CN1258230A - 将气凝胶粒化的方法 - Google Patents
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Abstract
本发明涉及气凝胶颗粒结构附聚的方法,其中在混合装置中加入气凝胶颗粒并充分混合,和在混合装置中加入粘合剂。
Description
本发明涉及一种将气凝胶粒化的方法。
气凝胶,特别是孔隙率高于60%和密度低于0.6克/立方厘米的气凝胶,具有特别低的导热能力,并因此可以作为绝热材料使用,正如在EP-A-0 171 722中描述的一样,还可以作为催化剂或作为催化剂载体以及作为吸附材料使用。此外,由于它们对固体物质具有非常低的折射率,已知它们可以用于Cerenkov探测器。另外,由于它们特殊的声阻抗,公开文献中描述了例如在超声领域中作为阻抗调节装置。
它们也可以在药物学和农业中作为活性物质的载体。
在广义上,即“以空气作为分散介质的凝胶”的意义上,气凝胶是通过干燥合适的凝胶制备的。在此意义上,术语“气凝胶”包括狭义的气凝胶,干凝胶和冷凝胶(Kryogel)。在此,当凝胶中的液体在超过临界温度的温度下并从超过临界压力的压力开始基本上被脱除时,则干燥的凝胶被称作狭义上的气凝胶。相反,如果凝胶的液体在亚临界条件下,例如伴随形成液体-蒸汽界面相而被除去,那么生成的凝胶通常被称为干凝胶。
本发明中使用的术语气凝胶是广义上的气凝胶,即“以空气作为分散介质的凝胶”。
该术语不包括早期文献中公开的例如通过硅酸沉淀(例如DE3025437,DD296 898)或作为火成硅酸例如AerosilTM产生的干凝胶。在这些情况中,在制备期间,未形成在相当长的距离内均匀的三维凝胶网状物。
气凝胶基本上可以划分为无机和有机气凝胶。
从1931年以来,就已经已知无机气凝胶(S.S.Kistler,自然(Nature)1931,127,741)。之后,由各种不同的原材料制备气凝胶。在这方面,例如可以制备SiO2-、Al2O3-、TiO2-、ZrO2-、SnO2-、Li2O-、CeO2-、V2O5-气凝胶以及它们的混合物(H.D.Gesser,P.C.Goswami,《化学评论》(Chem.Rev.)1989,89,765ff)。
几年来,也公开了由各种各样的原材料例如蜜胺甲醛(R.W.Pekala,《材料科学杂志》(J.Mater.Sci.),1989,24,3221)制备的有机气凝胶。
无机气凝胶可以按照不同的方法制备。
一方面,SiO2气凝胶例如可以通过原硅酸四乙基酯在乙醇中酸式水解和缩合来制备。在该方法中,获得一种可以通过超临界干燥来干燥同时保持其结构的凝胶。例如EP-A-0 396 076、WO92/03378或WO95/06617中公开了基于这种干燥技术的制备方法。
然而,气凝胶的超临界干燥中涉及的高压技术在工艺上是非常昂贵的,且具有高的安全危险性。此外,气凝胶的超临界干燥是一种成本非常高的生产方法。
已提供一种亚临界干燥SiO2-凝胶的方法以代替超临界干燥方法。
由于其工艺简单、能耗低和安全危险性低,所以亚临界干燥的成本显著降低。
例如,SiO2-凝胶可以通过在合适有机溶剂中借助于水使四烷氧基硅烷酸式水解来制备。用合适的有机溶剂交换该溶剂之后,得到的凝胶在下一步骤中与甲硅烷基化剂反应。最后在空气中从有机溶剂中干燥出因此制得的SiO2-凝胶。由此,可以获得密度低于0.4克/立方厘米和孔隙率高于60%的气凝胶。WO94/25149中详细地描述了基于该干燥技术的制备方法。
此外,如WO92/20623中公开的一样,在干燥之前,上述凝胶可以与四烷氧基硅烷在醇的水溶液中混合并且老化,以提高凝胶网状物的强度。
然而,在上述方法中作为原材料的四烷氧基硅烷同样是十分昂贵的。
通过使用水玻璃作为原材料来制备SiO2-凝胶可以显著降低成本。为此,例如借助于离子交换树脂由水玻璃水溶液制备硅酸,然后通过加入碱使该硅酸缩聚为SiO2-凝胶。在用合适的有机溶剂交换含水介质之后,获得的凝胶在下一步骤中可以与含氯甲硅烷基化剂反应。最后同样在空气中从有机溶剂中干燥出其表面用例如甲基甲硅烷基改性的SiO2-凝胶。DE-A-43 42 548中详细地描述了基于该技术的制备方法。
在德国专利申请195 41 715.1和195 41 992.8中描述了另一基于水玻璃和随后亚临界干燥制备SiO2-气凝胶的方法。
此外,在DE-A 195 02 453中描述了无氯的甲硅烷基化剂在制备亚临界干燥的气凝胶中的用途。
此外,在DE-A-195 34 198中描述了在亚临界干燥的气凝胶制备中借助于有机官能化的甲硅烷基化剂的有机官能化。
然而,由于生产工艺和制备成本方面的原因,工业规模生产的气凝胶颗粒的颗粒尺寸被限为小于5毫米和优选小于2毫米。
根据制备气凝胶方法的种类,原则上多次洗涤和溶剂交换是需要的。因为这些与扩散有关,所以所需时间与凝胶颗粒半径的平方成正比。结果,不考虑干燥方法,气凝胶的制造成本也随颗粒尺寸的增大而显著增加。由于成本方面的原因,造成试图生产尽可能小的气凝胶颗粒的局面。
另一方面,非常小的颗粒的操作非常复杂,并且因此所需的成本不是令人满意的,而且不是所有气凝胶的工业应用均与颗粒尺寸无关。
因此,从可操作性和对许多应用来看,较大的气凝胶颗粒是需要的或者至少是有利的。
因此,本发明的目的是提供一种方法,通过该方法尺寸小于2毫米的小气凝胶颗粒可以形成较大的气凝胶颗粒。
该问题是通过这样一种方法解决的,在该方法中,将气凝胶颗粒送入混合装置中并充分混合,并在混合装置中加入粘合剂。
可在气凝胶颗粒加入之前、期间和/或之后,在混合装置中加入粘合剂,在此随后加入是优选的。
借助于所述的混合装置使气凝胶颗粒处于运动中以使它们之间相对移动,该混合装置例如是附聚板(Agglomerierteller)、混合器或流化床单元。
有利地,粘合剂作为水溶液或非水性溶液或悬浮液或甚至作为熔体例如通过喷射加入。该粘合剂导致原来提供的气凝胶颗粒相互团聚,形成较大的颗粒。
在该方法中,通过化学反应、硬化、由于溶剂蒸发或气化引起的结晶,该粘合剂导致混合物组分相互粘结。
根据另一有利的实施方案,粘合剂作为固体物质加入。然后通过固体物质与混合物中的一种或多种组分进行化学反应发生粘结,或通过固体粘合剂的软化例如通过升高温度使其具有粘性并粘结混合物的颗粒而发生粘结。
另一有利的实施方案是除气凝胶颗粒外,也可以在混合装置中加入以颗粒或纤维形式的添加剂和/或填料。
根据一优选的实施方案,根据附聚物的尺寸将它们分离。有利地,从制备的颗粒中,根据所希望的颗粒范围筛分出目标级分。太大的颗粒可以例如使用切碎机或铣头来粉碎并筛分,这样使它们处于所希望的颗粒范围中或在粉碎之后返回附聚装置中。太小的颗粒可以返回附聚装置中。
根据另一方案,在进一步加工之前干燥附聚物。
Claims (9)
1、气凝胶颗粒结构附聚的方法,其中在混合装置中加入气凝胶颗粒并充分混合,和在混合装置中加入粘合剂。
2、根据权利要求1的方法,其特征在于,在混合装置中先加入气凝胶颗粒,然后加入粘合剂。
3、根据权利要求1或2的方法,其特征在于,粘合剂作为水溶液或非水性溶液、作为悬浮液、作为熔体或作为固体物质加入。
4、根据上述权利要求至少之一的方法,其特征在于,除气凝胶颗粒外,在混合装置中还加入添加剂和/或填料。
5、根据上述权利要求至少之一的方法,其特征在于,根据它们的尺寸分离附聚物。
6、根据权利要求5的方法,其特征在于,将在所希望颗粒范围之下的附聚物返回混合装置中。
7、根据权利要求5的方法,其特征在于,在所希望颗粒范围之上的附聚物被粉碎。
8、根据权利要求7的方法,其特征在于,将粉碎和在所希望颗粒范围之下的附聚物送入混合装置中。
9、根据上述权利要求至少之一的方法,其特征在于,在进一步加工之前干燥附聚物。
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DE19718740A DE19718740A1 (de) | 1997-05-02 | 1997-05-02 | Verfahren zur Granulierung von Aerogelen |
DE19718740.4 | 1997-05-02 |
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CN1258230A true CN1258230A (zh) | 2000-06-28 |
CN1126592C CN1126592C (zh) | 2003-11-05 |
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US (1) | US6481649B1 (zh) |
EP (1) | EP0979141A1 (zh) |
JP (1) | JP2001523162A (zh) |
KR (1) | KR20010012153A (zh) |
CN (1) | CN1126592C (zh) |
CA (1) | CA2287849A1 (zh) |
DE (1) | DE19718740A1 (zh) |
WO (1) | WO1998050144A1 (zh) |
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-
1997
- 1997-05-02 DE DE19718740A patent/DE19718740A1/de not_active Ceased
-
1998
- 1998-04-29 KR KR19997010098A patent/KR20010012153A/ko not_active Application Discontinuation
- 1998-04-29 WO PCT/EP1998/002519 patent/WO1998050144A1/de not_active Application Discontinuation
- 1998-04-29 CN CN98805627A patent/CN1126592C/zh not_active Expired - Fee Related
- 1998-04-29 CA CA002287849A patent/CA2287849A1/en not_active Abandoned
- 1998-04-29 JP JP54769598A patent/JP2001523162A/ja not_active Ceased
- 1998-04-29 EP EP98925496A patent/EP0979141A1/de not_active Ceased
-
1999
- 1999-11-01 US US09/433,931 patent/US6481649B1/en not_active Expired - Lifetime
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108147401A (zh) * | 2018-01-12 | 2018-06-12 | 昂星新型碳材料常州有限公司 | 石墨烯气凝胶粉末的制备方法和石墨烯气凝胶粉末 |
CN110077079A (zh) * | 2019-05-29 | 2019-08-02 | 浙江康廷电子科技有限公司 | 一种气凝胶与pet基材的复合结构及其制备工艺 |
Also Published As
Publication number | Publication date |
---|---|
WO1998050144A1 (de) | 1998-11-12 |
CA2287849A1 (en) | 1998-11-12 |
DE19718740A1 (de) | 1998-11-05 |
EP0979141A1 (de) | 2000-02-16 |
KR20010012153A (ko) | 2001-02-15 |
JP2001523162A (ja) | 2001-11-20 |
US6481649B1 (en) | 2002-11-19 |
CN1126592C (zh) | 2003-11-05 |
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