CN103619954B - 具有改善的绝热性质的异氰酸酯基聚合物泡沫 - Google Patents
具有改善的绝热性质的异氰酸酯基聚合物泡沫 Download PDFInfo
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- CN103619954B CN103619954B CN201180071786.0A CN201180071786A CN103619954B CN 103619954 B CN103619954 B CN 103619954B CN 201180071786 A CN201180071786 A CN 201180071786A CN 103619954 B CN103619954 B CN 103619954B
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- Prior art keywords
- isocyanate
- foam
- agent
- white carbon
- based polymer
- 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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- 150000001875 compounds Chemical class 0.000 claims description 17
- 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 15
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Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/3206—Polyhydroxy compounds aliphatic
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/4816—Two or more polyethers of different physical or chemical nature mixtures of two or more polyetherpolyols having at least three hydroxy groups
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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
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- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/6705—Unsaturated polymers not provided for in the groups C08G18/671, C08G18/6795, C08G18/68 or C08G18/69
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
本发明涉及包含炭黑组分的硬质异氰酸酯基聚合物泡沫,所述炭黑组分包含至少50重量%的氟化炭黑。具有改善的热性质的所述泡沫,具体地说,硬质聚氨酯和/或聚异氰脲酸酯泡沫用于绝缘应用。
Description
技术领域
本发明涉及包含氟化炭黑并具有改善的热性质的硬质异氰酸酯基聚合物泡沫,具体地,用于绝缘应用的硬质聚氨酯和/或聚异氰脲酸酯泡沫。
背景技术
USP4,795,763、5,192,607和5,373,026中公开了利用炭黑以降低闭孔硬质聚合物泡沫的老化k系数并由此改善绝缘值,所述文献在此以其全文通过引用并入。这些专利确定了均匀分散的炭黑填充剂引起泡沫的老化k系数显著的持久降低。不能恰当地分散炭黑和稳定所述分散体可导致泡沫生产设备的阻塞,并产生其中炭黑群集在泡沫孔的棱(strut)处或高度聚集在一部分孔壁中,得到很少改善或没有改善的绝缘值的泡沫。因此高度希望找到简单并且经济地将炭黑分散在用于泡沫生产的成分中并稳定所述分散体的方法,然后从所述分散的混合物形成高度绝缘的泡沫。
发明内容
本发明因此提供了这种具有改善的绝热性质的硬质异氰酸酯基聚合物泡沫,其由包含如下物质的混合物的反应性制剂制成:(A)A方,其包含:(i)有机异氰酸酯;(B)B方,其包含:(ii)异氰酸酯反应性组分,(iii)发泡剂,和(iv)一种或多种其他组分,选自催化剂、成核剂、表面活性剂、交联剂、扩链剂、阻燃剂、填充剂、着色剂、颜料、抗静电剂、补强纤维、抗氧化剂、防腐剂、红外线阻隔剂、或除酸剂,和(C)3至7份炭黑,其包含50至100重量%的(v)氟与碳(F/C)摩尔比为至少10/90的氟化炭黑,其中重量份是基于B方组分(B)的重量,并且组分(C)可以全部在A方(A)中、全部在B方(B)中、或部分在A方和部分在B方中。
本发明的一种实施方式是上文描述的硬质异氰酸酯基聚合物泡沫,其中所述有机异氰酸酯是2,4-甲苯二异氰酸酯(TDI)、2,6-甲苯二异氰酸酯、或其混合物;2,4′-二苯甲烷二异氰酸酯(MDI)、2,2′-二苯甲烷二异氰酸酯、4,4′-二苯甲烷二异氰酸酯、或其混合物;二苯甲烷二异氰酸酯及其异氰酸酯官能度大于2并且本领域称为“粗”或聚合MDI的低聚物的混合物;或包含氨基甲酸酯、脲基甲酸酯、脲、双缩脲、碳二亚胺、脲酮亚胺和/或异氰脲酸酯基团的MDI。
本发明的另一种实施方式是上文描述的硬质异氰酸酯基聚合物泡沫,其中所述异氰酸酯反应性组分是官能度从2至8并且羟值从100至850的多元醇。
本发明的另一种实施方式是上文描述的硬质异氰酸酯基聚合物泡沫,其中所述发泡剂是物理发泡剂、化学发泡剂、或其混合物。
本发明的优选实施方式是上文描述的硬质异氰酸酯基聚合物泡沫,其中所述炭黑组分(C)是100%氟化的炭黑(v)。
本发明的优选实施方式是上文描述的硬质异氰酸酯基聚合物泡沫,其中所述氟化炭黑具有5nm至500nm的平均粒度。
本发明的优选实施方式是上文描述的硬质异氰酸酯基聚合物泡沫,其中所述泡沫具有根据ISO12939-01测定的k-系数,使得所述泡沫的k-系数比相应泡沫的k-系数低至少0.2mW/mK,所述相应泡沫从除了省略氟化炭黑之外的相同的泡沫形成组合物制备。
本发明的另一种实施方式是通过以下步骤制造绝热性质改善的硬质异氰酸酯基聚合物泡沫的方法:
(I)形成:
(A)A方,其包含
(i)有机异氰酸酯,
(B)B方,其包含:
(ii)异氰酸酯反应性组分,
(iii)发泡剂
和
(iv)一种或多种其他组分,选自催化剂、成核剂、表面活性剂、交联剂、扩链剂、阻燃剂、填充剂、着色剂、颜料、抗静电剂、补强纤维、抗氧化剂、防腐剂、红外线阻隔剂、或除酸剂,
和
(C)3至7份炭黑,其包含:
(v)50至100重量%的氟与碳(F/C)摩尔比为至少10/90的氟化炭黑,其中重量份是基于B方组分(B)的重量,并且组分(C)可以全部在A方(A)中、全部在B方(B)中、或部分在A方和部分在B方中。
(II)将A方(A)和B方(B)混合在一起以形成反应性制剂,其中所述A方和所述B方之一或二者包含组分(C);
和
(III)将所得到的反应性制剂经受足以固化所述反应性制剂的条件,以形成绝热性质改善的硬质异氰酸酯基聚合物泡沫。
发明详述
根据本发明的硬质异氰酸酯基聚合物泡沫从反应性制剂制备,所述制剂包含A方(A)和B方(B)、以及氟化炭黑(C),所述A方包含一种或多种有机异氰酸酯(i),所述B方包含一种或多种异氰酸酯反应性组分(ii)、发泡剂(iii)和任选的一种或多种添加剂(iv)。
用于本发明的组合物和方法中的合适的有机异氰酸酯(i)包括本领域已知用于制备聚氨酯泡沫的任何有机异氰酸酯,如脂族、环脂族、芳脂族和优选的芳族异氰酸酯,例如甲苯二异氰酸酯以其2,4和2,6-异构体及其混合物的形式和二苯甲烷二异氰酸酯以其2,4′-、2,2′-和4,4′-异构体及其混合物的形式、二苯甲烷二异氰酸酯(MDI)与其异氰酸酯官能度大于2并且本领域称为“粗”或聚合MDI的低聚物(多亚甲基多亚苯基多异氰酸酯)的混合物、包含氨基甲酸酯、脲基甲酸酯、脲、双缩脲、碳二亚胺、脲酮亚胺和/或异氰脲酸酯基团的已知MDI变体。
优选地,单体MDI、粗MDI、聚合MDI、其组合和/或其液态变体是通过将脲酮亚胺和/或碳二亚胺基团引入到所述多异氰酸酯中而得到的,这样的碳二亚胺和/或脲酮亚胺改性多异氰酸酯的NCO值为29至33%,并包括1至45重量%的以单体和/或其碳二亚胺化产物的形式的2,4′-二苯甲烷二异氰酸酯。对这种碳二亚胺和/或脲酮亚胺改性多异氰酸酯的充分描述参见USP6,765,034,所述文献在此以其全部内容通过引用并入。
在本发明中,有机异氰酸酯组分除单体MDI之外和/或代替单体MDI,可以根据需要包括一种或多种有机多异氰酸酯,只要其他多异氰酸酯化合物对所述硬质异氰酸酯基聚合物泡沫的期望的消音、振动控制和阻燃性性能没有不良影响即可。这种其他多异氰酸酯化合物的典型实例包括上述单体MDI的至少一种化合物与合适的活性氢化合物之间反应而形成的端异氰酸酯预聚物。为了改善得到的泡沫的成形性和其他特性,所述其他多异氰酸酯化合物可以选自有机异氰酸酯例如甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)和二甲苯二异氰酸酯(XDI)、及其改性物。这些异氰酸酯可以以两种或更多种类型的组合来使用。最优选使用的多异氰酸酯具有2.1至3.0并优选2.2至2.8的平均异氰酸酯官能度。
用来制造弹性软质泡沫的多异氰酸酯的量通常足以提供0.6至1.5、优选0.6至1.2的异氰酸酯指数,但是特定情况可使用更宽的范围。优选的范围是0.7至1.05,更优选的范围是0.75至1.05。
本发明的B方包含异氰酸酯反应性组分(ii),所述异氰酸酯反应性组分(ii)包括本技术领域已知用于该目的的那些中的任何类型的化合物,例如多胺、氨基醇和多元醇。
合适的(聚醚)多元醇已经在现有技术中充分描述,并包括烯化氧例如氧化乙烯和/或氧化丙烯与官能度为2至8、优选3至8和平均羟值优选为约100至850、更优选约200至750并更优选200至650的引发剂的反应产物。根据ASTM D455测量,所述一种或多种多元醇在25℃可以具有至少约500cP的粘度。在一些实施方式中,可以优选至少约2,000cP的更高粘度。优选地,所述一种或多种多元醇具有100至10,000、更优选200至5,000的平均分子量。
本发明的合适的引发剂包括:多元醇,例如乙二醇、二乙二醇、丙二醇、二丙二醇、丁二醇、甘油、三羟甲基丙烷、三乙醇胺、季戊四醇、山梨糖醇和蔗糖;多胺,例如乙二胺、甲苯二胺(tolylene diamine)、二氨基二苯甲烷和多亚甲基多亚苯基多胺;和氨基醇,例如乙醇胺和二乙醇胺;和这些引发剂的混合物。其他合适的多元醇包括通过二醇和更高官能度的多元醇与多羧酸以适当比例缩合而得到的聚酯。仍然还合适的多元醇包括端羟基聚硫醚、聚酰胺、聚酯酰胺、聚碳酸酯、聚缩醛、聚烯烃和聚硅氧烷。仍然还合适的异氰酸酯反应性组分包括乙二醇、二乙二醇、丙二醇、二丙二醇、丁二醇、甘油、三羟甲基丙烷、乙二胺、乙醇胺、二乙醇胺、三乙醇胺和之前提到的其他引发剂。也可以使用这些异氰酸酯反应性组分的混合物。最优选使用的多元醇不包含伯、仲或叔氮原子。
对于制备本发明的硬质异氰酸酯基聚合物泡沫特别重要的是(聚醚)多元醇和多元醇混合物的羟值等于或大于50、优选等于或大于80、更优选等于或大于100。羟值指示反应可利用的反应性羟基数量。它表示为与一克多元醇的羟基含量相当的氢氧化钾的毫克数。对于制备本发明的硬质异氰酸酯基聚合物泡沫特别重要的是多元醇和多元醇混合物的羟值等于或小于1,200、优选等于或小于1,000、更优选等于或小于800。
对于制备硬质泡沫特别重要的是烯化氧例如氧化乙烯和/或氧化丙烯与每分子含有2至8个活性氢原子的引发剂的反应产物。合适的引发剂包括:多元醇,例如乙二醇、二乙二醇、丙二醇、二丙二醇、丁二醇、甘油、三羟甲基丙烷、三乙醇胺、季戊四醇和山梨糖醇;多胺,例如乙二胺、甲苯二胺、二氨基二苯甲烷和多亚甲基多亚苯基多胺;和氨基醇,例如乙醇胺和二乙醇胺;和这些引发剂的混合物。其他合适的多元醇包括通过二醇和更高官能度的多元醇与多羧酸以适当比例缩合而得到的聚酯。仍然还合适的多元醇包括端羟基聚硫醚、聚酰胺、聚酯酰胺、聚碳酸酯、聚缩醛、聚烯烃和聚硅氧烷。优选的多元醇是包含氧化乙烯和/或氧化丙烯单元的聚醚多元醇,最优选氧化乙烯含量为至少10重量%并优选10至85重量%的聚氧化乙烯聚氧化丙烯多元醇。优选的异氰酸酯反应性组分包括氧化乙烯封端的聚醚多元醇。
其他可以使用的多元醇包括加成或缩合聚合物在上述类型的多元醇中的分散体或溶液。这样的改性多元醇,经常被称为“共聚物”多元醇,已经在现有技术中充分描述,并包括通过一种或多种乙烯基单体例如苯乙烯和丙烯腈在聚合多元醇例如聚醚多元醇中原位聚合、或通过多异氰酸酯与氨基或羟基官能化合物例如三乙醇胺之间在聚合多元醇中的原位反应而得到的产物。
根据本发明特别有利的聚合物改性多元醇是通过苯乙烯和/或丙烯腈在聚氧化乙烯聚氧化丙烯多元醇中的原位聚合而得到的产物、以及通过多异氰酸酯与氨基或羟基官能化合物(例如三乙醇胺)在聚氧化乙烯聚氧化丙烯多元醇中原位反应而得到的产物。
含有5至50%分散聚合物的聚氧化烯多元醇是特别有用的。优选所述分散聚合物的粒度小于50微米。也可以使用这些异氰酸酯反应性组分的混合物。最优选使用的多元醇不包含伯、仲或叔氮原子。
所述B方还包含发泡剂(iii)。为了制备本发明的硬质异氰酸酯基聚合物泡沫,发泡剂是必需的。合适的发泡剂可以是有机发泡剂、无机发泡剂、化学发泡剂、或其混合物。例如,可使用多种多样的发泡剂,包括水;各种烃;各种氢氟烃;各种氯氟烃;气体如空气、N2和CO2;在发泡反应条件下产生氮气或二氧化碳的各种化学发泡剂;等等。也可以使用这些方式的组合来制造泡沫。
合适的物理发泡剂包括二氧化碳、氮气、氩气、水、空气、氮气和氦气。物理发泡剂包括具有1-9个碳原子的脂族烃以及具有1-4个碳原子的完全和部分卤代的脂族烃。脂族烃包括甲烷、乙烷、丙烷、正丁烷、异丁烷、正戊烷、异戊烷、新戊烷、乙醇、二甲醚等等。完全和部分卤代的脂族烃包括氟烃、氯烃和氯氟烃。氟烃的例子包括氟甲烷、全氟甲烷、氟乙烷、1,1-二氟乙烷、1,1,1-三氟乙烷(HFC-143a)、1,1,1,2-四氟乙烷(HFC-134a)、五氟乙烷、二氟甲烷、全氟乙烷、2,2-二氟丙烷、1,1,1-三氟丙烷、全氟丙烷、二氯丙烷、二氟丙烷、全氟丁烷、全氟环丁烷。用于本发明的部分卤代氯烃和氯氟烃包括氯甲烷、二氯甲烷、氯乙烷、1,1,1-三氯乙烷、1,1-二氯-1-氟乙烷(HCFC-141b)、1-氯-1,1-二氟乙烷(HCFC-142b)、1,1-二氯-2,2,2-三氟乙烷(HCFC-123)和1-氯-1,2,2,2-四氟乙烷(HCFC-124)。完全卤代的氯氟烃包括三氯一氟甲烷(CFC-11)、二氯二氟甲烷(CFC-12)、三氯三氟乙烷(CFC-113)、1,1,1-三氟乙烷、五氟乙烷、二氯四氟乙烷(CFC-114)、氯七氟丙烷和二氯六氟丙烷。化学发泡剂包括偶氮二甲酰胺、偶氮二异丁腈、苯磺酰肼、4,4-氧苯磺酰氨基脲、对甲苯磺酰氨基脲、偶氮二羧酸钡、N,N′-二甲基-N,N′-二亚硝基对苯二甲酰胺和三肼基三嗪。
发泡剂的量可以大幅变化,并主要取决于所用的发泡剂和所述硬质异氰酸酯基聚合物泡沫的期望密度。
如果水用作发泡剂,其使用范围基于B方的重量通常为0.1至5重量份。
如果烃、氢氟烃或氯氟烃用作发泡剂,其使用范围基于B方的重量通常为5至30重量份。
如果气体例如空气、CO2或N2用作发泡剂,其使用范围基于B方的重量通常为5至30重量份。
在本发明的一种实施方式中,特别合乎需要的发泡剂是水和氢氟烃的组合。
B方可以包含一种或多种其他组分(iv)。作为其他组分(iv),一种或多种催化剂可以存在于本发明的反应性制剂的B方中。一种优选的催化剂类型是叔胺催化剂。叔胺催化剂可以是对于多元醇和有机多异氰酸酯之间的反应具有催化活性和具有至少一个叔胺基的任何化合物。代表性的叔胺催化剂包括三甲胺、三乙胺、二甲基乙醇胺、N-甲基吗啉、N-乙基吗啉、N,N-二甲基苄胺、N,N-二甲基乙醇胺、N,N,N′,N′-四甲基-1,4-丁二胺、N,N-二甲基哌嗪、1,4-二氮杂双环-2,2,2-辛烷、双(二甲基氨基乙基)醚、双(2-二甲基氨基乙基)醚、4,4′-(氧二-2,1-乙二基)双吗啉、三乙二胺、五甲基二亚乙基三胺、二甲基环己胺、N-乙酰基N,N-二甲胺、N-椰油基吗啉、N,N-二甲基氨基甲基N-甲基乙醇胺、N,N,N’-三甲基-N’-羟乙基双(氨基乙基)醚、N,N-双(3-二甲基氨基丙基)N-异丙醇胺、(N,N-二甲基)氨基-乙氧基乙醇、N,N,N’,N’-四甲基己烷二胺、1,8-二氮杂双环-5,4,0-十一烯-7、N,N-二吗啉代二乙醚、N-甲基咪唑、二甲基氨基丙基二丙醇胺、双(二甲基氨基丙基)氨基-2-丙醇、四甲基氨基双(丙胺)、(二甲基(氨基乙氧基乙基))((二甲胺)乙基)醚、三(二甲基氨基丙基)胺、二环己基甲胺、双(N,N-二甲基-3-氨基丙基)胺、1,2-乙烯哌啶和甲基-羟乙基哌嗪。
反应性制剂的B方除之前提到的叔胺催化剂之外可以包含一种或多种其他催化剂,或可以包含一种或多种其他催化剂以代替之前提到的叔胺催化剂。其中特别有利的是羧酸锡和四价锡化合物。这些的实例包括辛酸亚锡、二乙酸二丁基锡、二月桂酸二丁基锡、二硫醇二丁基锡、二烷基巯基酸二烷基锡、二丁基氧化锡、二硫醇二甲基锡、二异辛基巯基乙酸二甲基锡等等。
催化剂通常以少量使用。例如,基于异氰酸酯反应性化合物(ii)的总重量,使用的催化剂总量可以是0.0015至5重量%、优选0.01至1重量%。有机金属催化剂通常以向着这些范围下限的量来使用。
B方还可以包含交联剂作为其他组分(iv)之一,交联剂如果确实使用的话,优选少量使用,基于异氰酸酯反应性化合物(ii)的总重量,最多2重量%、最多0.75重量%、或最多0.5重量%。所述交联剂每分子包含至少三个异氰酸酯反应性基团,并且每异氰酸酯反应性基团的当量为30至约125并优选30至75。氨基醇例如单乙醇胺、二乙醇胺和三乙醇胺是优选的类型,但也可以使用化合物例如甘油、三羟甲基丙烷和季戊四醇。
B方还可以包含表面活性剂作为其他组分(iv)。所述泡沫制剂中优选包括表面活性剂,以在泡沫膨胀和固化时帮助稳定所述泡沫。表面活性剂的例子包括非离子型表面活性剂和润湿剂,例如通过向丙二醇、固体或液体有机硅氧烷和长链醇的聚乙二醇醚相继添加氧化丙烯然后是氧化乙烯而制备的那些。离子型表面活性剂例如长链烷基酸硫酸酯、烷基磺酸酯和烷基芳基磺酸的叔胺或烷醇胺盐也可以使用。通过向丙二醇相继添加氧化丙烯然后是氧化乙烯而制备的表面活性剂是优选的,固体或液体有机硅氧烷也是优选的。有用的有机硅氧烷表面活性剂的例子包括可商购的聚硅氧烷/聚醚共聚物,例如可得自Goldschmidt ChemicalCorp.的TEGOSTABTM B-8729、和B-8719LF,以及出自MomentivePerformance Materials的NIAXTM L2171表面活性剂。更优选不可水解的液体有机硅氧烷。当使用表面活性剂时,基于所述有机异氰酸酯(i)的总重量,它的存在量通常为0.0015至1.5重量%。
扩链剂可以在本发明的反应性制剂的B方中作为其他组分(iv)使用。也可以存在扩链剂,它是实际具有两个异氰酸酯反应性基团并且每个异氰酸酯反应性基团的当量最多499、优选最多250的化合物。扩链剂,如果确实存在,通常少量使用,例如基于异氰酸酯反应性化合物(ii)的总重量,最多为10、优选最多5并更优选最多2重量%。合适的扩链剂的例子包括乙二醇、二乙二醇、三乙二醇、丙二醇、二丙二醇、三丙二醇、1,4-二羟甲基环己烷、1,4-丁二醇、1,6-己二醇、1,3-丙二醇、二乙基甲苯二胺、端胺基聚醚例如出自Huntsman Chemical Company的JEFFAMINETM D-400、氨乙基哌嗪、2-甲基哌嗪、1,5-二氨基-3-甲基-戊烷、异佛尔酮二胺、乙二胺、己二胺、肼、哌嗪、其混合物等等。
B方也可以包含填充剂作为其他组分(iv),填充剂降低产品的总成本、承重和其他物理性质。填充剂可以占所述聚氨酯反应性制剂总重量(即有机异氰酸酯(i)、异氰酸酯反应性化合物(ii)和阻燃组分(iii)的合并重量)的最多约50%。合适的填充剂包括滑石、云母、蒙脱土、大理石、硫酸钡(重晶石)、磨碎的玻璃花岗岩、磨碎的玻璃、碳酸钙、三水合铝、碳、芳纶、二氧化硅、二氧化硅-氧化铝、氧化锆、滑石、膨润土、三氧化锑、高岭土、炭基粉煤灰和氮化硼。
B方也可以包含成核剂作为其他组分(iv),可以添加成核剂以控制泡沫孔的尺寸。优选的成核剂包括无机物质例如碳酸钙、滑石、粘土、氧化钛、二氧化硅、硫酸钡、硅藻土、柠檬酸与碳酸氢钠的混合物,等等。每一百重量份聚合物树脂中成核剂的使用量量优选为约0.01至约5重量份。更优选的范围是0.1至约3重量份。
除了上文列出的其他组分之外,B方还可以包含选自如下的其它组分(iv):红外线阻隔剂(不同于组分(C)和除组分(C)之外)、阻燃剂例如磷酸酯型阻燃剂、油、抗氧化剂、脱模剂、哑光剂、紫外稳定剂、抗静电剂、抗微生物剂、助流剂、加工助剂、耐刮伤或擦伤剂、光滑剂、抗结块剂、颜料、触变剂、流动增强剂或其组合。每种添加剂可以以所述类型的添加剂在硬质异氰酸酯基聚合物泡沫中的通常量使用,所述量容易由本领域技术人员确定。
提供本发明硬质异氰酸酯基聚合物的反应性制剂还包含炭黑组分(C),其包含氟化碳,优选氟化炭黑组分(v)。所述氟化碳可以全部在A方中、全部在B方中、部分在每一方中,优选所述氟化碳是在B方中。氟化碳(v),有时称为石墨氟化物或碳氟化物,是用元素氟来氟化碳获得的固体物质。每个碳原子的氟原子数可以根据氟化条件而变化。氟化碳的可变的氟原子与碳原子的化学计量允许它的电阻率性质系统性地统一变化。
在本文中使用时,氟化碳是通过向许多形式的固体碳的一种或多种化学添加氟而制备的特定类别的组合物。另外,为了产生特定的期望电阻率,氟量可以变化。氟烃是脂族或芳族有机化合物,其中一个或多个氟原子连接到一个或多个碳原子,形成具有单一明确熔点或沸点的明确化合物。含氟聚合物是连接起来的单一相同分子,其包含通过共价键结合在一起的长链。此外,含氟弹性体是特定类型的含氟聚合物。因此,尽管本领域有一些明显的混淆,但很明显氟化碳既不是氟烃也不是含氟聚合物,并且所述术语在本文中以这种语境使用。
所述氟化碳材料可以是如本文中所述的任何氟化碳材料。制备氟化碳的方法是公知的并记录在文献中,例如在以下USP2,786,874、3,925,492、3,925,263、3,872,032和4,247,608中,它们的公开内容通过引用完全并入本文中。基本上,氟化碳是通过在升高的温度、通常150℃至600℃之间加热碳源例如无定形碳、焦、炭、炭黑或石墨与元素氟而产生的。稀释剂例如氮气可以优选与氟气(F2)混合。氟化碳的本质和特性随着具体的碳源、反应条件和在最终产物中得到的氟化度而变化。最终产物中的氟化度可以通过改变加工反应条件、主要是温度和时间而变化。通常,温度越高和时间越长,氟含量越高。
不同碳源和不同氟含量的氟化碳可从几种来源商购。优选的碳源是炭黑、结晶石墨和石油焦。适合用于本发明的一种形式的氟化碳是聚一氟化碳(polycarbon monofluoride),它通常以简写方式写成CFx,x通常最多约1.5、优选约0.01至约1.5、并且特别优选从约0.04至约1.4。CFx具有由稠合的六碳环的层构成的层状结构,其中氟原子连接到所述碳并位于所述碳原子平面的上方和下方。CFx型氟化碳的制备描述于例如上面提到的USP2,786,874和3,925,492中。通常,形成这种类型的氟化碳包括元素碳与F2催化反应。这种类型的氟化碳可以从许多经销商商购获得,包括Allied Signal,Morristown,N.J.;Central Glass International,Inc.,WhitePlains,N.Y.;Diakin Industries,Inc.,New York,N.Y.;Advanced ResearchChemicals,Inc.,Catoosa,Oklahoma;和Jiangsu Zhuoxi FluorinationTechnology Co.Ltd.,Taixing,China。
适合用于本发明的另一种形式的氟化碳是由Nobuatsu Watanabe假设的聚(一氟化二碳),通常以简写方式写成(C2F)n。(C2F)n型氟化碳的制备描述在例如上面提到USP4,247,608中,以及Watanabe等,"Preparationof Poly(dicarbon monofluoride)from Petroleum Coke",Bull.Chem.Soc.Japan,55,3197-3199(1982)中。
另外,所选的优选氟化碳包括Luly等的USP4,524,119中描述的那些,其主题在此以其全部内容通过引用并入,和具有式CFx并通过C+F2=CFx的反应形成的那些。
优选的氟化碳是氟化炭黑。最优选通过表面处理而氟化的炭黑。制备氟化炭黑的优选方式是在高压釜内在95%F2气环境中反应炭黑。例如,F2压力起初保持在3巴,并在500℃至600℃的温度下反应1至2小时。然后,释放压力并降低温度以产生氟化炭黑。不同于氟化学处理,F2气直接与炭黑表面中的双键反应,在表面上形成C-F键。所生成的C-F键比通过化学反应的含氟聚合物处理更稳定得多,其允许C-F键在混合过程中的强剪切下存续。
可用于本发明的氟化炭黑中氟与碳(F/C)的摩尔比等于或大于5/95,优选等于或大于10/90,更优选等于或大于12/88,更优选等于或大于20/80,更优选等于或大于30/70。可用于本发明的氟化炭黑中氟与碳(F/C)的摩尔比等于或小于100/0,优选等于或小于95/5,更优选等于或小于90/10,更优选等于或小于80/20,更优选等于或小于70/30,更优选等于或小于60/40,更优选等于或小于50/50,并更优选等于或小于40/60。
在本发明的一种实施方式中,氟化炭黑的氟与碳(F/C)摩尔比为至少10/90。
在本发明的一种实施方式中,优选的氟化炭黑的氟与碳(F/C)摩尔比为10/90到100/0。
在本发明的一种实施方式中,优选的氟化炭黑的氟与碳(F/C)摩尔比为12/88到60/40。
在本发明的一种实施方式中,优选的氟化炭黑的氟与碳(F/C)摩尔比为12/88到30/70。
在另一种实施方式中,优选的氟化炭黑具有从5纳米到500纳米的平均粒度。
除了氟化炭黑组分(C)之外,本发明的反应性制剂中还可以存在非氟化碳(例如无定形碳、焦碳、木炭、炭黑和/或石墨),使得氟化炭黑与非氟化碳的重量比等于或大于50:50,换句话说,本发明的反应性制剂中存在的氟化炭黑的量占所有存在的碳的50重量%或更多。
氟化碳的存在量等于或大于1份,优选量等于或大于1.5份,优选量等于或大于2份,优选量等于或大于2.5份,优选量等于或大于3份,优选量等于或大于4份,并更优选量等于或大于5份,其中份数是基于B方重量(不包括(即排除)氟化炭黑和/或炭黑的重量,如果B方中存在的话)。氟化碳的存在量等于或小于8份,优选量等于或小于7份,优选量等于或小于6份,其中份数是基于B方重量(不包括(即排除)氟化炭黑和/或炭黑的重量,如果B方中存在的话)。
已经发现,本发明的包含氧化乙烯封端的聚氧化丙烯的混合物的聚氨酯泡沫制剂加工良好,特别是在水和氢氟烃的混合物用作发泡剂的制剂中。良好的加工在此是指在工业环境下,泡沫制剂始终产生优质泡沫的能力。加工良好通过随时间产生泡沫时,始终均匀的孔结构、完整的充模、始终良好的表面外观、一致的泡沫密度和泡沫物理性质的一致性来表明。所述泡沫制剂耐受工作温度、催化剂水平和其他工艺条件的小改变,而这些工艺条件在其他高含水泡沫制剂中经常导致显著的产物不一致性。
本发明的硬质异氰酸酯基聚合物还有利地具有25至45kg/m3、优选30至40kg/m3范围内的密度。密度按照ASTM D3574方便地测量。
所述硬质异氰酸酯基聚合物泡沫可以取决于应用而是闭孔或开孔。对于大多数绝缘应用而言,本发明的泡沫根据ASTM D2856-A理想地是大于90%闭孔。闭孔结构显著降低了对流效应、绝缘气体扩散、和水蒸汽渗透。
本发明的硬质异氰酸酯基聚合物泡沫所具有的k-系数有利地比相应泡沫的k-系数低等于或小于0.5mW/mK、优选等于或小于0.2mW/mK、优选等于或小于0.1mW/mK,所述相应泡沫从除了省略所述氟化炭黑之外的相同泡沫形成组合物制备。
为了制造本发明的硬质异氰酸酯基聚合物泡沫,制备反应性制剂,所述反应性制剂包含:A方,其包含(i)一种或多种有机多异氰酸酯和任选全部或部分的包含氟化炭黑组分(v)的炭黑组分(C)(如果组分(C)不是全部或部分在A方中,那么它是全部或部分在B方中);和B方,其包含:(ii)一种或多种异氰酸酯反应性组分,(iii)发泡剂,(iv)一种或多种其他组分,其选自催化剂、开孔剂、表面活性剂、交联剂、扩链剂、阻燃剂、填充剂、着色剂、颜料、抗静电剂、补强纤维、抗氧化剂、防腐剂或除酸剂,和优选全部或部分的包含氟化炭黑组分(v)的炭黑组分(C)。所述“B方”是预混合物,其包含适量的多元醇、任选的氟化炭黑、发泡剂、催化剂、发泡助剂、和特别用于期望的多元醇组分/最终泡沫的其他助剂。优选地,B方在低于40℃的温度下混合在一起,更优选它在环境温度(在此定义为20℃至30℃)下混合在一起。B方然后与任选含有部分或全部的炭黑组分(C)(所述炭黑组份(C)包含所述氟化炭黑(v))的特定有机(多)异氰酸酯组分混合,所述炭黑组分以所需比率包含在“A方”中,形成反应性制剂,所述制剂在混合时,允许发泡反应发生。所述多元醇预混合物(B方)和所述有机多异氰酸酯组分(A方)通过任何已知的氨基甲酸酯发泡设备混合一起。所得到的反应性制剂经受足以固化所述反应性制剂的条件,以形成绝热特性改善的硬质异氰酸酯基聚合物泡沫。注意,所述氟化炭黑组分(v)在本发明的反应性组合物中是必需的,换句话说,组分(v)不是任选的组分,然而,它可以任选全部添加到A方中、或任选全部添加到B方中、或任选部分可以添加到A方和部分可以添加到B方中。
所述多元醇预混合物(B方)和所述有机多异氰酸酯组分(A方)通过任何已知的氨基甲酸酯发泡设备混合一起。所得到的反应性制剂经受足以固化所述反应性制剂的条件,以形成硬质聚氨酯泡沫。所述反应性制剂被引入合适的模具,以在模具内发生发泡/固化反应,从而形成想要的聚氨酯泡沫,或者让它发泡/固化以形成块状原料或当场发泡。
本发明的绝热性质改善的硬质异氰酸酯基聚合物泡沫可以通过直接施加于表面或外壳、或者通过施加包含本发明泡沫的绝缘板而适合用于绝缘所述表面或外壳。这样的应用包括任何绝缘表面或外壳,例如房子、屋顶、建筑物、冰箱、冷冻机、电器、管道、汽车等等。此外,本发明的硬质异氰酸酯基聚合物泡沫可以形成为多个离散发泡粒子以供常规的松散填充缓冲应用和包装应用,或者可以研磨成碎片用作发泡绝缘材料。
实施例
在实施例1至11和比较例A至C中,将所有B方组分称重放入塑料瓶中并以4000rpm混合20分钟,然后接受20kHz超声1-2h以消除多元醇混合物中混合期间产生的气泡。如果所述氟化炭黑和/或未处理炭黑添加到B方的话,它们与其余的组分一起称重放入所述塑料瓶中。如果在A方中添加氟化炭黑的话,它经30分钟添加到所述异氰酸酯中,然后以3000rpm混合30分钟。通过以3000rpm的转头转速混合6秒来混合所述A方和B方组分,将由此产生的反应性制剂加工成硬质聚氨酯泡沫。所述混合物然后倒入封闭的30cm×20cm×5cm模具中并使之发泡。所述模具在15分钟之后打开并除去。从所述泡沫切割尺寸为20cm×20cm×2.5cm的样品,让其平衡24小时并在23℃下测量热导率(下板36℃和上板10℃)。通过混合上述A方和B方并向20cm×20cm×20cm开放模具添加所述混合物来制造自由泡沫(Free foams),以测定自由泡沫,乳白时间、胶凝时间和消粘时间,以秒(s)记录。
实施例1至11和比较例A至C中使用的材料归纳在表1中。表2中列出了实施例1至11和比较例A至C的A方(A)、B方(B方)以及氟化碳和或碳(C)组分的量。除非另外指出,在表2中,量是重量份,氟化炭黑和/或炭黑以重量份计的量是基于B方的总重量。
乳白时间(CT),其是从液相开始发生泡沫上升时的时间;此时液体混合物由于气泡形成而变得更澄清;
胶凝时间(GT),是泡沫混合物发展出足够的内部强度而变得尺寸稳定的时间;它记录为在金属抹刀放入然后抽出泡沫时,所述泡沫形成粘住金属抹刀的串的时间;和
消粘时间(TFT),是当轻触泡沫时,泡沫表皮不再粘住带手套的手指的时间。
自由起发密度利用倒入放在木盒内的聚乙烯袋中的自由起发泡沫来测定。测定反应时间(CT,GT,TFT)。所述泡沫应该达到约25至30cm的高度。泡沫样品在24小时之后以规则形状进行切割,测量样品重量和体积以计算密度。
K-系数在泡沫生产之后24小时从模制品的芯(20×30×5cm)中切出20×20×2.5cm泡沫板的泡沫样品上测定,这些样品在切割之后立即用于测试。λ,例如热导率或k-系数,根据ISO12939-01利用EKO InstrumentTrading Co.,Ltd.的热流计仪器HC-074在23℃(平均板温)下测量。
密度根据ASTM D941-88测定。
粘度用来自TA instrument的AR2000ex旋转流变仪测量;使用40mm平行板。温度通过peltier板控制在25℃。剪切速率设置为10分钟内从0.1至100S-1,粘度记录成每个十进位10个数据点。
表1
F=官能度
OH no.=羟值
PO基=氧化丙烯聚醚多元醇
FCB=氟化炭黑
F/C=氟与碳摩尔比
CB=未处理(即氟化)的炭黑
Claims (10)
1.一种绝热性质改善的硬质异氰酸酯基聚合物泡沫,其从包含如下物质的混合物的反应性制剂制成:
(A)A方,其包含
(i)有机异氰酸酯,
(B)B方,其包含:
(ii)异氰酸酯反应性组分,
(iii)发泡剂
和
(iv)一种或多种其他组分,选自催化剂、成核剂、表面活性剂、交联剂、扩链剂、阻燃剂、填充剂、着色剂、抗静电剂、补强纤维、抗氧化剂、防腐剂、红外线阻隔剂、或除酸剂,
和
(C)3至7份炭黑,其包含:
(v)50至100重量%的氟与碳(F/C)摩尔比为至少10/90的氟化炭黑,其中所述份数是基于B方组分(B)的重量的重量份,并且组分(C)可以全部在A方(A)中、全部在B方(B)中、或部分在A方中和部分在B方中。
2.权利要求1的硬质异氰酸酯基聚合物泡沫,其中所述(iv)一种或多种其他组分选自催化剂、成核剂、表面活性剂、交联剂、扩链剂、阻燃剂、填充剂、颜料、抗静电剂、补强纤维、抗氧化剂、防腐剂、红外线阻隔剂、或除酸剂。
3.权利要求1的硬质异氰酸酯基聚合物泡沫,其中所述有机异氰酸酯是2,4-甲苯二异氰酸酯(TDI)、2,6-甲苯二异氰酸酯、或其混合物;2,4'-二苯甲烷二异氰酸酯(MDI)、2,2'-二苯甲烷二异氰酸酯、4,4'-二苯甲烷二异氰酸酯、或其混合物;二苯甲烷二异氰酸酯及其异氰酸酯官能度大于2并且本领域称为“粗”或聚合MDI的低聚物的混合物;或包含氨基甲酸酯、脲基甲酸酯、脲、双缩脲、碳二亚胺、脲酮亚胺和/或异氰脲酸酯基团的MDI。
4.权利要求1的硬质异氰酸酯基聚合物泡沫,其中所述异氰酸酯反应性组分是官能度从2至8和羟值从100至850的聚醚多元醇。
5.权利要求1的硬质异氰酸酯基聚合物泡沫,其中所述发泡剂是物理发泡剂、化学发泡剂、或其混合物。
6.权利要求1的硬质异氰酸酯基聚合物泡沫,其中所述炭黑组分(C)是100%氟化炭黑(v)。
7.权利要求1的硬质异氰酸酯基聚合物泡沫,其中所述氟化炭黑具有5nm至500nm的平均粒度。
8.权利要求1的硬质异氰酸酯基聚合物泡沫,其中所述泡沫具有根据ISO 12939-01测定的k-系数,使得所述泡沫的k-系数比相应泡沫的k-系数低至少0.2mW/mK,所述相应泡沫从除了省略氟化炭黑之外的相同泡沫形成组合物制备。
9.一种通过以下步骤制造绝热性质改善的硬质异氰酸酯基聚合物泡沫的方法:
(I)形成:
(A)A方,其包含
(i)有机异氰酸酯,
(B)B方,其包含:
(ii)异氰酸酯反应性组分,
(iii)发泡剂
和
(iv)一种或多种其他组分,选自催化剂、成核剂、表面活性剂、交联剂、扩链剂、阻燃剂、填充剂、着色剂、抗静电剂、补强纤维、抗氧化剂、防腐剂、红外线阻隔剂、或除酸剂,
和
(C)3至7份炭黑,其包含:
(v)50至100重量%的氟与碳(F/C)摩尔比为至少10/90的氟化炭黑,其中所述份数是基于B方组分(B)的重量的重量份,并且组分(C)可以全部在A方(A)中、全部在B方(B)中、或部分在A方和部分在B方中;
(II)将所述A方(A)和所述B方(B)混合在一起以形成反应性制剂,其中所述A方和所述B方之一或二者包含组分(C);
和
(III)将所得到的反应性制剂经受足以固化所述反应性制剂的条件,以形成绝热性质改善的硬质异氰酸酯基聚合物泡沫。
10.权利要求9的方法,其中所述(iv)一种或多种其他组分选自催化剂、成核剂、表面活性剂、交联剂、扩链剂、阻燃剂、填充剂、颜料、抗静电剂、补强纤维、抗氧化剂、防腐剂、红外线阻隔剂、或除酸剂。
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