CN108290745B - 低粉尘、高绝热的气凝胶毡及其制备方法 - Google Patents
低粉尘、高绝热的气凝胶毡及其制备方法 Download PDFInfo
- Publication number
- CN108290745B CN108290745B CN201780003989.3A CN201780003989A CN108290745B CN 108290745 B CN108290745 B CN 108290745B CN 201780003989 A CN201780003989 A CN 201780003989A CN 108290745 B CN108290745 B CN 108290745B
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- silicon dioxide
- additive
- aerogel blanket
- dioxide gel
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- 239000000377 silicon dioxide Substances 0.000 claims abstract description 84
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- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 claims description 2
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
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- 229910002012 Aerosil® Inorganic materials 0.000 description 19
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/007—After-treatment
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Abstract
本发明涉及一种低粉尘、高绝热的气凝胶毡及其制备方法。更具体地,本发明提供一种低粉尘、高绝热的气凝胶毡的制备方法,其中,将片型Mg(OH)2·MgO·SiO2粉末添加到二氧化硅溶胶中,从而能够减少粉尘的产生同时具有优异的阻燃性和热导率;以及由所述制备方法制备的气凝胶毡。
Description
技术领域
相关申请的交叉引用
本申请要求于2016年10月12日提交到韩国知识产权局的韩国专利申请No.10-2016-0132168的权益,该申请的公开内容通过引用全部并入本说明书中。
技术领域
本发明涉及一种低粉尘(low-dust)、高绝热(high insulation)的气凝胶毡及其制备方法。
背景技术
气凝胶是孔隙率为约90%至99.9%并且孔尺寸在1nm至100nm的范围内的超多孔、高比表面积(≥500m2/g)的材料,并且是在超轻量、优异绝热性、超低介电性等方面优异的材料。因此,已经积极地进行对气凝胶材料的开发的研究,以及对其作为透明绝缘材料、环境友好的高温绝热材料、用于高度集成器件的超低介电薄膜、催化剂和催化剂载体、用于超级电容器的电极、以及用于海水脱盐的电极材料的实际用途的研究。
气凝胶的最大优点是气凝胶具有表现出0.03W/m·K以下的热导率的超绝热性,该热导率比有机绝热材料如常规泡沫聚苯乙烯的热导率更低,并且可以解决火灾情况下的火易损性和有害气体的产生,这些是有机绝热材料的致命弱点。
同时,由于这种气凝胶由于多孔结构而具有非常低的机械强度,因此,已经开发通过用织物毡浸渍气凝胶而粘结的气凝胶复合材料。气凝胶毡是柔性的并且可以弯曲、折叠或切割为任意尺寸或形状,并且容易处理。因此,气凝胶毡不仅用于工业用途,如用于LNG载体的绝热板、工业绝缘材料和航天服、运输工具和汽车、用于发电的绝缘材料,而且用于日用品如夹克和运动鞋。
气凝胶通常通过二氧化硅溶胶的制备、凝胶化、老化、表面改性和干燥步骤来制备。通常,为了改善气凝胶毡的绝热性和防火特性,使用诸如金属氢氧化物类阻燃剂的添加剂来降低二氧化硅溶胶制备步骤中的辐射热传导率并且改善阻燃性能。
然而,由于添加添加剂,SiO2键减弱以减少毡基底与气凝胶之间的粘合力,从而增加粉尘的产生。当将气凝胶毡应用于管道等中时,由于管道的振动,气凝胶不断地从毡基底分离,使得由于添加剂的使用,气凝胶分离现象进一步劣化。
为了解决上述问题,美国专利No.8,021,583B2已经尝试制备浆料形式的气凝胶颗粒或粉末以将它们填充在纤维之间,从而减少粉尘的产生,但是,与凝胶铸造方法相比,存在由于粘合剂等引起热导率增加的问题。
因此,本发明的发明人已经发明一种能够减少粉尘的产生,同时具有优异的阻燃性和热导率性能的低粉尘、高绝热的气凝胶毡的制备方法,以及由该制备方法制备的低粉尘、高绝热的气凝胶毡。
[现有技术文献]
(专利文献1)美国专利No.8,021,583B2(2011年9月20日)
发明内容
技术问题
本发明的一个方面提供一种低粉尘、高绝热的气凝胶毡的制备方法,其中,在所述制备方法中,将片型Mg(OH)2·MgO·SiO2粉末添加到二氧化硅溶胶中,从而能够减少粉尘的产生量,同时具有优异的阻燃性和热导率性能。
本发明的另一方面提供一种通过上述制备方法制备的低粉尘、高绝热的气凝胶毡。
技术方案
根据本发明的一个方面,提供一种气凝胶毡的制备方法,该制备方法包括以下步骤:1)混合二氧化硅前体、水和醇以制备二氧化硅溶胶;2)向所述二氧化硅溶胶中添加由下面的式1表示的添加剂;3)将碱性催化剂与混合有所述添加剂的二氧化硅溶胶混合,然后浸渍毡基底;4)在所述二氧化硅溶胶浸渍到所述毡基底中的状态下进行所述二氧化硅溶胶的凝胶化反应;以及5)之后,进行表面改性和干燥,
[式1]
M(OH)x·MyOz·SiO2
(其中,M是选自Mg、Ca和Al中的至少一种金属元素,x、y和z是3以下的正整数)。
另外,本发明提供一种通过上述制备方法制备的气凝胶毡。
有益效果
根据本发明的气凝胶毡的制备方法通过向二氧化硅溶胶中添加片型Mg(OH)2·MgO·SiO2粉末作为添加剂而具有减少粉尘的产生,同时提高阻燃性和绝热性能的效果。
附图说明
本说明书所附的下面的附图通过实例示出了本发明的优选实例,并且与下面给出的本发明的详细描述一起用于能够进一步理解本发明的技术概念,因此,本发明不应仅以这些附图中的事项来理解:
图1是示意性地示出根据本发明的一个实施方案的气凝胶毡的制备方法的流程图;
图2是示出根据本发明的实施例和比较例的气凝胶毡的阻燃性试验结果的照片。
具体实施方式
下文中,将更详细地描述本发明以更清楚地理解本发明。在这种情况下,应当理解的是,本说明书和权利要求书中所使用的词语或术语不应理解为在常用字典中所定义的含义。还应当理解的是,这些词语或术语应当基于发明人可以适当地定义词语或术语的含义以最好地说明本发明的原则,理解为具有它们在相关技术的背景中和在本发明的技术思想中的含义一致的含义。
二氧化硅气凝胶毡表示作为毡基底的二氧化硅气凝胶材料与织物等混合以制成垫子或片材形式,其中,二氧化硅气凝胶毡具有柔韧性,使得能够弯曲、折叠和切割。二氧化硅气凝胶赋予绝热性,并且诸如织物的毡基底用于提高二氧化硅气凝胶毡的柔韧性和机械强度。
这种二氧化硅气凝胶毡是一种新型材料,它比作为常规聚合物绝缘材料的聚苯乙烯泡沫塑料或聚氨酯泡沫在耐热性和绝缘性方面更优异,其作为能够解决未来发展中的节能和环境问题的高科技材料而引起关注。因此,二氧化硅气凝胶毡用作绝缘材料、绝热材料或不易燃材料,其不仅用于热和冷绝缘用工厂设备(如管道)和用于各种工业设施的工业炉,而且用于飞机、船舶、汽车、建筑结构等。
另外,为了改善气凝胶毡的各种性能,已经尝试通过在制备过程中使用各种添加剂来制备具有优异性能的气凝胶毡。
本发明以上述尝试为基础,并且本发明提供一种气凝胶毡的制备方法,所述气凝胶毡能够得到优异的绝热性能,同时解决添加常规使用的阻燃剂所引起的粉尘产生增加的问题。
下文中,将参照图1详细描述根据本发明的一个实施方案的气凝胶毡的制备方法。
根据本发明的一个实施方案的气凝胶毡的制备方法包括:1)混合二氧化硅前体、水和醇以制备二氧化硅溶胶;2)向所述二氧化硅溶胶中添加由下面的式1表示的添加剂;3)将碱性催化剂与混合有所述添加剂的二氧化硅溶胶混合,然后浸渍毡基底;4)在所述二氧化硅溶胶浸渍到所述毡基底中的状态下进行所述二氧化硅溶胶的凝胶化反应;以及5)之后,进行表面改性和干燥,
[式1]
M(OH)x·MyOz·SiO2
(其中,M是选自Mg、Ca和Al中的至少一种金属元素,x、y和z是3以下的正整数)。
步骤1)是二氧化硅溶胶的制备步骤,其中,二氧化硅溶胶可以通过混合二氧化硅前体、水和醇来制备。
具体地,二氧化硅前体的用量可以为使得二氧化硅溶胶中含有的二氧化硅含量为0.1重量%至30重量%。虽然二氧化硅前体可以根据其类型具有稍微不同的含量,但是,当二氧化硅含量小于0.1重量%时,最终制备的毡中二氧化硅气凝胶的含量会太低而不能实现理想的绝热效果;当含量超过30重量%时,二氧化硅气凝胶的过度形成会引起毡的机械性能,特别是柔韧性劣化。
可用于制备二氧化硅溶胶的二氧化硅气凝胶可以是含有硅的醇盐类化合物,具体地,可以是硅酸四烷基酯,如原硅酸四甲酯(TMOS)、原硅酸四乙酯(TEOS)、预水解的原硅酸四乙基(预水解的TEOS)、原硅酸甲基三乙酯、原硅酸二甲基二乙酯、原硅酸四丙酯、原硅酸四异丙酯、原硅酸四丁酯、原硅酸四仲丁酯、原硅酸四叔丁酯、原硅酸四己酯、原硅酸四环己酯和原硅酸四(十二烷基)酯。
另外,可用于制备二氧化硅溶胶的醇可以具体地是:一元醇,如甲醇、乙醇、异丙醇和丁醇;或多元醇,如甘油、乙二醇、丙二醇、二甘醇、二丙二醇和山梨糖醇,并且可以使用它们中的至少任意一种或两种的混合物。其中,考虑到与水和气凝胶的可混合性,醇可以是具有1至6个碳原子的一元醇,如甲醇、乙醇、异丙醇和丁醇。
考虑到最终制备的二氧化硅气凝胶中的疏水度同时促进表面改性反应,上述醇(极性有机溶剂)可以以适当的量使用。
根据本发明的一个实施方案的步骤2)是向二氧化硅溶胶中添加添加剂的步骤,具体地,可以是添加由下面的式1表示的添加剂的步骤,
[式1]
M(OH)x·MyOz·SiO2
(其中,M是选自Mg、Ca和Al中的至少一种金属元素,x、y和z是3以下的正整数,更具体地,x是2或3,y是1或2,z是1或3)。
更具体地,根据本发明的一个实施方案的添加剂可以是Mg(OH)2·MgO·SiO2。
通常,为了改善气凝胶毡的防火特性,已经在二氧化硅溶胶的制备步骤使用诸如金属氢氧化物类阻燃剂的添加剂。
然而,存在的问题是,添加剂使SiO2键减弱,并且毡基底与气凝胶之间的粘合力降低以增加粉尘的产生。当将气凝胶毡应用于管道等中时,由于管道的振动,粉尘产生问题进一步劣化。
本发明试图通过添加根据本发明的添加剂而解决上述问题,并且还改善绝热性能,同时得到阻燃性和低粉尘的特性。
另外,本发明的添加剂在化合物中含有SiO2,以赋予额外添加二氧化硅前体的效果,由此,气凝胶毡的气凝胶密度增加以降低热导率,从而能够提高最终的气凝胶毡的绝热性能。
另外,根据本发明的一个实施方案的添加剂粉末的特征在于为片型。
片型添加剂彼此交叉(cross),从而具有的效果为,与添加常规阻燃剂或具有其它形式如球形等的本发明的添加剂粉末的气凝胶毡相比,可以显著降低粉尘的产生。
根据本发明的一个实施方案的添加剂可以以适当的量添加,以使本发明的效果最大化,如优异的阻燃性和绝热性能以及低的粉尘产生。
具体地,基于100重量份的二氧化硅前体,本发明的添加剂的用量可以为2.5重量份至20重量份。
基于100重量份的二氧化硅前体,当所使用的添加剂以小于2.5重量份的过少的量添加时,通过本发明得到的改善阻燃性和绝热性能的效果会不显著;当以大于20重量份的过多量添加时,片型添加剂过度地彼此交叉,并且气凝胶在整个毡中不均匀地分布,使得在添加剂过度交叉而聚集的部分中,绝热效果会降低。
根据本发明的一个实施方案的步骤3)是二氧化硅气凝胶浸渍的复合材料的制备步骤,其可以通过在将碱性催化剂添加到二氧化硅溶胶之后浸渍毡基底来进行。
可用于制备本发明的二氧化硅凝胶的碱性催化剂用于提高二氧化硅溶胶的pH值以促进凝胶化。
碱性催化剂可以包括:无机碱,如氢氧化钠和氢氧化钾;或有机碱,如氢氧化铵,但是在无机碱的情况下,化合物中含有的金属离子会配位至Si-OH化合物,因此,可以优选有机碱。具体地,有机碱可以包括:氢氧化铵(NH4OH)、四甲基氢氧化铵(TMAH)、四乙基氢氧化铵(TEAH)、四丙基氢氧化铵(TPAH)、四丁基氢氧化铵(TBAH)、甲胺、乙胺、异丙胺、单异丙胺、二乙胺、二异丙胺、二丁胺、三甲胺、三乙胺、三异丙胺、三丁胺、胆碱、单乙醇胺、二乙醇胺、2-氨基乙醇、2-(乙氨基)乙醇、2-(甲氨基)乙醇、N-甲基二乙醇胺、二甲氨基乙醇、二乙氨基乙醇、次氨基三乙醇、2-(2-氨基乙氧基)乙醇、1-氨基-2-丙醇、三乙醇胺、单丙醇胺或二丁醇胺,并且可以使用它们中的至少一种或两种的混合物。更具体地,本发明的碱可以是NH4OH。
碱性催化剂的含量可以为使得二氧化硅溶胶的pH为4至8。当二氧化硅溶胶的pH超出上述范围时,不容易凝胶化,或者凝胶化速率会太低,从而使加工性能劣化。此外,由于当以固体形式添加时碱会沉淀,因此,其可以优选地以用醇(极性有机溶剂)稀释的溶液的形式添加。
可用于本发明的毡基底可以是薄膜、片材、网、纤维、多孔体、泡沫、无纺织物或包括两个以上层的层压体。此外,根据其应用,毡基底可以形成为在其表面上具有表面粗糙度,或者具有图案化的表面。更具体地,毡基底可以是通过包括二氧化硅气凝胶容易地进入毡基底的空间或孔而能够进一步改善绝热性能的纤维。此外,毡基底可以优选地具有低热导率。
具体地,毡基底可以是聚酰胺、聚苯并咪唑、芳族聚酰胺、丙烯酸树脂、酚醛树脂、聚酯、聚醚醚酮(PEEK)、聚烯烃(例如,聚乙烯、聚丙烯或它们的共聚物等)、纤维素、碳、棉、羊毛、大麻、无纺织物、玻璃纤维或陶瓷棉,更具体地,毡基底可以包括玻璃纤维或聚乙烯。
根据本发明的一个实施方案的步骤4)是制备二氧化硅凝胶复合材料的步骤,其中,可以在二氧化硅溶胶浸渍在毡基底中的状态下使混合有碱性催化剂的二氧化硅溶胶进行凝胶化反应。
根据本发明的一个实施方案的二氧化硅气凝胶毡的制备方法中的凝胶化可以是由二氧化硅前体材料形成网络结构,并且网络结构可以是具有一种或多种类型的原子排列的特定多边形互相连接的平面网状结构,或者是特定多面体互相共享它们的顶点、边、面等以形成三维骨架结构的结构。
二氧化硅溶胶的凝胶化可以在二氧化硅溶胶浸渍在毡基底中的状态下进行。
具体地,浸渍可以在能够容纳毡基底的反应容器中进行,并且可以通过将二氧化硅溶胶倒入反应容器中来进行,或者通过将填充有二氧化硅溶胶的毡基底放入反应容器中并润湿来进行。在这种情况下,为了改善毡基底与二氧化硅溶胶之间的粘合,可以轻轻按压毡基底以充分浸渍。下文中,在恒定压力下将毡基底压制成一定厚度,使得可以除去过量的二氧化硅溶胶以减少随后的干燥时间。
另外,根据本发明的一个实施方案的制备方法还可以在步骤4)之后包括进行老化的步骤。
老化是将二氧化硅凝胶保持在适当的温度下以完成化学变化的步骤,其可以通过在50℃至90℃下将二氧化硅凝胶保持在其中用有机溶剂将碱性催化剂(如氨)稀释至浓度为1%至10%的溶液中10小时来进行。本发明进行老化步骤,从而能够使形成的网状结构更牢固地形成,使得机械稳定性可以得到提高。
另外,根据本发明的一个实施方案的步骤5)是制备疏水性气凝胶毡的步骤,其可以通过对制备的二氧化硅湿凝胶复合材料进行表面改性和干燥来进行。
干燥后的二氧化硅气凝胶在干燥后即刻保持低热导率,但是具有的缺点是,由于二氧化硅表面上硅烷醇基(Si-OH)的亲水性而吸收空气中的水分以逐渐增加热导率,并且存在在干燥步骤的过程中孔严重塌陷的问题,使得难以预期回弹现象,因此,难以制备具有中孔的超绝热产品。因此,为了抑制空气中的水分吸收以保持低热导率,本质上需要将二氧化硅气凝胶的表面改性为疏水性的步骤。
本发明的表面改性通过添加选自三甲基氯硅烷(TMCS)、六甲基二硅氮烷(HMDS)、甲基三甲氧基硅烷、三甲基乙氧基硅烷、乙基三乙氧基硅烷、苯基三乙氧基硅烷和聚二甲基硅氧烷中的至少一种表面改性剂进行,更具体地,可以通过添加六甲基二硅氮烷(HMDS)进行。
下文中,疏水性二氧化硅气凝胶可以通过在保持表面改性后的疏水性二氧化硅气凝胶的孔结构没有任何改变的同时除去溶剂的干燥工艺来制备。所述干燥工艺可以通过常压干燥工艺或超临界干燥工艺进行。
二氧化碳(CO2)在室温和常压下为气态,但是当超过被称为临界点的特定温度和高压的界限时,不发生蒸发过程,从而变为气体和液体不能彼此区分的超临界状态,这种临界状态中的二氧化碳被称为超临界二氧化碳。
超临界二氧化碳具有接近于液体的分子密度,但是具有低的粘度,从而性能类似于气体,并且具有高扩散速率和高热导率,使得干燥效率高,因此,可以缩短干燥工艺时间。
在超临界干燥工艺中,将老化后的二氧化硅凝胶放入超临界干燥反应器中,接着填充液体状态的CO2并进行用CO2置换二氧化硅气凝胶中的醇溶剂的溶剂置换过程。之后,以特定的加热速率,具体地以0.1℃/分钟至1℃/分钟的加热速率将混合物加热至40℃至50℃,然后,在大于二氧化碳变为超临界的压力,具体地在100巴至150巴的压力下保持,从而在超临界状态中保持特定的时间,具体地为20分钟至1小时。通常,二氧化碳在31℃的温度和73.8巴的压力下变为超临界。将二氧化碳在二氧化碳变为超临界的特定温度和压力下保持2小时至12小时,具体地为2小时至6小时之后,缓慢地除去压力以完成超临界干燥工艺,使得可以制备二氧化硅气凝胶毡。
另外,常压干燥工艺可以根据常规方法,如在常压(1±0.3标准大气压)下的自然干燥来进行。
同时,根据本发明的一个实施方案的制备方法在干燥之前还可以进行洗涤步骤。洗涤是除去在反应过程中产生的杂质(钠离子、未反应物、副产物等)和在超临界干燥过程中与CO2反应以生成碳酸铵盐的残余铵的步骤,从而得到高纯度的疏水性二氧化硅气凝胶。洗涤可以通过使用非极性有机溶剂的稀释过程或置换过程来进行。
另外,本发明可以提供一种通过本发明的制备方法制备的气凝胶毡。此外,所述气凝胶毡的热导率可以为14mW/mK以下。
另一方面,随着毡中二氧化硅气凝胶的含量更高,气凝胶毡的绝热性能提高。然而,当含量太高时,由于二氧化硅气凝胶本身的低强度和粘合力,在用于毡制备的随后工艺中强度和粘合力会劣化,因此,考虑到毡的用途等,优选适当地调节毡中含有的二氧化硅气凝胶的含量。具体地,基于气凝胶毡的总重量,本发明中二氧化硅气凝胶的含量可以为20重量%至80重量%。
根据如上所述添加由式1表示的特定组成和形式的添加剂的本发明的制备方法,可以得到能够减少粉尘的产生,同时具有优异的阻燃性和优异的热导率的效果。
下文中,将详细描述本发明的实施例,使得本领域技术人员可以容易地实施本发明。然而,本发明可以以不同的形式实施,而不局限于本文中提出的实施方案。
实施例1
将原硅酸四乙酯、乙醇、水和HCl混合以制备SiO2浓度为20%的预水解的TEOS。将水和乙醇与混合物再次混合以制备二氧化硅浓度为4%的醇盐二氧化硅溶胶。之后,将片型Mg(OH)2·MgO·SiO2粉末以二氧化硅浓度为2.5重量份的量添加到二氧化硅溶胶中。将氨催化剂添加到制备的二氧化硅溶胶中之后,浸渍聚酯纤维并进行凝胶化。在这种情况下,完全凝胶化需要约10分钟。老化约1小时之后,用六甲基二硅氮烷(HMDS)进行表面改性。当表面改性结束时,将二氧化硅凝胶-纤维复合材料放入7.2L的超临界萃取器中并注入CO2。然后,经1小时20分钟将萃取器中的温度加热至50℃,并且当在50℃下达到100巴时,以0.4L/分钟的速率经150分钟连续注入CO2。此时,通过分离器的底部回收乙醇。然后通过排放CO2 2小时来制备气凝胶毡。
实施例2
除了在实施例1中添加5.0重量份的添加剂之外,以与实施例1中相同的方式制备气凝胶毡。
实施例3
除了在实施例1中添加7.5重量份的添加剂之外,以与实施例1中相同的方式制备气凝胶毡。
实施例4
除了在实施例1中添加10.0重量份的添加剂之外,以与实施例1中相同的方式制备气凝胶毡。
比较例1
除了在实施例1中不添加添加剂之外,以与实施例1中相同的方式制备气凝胶毡。
比较例2
除了在实施例1中添加5.0重量份的球形Mg(OH)2之外,以与实施例1中相同的方式制备气凝胶毡。
比较例3
除了在实施例1中添加球形粉末而不是片型的添加剂之外,以与实施例1中相同的方式制备气凝胶毡。
[表1]
实验例1:阻燃性测量
将金属丝与在实施例2和比较例1至3中制备的气凝胶毡样品接触之后,在将金属丝加热至1050℃的同时观察是否产生烟、气味和烟灰。结果示于表1和图2中。
如图2中所示,在没有添加阻燃剂或其它添加剂的比较例1中,可以观察到,最多地产生烟和烟灰并且出现火焰。
同时,在添加Mg(OH)2的比较例2中,可以观察到,与比较例1相比,阻燃性稍微改善,但是与添加Mg(OH)2·MgO·SiO2的实施例2和比较例3相比,出现大量的烟、烟灰和火焰。
根据实验结果,在添加本发明的Mg(OH)2·MgO·SiO2的实施例2和比较例3中,可以看出,阻燃性得到改善。在上述实施例中,在添加片型而不是球型Mg(OH)2·MgO·SiO2粉末的实施例2中,可以发现,阻燃性得到最大改善。
因此,可以确定,通过本发明的制备方法制备的气凝胶毡具有优异的阻燃性能。
实验例2:粉尘产生实验
将根据实施例1至4和比较例1至3制备的气凝胶毡切割成12.5cm×12.5cm,折叠14次,然后摇晃20次来测量重量变化(重量减少率=(气凝胶毡的初始重量-粉尘产生实验之后气凝胶毡的重量)/(气凝胶毡的初始重量)×100%)。测量结果示于上面的表1中。
如表1中所示,在未添加添加剂(比较例1)、添加Mg(OH)2(比较例2)或添加球形Mg(OH)2·MgO·SiO2粉末(比较例3)的气凝胶毡中,可以发现,通过粉尘产生实验,气凝胶毡的重量显著减少。
另一方面,在添加片型Mg(OH)2·MgO·SiO2粉末的本发明的实施例1至4中,可以发现,与比较例相比,气凝胶毡的重量减少率显著降低。
上述效果通过片型添加剂彼此交叉而得到,从而增加气凝胶对毡的粘合力,并且可以表明,与添加常规阻燃剂或具有诸如球形的其它类型的添加剂的气凝胶毡相比,粉尘的产生可以显著降低。
因此,可以确定,本发明的气凝胶毡的制备方法可以制备低粉尘气凝胶毡。
实验例3:热导率测量
通过使用NETZSCH Co.的GHP 456设备测量在实施例1至4和比较例1至3中制备的二氧化硅气凝胶毡的防护热板(GHP)高温热导率,结果示于表1中。
如表1中所示,在添加片型Mg(OH)2·MgO·SiO2粉末的本发明的实施例1至4中,可以发现,与比较例相比,气凝胶毡的热导率整体显著降低。
另外,可以确定,既没有添加阻燃剂也没有添加其它添加剂的比较例1具有最高的热导率,因此,可以发现,绝热性能最差。
另一方面,在添加Mg(OH)2的比较例2中,可以确定,与比较例1相比,热导率稍微提高,但是与添加Mg(OH)2·MgO·SiO2的实施例1至4和比较例3相比,热导率没有显著提高。
另外,即使当添加具有相同组成的Mg(OH)2·MgO·SiO2作为添加剂时,在添加剂粉末的类型为球形的比较例3中,可以确定,与添加相同量的片型粉末的实施例2相比,热导率的改善效果小。
因此,可以发现,通过本发明的气凝胶毡的制备方法制备的气凝胶毡具有优异的绝热性能,所述制备方法的特征在于添加片型粉末的Mg(OH)2·MgO·SiO2。
提出本发明的上述描述用于说明的目的。本领域技术人员应当理解的是,在不脱离本发明的精神和范围的情况下,可以对本说明书进行各种形式上和细节上的改变。因此,应当理解的是,上述实施方案在所有方面均是说明性的而不是限制性的。
Claims (7)
1.一种气凝胶毡的制备方法,该制备方法包括以下步骤:
1)混合二氧化硅前体、水和醇以制备二氧化硅溶胶;
2)向所述二氧化硅溶胶中添加由下面的式1表示的添加剂;
3)将碱性催化剂与混合有所述添加剂的二氧化硅溶胶混合,然后浸渍毡基底;
4)在所述二氧化硅溶胶浸渍到所述毡基底中的状态下进行所述二氧化硅溶胶的凝胶化反应;
5)之后,进行表面改性和干燥;以及
[式1]
M(OH)x·MyOz·SiO2
其中,M是选自Mg、Ca和Al中的至少一种金属元素,x、y和z是3以下的正整数,
其中,所述添加剂是Mg(OH)2·MgO·SiO2,所述添加剂是片型粉末。
2.根据权利要求1所述的制备方法,其中,基于100重量份的二氧化硅前体,所述添加剂的用量为2.5重量份至20重量份。
3.根据权利要求1所述的制备方法,其中,所述碱性催化剂是选自氢氧化铵(NH4OH)、四甲基氢氧化铵(TMAH)、四乙基氢氧化铵(TEAH)、四丙基氢氧化铵(TPAH)、四丁基氢氧化铵(TBAH)、甲胺、乙胺、异丙胺、二乙胺、二异丙胺、二丁胺、三甲胺、三乙胺、三异丙胺、三丁胺、胆碱、单乙醇胺、二乙醇胺、2-氨基乙醇、2-(乙氨基)乙醇、2-(甲氨基)乙醇、N-甲基二乙醇胺、二甲氨基乙醇、二乙氨基乙醇、次氨基三乙醇、2-(2-氨基乙氧基)乙醇、1-氨基-2-丙醇、三乙醇胺、单丙醇胺和二丁醇胺中的至少一种。
4.根据权利要求1所述的制备方法,其中,所述毡基底是选自薄膜、片材、网、纤维、多孔体、泡沫和无纺织物中的至少一种。
5.根据权利要求1所述的制备方法,在步骤4)之后,还包括进行老化的步骤。
6.根据权利要求1所述的制备方法,其中,所述表面改性通过添加选自三甲基氯硅烷(TMCS)、六甲基二硅氮烷(HMDS)、甲基三甲氧基硅烷、三甲基乙氧基硅烷、乙基三乙氧基硅烷、苯基三乙氧基硅烷和聚二甲基硅氧烷中的至少一种表面改性剂进行。
7.根据权利要求1所述的制备方法,其中,所述干燥通过超临界干燥工艺或常压干燥工艺进行。
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