CN113272352A - 包括富硅氧烷成核剂的刚性聚氨酯泡沫 - Google Patents
包括富硅氧烷成核剂的刚性聚氨酯泡沫 Download PDFInfo
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- CN113272352A CN113272352A CN201980087932.5A CN201980087932A CN113272352A CN 113272352 A CN113272352 A CN 113272352A CN 201980087932 A CN201980087932 A CN 201980087932A CN 113272352 A CN113272352 A CN 113272352A
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Classifications
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0042—Use of organic additives containing silicon
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/14—Manufacture of cellular products
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/166—Catalysts not provided for in the groups C08G18/18 - C08G18/26
- C08G18/168—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/4208—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/4211—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
本技术提供由泡沫制剂制造具有低热导率的聚氨酯泡沫的方法,所述泡沫制剂包括多元醇、异氰酸酯、聚氨酯催化剂、表面活性剂、水和富硅氧烷组成物。所述富硅氧烷组成物可充当用于减小泡沫的泡孔尺寸的成核剂并且可降低其热导率。
Description
相关申请的交叉引用
本申请要求2018年11月19日提交的名称为“包括富硅氧烷成核剂的刚性聚氨酯泡沫(Rigid Polyurethane Foams Comprising a Siloxane Rich Nucleating Agent)”的美国临时申请62/769,060的优先权和权益,该美国临时申请的公开内容以其整体并入本文中作为参考。
技术领域
本技术总体上涉及聚氨酯泡沫组合物和由这样的组合物制成的泡沫。更具体地,本技术涉及使用特定分子量的富硅氧烷化合物作为成核剂的刚性或半刚性聚氨酯泡沫。
背景技术
刚性聚氨酯泡沫分为两种类别,PUR和PIR类型。刚性PUR泡沫在异氰酸酯过量少的情况下制成并且主要包含由异氰酸酯反应形成的氨基甲酸酯键和脲键。刚性PIR泡沫在异氰酸酯过量多的情况下制成并且除氨基甲酸酯键和脲键外还导致由异氰酸酯三聚反应产生的大量异氰脲酸酯键。两种泡沫类型作为隔热(绝缘,insulation)材料广泛用在建筑工业中和用于家用或商用制冷装置。这些泡沫展现优异的隔热特性。
常规的刚性聚氨酯泡沫,例如可在隔热应用中使用的,通常是通过使至少一种多元醇与至少一种异氰酸酯在适合的催化剂、表面活性剂、化学和/或物理发泡剂和任选的其它添加剂(例如阻燃剂或其它的加工或泡沫性质改善添加剂)的存在下反应而制备的。
有机硅-聚醚共聚物作为表面活性剂在这样的刚性聚氨酯泡沫制剂(配方,formulation)中广泛使用。一直在试图优化这些类型的聚合物以使成核效果改善或最大化而不在其它泡沫性质方面妥协。仍存在机会来开发在隔热应用中使用的具有改善的热导率性质的刚性聚氨酯泡沫。
发明内容
本技术提供基于硅氧烷的添加剂组成物(组合物,composition),其将在半刚性或刚性聚氨酯泡沫制剂中使用以提供改善的热导率。
在一个方面中,本技术提供刚性聚氨酯或聚异氰脲酸酯泡沫组合物,其包括多元醇或其混合物、异氰酸酯、聚氨酯催化剂或其混合物、表面活性剂、富硅氧烷组成物、发泡剂(其为水、物理发泡剂或其混合物、或者这两者的组合)、任选的共化学发泡剂或其混合物、任选的阻燃剂添加剂或其混合物、和任选的其它加工添加剂。已经发现,特定分子量的富硅氧烷材料的使用当与常规的刚性泡沫表面活性剂和特别是基于有机硅-聚醚共聚物的那些组合使用时可充当成核剂。申请人已经发现,使用这些特定分子量和/或分子量分布的富硅氧烷材料可具有在初始混合阶段积极的成核效果而在以后的反应阶段不导致消泡或泡孔尺寸控制的不足,因此提供具有低泡孔尺寸的泡沫,导致低泡沫热导率。
在一个实施方式中,提供包括下式的富硅氧烷化合物的组成物:
M3 aD3 bD4 cTdQe (II)
其中
M3为三烷基封端单元R3R4R5SiO1/2—;
D3为二烷基单元-O1/2R6R7SiO1/2—;
D4为烷基单元-O1/2R8R9SiO1/2—;T为-O1/2Si(O1/2-)2R10;
Q为Si(O1/2-)4;
R3、R4、R6、R7、R8和R10独立地为氟、苯基、或者可被氟或苯基部分或完全取代的C1至C10烷基基团;
R5为氟;苯基;或者任选地被氟或苯基部分或完全取代的C1至C10烷基基团;或者-R11-Om-(CH2-CH2-O)q(CH2-CH(CH3)-O)p-R12;
R9为-R11-Om-(CH2-CH2-O)q(CH2-CH(CH3)-O)p-R12;
R11为C1至C10烃基团;
R12为氢、苯基、氟或C1-C8烃基团,所述C1-C8烃基团在一些实施方式中被氟或苯基部分或完全取代和任选地被氨基甲酸酯、脲或羰基基团中断;
a和b独立地为0至30;
c、d和e独立地为0至5;
m为0或1;
q和p独立地为0至10;
条件是b+c至少为1;
前提条件是富硅氧烷化合物具有至少25%的硅重量含量。
在一个实施方式中,富硅氧烷化合物或其混合物具有在200-3000道尔顿之间的数均分子量。
在一个实施方式中,富硅氧烷化合物或其混合物具有在300-2500道尔顿之间的数均分子量。
在一个实施方式中,富硅氧烷化合物或其混合物具有在450-2000道尔顿之间的数均分子量。
在任一前述实施方式的组成物的一个实施方式中,富硅氧烷化合物或其混合物具有在28%以上的硅重量含量。
在任一前述实施方式的组成物的一个实施方式中,富硅氧烷化合物或其混合物具有在25%以上且最高达约32重量%的硅重量含量。
在任一前述实施方式的组成物的一个实施方式中,富硅氧烷化合物或其混合物具有平均每分子2个或更少的能与异氰酸酯反应的反应性基团。
在任一前述实施方式的组成物的一个实施方式中,富硅氧烷化合物或其混合物具有平均少于2个或没有能与异氰酸酯反应的反应性基团。
在任一前述实施方式的组成物的一个实施方式中,富硅氧烷化合物的下标a为至少等于1。
在任一前述实施方式的组成物的一个实施方式中,下标a为1-30;2-20;或2-10。
在任一前述实施方式的组成物的一个实施方式中,富硅氧烷组成物基于这样的分子量分布:其包含2.5%或更少的分子量在400以下的基于硅氧烷的物种(species)。
在任一前述实施方式的组成物的一个实施方式中,富硅氧烷组成物基于这样的分子量分布:其包含2.5%或更少的数均分子量在400以下、350以下、300以下或250以下的基于硅氧烷的物种。
在任一前述实施方式的组成物的一个实施方式中,富硅氧烷组成物包含约5%或更少、3.5%或更少、2.5%或更少、1%或更少、或0.5%或更少的含有3-6个硅氧烷基团的常记为D3、D4和D6的环状硅氧烷物种。
在一个方面中,提供泡沫制剂,其包括:多元醇;异氰酸酯;催化剂;表面活性剂;物理发泡剂;和按照前述实施方式的任一项的富硅氧烷组成物。
根据另一方面,提供通过使制剂的不同组分反应制造聚氨酯泡沫的工艺,所述制剂包括:多元醇;异氰酸酯;催化剂;表面活性剂;物理发泡剂;和按照前述实施方式的任一项的富硅氧烷组成物。
在一个实施方式中,富硅氧烷组成物或混合物的用量为至少0.02重量%,相对于除物理发泡剂以外的制剂组分总重量。
在任一前述实施方式的工艺的一个实施方式中,富硅氧烷组成物或混合物的存在量为至少0.03重量%,相对于除物理发泡剂以外的制剂组分总重量。
在任一前述实施方式的工艺的一个实施方式中,富硅氧烷组成物或混合物的存在量为至少0.05重量%,相对于除物理发泡剂以外的制剂组分总重量。
在任一前述实施方式的工艺的一个实施方式中,富硅氧烷组成物或混合物的存在量为3重量%或更低,相对于除物理发泡剂以外的制剂组分总重量。
在任一前述实施方式的工艺的一个实施方式中,富硅氧烷组成物或混合物的存在量为约0.05重量%至约3重量%,相对于除物理发泡剂以外的制剂组分总重量。
在任一前述实施方式的工艺的一个实施方式中,富硅氧烷组成物或其混合物在配制的预共混物中加入,以与异氰酸酯组分混合而产生用作绝热材料的聚氨酯泡沫。
在任一前述实施方式的工艺的一个实施方式中,富硅氧烷组成物或其混合物作为单独组分在泡沫分配单元上加入以产生用作绝热材料的聚氨酯泡沫。
在任一前述实施方式的工艺的一个实施方式中,将富硅氧烷组成物或其混合物加入到异氰酸酯组分,以与对异氰酸酯具有反应性的成分混合而产生用作绝热材料的聚氨酯泡沫。
在任一前述实施方式的工艺的一个实施方式中,除任选地包含硅氧烷的表面活性剂外还将富硅氧烷组成物或其混合物加入到聚氨酯泡沫制剂中,其中这样的表面活性剂的包含硅氧烷的部分若存在则具有低于25%的硅含量和在2000道尔顿以上的数均分子量。
在任一前述实施方式的工艺的一个实施方式中,多元醇选自聚酯多元醇、聚醚多元醇、聚碳酸酯多元醇、聚硫醚多元醇、聚己内酯、溴化聚醚多元醇、丙烯酸类多元醇或其两种或更多种的组合。
在任一前述实施方式的工艺的一个实施方式中,催化剂包由提供发泡和胶凝催化活性的叔胺及任选的提供异氰脲酸酯催化活性的三聚催化剂形成。
在任一前述实施方式的工艺的一个实施方式中,物理发泡剂选自烃和特别地戊烷以及如下物质的任意异构体混合物:氢氟烃、氢氟烯烃、氢氯氟烃、氢氯氟烯烃,及其任意组合。
在任一前述实施方式的工艺的一个实施方式中,所述工艺形成刚性或半刚性聚氨酯泡沫。在一个实施方式中,刚性或半刚性聚氨酯泡沫具有10-100kg/m3密度和100-500异氰酸酯指数。
在一个实施方式中,所述泡沫用作绝热材料。
在一个实施方式中,所述泡沫具有约23mW/m·K或更小的在0至30℃的平均温度下的初始热导率。
在又一方面中,提供制品,其包括由所述工艺形成的聚氨酯泡沫。
在一个方面中,提供由前述实施方式任一项的组合物(组成物)形成的聚氨酯或聚异氰脲酸酯泡沫。
在一个实施方式中,所述泡沫的异氰酸酯组成物选自芳族聚异氰酸酯、脂族聚异氰酸酯或其任意组合。
在一个方面中,提供制品,其包括前述实施方式任一项的聚氨酯或聚异氰脲酸酯泡沫。
在一个方面中,提供聚氨酯或聚异氰脲酸酯泡沫的形成方法,其包括使前述实施方式任一项的组合物(组成物)反应。
具体实施方式
本技术提供在泡沫形成制剂中使用的添加剂组成物和由这样的制剂制成的泡沫。泡沫制剂包括:(a)多元醇组分;(b)异氰酸酯组分;(c)催化剂组分;(d)表面活性剂;和(e)富硅氧烷组成物。富硅氧烷组成物的使用提供具有良好性质(包括例如低热导率)的泡沫。在不局限于任何特定理论的情况下,富硅氧烷组成物可充当良好的成核剂并且容许控制或提供具有良好性质(包括例如低热导率)的泡沫。
多元醇组分没有特别限制并且对于特定意图或预期应用可按需选择。在多种实施方式中,多元醇可选自聚酯多元醇、聚醚多元醇、聚碳酸酯多元醇、羟基封端的聚烯烃多元醇等、或其两种或更多种的组合。多元醇可为例如聚酯二醇、聚酯三醇、聚醚二醇、聚醚三醇等。替代地,多元醇可选自聚硫醚多元醇、聚己内酯、溴化聚醚多元醇、丙烯酸类多元醇等,或其两种或更多种的组合。当使用高官能度聚醚多元醇时,高官能度聚醚多元醇可具有约3至约6的官能度。多元醇例如蔗糖或山梨糖醇引发剂可与较低官能度的二醇或胺混合以使多元醇的官能度在约3.5至约5范围内。
另外,尤为适合的多元醇包括芳族聚酯多元醇。芳族聚酯多元醇可由基本上纯的反应物材料制备,或可使用更复杂的起始材料例如聚对苯二甲酸乙二醇酯。另外,可使用对苯二甲酸二甲酯(DMT)工艺残余物形成芳族聚酯多元醇。
芳族聚酯多元醇可包括卤素原子。其可为饱和或不饱和的。芳族聚酯多元醇具有的芳环含量可至少为约30重量%、35重量%、甚至约40重量%,基于总的化合物重量。此处,如说明书和权利要求中的其它位置那样,数值可组合以形成新的或未公开的范围。具有酸组分的聚酯多元醇为特别有用的,所述酸组分有利地包括至少约30重量%的邻苯二甲酸残余物或其异构体残余物。
芳族聚酯多元醇可具有大于约50mg KOH/g、大于约100mg KOH/g、大于约150mgKOH/g、大于约200mg KOH/g和大于约250mg KOH/g的羟值。在一个实施方式中,芳族聚酯多元醇具有约100mg KOH/g至约300mg KOH/g的羟值。此处,如说明书和权利要求中的其它位置那样,数值可组合以形成新的和未公开的范围。
在一个实施方式中,芳族聚酯多元醇具有大于约1或大于约2的官能度。在一个实施方式中,芳族聚酯多元醇具有约1-约4或约1-约2的官能度。此处,如说明书和权利要求中的其它位置那样,数值可组合以形成新的和未公开的范围。
泡沫组合物还包括异氰酸酯组成物。异氰酸酯可包括至少一种异氰酸酯并且可包括多于一种异氰酸酯。异氰酸酯可选自芳族异氰酸酯、脂族异氰酸酯或其任意组合。异氰酸酯组成物可包括芳族异氰酸酯例如聚合MDI。若异氰酸酯组成物包括芳族异氰酸酯,则芳族异氰酸酯可对应于式R1(NCO)z,其中R1为芳族多价有机基团并且z为对应于R1化合价的整数。通常,z为至少2。
异氰酸酯组成物可包括但不限于1,4-二异氰酸基苯、1,3-二异氰酸基-邻二甲苯、1,3-二异氰酸基-对二甲苯、1,3-二异氰酸基-间二甲苯、2,4-二异氰酸基-1-氯苯、2,4-二异氰酸基-1-硝基苯、2,5-二异氰酸基-1-硝基苯、间亚苯基二异氰酸酯、对亚苯基二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、2,4-和2,6-甲苯二异氰酸酯的混合物、1,5-萘二异氰酸酯、1-甲氧基-2,4-亚苯基二异氰酸酯、4,4′-二苯基甲烷二异氰酸酯、2,4′-二苯基甲烷二异氰酸酯、4,4′-二亚苯基二异氰酸酯、3,3′-二甲基-4,4′-二苯基甲烷二异氰酸酯、和3,3′-二甲基二苯基甲烷-4,4′-二异氰酸酯、三异氰酸酯例如4,4′,4″-三苯基甲烷三异氰酸酯聚亚甲基聚亚苯基聚异氰酸酯和2,4,6-甲苯三异氰酸酯、四异氰酸酯例如4,4′-二甲基-2,2′-5,5′-二苯基甲烷四异氰酸酯、甲苯二异氰酸酯、2,2′-二苯基甲烷二异氰酸酯、2,4′-二苯基甲烷二异氰酸酯、4,4′-二苯基甲烷二异氰酸酯、聚亚甲基聚亚苯基聚异氰酸酯、其对应的异构体混合物,及其任意组合。
泡沫组合物还包括一种或多种催化剂。催化剂没有特别限制并且可选自适合于催化来自水、多元醇或任何羟基封端的化合物的羟基基团和异氰酸酯之间的反应以形成膨胀的(发泡的,expanded)基于聚氨酯的热固性聚合物的任意催化剂材料。适合的催化剂的实例选自但不限于胶凝催化剂、和或发泡催化剂、和或三聚催化剂。具体地,胶凝催化剂可催化羟基与异氰酸酯的反应以产生氨基甲酸酯键。发泡催化剂可促进水与异氰酸酯的反应以产生脲键。三聚催化剂可促进三个异氰酸酯基团的反应以形成异氰脲酸酯键。催化剂可包括一种或多种催化剂并且典型地包括催化剂组合。催化剂取决于其包含异氰酸酯反应性基团与否在放热反应中可消耗或可不消耗。催化剂可包括本领域中知晓的任何适合的催化剂或催化剂混合物。适合的催化剂的实例包括但不限于在适当的稀释剂例如一缩二丙二醇中的胺催化剂;和金属催化剂例如锡、铋、铅等。催化剂若包括则可以各种量包括。在一个实施方式中,催化剂选自N,N-二甲基环己胺(DMCHA)、N,N,N′,N′,N″-五甲基二亚乙基三胺(PMDETA)、双(2-二甲基氨乙基)醚、脒例如2,3-二甲基-3,4,5,6-四氢嘧啶、其它叔胺例如三乙胺、三丁胺、二甲基苄胺、N-甲基吗啉、N-乙基吗啉、N-环己基吗啉、N,N,N′,N′-四甲基亚乙基二胺、N,N,N′,N′-四甲基丁烷二胺、N,N,N′,N′-四甲基己烷-1,6-二胺、单或双(二甲基氨丙基)脲二甲基哌嗪、1,2-二甲基咪唑、1-氮杂双环[3.3.0]辛烷、1,4-二氮杂双环[2.2.2]辛烷、烷醇胺化合物例如三乙醇胺、三异丙醇胺、N-甲基二乙醇胺、N-乙基二乙醇胺、二甲基乙醇胺、三(二烷基氨基烷基)-s-六氢三嗪包括三(N,N-二甲基氨丙基)-s-六氢三嗪、四烷基铵氢氧化物包括四甲基铵氢氧化物、季铵羧酸盐、丙烯酸四甲基铵、丙烯酸四乙基铵、丙烯酸四丙基铵、丙烯酸四丁基铵、甲酸(2-羟丙基)三甲基铵、2-乙基己酸(2-羟丙基)三甲基铵、新戊酸四甲基铵、新戊酸四乙基铵、新戊酸四丙基铵、新戊酸四丁基铵、三乙基乙酸四甲基铵、三乙基乙酸四乙基铵、三乙基乙酸四丙基铵、三乙基乙酸四丁基铵、新庚酸四甲基铵、新庚酸四乙基铵、新庚酸四丙基铵、新庚酸四丁基铵、新辛酸四甲基铵、新辛酸四乙基铵、新辛酸四丙基铵、新辛酸四丁基铵、新癸酸四甲基铵、新癸酸四乙基铵、新癸酸四丙基铵、新癸酸四丁基铵、碱金属氢氧化物包括氢氧化钠和氢氧化钾、碱金属醇盐包括甲醇钠和异丙醇钾、具有5-20个碳原子和/或侧接(lateral)羟基基团的长链脂肪酸的碱金属盐、锡、铁、铅、铋、汞、钛、铪、锆、氯化亚铁(II)、氯化锌、经辛酸铅稳定的辛酸亚锡、有机羧酸的锡(II)盐例如乙酸锡(II)、辛酸锡(II)、乙基己酸锡(II)和月桂酸锡(II),和有机羧酸的二烷基锡(IV)盐例如二月桂酸二丁基锡、二乙酸二丁基锡、马来酸二丁基锡和二乙酸二辛基锡,钾盐包括甲酸钾、乙酸钾、丙酸钾、丁酸钾、戊酸钾、己酸钾、庚酸钾、辛酸钾、2-乙基己酸钾、癸酸钾、丁酸钾、异丁酸钾、壬酸钾、硬脂酸钾,辛酸2-羟丙基三甲基铵溶液,钠盐如辛酸钠、乙酸钠、己酸钠,锂盐如硬脂酸锂、辛酸锂等,或其任意组合。在多种实施方式中,所包括的催化剂的量可为总泡沫组合物的0.5-8重量%。此处,如说明书和权利要求中的其它位置那样,数值可组合以形成新的或未公开的范围。
泡沫组合物包括表面活性剂。表面活性剂可为适合用于制造刚性泡沫的任意表面活性剂(例如包括可有助于控制或调节泡孔尺寸的那些)。这样的表面活性剂的实例为磺酸蓖麻油酯的钠盐、脂肪酸的钠盐、脂肪酸与胺的盐、磺酸的碱金属或铵盐、聚醚硅氧烷共聚物、或者其两种或更多种的混合物。在一个方面中,所述组合物包括有机硅表面活性剂和特别地有机硅-聚醚型表面活性剂。可使用其它类型的表面活性剂例如非有机硅表面活性剂、或两者的组合。在一个实施方式中,表面活性剂可包括非离子表面活性剂、阳离子表面活性剂、阴离子表面活性剂、两性表面活性剂、及其组合。在多种实施方式中,表面活性剂可包括但不限于聚氧基亚烷基多元醇表面活性剂、烷基苯酚乙氧基化物表面活性剂及其组合。在一个实施方式中,磺酸盐,油酸、硬脂酸、十二烷基苯-二磺酸或二萘基甲烷-二磺酸、和蓖麻油酸的例如碱金属和/或铵盐,以及其它的有机聚硅氧烷、氧乙基化烷基苯酚、氧乙基化脂肪醇、石蜡油、蓖麻油、蓖麻油酯和蓖麻油酸酯,以及泡孔调节剂例如脂肪醇,及其组合。
在一个实施方式中,表面活性剂选自有机硅表面活性剂。通常,有机硅表面活性剂可在由树脂组成物和异氰酸酯组成物的反应产生的刚性泡沫中控制泡孔尺寸、闭孔含量、流动(flow)和限制空隙形成。适合的表面活性剂的实例包括有机硅-聚醚型表面活性剂,其包括如下式的那些:
M1D1 xD2 yM2 (I)
其中M1和M2独立地表示(CH3)3SiO1/2或(CH3)2R1SiO1/2,
D1表示(CH3)2SiO2/2,
D2表示(CH3)R1SiO2/2,
x+y通常为10至150;y通常为至少2;比率x/y正常为2-15;和R1为独立选择的聚醚或其混合,且平均上具有式:—CnH2nO(C2H4O)t(C3H6O)zR2其拥有150至5000的数均分子量,其中n为2-4,t为使得氧基亚乙基残基构成聚氧基亚烷基聚醚的亚烷基氧残基的40至100重量%的数字,z为使得亚丙基氧残基构成聚氧基亚烷基聚醚的亚烷基氧残基的60至0重量%的数字,和R2表示氢或具有1-4个碳原子的烷基基团或—C(O)CH3;
有机硅共聚物表面活性剂可通过若干种合成途径制备,所述合成途径包括分阶段加入聚醚。而且,聚氧基亚烷基聚醚组分为在本领域中公知的和/或可通过任何常规工艺制造。例如,羟基封端的聚氧基亚烷基聚醚(其是在三元共聚物的制备中便利的起始材料)可通过使适合的醇与环氧乙烷和环氧丙烷(1,2-环氧丙烷)反应以产生期望分子量的聚氧基亚烷基聚醚而制备。适合的醇为羟基烯基化合物例如乙烯基醇、烯丙基醇、甲基烯丙基醇等。通常,优选地将醇起始物与催化量的适合催化剂例如氢氧化钠、氢氧化钾、其它碱金属氢氧化物、或者钠或其它碱金属一起放置在高压釜或其它高压器皿中。制备的进一步细节阐述于例如美国专利No.3,980,688中。其全部内容并入本文中作为参考。
上述的醇-氧化物反应产生单羟基封端的聚氧基亚烷基聚醚,其中其它封端基团为由烯丙基或甲基烯丙基或乙烯基氧基基团组成的不饱和烯属基团。这些聚醚可通过将所述单羟基封端的聚(氧基亚乙基氧基亚丙基)共聚物的羟基末端基团经由任何常规手段封端而转化为非异氰酸酯反应性聚氧基亚烷基聚醚。
泡沫组合物可包括两种或更多种不同类型的有机硅表面活性剂。
对于泡沫组合物适合的常规的有机硅表面活性剂的非限制实例包括可得自Momentive Performance Materials Inc.的以商标得到的那些。适合的表面活性剂包括但不限于L-6900、L-5111、L-6972、L-6633、L-6635、L-6190、L-6100等或者其两种或更多种的组合。
表面活性剂可以任何适当量存在。在多种实施方式中,表面活性剂以泡沫组合物的0.5-5、1-3或约2重量%的量存在。此处,如说明书和权利要求中的其它位置那样,数值可组合以形成新的或未明确说明的范围。
泡沫组合物可还包括非有机硅表面活性剂。非有机硅表面活性剂可与有机硅表面活性剂一起或不与其一起使用。本领域中知晓的任何表面活性剂可在本发明中使用。因此,表面活性剂可包括非离子表面活性剂、阳离子表面活性剂、阴离子表面活性剂、两性表面活性剂及其组合。在多种实施方式中,表面活性剂可包括但不限于聚氧基亚烷基多元醇表面活性剂、烷基苯酚乙氧基化物表面活性剂及其组合。若表面活性剂包括在树脂组成物中,则表面活性剂可以任何适当量存在。
泡沫组合物包括包含限定分子量的富硅氧烷化合物的添加剂组成物。该添加剂在本文中也可称为富硅氧烷组成物。富硅氧烷组成物可包括如下式的化合物
M3 aD3 bD4 cTdQe (II)
其中M3为三烷基封端单元R3R4R5SiO1/2—;D3为二烷基单元-O1/2R6R7SiO1/2—;D4为烷基单元-O1/2R8R9SiO1/2—;T为-O1/2Si(O1/2-)2R10;和Q为Si(O1/2-)4;
R3、R4、R6、R7、R8和R10独立地为氟、苯基、或者可被氟或苯基部分或完全取代的C1至C10烷基基团;
R5为氟、苯基、或任选地被氟或苯基部分或完全取代的C1至C10烷基基团、或-R11-Om-(CH2-CH2-O)q(CH2-CH(CH3)-O)p-R12;
R9为-R11-Om-(CH2-CH2-O)q(CH2-CH(CH3)-O)p-R12;
R11为C1至C10烃基团;
R12为氢、苯基、氟、或C1-C8烃基团,所述C1-C8烃基团在一些实施方式中被氟或苯基部分或完全取代和任选地被氨基甲酸酯、脲或羰基基团中断;
a和b独立地为0至30;
c、d和e独立地为0至5;
m为0或1;
q和p独立地为0至10;
条件是b+c至少为1;
前提条件是富硅氧烷化合物具有至少25%的硅重量含量。
在实施方式中,富硅氧烷化合物具有约200至约3000道尔顿;约300至约2500道尔顿;约400至约2000道尔顿;约450至约2000道尔顿的数均分子量。数值可组合以形成新的和未明确说明的范围。数均分子量可通过硅NMR(29Si NMR)测定。
在实施方式中,富硅氧烷组成物基于这样的分子量分布:其包含以重量计2.5%或更少的分子量为400以下的基于硅氧烷的物种。在一个实施方式中,提供根据任一前述实施方式的组成物,其中富硅氧烷组成物基于这样的分子量分布:其包含以重量计2.5%或更少的分子量为400以下、350以下、300以下或250以下的基于硅氧烷的物种。分子量可使用气相色谱法评价和量化,使用校准因子再计算到重量%。
在实施方式中,富硅氧烷组成物以约5%或更少、4%或更少、2.5%或更少、1%或更少或0.5%或更少的量包括具有3-6个硅氧烷单元的标准低分子量环状硅氧烷。在实施方式中,富硅氧烷组成物具有各自在0.1%以下的非常低水平的所述残余环状硅氧烷物种。这样的低分子量环状硅氧烷典型地为六甲基环三硅氧烷(D3)、八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)和十二甲基环六硅氧烷(D6)。
富硅氧烷组成物的硅含量为至少25重量%或更大;至少28重量%或更大;至少30重量%或更大,最高达约32重量%。
在一个实施方式中,富硅氧烷组成物优选地平均具有每分子2个或更少的能与异氰酸酯反应的反应性基团;每分子1个或更少的能与异氰酸酯反应的反应性基团;或不具有能与异氰酸酯反应的反应性基团。
在一个实施方式中,富硅氧烷组成物为具有约200至3000道尔顿、约300至2500道尔顿、约450至2000道尔顿数均分子量的聚二甲基硅氧烷;其中具有400以下的分子量的物种少于2.5重量%。
包括富硅氧烷化合物的组成物可包括由式(II)描述的不同富硅氧烷化合物的组合。在泡沫制剂中提供富硅氧烷化合物,使得相对于不包括物理发泡剂的总制剂重量,富硅氧烷组成物以重量计为约0.02%至约5%;约0.03%至约4%;甚至约0.05%至约3%。
富硅氧烷组成物可作为单独添加剂提供或作为包括如下的组合物的一部分而加入:表面活性剂、所述富硅氧烷组成物和可能地稀释剂或者与在泡沫制剂中作为成分引入相关的另外组分。适合的稀释剂的实例包括例如一缩二丙二醇、己二醇或由从1至10的不同官能度的烷氧基化引发剂获得的聚合物等。
泡沫组合物可还包括一种或多种发泡剂,其包括但不限于物理发泡剂、化学发泡剂或其任意组合。在一个实施方式中,发泡剂可包括物理发泡剂和共化学发泡剂两者,并且该发泡剂可包括在泡沫组合物中。物理发泡剂典型地不与树脂组成物和/或异氰酸酯化学反应来提供发泡气体。物理发泡剂可为气体或液体。液体物理发泡剂当加热时可蒸发成气体并且当冷却时可返回到液体。物理发泡剂可降低刚性聚氨酯泡沫的热导率。发泡剂可包括但不限于二氯甲烷、丙酮、和液态二氧化碳、脂族和/或脂环族烃、卤代烃和烷烃、缩醛、水、醇、甲酸及其任意组合。在实施方式中,所述组合物包括选自水、甲酸或其组合的化学发泡剂。
在多种实施方式中,发泡剂可选自烃,氢氟烃,氢氯氟烯烃(HCFO)和氢氟烯烃(HFO),挥发性非卤代C2-C7烃例如烷烃(包括正戊烷、异戊烷和环戊烷),烯烃,具有最高达6个碳原子的环烷烃,二烷基醚,亚环烷基醚和酮,和氢氟烃,C1-C4氢氟烃,挥发性非卤代烃例如线型或支化的烷烃例如丁烷、异丁烷、2,3-二甲基丁烷、正和异己烷、正和异庚烷、正和异辛烷、正和异壬烷、正和异癸烷、正和异十一烷以及正和异十二烷,烯烃例如1-戊烯、2-甲基丁烯、3-甲基丁烯和1-己烯,环烷烃例如环丁烷和环己烷,线型和/或环状醚例如二甲醚、二乙醚、甲乙醚、乙烯基甲基醚、乙烯基乙基醚、二乙烯基醚、二甲氧基甲烷(甲缩醛)、四氢呋喃和呋喃,酮例如丙酮、甲乙酮和环戊酮,其异构体,羧酸酯例如蚁酸甲酯(甲酸甲酯),氢氟烃例如二氟甲烷(HFC-32)、1,1,1,2-四氟乙烷(HFC-134a)、1,1,2,2-四氟乙烷(HFC-134)、1,1-二氟乙烷(HFC-152a)、1,2-二氟乙烷(HFC-142)、三氟甲烷、七氟丙烷(R-227a)、六氟丙烷(R-136)、1,1,1-三氟乙烷、1,1,2-三氟乙烷、氟乙烷(R-161)、1,1,1,2,2-五氟丙烷、五氟丙烯(R-2125a)、1,1,1,3-四氟丙烷、四氟丙烯(R-2134a),二氟丙烯(R-2152b)、1,1,2,3,3-五氟丙烷、1,1,1,3,3-五氟正丁烷和1,1,1,3,3-五氟戊烷(245fa)、其异构体、1,1,1,2-四氟乙烷(HFC-134a)、其异构体,及其组合。在多种实施方式中,发泡剂可进一步限定为1,1,1,3,3-五氟戊烷(245fa),或者HFC 245fa、365MFC、227ea和134a的组合。在一种替代实施方式中,发泡剂可进一步限定为365MFC,其可与227ea共混。在一种进一步的实施方式中,发泡剂可进一步限定为1-氯-3,3,3-三氟丙烯或1,1,1,4,4,4-六氟-2-丁烯的顺式或反式异构体、或它们彼此或与以上提到的任意其它发泡剂的组合。
在多种实施方式中,发泡剂可以泡沫组合物的0.1-30、1-25、2-20、3-18、5-15重量%的量存在。此处,如说明书和权利要求中的其它位置那样,数值可组合以形成新的或未公开的范围。通常,发泡剂和/或水的量可基于刚性泡沫的期望密度和发泡剂在相关时的树脂组成物中的溶解度而选择。
泡沫组合物可还包括交联剂和/或扩链剂。交联剂可包括但不限于另外的多元醇、胺及其任意组合。若交联剂包括在泡沫组合物中,则交联剂可以任何适当量存在。对于在本技术中使用而想到的扩链剂包括但不限于肼、伯和仲二胺、醇、氨基酸、羟基酸、二醇及其组合。对于使用而想到的具体扩链剂包括但不限于单和双-乙二醇、单和双-丙二醇、1,4-丁烷二醇、1,3-丁烷二醇、丙二醇、一缩二丙二醇、一缩二乙二醇、甲基丙二醇、单、双-和三-乙醇胺、N-N′-双(2-羟基-丙基苯胺)、三羟甲基丙烷、甘油、氢醌、双(2-羟乙基)醚、4,4′-亚甲基-双(2-氯苯胺、二乙基甲苯二胺、3,5-二甲基巯基-甲苯二胺、肼、异佛尔酮二胺、己二酸、硅烷、及其任意组合。
泡沫组合物可还包括一种或多种添加剂。适合的添加剂包括但不限于非反应性阻燃剂(例如各种磷酸酯或盐、各种膦酸酯或盐、磷酸三乙酯、磷酸三氯丙酯、磷酸三苯酯或乙基膦酸二乙酯、磷酸三(2-氯乙基)酯、三乙基-磷酸酯、磷酸三(2-氯丙基)酯、磷酸三(1,3-二氯丙基)酯、磷酸二铵、各种卤代芳族化合物、氧化锑、氧化铝三水合物、聚氯乙烯及其任意组合)、不含OH/非反应性阻燃剂、链终止剂、改性或未改性的酚醛树脂、惰性稀释剂、胺、消泡试剂、空气释放试剂、润湿剂、表面改性剂、蜡、惰性无机填料、分子筛、反应性无机填料、短切玻璃、其它类型的玻璃例如玻璃毡、加工添加剂、表面活性剂、增粘剂、抗氧化剂、染料、颜料、紫外光稳定剂、触变剂、抗老化剂、抗静电添加剂、润滑剂、偶联剂、溶剂、流变促进剂、泡孔扩张剂、脱模添加剂、及其组合。一种或多种添加剂可以任意量存在于泡沫组合物中。
除泡沫组合物外,本技术还提供形成泡沫的方法和在表面上形成泡沫的方法。
形成刚性泡沫的方法典型包括将多元醇、异氰酸酯组成物、表面活性剂、富硅氧烷组成物和所有其它添加剂组合的步骤。泡沫的异氰酸酯指数通常没有限制。最典型地,将多元醇和异氰酸酯组成物组合使得异氰酸酯指数通常在120以上并且取决于所要制造的泡沫(PUR或PIR类型)可最高达500或甚至600的值。本领域技术人员将认识到,泡沫可为聚氨酯型泡沫(PUR,典型地在200以下的指数)或聚异氰脲酸酯(PIR,典型地远高于200和通常在250以上的指数)泡沫。然而,将认识到,不存在将PUR泡沫与PIR泡沫划分开的绝对指数值。
在表面上形成刚性泡沫的方法可包括将所述组分组合以形成泡沫混合物的步骤。通常,该组合步骤可在混合设备例如静态混合器、机械或撞击混合腔室、或混合泵中发生。在一个实施方式中,混合步骤在静态混合管中发生。替代地,泡沫组成物(组合物)和异氰酸酯组成物可在喷射喷嘴中组合。
当在工业混合设备上加工时,形成刚性或半刚性泡沫的方法可包括对制剂组分的一种或多种进行空气成核。
所述组分可当在表面上或离开表面时组合。在一个实施方式中,所述组分可在喷枪头中或在组合物正施加到其的表面上方的空气中组合。所述组分可通过本领域中知晓的任意方法组合并施加到表面,所述方法包括喷射、浸渍、倾倒、涂覆、上漆等。
本技术提供半刚性或刚性聚氨酯泡沫(“刚性或半刚性泡沫”)。刚性泡沫可为开孔的或闭孔的并且可包括高度交联的聚合物结构,其容许泡沫具有良好的热稳定性、在低密度下高的压缩强度、低热导率和良好的阻隔性质。典型地,本技术的刚性泡沫可具有大于室温(大约23℃+/-2℃(大约73.4°F+/-3.6°F))的玻璃化转变温度并且典型地在室温下为刚性的。通常,泡沫在其玻璃化转变温度以下、特别地在其储能模量的玻璃态区域中为刚性的。聚氨酯发泡材料可具有约10至约900kg/m3、约15至约800kg/m3、约20至约500kg/m3、约30至约400kg/m3的密度。在一个实施方式中,刚性泡沫可具有约10至约60kg/m3的密度。此处,如说明书和权利要求中的其它位置那样,数值可组合以形成新的或未公开的范围。
泡沫混合物可施加到任何适当的表面例如砖、混凝土、砌石、干墙、石膏夹心纸板、石膏、金属、石材、木材、塑料、聚合物复合材料或其任意组合。另外,所述表面可为模具表面并且因此刚性泡沫可在模具中形成。
所得的刚性或半刚性泡沫可以板材、成型体、面板或填充腔的形式使用。填充腔例如可为管道、隔热墙(insulated wall)、隔热外壳(隔热船体,insulated hull)结构。刚性泡沫可为喷射泡沫、起泡泡沫或连续制造的层压产品或非连续制造的层压产品,其包括但不限于用其它材料例如硬板、石膏板、塑料、纸、金属或其组合形成的层压体或层压产品。
根据本技术实施方式制备的刚性泡沫可显示改善的加工性。此泡沫可呈现减少的缺陷,包括但不限于减少的收缩和形变。该特性在夹心面板的制造中可为有用的。夹心面板可包括至少一个相对平坦的刚性泡沫层(即具有两个总体上大的维度和一个总体上小的维度的层),在其较大维度的各面上,每个这样的面面对至少一个柔性或刚性材料层例如金属或其它结构提供材料的箔或较厚层。这样的层可在某些实施方式中充当泡沫形成期间的基底。
另外,由以上指出的组分以上述方法制造的泡沫混合物可具有改善的绝热性例如较低的热导率。特别地,使用具有特定分子量的所述结构的硅氧烷组成物的本发明组合物可相对于没有所述硅氧烷组成物的类似泡沫组合物降低泡沫的热导率。
参考以下实施例可进一步理解包括上述富硅氧烷组成物的刚性泡沫。
实施例
泡沫制备和测试方法
泡沫总体上通过首先在1升塑料杯中制造包括不同多元醇、阻燃剂、催化剂和水的树脂共混物而制备。
在维持如表1a-1c和3中所示的制剂组分比率的情况下使用适当重量以获得足够自由的起发高度(rise height)。随后将常规的表面活性剂和富硅氧烷组成物单独加入或作为混合物加入以防一者具有低水平而妨碍良好的称量准确度。在两种情形中,用抹刀将它们轻轻地混合直至实现预混共混物的均匀性。物理发泡剂为戊烷异构体或其混合物并且被加入到该树脂共混物直到目标重量,然后用抹刀轻轻混合直至实现预混共混物的均匀性。加入少量额外的戊烷直至获得校正因在混合期间蒸发引起的少量损失所需的重量。其重复进行直至所需重量达到并且稳定。进一步使用机械混合器将所得混合物以4000rpm混合10秒。所需量的异氰酸酯在另一个杯中预称重并快速加入到容纳多元醇-戊烷预混物的杯以提供反应性共混物。使用装备有6cm环形螺旋桨的高能量机械混合器将反应性共混物以4000rpm进一步混合5秒并且在混合结束后立即倾倒在各面封闭在正方形木质框架中的23x23cm截面和20cm高度的正方形开口纸杯模具中。倾倒在正方形截面的中间进行。泡沫在竖直方向上自由膨胀。乳白时间和凝胶时间由杯中残留的反应性材料测量。获得刚性自由起发泡沫并且使其冷却并在室温下在开口纸模具内固化接下来的24小时。
然后,在24小时后从大小为20x20x4 cm的块状物的中心切下一片泡沫并且评价其热导率。使用该片测量芯泡沫密度测量和使用FOX Lasercomp 200热流计在0℃和20℃之间(10℃平均温度)或10和36℃之间(23℃平均温度)测量热导率(也称为λ值)。记录值称为初始热导率。
组合物中使用的原材料
Stepanpol PS 2412为得自Stepan Voranol的芳族聚酯多元醇。RN411为得自DowChemicals的聚醚多元醇。Daltocel R585为得自Huntsman Co.的聚醚多元醇。TCPP液体阻燃剂为(三(1-氯-2-丙基)磷酸酯。Niax A-1、C-5、C-8和辛酸钾为来自Momentive UrethaneAdditives系列产品的商业催化剂。Desmodur 44V70L和Suprasec 5025为分别得自Covestro和Huntsman Co的聚合MDI品级。
表1a-1c显示PIR泡沫例如用其中异氰酸酯指数典型地在200以上的制剂制成的泡沫的典型配方。对于所列出的实验,选择300的指数,其是用于PIR泡沫(例如用于柔性或金属面的建筑面板)的典型值。所使用的发泡剂为正戊烷并且λ值在0℃和20℃之间的板温在10℃平均温度下测量。
表1a
表1b
表1c
泡沫 | 14 | 15 | 16 | 17 |
制剂 | ||||
芳族聚酯多元醇,Stepanpol PS 2412 | 100 | 100 | 100 | 100 |
TCPP液体阻燃剂 | 15.0 | 15.0 | 15.0 | 15.0 |
水 | 0.8 | 0.8 | 0.8 | 0.8 |
Niax催化剂C-5 | 0.25 | 0.25 | 0.25 | 0.25 |
Niax辛酸钾 | 2.5 | 2.5 | 2.5 | 2.5 |
常规的刚性泡沫有机硅稳定剂 | 1.6 | 1.6 | 1.6 | 1.6 |
正戊烷 | 20 | 20 | 20 | 20 |
聚合MDI,Desmodur 44V70L | 218 | 218 | 218 | 218 |
添加的硅氧烷组成物1 | ||||
添加的硅氧烷组成物2 | ||||
添加的硅氧烷组成物3 | ||||
添加的硅氧烷组成物4 | ||||
添加的硅氧烷组成物5 | 5 | |||
添加的硅氧烷组成物6 | 0.2 | |||
添加的硅氧烷组成物7 | 1.2 | |||
添加的硅氧烷组成物8 | 1.2 | |||
添加的组成物中的硅氧烷化合物重量(%) | 100 | 100 | 87.3 | 87 |
硅氧烷化合物,计算的参数 | ||||
硅%* | 34.65 | 37.2 | 19.5** | 19.1** |
平均分子量* | 162.4 | 830 | 720** | 740** |
反应性基团/分子的平均数量* | 0 | 0 | 1 | 0 |
相对于总制剂,添加的硅氧烷化合物**(%) | 1.46 | 0.06 | 0.31 | 0.31 |
异氰酸酯指数 | 300 | 300 | 300 | 300 |
反应性-凝胶时间(s) | 65 | 65 | 62 | 60 |
泡沫密度(kg/m<sup>3</sup>) | 30 | 32 | 33 | 31 |
泡孔尺寸/结构 | 受控 | 受控 | 受控 | 受控 |
24小时后的热导率 | ||||
(λ0-20℃,以mW/K.m计) | 24.2 | 23.54 | 24.26 | 23.97 |
表1a-1c备注
*在硅氧烷改性的情形中不包括过量的聚醚反应物
**不包括物理发泡剂重量
对于表1a-c和表3两者,使用下面的基于有机硅的组成物:
常规的刚性泡沫有机硅稳定剂:由使65个D单元和7.5个D’单元的线型有机硅氢化物在烯丙基羟基封端的EO/PO聚醚上以30%聚醚过量进行反应而获得的共聚物,所述聚醚包含约12.8个EO单元和3.2个PO。硅氧烷共聚物具有约19%的有机硅含量和约11000道尔顿的数均分子量。
·基于硅氧烷的组成物1-4描述于表2中。
·硅氧烷组成物5:六甲基二硅氧烷或MM
·硅氧烷组成物6:未改性聚二甲基硅氧烷,平均结构M3D7T的T类型
·硅氧烷组成物7:由MD’M与烯丙基羟基封端的聚环氧乙烷(6.6个EO单位)反应而获得的改性硅氧烷
·硅氧烷组成物8:由MD’M与烯丙基甲氧基封端的聚环氧乙烷(6.6个EO单位)反应而获得的改性硅氧烷
表2
表2备注
*:通过29Si NMR作为每两个M末端的D单元平均数量测定
**:通过气相色谱法测定,使用校准因子再计算为重量%
***:通过凝胶渗透色谱法(GPC)作为对在低分子量侧上的总积分贡献小于0.5%的分子量测定-使用聚二甲基硅氧烷标准物进行校准
****:通过凝胶渗透色谱法(GPC)作为对在高分子量侧上的总积分贡献小于1%的分子量测定-使用聚二甲基硅氧烷标准物进行校准
*****:D4、D5和D6为硅氧烷组成物中的常见环状残留物种,分别为八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)和十二甲基环六硅氧烷(D6)。各水平通过对组成物进行液体提取、随后对提取的混合物进行气相色谱分析而获得。
结果表明,以每100份主要多元醇1.6-2.8份的标准水平引入的常规的有机硅表面活性剂导致在24-24.5mW/m.K范围内的初始的泡沫热导率值(或λ值)(泡沫1a至1c)。对于不具有任何添加的硅氧烷组成物的泡沫观察到一定的标准分散但仍在24-24.5mW/m.K的范围内。通过将常规的表面活性剂水平增至非常高的值例如5份,可获得稍低的λ值23.81mw/m.K,但这是被认为并非高度显著的十分小的益处。发现通过除常规的有机硅表面活性剂外还加入所选择的分子量的富硅氧烷组成物并且以每100份主要多元醇低至0.2份或更高的水平加入,可获得显著较低的泡沫λ值。这可在添加的硅氧烷组成物1-3或6的情况下看到,所述硅氧烷组成物1-3或6落在本发明的方面和实施方式内。使用添加的硅氧烷组成物4、5、7或8(其具有较小或较大的分子量或较低的硅含量且在本发明之外)的对比例未提供这样的益处。对于其它基本泡沫特性例如反应性(如通过凝胶时间量化的)和泡沫密度而言,由这些实验产生的所有泡沫并无显著不同。
表3显示PUR泡沫(例如用其中计算的异氰酸酯过量显著低于200的制剂制成)的典型制剂。对于表3中列出的实验,使用30摩尔%的异氰酸酯过量,意味着异氰酸酯指数为130。对于该制剂使用的发泡剂为环戊烷并且λ值在0℃和36℃之间的板温在23℃平均温度下测量。
表3
*在硅氧烷改性的情况下不包括过量的聚醚反应物
**不包括物理发泡剂重量
这些PUR制剂显示了如对于PIR制剂获得的相当的效果。相对于对照泡沫2,用落在本发明的方面和实施方式的范围内的添加的硅氧烷组成物2和6,实现0.4mW/m.K和更高的显著的热导率益处。使用落在本发明之外的添加的硅氧烷组成物5、7或8的对比例未改善λ值(硅氧烷组成物5和8)或显示大约0.2mW/m.K的微不足道的益处(硅氧烷组成物7)。再次地,泡沫产生的其它的基本泡沫特性例如通过凝胶时间量化的反应性和泡沫密度并无显著不同。
本技术实施方式已经在上文描述并且其他人员在阅读和理解本说明书时可想到变型和改变。如下的权利要求旨在以如下程度包括所有的变型和改变:它们进入权利要求或其等同物的范围内。
Claims (28)
1.聚氨酯泡沫制剂中作为添加剂使用的组成物,所述组成物包括式M3 aD3 bD4 cTdQe(II)的富硅氧烷化合物
其中
M3为三烷基封端单元R3R4R5SiO1/2—;
D3为二烷基单元-O1/2R6R7SiO1/2—;
D4为烷基单元-O1/2R8R9SiO1/2—;T为-O1/2Si(O1/2-)2R10;
Q为Si(O1/2-)4;
R3、R4、R6、R7、R8和R10独立地为氟、苯基、或者可被氟或苯基部分或完全取代的C1至C10烷基基团;
R5为氟;苯基;或者任选地被氟或苯基部分或完全取代的C1至C10烷基基团;或者-R11-Om-(CH2-CH2-O)q(CH2-CH(CH3)-O)p-R12;
R9为-R11-Om-(CH2-CH2-O)q(CH2-CH(CH3)-O)p-R12;
R11为C1至C10烃基团;
R12为氢、苯基、氟、或C1-C8烃基团,所述C1-C8烃基团在一些实施方式中被氟或苯基部分或完全取代和任选地被氨基甲酸酯、脲或羰基基团中断;
a和b独立地为0至30;
c、d和e独立地为0至5;
m为0或1;
q和p独立地为0至10;
条件是b+c为至少1;
前提条件是富硅氧烷化合物具有至少25%的硅重量含量。
2.如权利要求1所述的组成物,其中富硅氧烷化合物或其混合物具有在200和3000道尔顿之间的数均分子量。
3.如权利要求1所述的组成物,其中富硅氧烷化合物或其混合物具有在300和2500道尔顿之间的数均分子量。
4.如权利要求1所述的组成物,其中富硅氧烷化合物或其混合物具有在450和2000道尔顿之间的数均分子量。
5.如权利要求1-4任一项所述的组成物,其中富硅氧烷化合物或其混合物具有28%以上的硅重量含量。
6.如权利要求1-4任一项所述的组成物,其中富硅氧烷化合物或其混合物具有28%以上至最高达32%的硅重量含量。
7.如权利要求1-6任一项所述的组成物,其中富硅氧烷化合物或其混合物具有平均每分子2个或更少的能与异氰酸酯反应的反应性基团。
8.如权利要求1-7任一项所述的组成物,其中富硅氧烷化合物或其混合物具有平均少于2个或没有能与异氰酸酯反应的反应性基团。
9.如权利要求1-8任一项所述的组成物,其中富硅氧烷化合物的下标a至少等于1。
10.如权利要求1-9任一项所述的组成物,其中富硅氧烷组成物基于包括2.5重量%或更少的分子量在400以下的基于硅氧烷的物种的分子量分布。
11.如权利要求1-10任一项所述的组成物,其中富硅氧烷组成物包含约5重量%或更少的具有3-6个硅氧烷基团的环状硅氧烷物种,所述具有3-6个硅氧烷基团的环状硅氧烷物种选自六甲基环三硅氧烷(D3)、八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)和十二甲基环六硅氧烷(D6)。
12.用于通过使制剂的不同组分反应而制造聚氨酯泡沫的工艺,所述制剂包括:
多元醇;
异氰酸酯;
催化剂;
表面活性剂;
物理发泡剂;和
如权利要求1-11任一项所述的富硅氧烷组成物。
13.如权利要求12所述的工艺,其包括量为至少0.02重量%的富硅氧烷组成物或混合物,相对于除物理发泡剂以外的制剂组分总重量。
14.如权利要求12-13任一项所述的工艺,其包括量为至少0.03重量%的富硅氧烷组成物或混合物,相对于除物理发泡剂以外的制剂组分总重量。
15.如权利要求12-13任一项所述的工艺,其包括量为至少0.05重量%的富硅氧烷组成物或混合物,相对于除物理发泡剂以外的制剂组分总重量。
16.如权利要求12-15任一项所述的工艺,其包括量为3重量%或更低的富硅氧烷组成物或混合物,相对于除物理发泡剂以外的制剂组分总重量。
17.如权利要求12-16任一项所述的工艺,其包括量为约0.05重量%至约3重量%的富硅氧烷化合物或混合物,相对于除物理发泡剂以外的制剂组分总重量。
18.如权利要求12-17任一项所述的工艺,其中将富硅氧烷组成物或其混合物加入配制的预共混物中,以与异氰酸酯组分混合而产生用作绝热材料的聚氨酯泡沫。
19.如权利要求12-18任一项所述的工艺,其中将富硅氧烷组成物或其混合物作为单独组分加入到泡沫分配单元上以产生用作绝热材料的聚氨酯泡沫。
20.如权利要求12-19任一项所述的工艺,其中将富硅氧烷组成物或其混合物加入到异氰酸酯组分,以与对异氰酸酯具有反应性的成分混合而产生用作绝热材料的聚氨酯泡沫。
21.如权利要求12-20任一项所述的工艺,其中除任选地包含硅氧烷的表面活性剂外,还将富硅氧烷组成物或其混合物加入到聚氨酯泡沫制剂中,其中这样的表面活性剂的包含硅氧烷的部分若存在则具有低于25%的硅含量和2000道尔顿以上的数均分子量。
22.如权利要求12-21任一项所述的工艺,其中所述工艺形成刚性或半刚性聚氨酯泡沫。
23.如权利要求22所述的工艺,其中所述刚性或半刚性聚氨酯泡沫具有在10和100kg/m3之间的密度以及在100和500之间的异氰酸酯指数。
24.聚氨酯泡沫,其由如权利要求1-11任一项所述的组成物形成。
25.如权利要求23所述的聚氨酯泡沫,其中泡沫为刚性或半刚性聚氨酯泡沫,其具有在10和100kg/m3之间的密度以及在100和500之间的异氰酸酯指数。
26.如权利要求24所述的聚氨酯泡沫,其中泡沫在0至30℃的平均温度下具有约23mW/m·K或更小的初始热导率。
27.绝热材料,其包括如权利要求25或26所述的聚氨酯泡沫。
28.制品,其包括如权利要求24-26任一项所述的聚氨酯泡沫。
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Publication number | Publication date |
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JP2022509109A (ja) | 2022-01-20 |
CA3120512A1 (en) | 2020-05-28 |
WO2020106538A1 (en) | 2020-05-28 |
MX2021005881A (es) | 2021-08-11 |
BR112021009742A2 (pt) | 2021-08-24 |
CN113272352B (zh) | 2024-02-06 |
KR20210094008A (ko) | 2021-07-28 |
US20220017717A1 (en) | 2022-01-20 |
EP3883981A1 (en) | 2021-09-29 |
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