用本领域技术人员已知的任何方法进行结合和聚合。优选地,根据本领域技术人员已知的方法将气相二氧化硅分散在多元醇中,然后可在与多异氰酸酯结合和聚合之前与聚氨酯的一种或多种剩余非异氰酸酯组分结合。聚氨酯泡沫可为自由起发泡沫,其中聚合发生在对大气压开放的容器中,或经模塑的泡沫,其中聚合发生在封闭的模具中。在将未聚合的材料装入到模具中之后封闭模具为聚氨酯泡沫的膨胀创造了受限的空间。因此,泡沫的密度可通过改变封闭的模具中的材料的量来部分地控制,而自由起发泡沫的密度可通过调整配制物以控制二氧化碳的生成以及聚合和二氧化碳形成的相对速率来控制。典型的自由起发泡沫的密度为1.8至3pcf,而典型的经模塑的泡沫的密度为2至4pcf。
对于自由起发或经模塑的泡沫,如本文所述的二氧化硅的使用为泡沫提供了增强,而不显著降低由泡沫的开孔结构所赋予的柔韧性。优选地,聚氨酯泡沫具有至少40%,例如40%至70%的回弹性。替代地或另外,聚氨酯泡沫具有不大于15%,例如3%至15%的干压缩永久变形。替代地或另外,如本文所述的气相二氧化硅的添加提高压缩力挠度。例如,相对于无二氧化硅配制物,通过ASTM D3574、Test C测量的在50%的CFD可提高至少30%,例如至少50%,至少70%,或30%至155%。
本发明将通过以下实施例进一步阐明,这些实施例旨在性质上仅为示例性的。
实施例
实施例1
将CAB-O-SIL TG-6110疏水气相二氧化硅(具有85m2/g的BET表面积和在表面处的三甲基硅烷基)(Cabot Corporation)分散在Pluracol 2090聚醚多元醇三醇(BASF)中,以形成15wt%的分散体。使用SpeedMixer(Flackteck,Landrum,Sc)然后使用全混合器(plenary mixer)(PC Laborsystem Labotop)以350g批次生产二氧化硅分散体。将多元醇称重到600g塑料容器中,以及分阶段添加二氧化硅,直到所有材料都加入。然后将材料以2350rpm混合5分钟以及冷却至室温。该混合序列再重复三次,总共混合20分钟,以确保完全混合。将两批次结合以及在全混合器中在1bar真空下脱气15分钟。如表1-1中所示将适当量的分散体和另外的Pluracol 2090多元醇装入到400mL聚乙烯烧杯中,与表1-2中列出的量的另外的组分一起,以制备具有按多元醇组分的总重量计0%、2%、4%、6%、8%和10%气相二氧化硅的多元醇组分配制物。二氧化硅-多元醇分散体可用作基于质量的等量的纯多元醇的直接(drop-in)替代物,以在多元醇组分中实现期望的气相二氧化硅浓度。用97gPluracol 2090多元醇和表1-2中列出的量的另外的原材料制备无二氧化硅对照多元醇组分。使用高扭矩混合器(CRAFSTMAN 10-Inch Drill Press,Model No.137.219000)在环境温度下以3,100rpm持续7s将多元醇组分与多异氰酸酯(Suprasec 7007多异氰酸酯;Huntsman)以表1-3中所示的量(异氰酸酯指数=90)在400mL三倒(tri-pour)聚乙烯杯中结合,然后转移到聚乙烯衬里盒(6”x6”x3”;15.24x15.24x7.62cm)中。在泡沫起发完成之后,将所有泡沫放入到预热至70℃的空气循环烘箱中持续30min以完成固化。对于每种配制物制备三个样品。
表1-1
实施例 | 1C(无二氧化硅) | 1-1 | 1-2 | 1-3 | 1-4 | 1-5 |
多元醇组分中的气相二氧化硅% | 0 | 2 | 4 | 6 | 8 | 10 |
分散体的量(g) | 0 | 14.2 | 28.36 | 42.54 | 56.71 | 70.89 |
另外的Pluracol 2090(g) | 97 | 82.8 | 68.64 | 54.46 | 40.29 | 26.11 |
添加的水(g) | 3.45 | 3.44 | 3.44 | 3.44 | 3.44 | 3.44 |
表1-2
表1-3
实施例 | 1C(无二氧化硅) | 1-1 | 1-2 | 1-3 | 1-4 | 1-5 |
多元醇组分的总质量(g) | 106.35 | 106.34 | 106.34 | 106.34 | 106.34 | 106.34 |
异氰酸酯量(g) | 61.74 | 61.60 | 61.45 | 61.31 | 61.16 | 61.01 |
矩形泡沫通过以下表征:泡沫密度(ASTM D3574,Test A),通过球反弹的回弹性(ASTM D3574,Test H),断裂拉伸强度(ASTM D3574,Test E),断裂伸长率(ASTM D3574,Test E),在25%、50%和65%的压缩力挠度(ASTM D3574,Test C),撕裂强度(ASTM D-624,Die C),和平均孔尺寸(ASTM D3576)。
具有基于总多元醇组分计2%和4%气相二氧化硅(基于总泡沫重量计分别为1.3%和2.5%)的泡沫的表观泡孔结构是均匀的,并且与参照泡沫相比,气相二氧化硅对孔尺寸没有显著影响(表1-4)。然而,具有基于总多元醇组分计6%气相二氧化硅(基于总泡沫重量计3.8%)的泡沫表现出略微粗糙的孔结构。随着配制物中的气相二氧化硅的量的进一步增加,孔结构变得更粗糙。
表1-4
基于总泡沫重量计的1.3%和2.5%的气相二氧化硅的引入对密度、回弹性、拉伸强度和伸长率没有显著影响(表1-4)。然而,随着引入如此少量的气相二氧化硅,撕裂强度和压缩力挠度(CFD)值显著增加(表1-4)。
在用基于总泡沫重量计的3.8%、5.1%和6.4%的气相二氧化硅(采用具有6%、8%和10%的气相二氧化硅的多元醇组分)生产的泡沫的泡沫起发期间观察到排气。孔结构也更粗糙。据推测,这是由气相二氧化硅的孔开放效应(cell-opening effect)引起的。然而,这些样品分别表现出3.29±0.21、3.86±0.20和4.21±0.46的在50%的CFD,表明二氧化硅仍然为泡沫提供增强。
实施例2
为了优化孔结构,使用具有10%气相二氧化硅的多元醇组分,使用上述方法和以下表2-1中所列出的配制物制备另外的泡沫,其中调节表面活性剂(Tegostab B 4690表面活性剂)和开孔多元醇(Lumulse POE 26多元醇)浓度以及碳酸亚丙酯(1,2丙二醇环状碳酸酯99.7%,Sigma-Aldrich)至一些配制物的多元醇组分以降低粘度。将约一半的多元醇组分(如表2-1中所示的量)与足够的异氰酸酯(异氰酸酯指数为90)在400mL三倒聚乙烯杯中(表2-1中的确切量)结合,如实施例1所述混合7s,倒入到1000mL聚乙烯三倒烧杯中以及允许自由起发。
表2-1
*添加的水加上残留的水=3.6g
如表2-1中所示,当表面活性剂浓度增加时,孔结构没有改进(实施例2-1和2-2)。然而,当孔开口多元醇(cell-opening polyol)的量减少时,孔结构显著改进(实施例2-3和2-4)。粘度也可影响发泡过程-添加碳酸亚丙酯也降低了孔结构的粗糙度,尤其是与减少量的开孔多元醇结合时(实施例2-5、2-6、2-7)。
实施例3
如下生产开孔聚氨酯泡沫:用以下表3-1中所示的在多元醇组分配制物中具有0%(对比)、6%、8%和10%CAB-O-SIL TG-6110气相二氧化硅的多元醇组分(类似于实施例2-6),使用实施例1中描述的方法(异氰酸酯指数为90)与以下所示的量的异氰酸酯结合,以及如实施例1中所述分配到6”x6”x3”聚乙烯衬里盒中以及允许自由起发。所得泡沫具有0%、3.8%、5.1%和6.4%的气相二氧化硅。所有泡沫的孔结构都均匀。对于每种配制物制备三个样品。
表3-1
孔尺寸测量和机械测试(如实施例1所述进行)的结果提供在表3-2中。具有3.8%气相二氧化硅的泡沫的孔尺寸显著小于对比泡沫的孔尺寸。孔尺寸随着气相二氧化硅负载而增加,但始终小于对比泡沫的孔尺寸。随着配制物中FS的量的增加,回弹性和断裂伸长率降低。在相同密度下与参照泡沫相比,用FS制备的泡沫的拉伸强度、撕裂强度和CFD值均显著更高。
表3-2
性质 | 实施例3-Comp | 实施例3-1 | 实施例3-2 | 实施例3-3 |
密度,pcf | 2.44±0.03 | 2.41±0.03 | 2.38±0.02 | 2.43±0.04 |
通过球反弹的回弹性,% | 60±1 | 49±1 | 49±1 | 47±1 |
断裂拉伸强度,psi | 15.8±1.3 | 18.8±1.4 | 21.0±1.4 | 17.0±0.8 |
断裂伸长率,% | 123±8 | 120±8 | 113±7 | 98±7 |
撕裂强度,lbf/in | 3.06±0.26 | 4.24±0.25 | 3.92±0.25 | 4.04±0.13 |
CFD@25%,kPa | 1.19±0.06 | 2.20±0.12 | 2.56±0.16 | 2.95±0.23 |
CFD@50%,kPa | 2.36±0.12 | 4.13±0.29 | 4.70±0.30 | 5.53±0.45 |
CFD@65%,kPa | 5.18±0.45 | 8.10±0.58 | 8.40±0.76 | 9.97±0.56 |
孔尺寸,mm | 1.06±0.08 | 0.78±0.07 | 0.94±0.06 | 0.92±0.08 |
实施例4
将无二氧化硅(对比)多元醇组分和根据实施例1中的配制物的含有2%、4%、6%、8%和10%的气相二氧化硅的多元醇组分密封并且在封闭的柜中在环境温度下老化。在两周之后,具有2%气相二氧化硅的多元醇组分为稠液体,并且仅缓慢流动,而具有较高气相二氧化硅浓度的剩余样品则具有糊状外观并且在倒置时不流动。相比之下,参照组合物保持流动(流体)。
用10%气相二氧化硅制备另外的多元醇组分配制物,如以下表4-1中所示;还显示了这些配制物在环境温度下老化各种时间之后的粘度(箭头指示在进行测量时粘度仍在上升)。粘度是在Brookfield Viscometer,Model LVF中根据ASTM D-4878测量的。
表4-1
组分(g) | 实施例4-1 | 实施例4-2 | 实施例4-3 | 实施例4-4 | 实施例4-5 | 实施例4-6 |
气相二氧化硅-多元醇分散体 | 70.89 | 70.89 | 70.89 | 70.89 | 70.89 | 70.89 |
Pluracol 2090 | 26.11 | 26.11 | 26.11 | 26.11 | 26.11 | 26.11 |
Lumulse POE26 | 3 | 3 | 3 | 3 | 3 | 3 |
Tegostab B 4690 | 1 | 1 | 1 | 1 | 1 | 1 |
Dabco 33LV | 0.8 | 0.8 | 0 | 0 | 0.8 | 0 |
二乙醇胺LF 85% | 1 | 0 | 0 | 1 | 0 | 0 |
三乙醇胺 | 0 | 0 | 0 | 0 | 1 | 1 |
Toyocat ET | 0.1 | 0.1 | 0 | 0 | 0.1 | 0 |
添加的水 | 3.44 | 3.44 | 3.44 | 3.44 | 3.44 | 3.44 |
粘度(mPa-s) | ||||||
初始 | 5,530 | 5,750 | 5,580 | 6,620 | 6,340 | 6,200 |
1天 | 9,960 | 7,800 | 5,570 | 9,000 | 8,400 | 6,480 |
2天 | 25,500 | 7,840 | 5,500 | 27,350 | 10,180 | 6,480 |
3天 | 糊 | 9,440 | 5,490 | 糊 | 12,120 | - |
5天 | 糊 | - | - | 糊 | - | 6,730 |
6天 | 糊 | 19,500↑ | 5,400 | 糊 | 21,700↑ | 6,740 |
在不使用Dabco 33LV催化剂的情况下和在没有任何二乙醇胺(DEA)的情况下制备的多元醇组分的粘度不随时间变化(实施例4-3)。含有这两种产品之一(Dabco 33LV或DEA)的多元醇组分的粘度随时间增加(实施例4-2和4-4)。在具有DEA的情况下和在没有Dabco33LV的情况下制备的多元醇组分在仅三天之后就具有糊的稠度。在具有Dabco 33LV的情况下和在没有DEA的情况下制备的多元醇组分在6天之后变为非常粘稠的液体。
用三乙醇胺(TEOA)代替DEA以及在没有Dabco 33LV的情况下制备的多元醇组分的粘度在存储6天之后仅略微变化(如果有的话)(实施例4-6)。在具有TEOA和Dabco 33LV的情况下制备的多元醇组分的粘度的变化与在没有任何胺扩链剂的情况下在具有Dabco 33LV的情况下制备的多元醇组分的粘度的变化相当(实施例4-2和4-5)。这些结果清楚地表明,气相二氧化硅与仲胺的相互作用多于与叔胺。此外,在采用气相二氧化硅的开孔PU体系中可能不必须使用胺扩链剂或交联剂。
实施例5
如上所述,将CAB-O-SIL TG-6110疏水气相二氧化硅(Cabot Corporation)分散在Pluracol 2090聚醚三醇(BASF)中,以形成15wt%分散体。将分散体与另外的组分(包括聚-G 85-29环氧乙烷封端的聚醚多元醇三醇(Monument Chemical))以以下表5-1中列出的比例结合,以形成多元醇组分。与实施例1类似,二氧化硅-多元醇分散体可用作基于质量的等量的纯多元醇的直接替代物,以制备具有0%、2%、4%、6%、8%和10%的二氧化硅浓度的多元醇组分。使用高扭矩混合器(CRAFSTMAN 10-Inch Drill Press,ModelNo.137.219000)在环境温度下以3,100rpm持续7s将总共223.34g的多元醇组分与131.52gSuprasec 7007多异氰酸酯(以实现90的异氰酸酯指数)在1000mL三倒聚乙烯杯中结合,然后,在液体混合物变得浑浊并且开始膨胀之前,倒入到预热至70℃的12”x12”x2”(30cmx30cmx5cm)铝模具中。在倒入之后,封闭模具并且允许泡沫固化260s,然后打开模具并且泡沫脱模。在测试之前将所有经模塑的泡沫在环境气氛中老化至少一周。在脱模之后立即手工撞击泡沫垫(即用手压缩以打开孔窗口)。除了实施例1中描述的测试外,泡沫还通过在ASTM D-3574下的以下测试来表征:干恒定挠度压缩永久变形(Test D),湿老化压缩永久变形(Test D与Test L湿热老化),湿老化负荷(CFD)损失(Test C与Test L-湿热老化;22h@50℃和95%相对湿度,以及Test C与Test J2-蒸汽高压釜老化;5h@120℃)。如实施例1所述,还评估了经模塑的泡沫的在25%、50%和65%挠度(偏移,deflection)的CFD,但具有60s停留时间。使用每种配制物测量两个泡沫样品。
表5-1
用基于总泡沫重量计0%、1.3%、2.5%、3.8%的FS(基于总多元醇组分计分别为0%、2%、4%和6%的FS)制备的经模塑的泡沫表现出均匀的表面(表皮)和均匀的表观孔结构。在用基于总泡沫重量计5.1%和6.3%的气相二氧化硅(基于总多元醇组分计分别为8%和10%的FS)制备的泡沫中观察到在表皮上的一些瑕疵。然而,不管轻微表皮瑕疵如何,这些泡沫的孔结构都是均匀的。所得泡沫的机械性质在表5-2中列出。经模塑的泡沫的回弹性随着气相二氧化硅的浓度的增加而降低。
表5-2
实施例6
在Jeffol G 31-28甘油基环氧乙烷尖端(tipped)三醇(Huntsman)中制备CAB-O-SIL TG-6110(实施例6-x)和CT1221(实施例6-Cx)二氧化硅(Cabot Corporation;CT1221二氧化硅具有180-250m2/g的BET表面积和在表面处的三甲基硅烷基)的15%分散体,如实施例1所述。使用表6-1中所列出的配制物(包括Voranol-Voractiv 6340聚醚多元醇(Dow)、Dabco NE300吹泡催化剂(Evonik)、Dabco NE1091胶凝催化剂(Evonik)、Dabco DC193表面活性剂(Evonik)、碳酸亚丙酯(见实施例2)和二乙醇胺LF 85%(Webb Chemical))制备如实施例1中所述的多元醇组分。将多元醇组分与Lupranate T80异氰酸酯(2,4-和2,6-甲苯二异氰酸酯的混合物,Huntsman)以表6-2中所规定的量(异氰酸酯指数为90)结合,以及如实施例1中所述浇注在聚乙烯衬里盒中(“自由起发泡沫”)。一式两份制备自由起发泡沫。表6-2中所规定的聚氨酯配制物对于实施例6-C1放大250%以及对于实施例6-1和6-2放大257%,以根据实施例5中所述的方法制备经模塑的泡沫。一式两份制备经模塑的泡沫。泡沫如上所述进行评估。
表6-1a
*添加的水=配制物中的总的水
表6-1b
*添加的水=配制物中的总的水
表6-2
实施例No. | 多元醇组分的量(g) | Lupranate T80异氰酸酯的量 | 自由起发泡沫外观 |
6-C1 | 106.1 | 30.63 | 均匀、细 |
6-1 | 106.1 | 30.43 | 均匀、细 |
6-2 | 106.1 | 30.36 | 均匀、细 |
6-C2 | 106.1 | 30.47 | 在71-74s塌陷 |
6-C3 | 106.6 | 30.50 | 在75s塌陷 |
6-C4 | 106.1 | 30.49 | 在中心的水平*** |
6-C5 | 106.1 | 30.48 | 在81s塌陷 |
6-C6 | 108.1 | 30.47 | 在75s塌陷 |
6-C7 | 106.1 | 30.55 | 完全上升后缓慢下降 |
表6-2证实,用较低表面积TG-6110二氧化硅制备了稳定的泡沫。据推测,二氧化硅的开孔性质补偿了配制物中的开孔多元醇的缺失。然而,即使在不存在开孔多元醇的情况下,具有较高表面积CT-1221二氧化硅的泡沫也塌陷。泡沫稳定性没有随着表面活性剂浓度的变化、用替代分散剂Dabco DC 193表面活性剂部分替代Tegostab分散剂、添加碳酸亚丙酯或二氧化硅浓度的降低而改进。
除了上述测试之外,还根据ASTM D-3574(Procedure B-CFD Hysteresis loss)表征泡沫的滞后损失。表6-3显示了含有TG-6110二氧化硅的经模塑的泡沫相对于无二氧化硅对照的机械和其他性质。TG-6110二氧化硅的引入增加了CFD,并且没有显著影响自由起发泡沫的回弹性。在经模塑的泡沫中,引入TG-6110二氧化硅增加了CFD和撕裂强度,但没有显著影响拉伸强度。
表6-3
实施例7
在Jeffol G 31-28甘油基环氧乙烷尖端三醇(Huntsman)中制备CAB-O-SIL TG-6110和CT 1221二氧化硅的15%分散体,如上所述。使用表7-1中所列出的配制物如实施例1中所述制备具有6wt%二氧化硅的多元醇组分(包括Lumulse POE 26乙氧基化甘油、Tegostab B 4690表面活性剂、二乙醇胺LF 85%交联剂、Dabco 33LV三亚乙基二胺和Toyocat ET双(2-二甲基氨基乙基)醚)。如实施例1中所述将多元醇组分与Suprasec 7007异氰酸酯以表7-1中所列出的量结合,以及如实施例1中所述浇铸在聚乙烯衬里盒中(“自由起发泡沫”)以形成具有3.8wt%二氧化硅的泡沫。目视评估泡沫外观。
表7-1
在没有二氧化硅的情况下生产的泡沫和用较低表面积TG-6110二氧化硅生产的两种泡沫均表现出均匀并且细的孔结构。用较高表面积CT-1221二氧化硅和Lumulse POE开孔多元醇生产的泡沫表现出部分泡沫塌陷,而用CT-1221二氧化硅在没有开孔多元醇的情况下生产的泡沫在泡沫的核心中表现出粗孔。
实施例8
将气相二氧化硅(参见以下表8-1,所有二氧化硅来自Cabot Corporation)与Voranol 220-046聚醚多元醇(Dow)在Hauschild Speedmixer DAC-150中在6wt%的负载下结合,直到实现5的Hegman研磨。在TA Instruments AR2000Rheometer中使用4cm平行板几何形状和500微米间隙在25℃下评估分散。粘度数据示于图1中。数据显示,与经过具有三个或更少个碳的烷基硅烷基处理的气相二氧化硅相比,用辛基硅烷基或硅氧烷聚合物处理的气相二氧化硅显著增加了粘度。
表8-1
实施例9
将CAB-O-SIL TG-6110(圆圈)和CT-1221(三角)二氧化硅与Voranol 6340(封闭符号)和Jeffol G 31-28f(开放符号)多元醇在15%的负载下结合,如实施例1中所述。如实施例8中所述测量粘度,并且针对剪切速率绘图。结果示于图2中并且显示了较高表面积CT-1221二氧化硅也导致粘度的显著增加。
实施例10
将CAB-O-SIL TG-6110(圆圈)和L90(三角)二氧化硅与Voranol 232-034(封闭符号)多元醇在10%的负载下结合,如实施例1中所述。如实施例8中所述测量粘度,并且针对剪切速率绘图。通过向样品添加1wt%三乙醇胺,在SpeedMixer(Flackteck,Landrum,SC)中混合30s,允许样品在环境温度下孵育30min,然后再次测量粘度(开放符号),评估疏水TG-6110二氧化硅和未经处理的亲水L90二氧化硅与胺催化剂的相互作用。结果示于图3中并且显示了未经处理的L90二氧化硅导致多元醇粘度的显著增加。在聚合体系中,粘度的这种增加可阻止泡沫中的气泡的正常(proper)发展。
本发明的优选的实施方案的上述描述已出于说明和描述的目的而提出。其不旨在穷尽性的或将本发明限制到所公开的精确形式。修改和变化根据以上教导是可能的,或者可从本发明的实践中获得。选择和描述实施方案是为了解释本发明的原理及其实际应用,以使本领域技术人员能够在各种实施方案中利用本发明,并且根据所设想的特定用途进行各种修改。目的是通过本文所附的权利要求及其等同物来定义本发明的范围。
Claims (20)
1.生产柔性聚氨酯泡沫的方法,包括:
提供包含至少第一多元醇以及最高达10wt%的具有50至150m2/g的表面积的气相二氧化硅的多元醇组合物,所述第一多元醇具有3000至6000的重均分子量和2.5至3.5的官能度,其中气相二氧化硅在其表面处具有C1-C3烷基硅烷基;
将该多元醇组合物、具有1.8至2.5的官能度的多异氰酸酯、水、和叔胺催化剂结合以形成预聚物组合物;以及
允许预聚物组合物聚合以形成具有1.8至4pcf的密度以及如下中的一种或多种的开孔泡沫结构:a)至少40%、例如40%至70%的回弹性和b)不大于15%、例如3%至15%的干压缩永久变形。
2.权利要求1的方法,其中柔性聚氨酯泡沫呈现出1.8至3pcf的密度或2至4pcf的密度。
3.权利要求1或权利要求2的方法,其中多异氰酸酯包含六亚甲基二异氰酸酯(HDI)、亚苯基二异氰酸酯(PDI)、2,4-甲苯二异氰酸酯(2,4-TDI)、2,6-甲苯二异氰酸酯(2,6-TDI)、4,4’-二苯基甲烷二异氰酸酯(MDI)、二苯基甲烷二异氰酸酯的异构体混合物、或这些中的两种或更多种的混合物。
4.权利要求1-3中任一项的方法,其中第一多元醇包含聚醚多元醇或聚酯多元醇。
5.权利要求1-4中任一项的方法,其中所述多元醇组合物进一步包含第二多元醇,所述第二多元醇具有2000至10000的重均分子量。
6.权利要求1-5中任一项的方法,其中气相二氧化硅具有50至150m2/g或50至100m2/g的BET表面积。
7.权利要求1-6中任一项的方法,其中允许包括将预聚物组合物装入到具有对气氛开放的一侧的模具中。
8.权利要求7的方法,其中柔性聚氨酯泡沫具有1.8至3pcf的密度。
9.权利要求1-6中任一项的方法,其中允许包括将预聚物组合物装入到模具中并且封闭该模具。
10.权利要求9的方法,其中柔性聚氨酯泡沫具有2至4pcf的密度。
11.权利要求1-10中任一项的方法,其中C1-C3烷基硅烷基为三甲基硅烷基或二甲基硅烷基。
12.权利要求1-11中任一项的方法,其中柔性聚氨酯泡沫具有如下的通过ASTM D3574测量的在50%的压缩力挠度:相对于通过相同方法但其中用相等质量份的第一多元醇代替二氧化硅生产的柔性聚氨酯泡沫,改善至少30%,例如,至少50%、至少70%、或30%至155%。
13.通过权利要求1-12中任一项的方法生产的聚氨酯泡沫。
14.柔性聚氨酯泡沫,其包含最高达10wt%的具有50至150m2/g的表面积的气相二氧化硅,其中该气相二氧化硅在其表面处具有C1-C3烷基硅烷基,柔性聚氨酯泡沫表现出具有至少40%例如40%至70%的回弹性、不大于15%例如3%至15%的干压缩永久变形、或这两者。
15.权利要求14的柔性聚氨酯泡沫,其中气相二氧化硅具有50至150m2/g或50至100m2/g的BET表面积。
16.权利要求14或权利要求15的柔性聚氨酯泡沫,其中C1-C3烷基硅烷基为三甲基硅烷基或二甲基硅烷基。
17.权利要求14-16中任一项的柔性聚氨酯泡沫,其中该泡沫为经模塑的泡沫或自由起发泡沫。
18.权利要求14-17中任一项的柔性聚氨酯泡沫,其中聚氨酯包含聚醚聚氨酯或聚酯聚氨酯。
19.权利要求14-18中任一项的柔性聚氨酯泡沫,具有1.8至4pcf的密度,例如,1.8至3pcf的密度或2至4pcf的密度。
20.权利要求14-19中任一项的柔性聚氨酯泡沫,具有如下的通过ASTM D3574测量的在50%的压缩力挠度:与具有相同组成但用多元醇代替二氧化硅的柔性聚氨酯泡沫相比大至少30%,例如,至少50%、至少70%、或30%至155%。
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