CN1171093A - 含气凝胶的组合材料及其制备方法和用途 - Google Patents
含气凝胶的组合材料及其制备方法和用途 Download PDFInfo
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Abstract
本发明涉及包含10—95%(体积)气凝胶和至少一种无机粘合剂的组合材料及其制备方法和用途。
Description
本发明涉及包含10-95%(体积)的气凝胶微粒及至少一种无机粘合剂的组合材料,以及制备这种材料的方法及其用途。
因为固体材料能高效地传导热量,因而大多数无孔的无机固体具有较高的热导率。为了降低热导率,因此常常采用多孔材料,如以蛭石为主要成分的材料。对多孔材料来说,仍有能有效地传导热量的固体骨架,而只是孔中的空气较固体本身导热能力差一些。
然而,固体中小孔通常会使固体的机械稳定性下降,因为应力只能通过固体骨架传递。因此,有孔的、仍具有机械稳定性的材料同样仍具有较高的热导率。
然而,对于许多用途来说,需要有低的热导率,同时又要具有好的机械性能,如高抗压强度和高抗弯强度。这是因为:首先,成型的制品需要机加工;第二,根据用途,制品必须能经得起机械载荷,即使在高温下也不会发生断裂或龟裂。
因为气凝胶具有很低的密度、很高的孔隙度、孔径小,特别是孔隙度高于60%、密度低于0.6克/厘米3的气凝胶具有极低的热导率,因而可用作绝热材料,如EP-A-0171722中所述。直径小于空气分子平均自由路径的小孔,对于热导率来说是特别重要的,因为这种小孔中空气的导热性较大孔中空气的导热性低。因此,气凝胶的热导率较其它具有类似孔隙度、但孔径较大(如泡沫或蛭石基材料)的材料的热导率低得多。
然而,由干燥气凝胶制的凝胶和干燥气凝胶本身都是高孔隙度的,而高孔隙度又会降低机械稳定性。
在广泛意义上说,气凝胶是指“以空气为分散介质的凝胶”,是由合适的凝胶经干燥而制得的。术语“气凝胶包括狭义的气凝胶、干凝胶和Cryogel。假如在温度高于临界温度、起始压力高于临界压力下除去凝胶液体的话,干燥的凝胶称为狭义上的气凝胶。如果,与此不同,以亚临界方法例如,形成液体一蒸气界面相来除去凝胶液体。所得的凝胶常常称为干凝胶。应该指出,根据本发明的凝胶是指以空气为分散介质的气凝胶。
然而,对于许多用途来说,需要使用能成形为具有适当机械稳定性的制品的气凝胶。
EP-A-0340707公开了密度为0.1-0.4克/厘米3、含至少50%(体积)直径在0.5-5毫米之间的二氧化硅气凝胶微粒,并由至少一种有机和/或无机粘合剂粘合在一起的绝缘材料。由粒度较粗的绝缘材料制得的成形制品中,气凝胶材料分布不均匀。这种现象尤其存在于成形制品中尺寸最小部分(对薄膜或片材来说是厚度)不比气凝胶微粒直径大很多的情况中。特别在周边上,需要提高粘合剂的用量比例,这就会对成形制品的热导率产生不良的影响,尤其是在表面上。
此外,在由这种绝缘材料制的成形制品中,含直径在0.5-5毫米之间的气凝胶材料的低机械稳定性的区域会出现在表面上,并在机械载荷下,最终会使表面因直径不同而变成不均匀或者在表面气凝胶遭到破坏可深达5毫米。
此外,制造这种只包括少量液体的绝缘材料是不容易的,如EP-A0340707中指出,由于气凝胶微粒机械强度低,因而在混合期间经剪切作用时易被破坏。
因此,本发明的目的是提供具有低热导率和高机械强度以气凝胶为主要成分的复合材料。
本发明目的是通过包含10-95%(体积)的气凝胶微粒和至少一种无机粘合剂的复合材料来实现的,其中气凝胶微粒的直径小于0.5毫米。
无机粘合剂将气凝胶微粒粘合在一起形成基体并使连续相延伸到整个组合材料。
当组合材料中气凝胶微粒含量明显低于10%(体积)时,组合物会因其气凝胶微粒的比例太低而在很大程度上丧失了有利性质。这种类型的复合物不再具有低密度和低热导率。
气凝胶微粒含量明显高于95%(体积),就会使粘合剂含量低于5%(体积),粘合剂含量太低就不能保证气凝胶微粒相互间有充分的粘合和足够的机械抗压强度和挠曲强度。
气凝胶微粒的比例优选为20-90%(体积)之间。
根据本发明,气凝胶微粒的微粒直径小于0.5毫米,优选小于0.2毫米。微粒直径指的是单个气凝胶微粒的平均直径,因为制备气凝胶微粒的方法,如研磨法,意味着制成的微粒并不一定呈球形。
采用能在组合材料中均匀分布的小气凝胶微粒,因此,组合材料具有几乎完全均一的、在所有各点,特别在表面上各点都具有低的热导率。
而且,在气凝胶比例相同的情况下,小气凝胶微粒还能提高耐破裂和龟裂的机械稳定性,因为它们能降低载荷下局部应力集中。
气凝胶可以是亲水的或憎水的,这取决于材料和孔表面的表面基团类型。
如果亲水气凝胶与极性物质,具体说与水蒸气或液态水相接触,它的孔结构可能被削弱,削弱程度决定于作用的时间和材料的物理状态;在不利的情况下,亲水气凝胶甚至发生塌陷。
孔结构的这种改变,尤其是塌陷可能会导致绝热效率急剧下降。
考虑到组合材料中可能存在水分(如水)例如在温度变化时空气中湿气的冷凝和制造过程中一般是免不了有水的,因此憎水气凝胶是优选的。
为了避免由复合材料制的成形制品在预期的长使用期限内受到水分和/或周围大气的影响,而使复合材料的绝热效率变坏,因此能长期保持憎水,即使在稍有酸性的环境中仍保持憎水的气凝胶是特别优选的。
当采用具有憎水表面基团的气凝胶时,由很小粒径的气凝胶能制成憎水性陶瓷材料,因为憎水气凝胶在其中是呈均匀和精细分布的。
通过采用粒径的双峰分布可以使组合材料中气凝胶微粒达到特别高的比例。
优选的无机粘合剂是水泥、石灰或石膏以及它们的混合物。其它无机粘合剂,如以硅溶胶为主要成分的那些粘合剂也是可采用的。
无机粘合剂是制造气凝胶成形制品优良的基础。以水凝固能产生具有高强度的细密结构。无机粘合剂与气凝胶相结合能制得适合应用部门(如建筑部门)性能需要的成形材料。
此外,该组合材料还可包含至少一种作为无机基体材料的未焙烧的和/或焙烧的页硅酸盐;这种页硅酸盐可以是天然的页硅酸盐如高岭土、白土或膨润土,或合成的页硅酸盐,如magadiite或kenyaite或它们的混合物。
含尽可能低的碱金属、同时具有高成型性的页硅酸盐是优选的。而白土或合成的无碱金属(无钠)的页硅酸盐,如magadiite是特别优选的。
组合材料中页硅酸盐的比例优选低于50%(重量,以无机粘合剂含量计)。无机粘合剂与页硅酸盐混合物优选适用于浇铸。页硅酸盐可用来调节这种水性混合物的流变性质。
适用于新颖组合材料的气凝胶是那些藉溶胶-凝胶技术(C.J.Brinker,G.W.Scherer,溶胶-凝胶科学Sol-gel science,1990,第2和第3章)制的以金属氧化物为主要成分的物质,例如硅或铝化合物,或是那些藉溶胶-凝胶技术制的以有机物质为主要成分的物质,例如三聚氰胺-甲醛缩合物(US-A-5086085)或间苯二酚-甲醛缩合物(US-A-4873218)。以上述物质的混合物为主要成分的气凝胶也是适用的。优选的气凝胶是硅化合物,具体说是SiO2气凝胶,更特别优选的是SiO2干凝胶。为了降低辐射引起的导热性,气凝胶可包含红外不透明材料,例如碳黑、二氧化钛、氧化铁或二氧化锆或它们的混合物。
在优选的实施方案中,气凝胶微粒具有憎水表面基团。具有持久憎水作用的基团是,例如式为-Si(R)3的三取代甲硅烷基团,优选的是三烷基甲硅烷基团和/或三芳基甲硅烷基团,其中每一R各自独立地为无反应活性的有机基团,如C1-C18烷基或C6-C14芳基,优选C1-C6烷基或苯基,具体地说为甲基、乙基、环己基或苯基,它们也是可被官能基团取代的。三甲基甲硅烷基团特别有利于使气凝胶具有持久憎水作用。可按WO94/25149所述方法或通过气凝胶与,例如活化的三烷基硅烷衍生物(如氯代三烷基硅烷或六烷基二硅氮烷,参看R.Iler,硅化学The Chemistry ofSilica,Wiley & Sons,1979)进行气相反应将这些基团引入气凝胶表面。
气凝胶的热导率会随孔隙度的增加和密度的降低而降低。为此,优选气凝胶的孔隙度高于60%,密度低于0.6克/厘米3。密度低于0.4克/厘米3的气凝胶是特别优选的。
为了减少辐射对导热性的影响,组合材料中可包含红外不透明材料,例如碳黑、二氧化钛、氧化铁或二氧化锆或它们的混合物;这特别有利于气凝胶在高温下的应用。
如果组合材料中含有纤维,对于提高抗裂强度和破坏强度也可能是有利的。这种纤维可以是有机纤维,如聚丙烯、聚酯、尼龙或三聚氰胺-甲醛纤维和/或无机纤维,如玻璃纤维、矿物或SiC纤维和/或碳纤维。
根据气凝胶、无机粘合剂及纤维材料(如果采用的话)可燃性等级来确定干燥后所得到的组合材料的可燃性等级。为使组合材料获得最好的可燃性等级(低可燃性或不会燃烧),纤维应是由不会燃烧的材料,例如矿物、玻璃或SiC纤维制造的。
为了避免由于添加纤维而引起导热性增加,
a)纤维用量的体积比应当为0.1-30%,优选1-10%,及
b)纤维材料的热导率优选小于1瓦/米·开尔文。
通过适当选择纤维的直径和/或纤维材料,能够降低辐射对热导率的影响并能提高机械强度。为此,纤维直径优选应当在0.1-30微米之间。
如果采用碳纤维或含碳纤维,则能格外显著地降低辐射对热导率的影响。
纤维的长度和在组合材料中的分布也会对机械强度产生影响。长度在0.5-10厘米之间的纤维是优选的。对薄片状制品也可采用由纤维构成的织物。
组合材料也可含其它辅助材料,如甲基纤维素、淀粉、聚乙烯醇和/或蜡乳液。在先有技术领域中,这些材料在工业上用于陶瓷体的成形。
如果组合材料用于形成片状结构,例如片材,可在至少一面上叠合至少一层覆盖层来提高其表面性能,例如提高耐磨性、使表面形成防潮层或保护表面以免被弄脏。覆盖层也能提高由组合材料制的制品的机械稳定性。如果两面都采用覆盖层,则这两覆盖层可以是相同的或不相同的。
本领域技术熟练人员熟知的所有材料都适用作覆盖层,其中无孔材料能作为有效的防潮层,例如塑料薄膜、金属箔或能反射热辐射的喷涂金属的塑料膜;能允许空气进入到组合材料中、从而能阻隔声音的多孔性覆盖层例如多孔薄膜、纸张、织物及纤维结构片状物,也是可采用的。基体材料本身也可用作覆盖层。
覆盖层本身可包括许多层,并可用粘合剂或基它粘结材料粘固。
也可通过引入至少一种适用材料的表面层使组合材料表面密封和固结。
本发明还有一个目的是提供制造新颖组合材料的方法。
该目的可通过包括下列步骤的方法来达到:
a)在混合设备中混合气凝胶微粒、无机粘合剂、水,根据需要还有纤维、页硅酸盐和/或辅助材料,
b)将所得混合物经成形工艺成形,
c)干燥已成形的物件,
d)根据需要,对已干燥的物体作初加工。
在步骤a)中,预先将固体成分装入混合设备中,然后再添加液体成分是优选的。
将含水量约50%的蜡乳液添加到干燥的原材料固体成分中是特别优选的,所需的其余水分可通过加入水玻璃来补充。还可向混合物追加水使其达到所必需的含水量。
可利用混合的水量来改变混合物的机械性能。混合物的特征流变性能可根据纤维、页硅酸盐和/或辅助材料的类型、用量及组合与气凝胶微粒和无机粘合剂性能相配合的情况来确定。
如果混合物含页硅酸盐,优选在能对混合物实施剪切力的混合机中混合。施加剪切力的目的在于尽可能完全地打开页硅酸盐使其成为单个片晶。
在接着的成形工艺步骤,例如挤出成形过程中,借助剪切力和垂直作用在混合物上的成形力能使页硅酸盐取向。这种取向作用能提高机械强度。对于用作绝热材料来说,取向有助于降低热导率。此外,为达到同等的物理性能只需较少量的页硅酸盐。
由于页硅酸盐的塑性性质,因此能够以挤出的方法与水混合。含水量应调整到保证混合物具有良好的成形性。根据气凝胶的吸水能力,必须提高含水量。
在一个优选的实施方案中,在混合机或有搅拌的罐中增加外加水使混合物均化。优选的粘度设在100-2000毫帕·秒之间。然后使混合物倾入预定模子之前进行脱气。
对由成形步骤得到的制品进行干燥,然后,根据需要可经初加工,即修整成所需的大小。
该新颖复合材料由于其低热导率,适宜作绝热用成形制品。根据不同用途,该制品可成形为片材、长条形或形状不规则的物件。
通过下面具体实施例对本发明作更详细的说明;所有实验中所用的以原硅酸四乙酯(TEOS)为主要成分的憎水气凝胶是按公开在WO94/25149中类似的方法由三甲基氯硅烷制备的,气凝胶的密度为0.17克/厘米3,热导率为30毫瓦/米·开尔文。
实施例1
将1000毫升气凝胶
200克α-半水合石膏
50克SAVC白土
40克FL6000×甲基纤维素
250毫升水
50毫升Baykiesol置于反应罐中,借助搅拌器混合至成为外观均匀的混合物,即用肉眼不能分辨各个成分时为止。
将混合物倾入模具中,放置3小时然后卸出制品。为了除去过量水分,将成形的制品在50℃下干燥。干燥后成形制品的密度为0.6克/厘米3,热导率为0.2瓦/米·开尔文
实施例2
将1000毫升气凝胶
250克微孔水泥
40克FL600×甲基纤维素
300毫升水
100毫升Baykiesol置于反应罐内借助搅拌器混合至成为外观均匀的混合物,即用肉眼不能分辨各个成分为止。
将混合物倾入模具中,放置3小时,然后卸出制品。为了除去过量水分,将成形的制品在50℃下干燥。干燥后的成形制品的密度为0.63克/厘米3,热导率为0.25瓦/米·开尔文。
实施例3
将1000毫升气凝胶
50克SAVC白土
40克甲基纤维素
300毫升Baykiesol置于反应罐中借助搅拌器混合至成为外观均匀的混合物,即用肉眼不能分辨各个成分为止。
将混合物倾八模具中,放置3小时,然后卸出制品。然后在600℃下烧结成形制品30分钟,烧结成形的制品的密度为0.45克/厘米3,热导率为0.15瓦/米·开尔文。
Claims (12)
1.包含10-95%(体积)气凝胶微粒和至少一种无机粘合剂的组合材料,其中气凝胶微粒直径小于0.5毫米。
2.权利要求1的组合材料,其中无机粘合剂是水泥、石灰和/或石膏。
3.权利要求1的组合材料,其中组合材料中还包含页硅酸盐。
4.权利要求1-3项中至少一项的组合材料,其中气凝胶是SiO2气凝胶。
5.权利要求1-4项中至少一项的组合材料,其中气凝胶微粒具有憎水表面基团。
6.权利要求1-5项中至少一项的组合材料,其中气凝胶微粒的孔隙率高于60%,密度低于0.6克/厘米3。
7.权利要求1-6项中至少一项的组合材料,其中组合材料包括0.1-30%(体积)纤维。
8.权利要求1-7项中至少一项的组合材料,其中组合材料包括辅助材料。
9.权利要求1-8项中至少一项的组合材料,其中组合材料具有片材形状,且在至少一个面上叠合有至少一层覆盖层。
10.制造权利要求1组合材料的方法,该方法包括:
a)在混合设备中混合气凝胶微粒,无机粘合剂、水及根据需要还有纤维、页硅酸盐和/或辅助材料,
b)将所得混合物经成形工艺成形,
c)干燥已成形的物件,
d)根据需要,对已干燥的物件作初加工。
11.根据权利要求10的方法,该方法包括进行下列成形步骤,
a)通过加水调整所得混合物的粘度至100-2000毫帕·秒之间,
b)根据需要,使得到的混合物脱气,及
c)将脱气后的混合物倾入预定的模具中。
12.权利要求1-9中至少一项的组合材料作为绝热材料的用途。
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-
1994
- 1994-11-23 DE DE19944441567 patent/DE4441567A1/de not_active Withdrawn
-
1995
- 1995-11-22 CN CN95197060A patent/CN1077089C/zh not_active Expired - Lifetime
- 1995-11-22 EP EP95941621A patent/EP0793627B1/de not_active Expired - Lifetime
- 1995-11-22 PL PL95320427A patent/PL180770B1/pl not_active IP Right Cessation
- 1995-11-22 US US08/008,492 patent/US6080475A/en not_active Expired - Lifetime
- 1995-11-22 DE DE59508149T patent/DE59508149D1/de not_active Expired - Lifetime
- 1995-11-22 AU AU42997/96A patent/AU4299796A/en not_active Abandoned
- 1995-11-22 JP JP51657796A patent/JP4361602B2/ja not_active Expired - Lifetime
- 1995-11-22 CA CA 2205923 patent/CA2205923A1/en not_active Abandoned
- 1995-11-22 WO PCT/EP1995/004599 patent/WO1996015997A1/de not_active Application Discontinuation
- 1995-11-22 MX MX9703828A patent/MX9703828A/es not_active IP Right Cessation
- 1995-11-22 ES ES95941621T patent/ES2147310T3/es not_active Expired - Lifetime
- 1995-11-22 RU RU97110217A patent/RU2161143C2/ru active
-
1997
- 1997-05-21 FI FI972165A patent/FI972165A/fi not_active IP Right Cessation
- 1997-05-22 NO NO19972354A patent/NO312454B1/no unknown
Cited By (9)
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CN1331588C (zh) * | 2002-05-15 | 2007-08-15 | 卡伯特公司 | 气凝胶和中空颗粒粘结剂组合物、绝缘复合物和其制备方法 |
CN101124371B (zh) * | 2004-12-15 | 2013-07-17 | 卡伯特公司 | 含气凝胶的垫层 |
CN105143141A (zh) * | 2009-04-27 | 2015-12-09 | 罗克伍尔国际公司 | 气凝胶组合物及其制备方法和使用方法 |
CN102725243A (zh) * | 2009-11-25 | 2012-10-10 | 卡博特公司 | 气凝胶复合材料及其制造和使用方法 |
CN105669101A (zh) * | 2009-11-25 | 2016-06-15 | 卡博特公司 | 气凝胶复合材料及其制造和使用方法 |
CN104692757A (zh) * | 2015-02-15 | 2015-06-10 | 金成� | 短碳化硅纤维/SiO2气凝胶复合材料及其制备方法 |
CN104692757B (zh) * | 2015-02-15 | 2017-01-25 | 金成� | 短碳化硅纤维/SiO2气凝胶复合材料及其制备方法 |
CN105967621A (zh) * | 2016-05-09 | 2016-09-28 | 天津城建大学 | 保温防水阻燃一体板及其制备方法 |
CN109369129A (zh) * | 2018-11-06 | 2019-02-22 | 航天材料及工艺研究所 | 纤维增强氧化铝气凝胶隔热材料及其制备方法 |
Also Published As
Publication number | Publication date |
---|---|
US6080475A (en) | 2000-06-27 |
CN1077089C (zh) | 2002-01-02 |
DE4441567A1 (de) | 1996-05-30 |
EP0793627A1 (de) | 1997-09-10 |
RU2161143C2 (ru) | 2000-12-27 |
PL320427A1 (en) | 1997-09-29 |
DE59508149D1 (de) | 2000-05-11 |
NO972354D0 (no) | 1997-05-22 |
PL180770B1 (pl) | 2001-04-30 |
WO1996015997A1 (de) | 1996-05-30 |
MX9703828A (es) | 1997-08-30 |
NO312454B1 (no) | 2002-05-13 |
NO972354L (no) | 1997-06-26 |
FI972165A (fi) | 1997-07-21 |
EP0793627B1 (de) | 2000-04-05 |
FI972165A0 (fi) | 1997-05-21 |
JP4361602B2 (ja) | 2009-11-11 |
AU4299796A (en) | 1996-06-17 |
JPH10509940A (ja) | 1998-09-29 |
ES2147310T3 (es) | 2000-09-01 |
CA2205923A1 (en) | 1996-05-30 |
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