CN103339164B - 用于聚氨酯硬质泡沫体改进的低温表皮固化的多元醇配方 - Google Patents
用于聚氨酯硬质泡沫体改进的低温表皮固化的多元醇配方 Download PDFInfo
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- CN103339164B CN103339164B CN201180060936.8A CN201180060936A CN103339164B CN 103339164 B CN103339164 B CN 103339164B CN 201180060936 A CN201180060936 A CN 201180060936A CN 103339164 B CN103339164 B CN 103339164B
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本发明提供了一种包括某些类型的聚酯多元醇的多元醇配方,所述多元醇配方用于制备具有低表面脆性的硬质聚氨酯泡沫体。在一种实施方式中,提供了用于制备硬质泡沫体的反应体系。该反应体系包括聚酯多元醇和一种或多种多异氰酸酯,其中该聚酯多元醇和多异氰酸酯以足以提供硬质聚氨酯泡沫体的量混合。该聚酯多元醇包括以下物质的反应产物:20到60重量%的包括至少80摩尔%或更多对苯二甲酸的芳族组分、20到60重量%的具有150到1000的数均分子量的聚乙二醇、5到20重量%的官能度为2且分子量为60到250的二醇和5到20重量%的官能度为至少3且分子量为60到250的二醇。
Description
技术领域
本发明涉及用于制备聚氨酯硬质泡沫体的包括某些聚酯多元醇的多元醇配方。这种泡沫体特别用于制造复合元件,例如夹心板。
背景技术
聚氨酯泡沫体用于各种应用,从缓冲(如床垫、枕头和座位垫)至包装至热绝缘和用于医疗应用。聚氨酯具有下述能力,即,经过选择用来形成聚合物的原材料,可以将其剪裁以适应特定应用。硬质类型的聚氨酯泡沫体用作器具绝缘泡沫体和其它热绝缘应用。
通过多元醇与多异氰酸酯在催化剂和其他可能的组分的存在下反应而在聚氨酯的制备中使用多元醇是公知的。芳族聚酯多元醇,例如基于对苯二甲酸二甲酯(DMT)基底的那些广泛用于制造定速燃烧(flame rated)的硬质聚氨酯面板以便有利于泡沫体的燃烧性能。使用这些芳族聚酯多元醇的典型配方显示了趋向高表面脆性的趋势,这要求了相对高的模具或“表皮固化”温度以避免产生缺陷,例如面板表皮起泡。这种高表皮固化温度导致增加的加工时间,而在一些情况中还导致最终产品品质的降低。改进聚氨酯配方以减少表面脆性的尝试导致了在泡沫体加工和/或性质方面的其他负面结果。
可以期望的是在接近环境温度的模具温度下降低表面脆性并且改进这种硬质聚氨酯泡沫体系的表皮固化,同时降低硬质泡沫体起泡趋势而又对泡沫体加工或泡沫体产品的材料性质没有负面影响。
发明内容
本发明涉及一种用于在给定的模具温度制备具有降低的表面脆性和改进的表皮固化的聚氨酯硬质泡沫体的多元醇配方,该聚氨酯泡沫体用作结构应用中的绝缘体。本发明的一种实施方式提供了一种多元醇共混物,其包括官能度为2到8且分子量为100到2000的聚醚多元醇、20到90重量%的包括至少以下物质的反应产物的芳族聚酯多元醇:
A)包括80摩尔%或更多对苯二甲酸的芳族组分;
B)至少一种聚醚多元醇,其标称官能度为2、分子量为150到1000,并且聚环氧乙烷含量为多元醇的至少70重量%;以及
C)至少一种分子量为60到250的不是B的二醇;
D)至少一种分子量为60到250且标称官能度为至少3的二醇;
其中A、B、C和D在所述反应中的存在量基于重量百分比为:20到60重量%的A)、20到60重量%的B)和5到20重量%的C)以及5到20重量%的D)。
在其他方面,本发明提供了一种用于制备硬质泡沫体的反应体系,该反应体系包括以下物质的反应产物:
(1)如上所述的多元醇共混物,
(2)多异氰酸酯,和
(3)任选的本身公知的添加剂和助剂。这些任选的添加剂或助剂选自染料、颜料、内脱模剂、物理发泡剂、化学发泡剂、阻燃剂、填料、增强剂、增塑剂、烟雾抑制剂(smoke supresants)、芳香剂、抗静电剂、生物杀灭剂、抗氧剂、光稳定剂、粘合促进剂以及它们的联合。
在另一方面,本发明提供了一种用于制备硬质聚氨酯泡沫体的方法,其包括:
a)形成包含至少以下物质的反应混合物:
1)如上所述的多元醇共混物,
2)多异氰酸酯,
3)至少一种烃、氢氟烃、氢氯氟烃、氟烃、二烷基醚或氟取代的二烷基醚物理发泡剂;
b)使反应混合物经受使得反应混合物膨胀并且固化以形成硬质聚氨酯泡沫体的条件。
本发明的另一方面提供了一种复合元件,其包括:
i)下覆盖面,
ii)包括以下物质的反应产物的硬质泡沫体产品
(1)异氰酸酯和
(2)多元醇混合物,其中多元醇混合物包括:
第一多元醇,其为包括至少以下物质的反应产物的聚酯多元醇:
A)包括80摩尔%或更多对苯二甲酸的芳族组分;
B)至少一种聚醚多元醇,其官能度为2、分子量为150到1000,且聚环氧乙烷含量为多元醇的至少70重量%;以及
C)至少一种分子量为60到250的不是B的二醇;
D)至少一种分子量为60到250的且标称官能度为至少3的二醇;
其中A、B、C和D在所述反应中的存在量基于重量百分比为:20到60重量%的A)、20到60重量%的B)和5到20重量%的C)以及5到20重量%的D)。
以及
第二多元醇,其为官能度为2到8且分子量为100到2000的聚醚多元醇;其中第一多元醇与第二多元醇在多元醇混合物中存在的重量百分比为20到90重量%的第一多元醇和10到80重量%的第二多元醇。
iii)上覆盖面。
在另一种实施方式中,本发明提供了一种用于制备复合元件的方法,其中硬质泡沫体(ii)与(i)和(iii)粘合并且通过在25℃到50℃的温度使异氰酸酯和多元醇混合物反应而在(i)和(iii)之间制备。在进一步的实施方式中,其中发生发泡的模具温度小于35℃。
具体实施方式
本发明的多元醇共混物包括高官能度的聚醚多元醇和某些由包括至少以下物质的反应混合物制备的芳族聚酯多元醇:A)对苯二甲酸;B)至少一种聚醚多元醇,其中该聚醚多元醇的官能度为2且聚环氧乙烷含量为多元醇的至少70重量%;以及C)至少一种分子量为60到250的不是B)的二醇组分;和D)至少一种分子量为60到250且标称官能度为至少3的二醇。已经发现这种多元醇共混物可以用于在给定的模具温度制备具有降低的表面脆性和改进的表皮固化的聚氨酯泡沫体,同时降低硬质泡沫体起泡的趋势,而又对泡沫体加工或泡沫体的材料性质没有负面影响。特别的,还发现通过在制备这种面板中使用公开的聚酯而降低了在降低的模具温度下泡沫体起泡的趋势。
本发明聚酯多元醇的芳族组分(组分A)主要源自对苯二甲酸。该对苯二甲酸组分将通常占芳族组分的80摩尔%或更多。在进一步的实施方式中,对苯二甲酸将占芳族组分的85摩尔%或更多。在另一种实施方式中,对苯二甲酸将占用于制备芳族聚酯多元醇的芳族组分的90摩尔%或更多。在另一种实施方式中,芳族组分包括大于95摩尔%的对苯二甲酸。在另一种实施方式中,芳族组分基本上源自对苯二甲酸。虽然聚酯多元醇可以由基本上纯的对苯二甲酸制备,但是还可以使用更复杂的成分,例如来自对苯二甲酸制造的侧物流、废弃物或废料剩余物。可以使用可以分解为对苯二甲酸和二甘醇的再循环材料,例如聚对苯二甲酸乙二醇酯的消化产物(digestionproducts)。可以存在的其他类型的芳族材料包括,例如邻苯二甲酸酐、偏苯三甲酸酐、对苯二甲酸二甲酯剩余物。
组分A)通常占反应混合物的20到60wt%。在进一步的实施方式中,组分A)占反应混合物的30wt%或更多。在进一步的实施方式中,组分A)占反应混合物的35wt%或更多。
组分B)是通过合适的起始分子(引发剂)与C2至C4环氧烷烃的的烷氧基化获得的聚醚多元醇,所述环氧烷烃例如环氧乙烷、环氧丙烷,1,2-环氧丁烷或2,3-环氧丁烷,四氢呋喃或它们中的两种或多种的组合。聚醚多元醇通常将包含大于70重量%的源自环氧乙烷(EO)单元的环氧烷烃单元,优选为至少75重量%源自EO的环氧烷烃单元。在其他的实施方式中,多元醇将包含大于80wt%的源自EO的环氧烷烃单元,在进一步的实施方式中,其包括85wt%或更多的源自EO的环氧烷烃单元。在一些实施方式中,环氧乙烷将是用于多元醇制备中唯一的环氧烷烃。当使用不是EO的环氧烷烃时,优选将另外的环氧烷烃,例如环氧丙烷或环氧丁烷作为共进料与EO一起进料或者作为内嵌段(internal block)进料。对这种聚合的催化可以是阴离子的或阳离子的,使用催化剂如氢氧化钾、氢氧化铯、三氟化硼,或者是双氰化物络合物(DMC)催化剂例如六氰基钴酸锌或季磷腈化合物。在碱性催化剂的情况,这些碱性催化剂优选在生产结束时通过适当的修整步骤(如凝结、硅酸镁分离或酸中和)从多元醇中移除。
基于聚环氧乙烷的多元醇通常具有150到1000的分子量。在一种实施方式中,其数均分子量为160或更高。在进一步的实施方式中,其数均分子量低于800,或者甚至低于600。在进一步的实施方式中,其数均分子量低于500。
用于制备组分B)的引发剂的官能度为2。正如本申请使用的,除非另有说明,否则官能度指的是标称官能度。这些引发剂的非限制性实例包括,例如乙二醇、二甘醇和丙二醇。
基于聚环氧乙烷的多元醇通常占反应混合物的20到60重量%。在进一步的实施方式中,基于聚环氧乙烷的多元醇将占反应混合物的30到60wt%。在另一种实施方式中,基于聚环氧乙烷的多元醇将占反应混合物的至少35wt%或40wt%。
除了芳族组分A)和基于聚环氧乙烷的多元醇组分B)之外,用于制备聚酯多元醇的反应混合物还包含一种或多种分子量为60到250的不同于B)的二醇(组分C)。这种二醇或二醇的共混物的标称官能度通常为2。
在一种实施方式中,组分C)的2官能的二醇可以通过下式表示:
OH-(CH2-CH-O)n-H
Ι (式I)
R
其中R为氢或具有1到4个碳原子的低级烷基,且选择n以获得250或更低的分子量。在进一步的实施方式中,选择n以获得低于200的分子量。在进一步的实施方式中,R为氢。可以用于本发明的二甘醇的非限制性实例包括乙二醇、二甘醇,和其他聚乙二醇、丙二醇、一缩二丙二醇等。
组分C)通常占反应混合物的至少5重量%,且通常占用于制备聚酯的反应混合物的少于20重量%。在另一种实施方式中,二醇组分将占反应混合物的大于7wt%。在进一步的实施方式中,二醇组分将占反应混合物的少于18wt%。
组分D)是标称官能度为3或更大的二醇。三官能的二醇包括,例如甘油和三羟甲基丙烷。更高官能的二醇包括,例如季戊四醇。组分D)通常占反应混合物的至少5重量%,且通常占用于制备聚酯的反应混合物的少于20重量%。在另一种实施方式中,二醇组分将占反应混合物的大于7wt%。在进一步的实施方式中,二醇组分将占反应混合物的少于18wt%。
基于制备聚酯的组分,聚酯的标称官能度大于2.3且通常不大于3.1。在进一步的实施方式中,聚酯将具有2.4到2.9的官能度。在进一步的实施方式中,聚酯具有2.5或更大的官能度。用于制备聚酯的材料的量将通常提供具有200到400的羟值的聚酯。在进一步的实施方式中,聚酯的羟值少于350。
通过引入特定量的基于聚环氧乙烷的多元醇和以上指出的其他二醇、以及芳族组分,得到的聚酯在25℃下根据UNI EN ISO3219测得的粘度通常小于30,000mPa*s。在进一步的实施方式中,聚酯多元醇的粘度小于20,000mPa*s。虽然期望获得具有尽可能低的粘度的多元醇,但是由于实际的化学限制和最终用途应用,多元醇的粘度通常大于1,000mPa*s。
本发明的芳族聚酯多元醇包括任何少量在制备聚酯多元醇后剩余的未反应的二醇。虽然不期望,但是芳族聚酯多元醇可以包括至多约30重量%的游离二醇/多元醇。基于聚酯多元醇组分的总重量,本发明的芳族聚酯多元醇的游离二醇含量通常为约0到约30重量%,且通常为1到约25重量%。聚酯多元醇还可以包括少量残留的未相互酯化的芳族组分。基于合并以形成本发明的芳族聚酯多元醇的组分的总重量,通常该未相互酯化的芳族物质的存在量低于2%重量。
聚酯多元醇可以通过在本领域公知的条件下组分A、B和C之间的缩聚反应/酯交换反应和聚合反应而形成。例如参见G.Oertel,PolyurethaneHandbook,Carl Hanser Verlag,Munich,Germany1985,pp54-62和MihailIonescu,Chemistry and Technology of Polyols for Polyurethanes,RapraTechnology,2005,pp263-294。通常,该合成反应在180到280℃的温度进行。在另一种实施方式中,该合成反应在至少200℃的温度进行。在进一步的实施方式中,该合成反应在215℃或更高的温度进行。在进一步的实施方式中,该合成反应在260℃或更低的温度进行。
虽然该合成反应可以在降低或升高的压力下发生,但是该反应通常在接近大气压力的条件下进行。
虽然该合成反应可以在没有催化剂的存在下发生,但是可以使用促进酯化反应/酯交换反应/聚合反应的催化剂。这些催化剂的实例包括四丁基钛酸盐,氧化二丁基锡,甲醇钾,或锌、铅或锑的氧化物;钛化合物,例如异丙醇钛(IV)和乙酰丙酮钛。当使用时,这种催化剂的用量为全部混合物的0.005到1重量%。在进一步的实施方式中,该催化剂的存在量为全部混合物的0.005到0.5重量%。
反应的挥发性产物,例如水和/或甲醇,通常在过程中顶部馏出除去并且迫使酯交换反应完成。
该合成反应通常进行1到5个小时。当然所需要的实际时间长度会随着催化剂浓度、温度等变化。出于经济原因和如果聚合反应循环太长会发生热降解的原因,通常不期望有太长的聚合反应循环。
本发明描述的聚酯多元醇用作用于制备多种聚氨酯或多异氰脲酸酯产品的多元醇配方的一部分。多元醇也称为异氰酸酯反应性组分,它与异氰酸酯组分一起构成用于制备聚氨酯或多异氰脲酸酯泡沫体的体系。根据应用,该聚酯通常在总的多元醇配方的20到90wt%的范围内。可以用于特殊应用的聚酯多元醇的量可以由本领域技术人员容易的确定。
配方中其他代表性的多元醇包括聚醚多元醇、不同于本发明的聚酯的聚酯多元醇、多羟基封端的缩醛树脂和羟基封端的胺。可以使用的可替换的多元醇包括基于聚碳酸亚烷基酯的多元醇和基于多磷酸酯的多元醇。优选的是聚醚或聚酯多元醇。聚醚多元醇通过向具有2到8个活性氢原子的引发剂中添加环氧烷烃制备,所述环氧烷烃例如环氧乙烷、环氧丙烷、环氧丁烷或它们的组合。用于配方中的多元醇的官能度将取决于本领域技术人员已知的最终用途应用。这些多元醇的官能度有利地为至少2个活性氢原子/分子(优选为3个活性氢原子/分子)且至多为8个活性氢原子/分子(优选为至多6个活性氢原子/分子)。用于硬质泡沫体的多元醇的羟值通常为约200到约1200,且更优选为约250到约800。
源自例如植物油或动物脂肪的可再生原料的多元醇也可以用作另外的多元醇。这样的多元醇的实例包括蓖麻油、WO04/096882和WO04/096883中描述的羟甲基化的聚酯、美国专利4,423,162、4,496,487和4,543,369中描述的羟甲基化的多元醇以及美国公开专利申请2002/0121328、2002/0119321和2002/0090488中描述的“吹制”植物油。
为了增加交联网络,多元醇共混物可以包含官能度为5到8的较高官能的多元醇。这样的多元醇的引发剂包括,例如季戊四醇、山梨醇、蔗糖、葡萄糖、果糖或其他糖类以及类似物。这些较高官能的多元醇的平均羟值为约200到约850,优选为约300到约770。可以将其他引发剂添加到较高官能的多元醇例如丙三醇中,以获得共引发的多元醇,该多元醇的官能度为4.1到7个羟基/分子且羟基当量为100到175。根据特别的应用,当使用这种多元醇时,其通常占用于制备硬质泡沫体的多元醇配方的30到70wt%。
多元醇混合物可以包含至多20重量%的再另一种多元醇,该多元醇不是聚酯、胺引发的多元醇或较高官能的多元醇,并且其羟基官能度为2.0到3.0和羟基当量为90到600。
为了结构应用,多元醇共混物还可以包括酚醛树脂的烷氧基化产物形成的多元醇。这样的多元醇在本领域称为线型酚醛清漆多元醇。当在配方中使用时,它们的存在量可以为至多20wt%。
在一种实施方式中,本发明提供了多元醇共混物,其包括30到80重量%的如上所述的芳族聚酯多元醇,且剩余物为官能度为2到8且分子量为100到10000的至少一种多元醇或该多元醇的组合。
适用于制备用于结构应用(具有改进的表皮固化)的硬质泡沫体的多元醇混合物的特殊实例包括以下物质的混合物:30到80重量%的本发明的聚酯;20到70重量%的山梨醇或蔗糖/甘油引发的聚醚多元醇,其中多元醇或多元醇共混物的官能度为3到8且羟基当量为200到850;和至多20重量%的另外的多元醇,其羟基官能度为2.0到3.0且羟基当量为90到500。
所述的多元醇混合物可以如下制备:单独制备组分多元醇,然后将它们共混在一起。可替换地,不包括聚酯的多元醇混合物可以如下制备:形成各引发剂化合物的混合物、然后烷氧基化该引发剂混合物以直接形成多元醇混合物。还可以使用这些方法的组合。
用于制备聚氨酯产物的合适的多异氰酸酯包括芳族、脂环族和脂族异氰酸酯。这样的异氰酸酯是本领域公知的。
合适的芳族异氰酸酯的实例包括二苯基甲烷二异氰酸酯的4,4'-异构体、2,4'-异构体和2,2'-异构体(MDI),它们的共混物以及聚合MDI共混物和单体MDI共混物,甲苯-2,4-二异氰酸酯和甲苯-2,6-二异氰酸酯(TDI),邻苯二异氰酸酯和对苯二异氰酸酯,氯苯-2,4-二异氰酸酯,二亚苯基-4,4'-二异氰酸酯,4,4'-二异氰酸酯-3,3'-二甲基二苯基,3-甲基二苯基-甲烷-4,4'-二异氰酸酯和二苯基醚二异氰酸酯和2,4,6-三异氰酸基甲苯以及2,4,4'-三异氰酸基二苯基醚。
在本发明的实践中还可以使用粗制多异氰酸酯,例如通过甲苯二胺的混合物的光气化作用获得的粗制甲苯二异氰酸酯或通过粗制亚甲基二苯基胺的光气化作用获得的粗制二苯基甲烷二异氰酸酯。在一种实施方式中,使用TDI/MDI共混物。
脂族多异氰酸酯的实例包括亚乙基二异氰酸酯,1,6-六亚甲基二异氰酸酯,1,3-二(异氰酸基甲基)环己烷和/或1,4-二(异氰酸基甲基)环己烷(包括任一种的顺式异构体或反式异构体),异佛尔酮二异氰酸酯(IPDI),四亚甲基-1,4-二异氰酸酯,亚甲基二(环己烷异氰酸酯)(H12MDI),环己烷1,4-二异氰酸酯,4,4'-二环己基甲烷二异氰酸酯,以上提及的芳族异氰酸酯的饱和类似物以及它们的混合物。
也可以使用包含缩二脲、脲、碳化二亚胺、脲基甲酸酯和/或异氰脲酸酯基团的任何前述多异氰酸酯基团的衍生物。这些衍生物通常具有增加的异氰酸酯官能度,并且当期望更加高度交联的产物时,可以期望地使用该衍生物。
为了制备硬质聚氨酯或多异氰脲酸酯材料,多异氰酸酯通常为二苯基甲烷-4,4'-二异氰酸酯,二苯基甲烷-2,4'-二异氰酸酯,它们的聚合物或衍生物,或者它们的混合物。在一种优选的实施方式中,使用4,4’-MDI或包含显著部分的4,4’-异构体或如上所述改性的MDI的其它MDI共混物制备异氰酸酯封端的预聚物。优选MDI包含45到95重量%的4,4’-异构体。
多异氰酸酯以足以提供80到200的异氰酸酯指数的量使用。异氰酸酯指数计算为由多异氰酸酯组分提供的反应性异氰酸酯基团的数目除以形成聚氨酯的组合物(包括由异氰酸酯反应性发泡剂包含的那些物质,例如水)中异氰酸酯反应性基团的数目再乘以100。针对计算异氰酸酯指数的目的,认为水每分子具有2个异氰酸酯反应性基团。对于硬质聚氨酯泡沫体应用,优选的异氰酸酯指数通常为100到150。
也可以在用于制备聚氨酯产物的配方中使用一种或多种扩链剂。扩链剂的存在为所得聚合物提供了期望的物理性质。在聚氨酯聚合物形成期间,扩链剂可以与多元醇组分共混或者可以作为单独的物流存在。扩链剂是每分子具有两个异氰酸酯反应性基团且当量/异氰酸酯反应性基团的小于400道尔顿、优选小于300道尔顿且特别为31-125道尔顿的物质。在用于制备本发明的聚氨酯聚合物的配方中还可以包括交联剂。“交联剂”是每分子具有三个或更多个异氰酸酯反应性基团且当量/异氰酸酯反应性基团小于400的物质。交联剂优选每分子含有3-8个(特别是3-4个)羟基、伯胺或仲胺基团并且当量为30到约200,特别为50-125。
本发明的多元醇共混物可以与多种发泡剂一起使用。用于形成聚氨酯的组合物的发泡剂包括至少一种物理发泡剂,该物理发泡剂为烃、氢氟烃、氢氯氟烃、氟烃、氢氯氟烯烃(HCFO)、氢氟烯烃(HFO)、二烷基醚或氟代二烷基醚、或它们中的两种或更多种的混合物。这些类型的发泡剂包括丙烷、异戊烷、正戊烷、正丁烷、异丁烷、异丁烯、环戊烷、二甲基醚、1,1-二氯-1-氟乙烷(HCFC-141b)、一氯二氟甲烷(HCFC-22)、1-氯-1,1-二氟乙烷(HCFC-142b)、1,1,1,2-四氟乙烷(HFC-134a)、1,1,1,3,3-五氟丁烷(HFC-365mfc)、1,1-二氟乙烷(HFC-152a)、1,1,1,2,3,3,3-七氟丙烷(HFC-227ea)和1,1,1,3,3-五氟丙烷(HFC-245fa)。HFO和HFCO发泡剂的实例包括五氟丙烯,例如HFO-1225yez和HFO-1225ye;四氟丙烯,例如HFO-1234yf和HFO-1234ez;1,1,1,4,4,4-六氟-2-丁烯(HFO-1336mzz);1-氯-3,3,3-三氟丙烯(HCFO-1233zd);1,2-二氟-3,3,3-三氟丙烯(HCFO-1223xd);2-氯-3,3,3-三氟丙烯(HCFO-1233xf)。这些发泡剂已经在大量的公开物中公开,例如公开WO2008121785A1、WO2008121790A1、WO2011/135395、US2008/0125506、US2011/0031436、US2009/0099272、US2010/0105788、US2011/0210289和2011/0031436。烃和氢氟烃发泡剂是优选的。除了物理发泡剂之外,通常优选的是在配方中进一步包括水。
优选地,发泡剂的用量足以使得,配方固化以形成具有下述模塑密度的泡沫体:16到160kg/m3、优选16到64kg/m3,特别为20到48kg/m3。为了达到这些密度,烃或氢氟烃发泡剂的用量便利地为约10到约40重量份,优选为约12到约35重量份,相对于每100重量份的多元醇。水与异氰酸酯基团反应,产生二氧化碳,二氧化碳用作膨胀气体。水的用量适当地为0.5到3.5重量份,优选为1.0到3.0重量份,相对于100重量份的多元醇。
形成聚氨酯的组合物典型地包括至少一种用于多元醇和/或水与多异氰酸酯的反应的催化剂。合适的形成氨基甲酸酯的催化剂包括美国专利4,390,645和WO02/079340中描述的那些,二者通过参考文献并入本发明。代表性的催化剂包括季胺和膦化合物,多种金属的螯合物,强酸的酸性金属盐,强碱,多种金属的醇盐和酚盐,有机酸与多种金属的盐,四价锡、三价和五价As、Sb和Bi的有机金属衍生物,以及铁和钴的金属羰基化物。
叔胺催化剂通常是优选的。在各种叔胺催化剂中,有二甲基苄基胺(如得自Rhine Chemie的DB)、1,8-二氮杂(5,4,0)十一烷-7(如得自Air Products的SA-1)、五甲基二亚乙基三胺(如得自Air Products的5)、二甲基环己基胺(如得自Air Products的8)、三亚乙基二胺(如得自Air Products的33LV)、二甲基乙基胺、N-乙基吗啉、N-烷基二甲基胺化合物如N-乙基N,N-二甲基胺和N-十六烷基N,N-二甲基胺、N-烷基吗啉化合物如N-乙基吗啉和N-椰油吗啉等等。可用的其他叔胺催化剂包括Air Products所售商品名为NE1060、NE1070、NE500、TMR-2、TMR-4、TMR30、1058、 和MD45的那些,以及Huntsman所售商品名为ZR50和ZR70的那些。另外,某些胺引发的多元醇在本文中可用作催化剂材料,包括在WO01/58976A中所描述的那些。可使用前述两种或更多种的混合物。
催化剂以催化足够量使用。对于优选的叔胺催化剂而言,催化剂的适宜量为每100重量份多元醇约0.3~约2份,尤其是约0.3~约1.5份叔胺催化剂。
形成聚氨酯的组合物还优选含有至少一种表面活性剂,表面活性剂有助于当气体放出形成气泡并使泡沫膨胀时稳定组合物的泡孔。适宜的表面活性剂的实例包括脂肪酸的碱金属盐和胺盐,如油酸钠、硬脂酸钠、蓖麻油酸钠、二乙醇胺油酸盐、二乙醇胺硬脂酸盐、二乙醇胺蓖麻油酸盐等等:磺酸(如十二烷基苯磺酸和二萘基甲烷二磺酸)的碱金属盐和胺盐;蓖麻油酸;硅氧烷-氧化烯烃聚合物或共聚物和其他有机聚硅氧烷;乙氧基化烷基苯酚(如Tergitol NP9和Triton X100,得自The Dow Chemical Company);乙氧基化脂肪醇(如Tergitol15-S-9,得自The Dow Chemical Company);石蜡油;蓖麻油;蓖麻油酸酯;土耳其红油;花生油;石蜡;脂肪醇;二甲基聚硅氧烷和含有聚氧化烯烃和氟烷烃侧基的低聚丙烯酸酯。通常这些表面活性剂的用量为0.01~6重量份,基于100重量份多元醇。
有机硅氧烷表面活性剂通常为优选的类型。各种各样的这些有机硅氧烷表面活性剂是市售可得的,包括Goldschmidt所售名称为的那些(如Tegostab B-8462、B8427、B8433和B-8404表面活性剂),OSi Specialties所售名称为的那些(如L6900和L6988表面活性剂),以及市售可得自Air Products and Chemicals的各种表面活性剂产品,如DC-193、DC-198、DC-5000、DC-5043和DC-5098表面活性剂。
除了前述组分以外,形成聚氨酯的组合物可包括各种辅助组分,如填料、着色剂、气味掩蔽剂、阻燃剂、生物杀灭剂、抗氧化剂、UV稳定剂、抗静电剂、粘度改进剂等等。
适宜的阻燃剂的实例包括磷化合物、含卤素的化合物和三聚氰胺。
填料和颜料的实例包括碳酸钙、二氧化钛、氧化铁、氧化铬、偶氮/重氮染料、酞菁、二噁嗪、再生的硬质聚氨酯泡沫材料和炭黑。
UV稳定剂的实例包括羟基苯并三唑、二丁基硫代氨基甲酸锌、2,6-二叔丁基邻苯二酚、羟基二苯甲酮、受阻胺和亚磷酸盐。
除了填料以外,前述添加剂通常用量少。每一种添加剂占聚氨酯配方总重量的0.01%~3%。填料的用量可高达聚氨酯配方总重量的50%。
形成聚氨酯的组合物采用以下方式制备,在使多元醇与异氰酸酯反应的条件下使各种组分合并在一起,发泡剂产生气体,组合物膨胀并固化。可将除多异氰酸酯以外的所有组分(或其任何亚组合)预共混为配制的多元醇组合物,如果需要,然后在制备泡沫体时与多异氰酸酯混合。在需要时可将各种组分预热,但通常不必要,可在约室温(~22℃)下使各种组分在一起进行反应。通常不必要对组合物施加热量以驱动固化,但如果希望的话,也可以这么做。
本发明特别用于制造夹心复合元件,该夹心复合元件包括至少两个硬质或软质材料的外层和一个硬质泡沫体的芯层的。
对于外层或饰面(facings),原则上可以使用任何方便使用的软质或硬质饰面,例如铝(涂漆的和/或阳极电镀的)、钢(镀锌的和/或涂漆的)、铜、不锈钢和非金属,例如无纺布有机纤维、塑料片材(例如聚苯乙烯)、塑料箔片(例如PE箔片)、木质片材、玻璃纤维、浸渍纸板、纸张、或这些的层压物的混合物。通常优选使用金属饰面,特别是铝和/或钢制造的饰面。饰面的厚度通常为200μm到5mm。在进一步的实施方式中,该厚度大于300μm或大于400μm。在进一步的实施方式中,该厚度小于3mm或小于2mm。可商购获得的饰面的实例是GalvalumneTM金属饰面。
这种复合元件的制造可以通过本领域已知的方法制备。例如,在将各组分混合后,可以将静置的液态反应混合物注射到空的预先安装的面板中,该面板包含在压机/夹具中。这些预先安装的面板通常由两个饰面组成,即典型由木材、金属或高密度聚氨酯制备的外围围栏(rail)和用于将最终发泡的面板连接在一起的锁定装置。在泡沫体固化后,从压机或夹具上取下面板。
通常,泡沫体层的厚度为2cm到25cm。在其他实施方式中,泡沫体层为2.5到21cm且在特别的实施方式中为6到16cm。通常在25℃到50℃的温度加热模具。特别的,发现包含本发明聚酯的配方显示了良好的粘合性且其表面缺陷也减少,甚至当模具温度降低到低于35℃时也是如此。
具有硬质外层的复合元件的应用包括用作卡车车身、客厅门和大门以及用在容器结构中。具有柔性外层的绝缘板、复合元件用作屋顶、外墙和地板的绝缘材料。
应当理解的是本说明书仅用于说明的目的且不应当以任何方式构成对本发明范围的限制。因此本领域技术人员可知,可以在不背离本发明预设的精神和范围的情况下对本发明公开的实施方式进行多种改进和变形。在审查以下对实施例和所附权利要求之后,本发明其他的优点和细节是明显的。
提供以下实施例以说明本发明的实施方式,但是其并不意在限制本发明的范围。除非另有说明,否则所有的份和百分比均基于重量。
对实施例中使用的原料的描述如下。
DABCO DC193是获自Air Products的硅表面活性剂(DABCO是AirProducts的商标)。
-2031多元醇是获自Invista的基于对苯二甲酸二甲酯的聚酯多元醇。
聚酯A是基于本发明描述的对苯二甲酸、二甘醇和聚乙二醇200的聚酯多元醇。
VORANOLTMRH490是蔗糖/甘油引发的聚环氧丙烷多元醇,其官能度为约4.3,羟值为约490,以商品名Voranol RH490获自The Dow ChemicalCompany。
8是获自Air Products的N,N-二甲基环己基胺催化剂。
TCPP,即磷酸三(氯异丙基)酯,是获自Supresta的低粘性且低酸性的阻燃添加剂。
HFC-245fa,即1,1,1,3,3-五氟丙烷,是以商品名获自Honeywell的发泡剂。
PAPITM27聚合MDI是获自The Dow Chemical Company的含有MDI的聚亚甲基聚苯基异氰酸酯。
表1和2分别给出了聚酯多元醇和添加了这些聚酯的配方的性质。
表1:聚酯多元醇的性质
a通常用于制备阻燃聚氨酯泡沫体的商购多元醇,其确切的组成是未知的。
表2.配方
表3中给出了制得的聚氨酯泡沫体的性质。
表3.结果
制备的硬质聚氨酯泡沫体的性质使用以下过程测量。对于表皮完整性百分比,将各个配方倾倒在用脱模剂处理并且在指定的温度加热的铝模具(30x20x5cm)中。30分钟后,打开模具并且测量附着在模具两个相对表面上的表皮的量。粘着在模具上的量可指出泡沫体的脆性,即,粘着在模具上的量越大,其表面越脆。
以psi为单位的压缩强度根据ASTM D-1621在泡沫体上测量,该泡沫体在37.8℃(100°F)的模具温度模塑、在30分钟后脱模制备,并且该泡沫体在测试前固化至少24小时。尺寸稳定性表示将泡沫体暴露于158°F(70℃)、97%的相对湿度(RH)下14天后的体积变化%。尺寸稳定性在泡沫体上测量,该泡沫体是在加热到37.8℃(100°F)的模具中制备的。
对于生坯强度测试,手动混合自由起发的样品并且将其倾倒在8英寸(30.3cm)长乘8英寸(20.3cm)宽乘9.5英寸(24.1cm)高的木质模具(室温)中。混合足够的材料以制备泡沫体,使得最终的样品充分起发以便在至少8英寸(20.3cm)高的侧面上形成平面。使泡沫体在模具中固化,直至期望的测试时间到达前1分钟,,即对于30分钟测试结果的29分钟。
生坯强度测试过程在Instron5566Extra wide Materials测试系统中进行。将测压元件(load cell)(UK537/2000lb)安装在十字头上,该十字头依托在载荷框架的立导(vertical guides)上。将试样放置在测试台上,然后通过固定在测压元件上的直径8英寸(20.3cm)的刻压机脚压制。
为了开始生坯强度测试,将泡沫体样品水平定位(与倾倒相比)并且居于Instron测试台中心。在期望的时间到达之前的15秒时[对于30分钟的测试而言,在从的模具上取下之后的29分45秒],开始测试。这启动Instron将十字头从228.6mm(9英寸(22.9cm))高的位置开始以100mm/min的速率降低,直到测压元件与泡沫体样品接触。十字头继续降低直到达到8.9N(2.0lbf)的力,在该时间点自动记录厚度。接着,再次降低十字头;这次以305mm/min的速率直到获得25.4mm的压缩(与2.0lbf的厚度相比),自动记录该时间点的最大压制载荷(生坯强度)。生坯强度值可指出在完全固化或硬化之前,模塑或流延产品以经受处理、模塑排出和机械加工的能力。
使用表3的配方制备的泡沫体表明,使用实施例#1的配方制备的硬质泡沫体显示了在90°F和100°F的表皮固化%的显著改进,相对于对照(C1)而言。获得了完整的表皮性质,同时又保持或略微改进泡沫体的其他性质。
虽然前述内容涉及本发明的实施方式,但是在不背离本发明基本范围的情况也可设计本发明的其他或进一步的实施方式。
Claims (9)
1.一种芳族聚酯多元醇,其由以下物质的反应产物构成:
A)包括80摩尔%或更多对苯二甲酸的芳族组分;
B)至少一种聚醚多元醇,其具有的标称官能度为2,分子量为150到1000,并且聚环氧乙烷含量为多元醇的至少70重量%;以及
C)至少一种分子量为60到250的不是B的二甘醇;和
D)甘油;
其中A、B、C和D在所述反应中的存在量基于重量百分比为:20到60重量%的A)、20到60重量%的B)和5到20重量%的C)以及5到20重量%的D)。
2.制备硬质泡沫体的多元醇混合物,其包括
1)第一多元醇,其为由以下物质的反应产物构成的聚酯多元醇:
A)包括80摩尔%或更多对苯二甲酸的芳族组分;
B)至少一种聚醚多元醇,其标称官能度为2、分子量为150到1000,且聚环氧乙烷含量为多元醇的至少70重量%;和
C)至少一种分子量为60到250的不是B的二甘醇;和
D)甘油;
其中A、B、C和D在所述反应中的存在量基于重量百分比为:20到60重量%的A)、20到60重量%的B)和5到20重量%的C)以及5到20重量%的D),以及
2)第二多元醇,其为官能度为2到8且分子量为100到2000的聚醚多元醇;其中第一多元醇与第二多元醇在多元醇混合物中存在的重量百分比为20到90重量%的第一多元醇和10到80重量%的第二多元醇。
3.一种复合元件,其包括:
i)下覆盖面,
ii)包括以下物质的反应产物的硬质泡沫体产物:
(1)异氰酸酯和
(2)多元醇混合物,其中多元醇混合物包括:
第一多元醇,其为由以下物质的反应产物构成的聚酯多元醇:
A)包括80摩尔%或更多对苯二甲酸的芳族组分;
B)至少一种聚醚多元醇,其标称官能度为2、分子量为150到1000,且聚环氧乙烷含量为多元醇的至少70重量%;和
C)至少一种分子量为60到250的不是B的二甘醇;和
D)甘油;
其中A、B、C和D在所述反应中的存在量基于重量百分比为:20到60重量%的A)、20到60重量%的B)和5到20重量%的C)以及5到20重量%的D),
以及
第二多元醇,其为官能度为2到8且分子量为100到2000的聚醚多元醇;其中第一多元醇与第二多元醇在多元醇混合物中存在的重量百分比为20到90重量%的第一多元醇和10到80重量%的第二多元醇,以及
iii)上覆盖面。
4.权利要求3的复合元件,其中B)具有小于500的数均分子量。
5.权利要求3或4的复合元件,其中所述聚醚多元醇B)是聚乙二醇,芳族组分和聚乙二醇各自以35到45重量%的量添加到聚酯多元醇中。
6.权利要求5的复合元件,其中异氰酸酯指数为80到200。
7.权利要求5的复合元件,其中硬质泡沫体具有16到64kg/m3的密度。
8.权利要求5的复合元件,其中异氰酸酯指数为100到150。
9.一种用于制备根据权利要求3到8中任一项的复合元件的方法,其中通过在25℃到50℃的温度使异氰酸酯和多元醇混合物反应而在(i)和(iii)之间制备与(i)和(iii)粘合的硬质泡沫体(ii)。
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2011
- 2011-12-13 WO PCT/US2011/064628 patent/WO2012087667A1/en active Application Filing
- 2011-12-13 US US13/880,898 patent/US20140364528A1/en not_active Abandoned
- 2011-12-13 MX MX2013007318A patent/MX2013007318A/es unknown
- 2011-12-13 CN CN201180060936.8A patent/CN103339164B/zh not_active Expired - Fee Related
- 2011-12-13 KR KR1020137015955A patent/KR101853153B1/ko active IP Right Grant
- 2011-12-13 EP EP11806060.7A patent/EP2655464A1/en not_active Withdrawn
- 2011-12-13 JP JP2013546207A patent/JP5931913B2/ja not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
---|---|
US20140364528A1 (en) | 2014-12-11 |
WO2012087667A1 (en) | 2012-06-28 |
JP5931913B2 (ja) | 2016-06-08 |
JP2014502651A (ja) | 2014-02-03 |
MX2013007318A (es) | 2013-07-22 |
CN103339164A (zh) | 2013-10-02 |
KR20140030103A (ko) | 2014-03-11 |
EP2655464A1 (en) | 2013-10-30 |
KR101853153B1 (ko) | 2018-04-27 |
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