CN101316886B - 由反应性缩聚树脂构成的纳米孔聚合物泡沫 - Google Patents

由反应性缩聚树脂构成的纳米孔聚合物泡沫 Download PDF

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CN101316886B
CN101316886B CN2006800444472A CN200680044447A CN101316886B CN 101316886 B CN101316886 B CN 101316886B CN 2006800444472 A CN2006800444472 A CN 2006800444472A CN 200680044447 A CN200680044447 A CN 200680044447A CN 101316886 B CN101316886 B CN 101316886B
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V·舍德勒
V·I·莱曼
C·杜弗莱森冯霍奈施
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Abstract

本发明涉及一种平均孔径为10nm～1000nm的纳米孔聚合物泡沫，该泡沫根据包括如下步骤的方法获得：a)制备反应性缩聚树脂在有机溶剂中的溶液，b)将所述溶液与用于反应性缩聚树脂的固化催化剂混合并固化所述反应性组分以形成凝胶，和c)除去所述有机溶剂。本发明还涉及所述泡沫用于绝热的用途。

Description

由反应性缩聚树脂构成的纳米孔聚合物泡沫
本发明涉及一种生产反应性缩聚树脂的纳米孔
Figure S2006800444472D00011
聚合物泡沫的方法。
理论上来说，孔径明显低于1μm且总孔隙率大于90％的纳米孔聚合物泡沫是非常优良的绝热体。
溶胶-凝胶技术被广泛用于生产这类纳米孔聚合物泡沫。WO00/24799描述了可以通过将有机多异氰酸酯与异氰酸酯三聚催化剂混合以形成中间聚合物凝胶，然后将该凝胶干燥而获得的保温体。在“非结晶性固体杂志(Journal of Non-Crystalline Solids)”350(2004)，第372～378页中，A.Rigacci等人描述了一种生产基于聚氨酯的气凝胶和干凝胶的方法。这些产品显示出比标准的聚氨酯泡沫显著降低的热导率。
US5128382公开了基于环氧树脂或甲基丙烯酸酯的微孔泡沫。它们可通过在溶剂/非溶剂中聚合并随后在次临界条件下干燥得到。
为了生产基于三聚氰胺树脂的水凝胶，通常在水介质中通过交联反应生产亲水的三聚氰胺。随后将这些水凝胶在次临界条件或超临界条件下干燥以形成气凝胶或干凝胶。干燥步骤通常在用有机溶剂对水进行一次或多次替换后进行。在用二氧化碳提取的情况下，有机溶剂起到设定适当极性的作用。在次临界干燥情况下，溶剂替换的作用是提供适当表面张力和适当润湿性。对于该目的来说，通常需要一次以上的溶剂替换。
WO05/049708涉及可通过微乳液固化获得的纳米孔聚合物泡沫。该微乳液含有含反应性树脂的水相、合适的两亲性试剂和油相，在该微乳液中所述反应性组分进行缩聚。在随后的干燥过程中，例如通过冷冻干燥的方法从由此获得的凝胶体中除去流体组分。
在上面提及的生产纳米孔聚合物泡沫的方法中，干燥步骤要么在复杂的超临界条件下进行，要么存在聚合物泡沫由于出现高毛细力而皱缩。
本发明的目的是为了克服上述缺点，并提供一种生产纳米孔聚合物泡沫的方法，其中可以在次临界条件下干燥凝胶体，且凝胶体仅发生低程度的皱缩。
因此，发现了一种生产纳米孔聚合物泡沫的方法，所述方法包括以下步骤a)～c)：
a)提供反应性缩聚树脂在有机溶剂中的溶液，
b)将所述溶液与用于反应性缩聚树脂的固化催化剂混合并固化所述反应性组分以形成凝胶，和
c)除去所述有机溶剂。
术语“反应性缩聚树脂”应理解为：可通过缩聚反应获得并且可通过在室温下加入固化剂或在升高的温度下无固化剂的条件下发生反应的那些树脂。这些树脂的例子为氨基树脂如脲甲醛树脂、苯胍胺甲醛树脂、三聚氰胺甲醛树脂以及它们的混合物。根据本发明，所用的反应性缩聚树脂可溶于有机溶剂。优选使用与少于10％重量、优选少于5％重量、更优选少于0.01％重量的水可互混(Mischbar)的疏水性树脂。
醚化的反应性缩聚树脂是特别优选的，这类树脂在步骤b)中固化而消去醇。由于醇的消去，溶解性能在凝胶形成期间受到影响。正丁醇醚化的高度烷基化三聚氰胺甲醛树脂是特别优选的，该树脂不能由水和甲醇稀释。
在优选的三聚氰胺甲醛树脂中，三聚氰胺与甲醛的比率为1∶1～1∶10，优选1∶2～1∶6。
用于反应性缩聚树脂的合适有机溶剂为非极性化合物，如烃、醇、酮、醚和烷基酯。优选在标准压力下沸点低于120℃的溶剂，以便在蒸发期间容易从聚合物凝胶中将其除去。合适的有机溶剂的例子为含有1～6个碳原子的直链或支链烃，特别是戊烷、己烷和庚烷。特别优选的溶剂为四氢呋喃、丙酮、甲乙酮、乙酸乙酯和氯仿。
步骤a)的所述溶液中的反应性缩聚树脂的浓度通常为5％重量～25％重量，优选8％重量～15％重量。
固化催化剂的种类和数量取决于使用的缩聚树脂。对于氨基树脂，例如可以使用有机或无机酸，如磷酸、盐酸、对甲苯磺酸和羧酸，如醋酸或甲酸。
通常步骤b)中的固化在反应性缩聚树脂与固化催化剂的重量比率基于固体为1∶1～20∶1、优选在4∶1～10∶1的条件下发生。此外，与盐组合对于控制反应动力学也是有帮助的。水分含量应低于10％重量，优选低于5％重量，更优选低于0.01％重量。
此外，可以使用交联组分(固化剂)，例如在三聚氰胺甲醛树脂情况下，可以使用尿素或2，4-二氨基-6-壬基-1，3，5-三嗪。
固化通常在30～100℃、优选50～70℃的温度下进行。凝胶化在约0.5小时～10小时、优选1小时～4小时的时间范围内进行。微观结构通过聚合物网络的相分离而形成。
有机溶剂然后在步骤c)中除去。该步骤优选在次临界条件下、更优选在室温和标准压力下实施。
干燥后可获得的纳米孔聚合物泡沫的特征在于高总孔隙率以及由此带来的较低密度和较小孔径。平均孔径优选为10nm～1000nm，优选30nm～300nm。
本发明的纳米孔聚合物泡沫的热导率低，通常低于33mW/mK，因此特别适合于绝热应用，如在建筑业以及在制冷组件、车辆和工业厂房中的绝热板。
实施例
在各实施例中使用正丁醇醚化的高度烷基化三聚氰胺甲醛树脂(Luwipal 44，由BASF AG提供)作为反应性缩聚树脂。
孔隙率根据DIN 66133通过压汞法进行测定。比表面积根据BET(DIN66131)进行测定。
实施例1
将在四氢呋喃中的10％重量Luwipal 44溶液与37％重量盐酸以基于固体为5∶1的重量比混合，并在烘箱中于60℃下凝胶化3小时。将所得有机凝胶于室温下在空气中干燥。对所得干凝胶的水银孔隙率结果表明：总孔隙率为80％，其中大部分孔的孔径小于1000nm。比表面积为170m2/g。
实施例2
将在丙酮中的10％重量Luwipal 44溶液与37％重量盐酸以基于固体为5∶1的重量比混合。在烘箱中于60℃下进行凝胶化3小时。将所得有机凝胶在空气中干燥。水银孔隙率结果表明：总孔隙率为86％，大部分孔的孔径小于1000nm。比表面积为25m2/g。
实施例3
将在四氢呋喃中的10％重量Luwipal 44溶液与对甲苯磺酸以基于固体为5∶1的重量比混合，并以每30毫升该混合物1g软化水的比例与软化水混合。在烘箱中于60℃下进行凝胶化3小时。将所得有机凝胶在空气中干燥。对该纳米孔聚合物泡沫的水银孔隙率结果表明：总孔隙率为75％，大部分孔的孔径小于1000nm。比表面积为82m2/g。

Claims (13)

1.一种生产纳米孔聚合物泡沫的方法，包括以下步骤：
a)提供反应性缩聚树脂在有机溶剂中的溶液，该“反应性缩聚树脂”为可通过缩聚反应获得并且可通过在室温下加入固化剂或在升高的温度下无固化剂的条件下发生反应的那些树脂，
b)将所述溶液与用于反应性缩聚树脂的固化催化剂混合并固化所述反应性缩聚树脂而消去醇，以形成凝胶，和
c)除去所述有机溶剂，
其中所述反应性缩聚树脂是醚化的反应性缩聚树脂，它们在步骤b)中固化而消去醇。
2.根据权利要求1的方法，其中使用的反应性缩聚树脂为氨基树脂。
3.根据权利要求1的方法，其中使用的反应性缩聚树脂为脲甲醛树脂或三聚氰胺甲醛树脂。
4.根据权利要求1的方法，其中使用的所述反应性缩聚树脂为与少于10％重量的水可互混的疏水性树脂。
5.根据权利要求2的方法，其中使用的所述反应性缩聚树脂为与少于10％重量的水可互混的疏水性树脂。
6.根据权利要求3的方法，其中使用的所述反应性缩聚树脂为与少于10％重量的水可互混的疏水性树脂。
7.根据权利要求1～6任一项的方法，其中使用的溶剂为在标准压力下沸点低于120℃的烃、醇、酮、醚、烷基酯或它们的混合物。
8.根据权利要求1～6任一项的方法，其中步骤b)中的所述溶液的水含量低于10％重量。
9.根据权利要求7的方法，其中步骤b)中的所述溶液的水含量低于10％重量。
10.根据权利要求1～6任一项的方法，其中使用的固化催化剂为有机酸或无机酸。
11.根据权利要求7的方法，其中使用的固化催化剂为有机酸或无机酸。
12.根据权利要求8的方法，其中使用的固化催化剂为有机酸或无机酸。
13.根据权利要求9的方法，其中使用的固化催化剂为有机酸或无机酸。
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US20090005468A1 (en) 2009-01-01
WO2007065847A1 (de) 2007-06-14
PL1960459T3 (pl) 2011-07-29
DE502006008858D1 (de) 2011-03-17
EP1960459B1 (de) 2011-02-02
BRPI0619589A2 (pt) 2012-12-11
JP5124473B2 (ja) 2013-01-23
ATE497516T1 (de) 2011-02-15
KR101369681B1 (ko) 2014-03-04
DE102005059303A1 (de) 2007-06-21
CN101316886A (zh) 2008-12-03
EP1960459A1 (de) 2008-08-27
KR20080081026A (ko) 2008-09-05

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