CN112321313A - 一种陶瓷纤维气凝胶复合材料及其制备方法 - Google Patents

一种陶瓷纤维气凝胶复合材料及其制备方法 Download PDF

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CN112321313A
CN112321313A CN202011375280.6A CN202011375280A CN112321313A CN 112321313 A CN112321313 A CN 112321313A CN 202011375280 A CN202011375280 A CN 202011375280A CN 112321313 A CN112321313 A CN 112321313A
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aerogel
ceramic fiber
powder
aerogel powder
parts
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陈智明
杨浩
罗肖宁
郭海建
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Henan Aibiaihe New Material Co ltd
Contemporary Amperex Technology Co Ltd
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Henan Aibiaihe New Material Co ltd
Contemporary Amperex Technology Co Ltd
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Abstract

本发明属于气凝胶材料领域，公开了一种陶瓷纤维气凝胶复合材料及其制备方法，降低传统浸渍或喷淋工艺的生产成本，并解决现有陶瓷纤维气凝胶毡粉体复合不均匀的问题，陶瓷纤维气凝胶毡，主要由陶瓷纤维和气凝胶粉体组成，在制备陶瓷纤维混合浆料时，加入气凝胶粉体同步改性，或直接加入经过高温表面改性气凝胶粉，再高温干燥，制备出具有防火隔热性能，且气凝胶分布均匀的陶瓷纤维气凝胶毡，可广泛应用于新能源、动力电池、建筑、工业等有防火隔热需求的领域。

Description

一种陶瓷纤维气凝胶复合材料及其制备方法
技术领域
本发明涉及气凝胶材料领域，特别涉及了一种陶瓷纤维气凝胶复合材料及其制备方法。
背景技术
气凝胶是一种三维网络结构的纳米先进材料，气凝胶的空间网状结构中充满的介质是空气，因此具有极低密度、低导热系数、高孔隙率等优越性能，在保温隔热，节能降耗领域具有非常广阔的应用前景。陶瓷纤维耐火性能优越，在防火领域应用十分广泛。陶瓷纤维气凝胶复合材料同时具备陶瓷纤维良好的防火性能，以及气凝胶的保温隔热性能，是一种高性能的防火隔热复合材料。
传统陶瓷纤维气凝胶复合材料是采用两步法的工艺制备而成的，即先制备出陶瓷纤维材料，再将其与气凝胶复合，此方法，工艺复杂，且气凝胶复合不均匀，导致气凝胶和陶瓷纤维复合材料的制备效果降低，使用效果不好。
发明内容
针对上述现有技术的不足，本发明制备出一种陶瓷纤维气凝胶复合材料，并提供了一种工艺简单，气凝胶粉分布均匀的制备方法。
本发明的目的是这样实现的：
一种陶瓷纤维气凝胶复合材料，包括陶瓷纤维和气凝胶粉，气凝胶粉体均匀的附着在陶瓷纤维表面。
所述陶瓷纤维为硅酸铝纤维、氧化锆纤维、玄武岩纤维、莫来石纤维中的一种或几种，直径为0.0001mm-3mm。
所述气凝胶粉体为SiO2气凝胶粉、TiO2气凝胶粉、Al2O3气凝胶、LiO气凝胶、石墨烯气凝胶等气凝胶材料中的一种或几种，气凝胶粉体的粒度在50目-1000目。
一种陶瓷纤维气凝胶复合材料的制备方法，包括以下步骤：a. 气凝胶粉体的高温表面改性：称取一定量的气凝胶粉，放置于烘箱中，经过高温一段时间，得到高温表面改性的气凝胶粉；b. 陶瓷纤维气凝胶混合浆料配制：以下原料组分按重量份数计算，称取陶瓷纤维20-100份，称取气凝胶粉或步骤a中的改性后的气凝胶粉5-40份，有机结合剂10-30份，润湿剂1-15份，分散剂1-15份，增稠剂1-15份、去离子水60-100份放入搅拌釜中并搅拌，直至混合均匀并冷却至室温，制成陶瓷纤维气凝胶浆料；c. 将步骤b中陶瓷纤维气凝胶浆料通过压板控制厚度为0.2-20mm，在30-150℃的烘干隧道中烘0.5-2h，收卷或切片后得到陶瓷纤维气凝胶复合材料。
所述步骤a中烘箱的温度为150-600℃，在烘箱中烘烤0.5-4h。
所述步骤b中的搅拌釜的温度为25-85℃时，搅拌速率为1000-5000r/min，在搅拌釜中搅拌时间为0.5-2h。
所述有机结合剂为丙烯酸乳液、EVA乳液，聚氨酯乳液等可以作为结合剂的有机树脂乳液中的一种或几种；
所述润湿剂包括氨水、聚乙二醇、三乙醇胺、多元醇中的一种或几种；
所述分散剂为5040分散剂、六偏磷酸钠、十二烷基苯磺酸钠、聚丙烯酸、聚丙烯酸钠、聚丙烯酸钙、十二烷基硫酸钠、聚乙烯醇等中的一种或几种；
所述增稠剂为的羟乙基纤维素、羧甲基纤维素钠、锂基膨润土中的一种或多种。
本发明的有益效果是：采用一步法制备的陶瓷纤维气凝胶复合材料，在陶瓷纤维浆料中加入改性的气凝胶水性浆料，同步干燥后收卷或切片，工序简单，气凝胶分布均匀，一致性好，应用范围广泛。
具体实施方式
下面结合实施例对本发明作以下说明：
实施例1：
一种陶瓷纤维气凝胶复合材料制备方法，包括以下步骤：a. 气凝胶粉体的高温表面改性：称取粒径为600目的SiO2气凝胶粉体20份，放置于温度为300℃的烘箱中，经过高温烘烤2h，得到高温表面改性的气凝胶粉；b. 陶瓷纤维气凝胶混合浆料配制：以重量份称取直径0.02mm-1mm的硅酸铝纤维80份，SiO2气凝胶粉20份，氨水5份，EVA胶粘剂20份，六偏磷酸钠和聚乙烯醇各5份，聚丙烯酸钠10份，羧甲基纤维素钠5份，去离子水70份；在40℃时，以1500r/min的转速在搅拌釜中搅拌1h，冷却至室温，制成陶瓷纤维气凝胶浆料备用，。c：对陶瓷纤维气凝胶浆料进行压制：将步骤b中陶瓷纤维气凝胶浆料经压板控制厚度为3mm，压板压制后的瓷纤维气凝胶浆料在80℃的烘干隧道中烘30min，烘干后进行收卷，得到3mm厚的陶瓷纤维气凝胶毡卷材，陶瓷纤维气凝胶毡卷材包括陶瓷纤维和气凝胶粉，气凝胶粉体均匀的附着在陶瓷纤维表面，陶瓷纤维气凝胶毡可广泛应用于新能源、动力电池、建筑、工业等有防火隔热需求的领域，增稠剂增加陶瓷纤维气凝胶混合浆料的粘稠度，增大液体对体系内纤维、粉体等易沉降物和易漂浮物的浮力和束缚力，提高纤维和粉体的悬浮稳定性，从而保障气凝胶粉体与陶瓷纤维复合的均匀性，润湿剂主要是为了增加气凝胶粉和陶瓷纤维表面的浸润性，使其二者表面更好的被去离子水润湿，一方面可提高二者在水相中的悬浮稳定性，另一方面可提高二者直接的亲和性，最终提高纤维和粉体的亲和性及均匀性，主要是用于对气凝胶粉体进行表面疏水改性，提高气凝胶粉体表面的亲水性，使之更均匀的悬浮于整个体系中，现有工艺均需额外加入改性剂对粉体进行改性。本发明中创造性的使用高温热解气凝胶粉体表面的疏水基团，但不破环其内部孔隙结构，无需添加改性剂，即可达到表面亲水改性的效果，本发明在浆料制备阶段加入增稠剂、润湿剂，并通过高温实现气凝胶粉体表面的亲水改性，降低了生产成本，提高气凝胶粉体与陶瓷纤维的亲和性及均匀性。
实施例2：
一种陶瓷纤维气凝胶复合材料制备方法，包括以下步骤：a：称取粒径为600目的SiO2气凝胶粉体20份，在300℃环境下加热2h，得到高温表面改性的SiO2气凝胶粉；b：以重量份称取直径0.04mm的莫来石纤维100份， 步骤a中的高温表面改性的SiO2气凝胶粉20份，丙烯酸胶粘剂30份，5040和十二烷基苯磺酸钠各10份，聚丙烯酸5份，羟丙基纤维素5份，去离子水100份。在60℃时，以2500r/min的转速在搅拌釜中搅拌1h，冷却至室温，制成陶瓷纤维气凝胶浆料备用。c：对陶瓷纤维气凝胶浆料进行压制：将步骤b中陶瓷纤维气凝胶浆料经压板控制厚度为10mm，压板压制后在80℃的烘干隧道中烘60min，烘干后进行切片，得到10mm厚的陶瓷纤维气凝胶毡片材，陶瓷纤维气凝胶毡卷材包括陶瓷纤维和气凝胶粉，气凝胶粉体均匀的附着在陶瓷纤维表面，陶瓷纤维气凝胶毡可广泛应用于新能源、动力电池、建筑、工业等有防火隔热需求的领域，增稠剂增加陶瓷纤维气凝胶混合浆料的粘稠度，增大液体对体系内纤维、粉体等易沉降物和易漂浮物的浮力和束缚力，提高纤维和粉体的悬浮稳定性，从而保障气凝胶粉体与陶瓷纤维复合的均匀性，润湿剂主要是为了增加气凝胶粉和陶瓷纤维表面的浸润性，使其二者表面更好的被去离子水润湿，一方面可提高二者在水相中的悬浮稳定性，另一方面可提高二者直接的亲和性，最终提高纤维和粉体的亲和性及均匀性，主要是用于对气凝胶粉体进行表面疏水改性，提高气凝胶粉体表面的亲水性，使之更均匀的悬浮于整个体系中，现有工艺均需额外加入改性剂对粉体进行改性。本发明中创造性的使用高温热解气凝胶粉体表面的疏水基团，但不破环其内部孔隙结构，无需添加改性剂，即可达到表面亲水改性的效果，本发明在浆料制备阶段加入增稠剂、润湿剂，并通过高温实现气凝胶粉体表面的亲水改性，降低了生产成本，提高气凝胶粉体与陶瓷纤维的亲和性及均匀性。
实施例3：
一种陶瓷纤维气凝胶复合材料制备方法，包括以下步骤：a：称取粒径为600目的Al2O3气凝胶粉体30份，在400℃环境下加热2h，得到高温表面改性的Al2O3气凝胶粉；b：以重量份称取直径0.05mm的氧化锆纤维80份，步骤a中的高温表面改性的Al2O3气凝胶粉30份，聚氨酯胶粘剂30份，六偏磷酸钠和十二烷基苯磺酸钠各5份，聚丙烯酸5份，羧甲基纤维素钠5份，去离子水100份。在80℃时，以3000r/min的转速在搅拌釜中搅拌1.5h，冷却至室温，制成陶瓷纤维气凝胶浆料备用。
c：对陶瓷纤维气凝胶浆料进行压制；将步骤b获得的陶瓷纤维气凝胶浆料经压板控制厚度，厚度为5mm，压板压制后在80℃的烘干隧道中烘30min，烘干后进行收卷，得到5mm厚的陶瓷纤维气凝胶毡卷材，陶瓷纤维气凝胶毡卷材包括陶瓷纤维和气凝胶粉，气凝胶粉体均匀的附着在陶瓷纤维表面，陶瓷纤维气凝胶毡可广泛应用于新能源、动力电池、建筑、工业等有防火隔热需求的领域，增稠剂增加陶瓷纤维气凝胶混合浆料的粘稠度，增大液体对体系内纤维、粉体等易沉降物和易漂浮物的浮力和束缚力，提高纤维和粉体的悬浮稳定性，从而保障气凝胶粉体与陶瓷纤维复合的均匀性，润湿剂主要是为了增加气凝胶粉和陶瓷纤维表面的浸润性，使其二者表面更好的被去离子水润湿，一方面可提高二者在水相中的悬浮稳定性，另一方面可提高二者直接的亲和性，最终提高纤维和粉体的亲和性及均匀性，主要是用于对气凝胶粉体进行表面疏水改性，提高气凝胶粉体表面的亲水性，使之更均匀的悬浮于整个体系中，现有工艺均需额外加入改性剂对粉体进行改性。本发明中创造性的使用高温热解气凝胶粉体表面的疏水基团，但不破环其内部孔隙结构，无需添加改性剂，即可达到表面亲水改性的效果，本发明在浆料制备阶段加入增稠剂、润湿剂，并通过高温实现气凝胶粉体表面的亲水改性，降低了生产成本，提高气凝胶粉体与陶瓷纤维的亲和性及均匀性。
测试方法：①、防火测试；取200*200*3mm规格的陶瓷纤维气凝胶毡，使用丁烷喷枪（火焰温度1200℃）对样品进行火焰灼烧，测试烧穿时间，如1h未烧穿，则停止测试，记录灼烧状态
②、隔热测试：取200*200*3mm规格的陶瓷纤维气凝胶毡，使用热台加热到800℃，将样品置于加热台面上，20min后测试样品冷面温度；
测试结果：使用1200℃的火焰喷枪对样品灼烧1h，样品未烧穿；800℃加热20min，三个实例中的样品冷面温度均超过220℃，冷热面温差超过580℃，具有优异的隔热效果。
实例1：SiO2气凝胶+硅酸铝纤维：耐火温度1300℃，1200℃火焰喷枪灼烧1h，未烧穿，800℃加热台加热20min后，冷面温度＜220℃；
实例2：SiO2气凝胶+莫来石纤维：耐火温度1600℃，1200℃火焰灼烧1h，未烧穿，800℃加热台加热20min后，冷面温度＜220℃；
实例3：Al2O3气凝胶+氧化锆纤维：耐火温度2000℃，1200℃火焰灼烧1h，未烧穿，800℃加热台加热20min后，冷面温度＜200℃；
实例1和实例2隔热较实例3略低，是因为SiO2气凝胶极限耐温较Al2O3气凝胶低，在800℃下，SiO2气凝胶的三维纳米网络结构受到一定破坏，隔热受到一定影响；而Al2O3气凝胶的网络结构仍保持稳定，隔热性能稳定。

Claims (10)

1.一种陶瓷纤维气凝胶复合材料，其特征在于：包括陶瓷纤维和气凝胶粉，气凝胶粉体均匀的附着在陶瓷纤维表面。
2.根据权利要求1所述的陶瓷纤维气凝胶复合材料，其特征在于：所述陶瓷纤维为硅酸铝纤维、氧化锆纤维、玄武岩纤维、莫来石纤维中的一种或几种，直径为0.0001mm-3mm。
3.根据权利要求1所述的陶瓷纤维气凝胶复合材料，其特征在于：所述气凝胶粉体为SiO2气凝胶粉、TiO2气凝胶粉、Al2O3气凝胶、LiO气凝胶、石墨烯气凝胶等气凝胶材料中的一种或几种，气凝胶粉体的粒度在50目-1000目。
4.一种如权利要求1-3任一项陶瓷纤维气凝胶复合材料的制备方法，其特征在于：包括以下步骤：a. 气凝胶粉体的高温表面改性：称取一定量的气凝胶粉，放置于烘箱中，经过高温一段时间，得到高温表面改性的气凝胶粉；b. 陶瓷纤维气凝胶混合浆料配制：称取陶瓷纤维，称取气凝胶粉或步骤a中的改性后的气凝胶粉、有机结合剂、润湿剂、分散剂、增稠剂、去离子水放入搅拌釜中并搅拌，直至混合均匀并冷却至室温，制成陶瓷纤维气凝胶浆料；c.将步骤b中陶瓷纤维气凝胶浆料通过压板控制厚度，在烘干隧道中烘干，收卷或切片后得到陶瓷纤维气凝胶复合材料。
5.一种如权利要求1-3任一项陶瓷纤维气凝胶复合材料的制备方法，其特征在于：包括以下步骤：a. 气凝胶粉体的高温表面改性：称取一定量的气凝胶粉，放置于烘箱中，经过高温一段时间，得到高温表面改性的气凝胶粉；b. 陶瓷纤维气凝胶混合浆料配制：以下原料组分按重量份数计算，称取陶瓷纤维20-100份，称取气凝胶粉或步骤a中的改性后的气凝胶粉5-40份，有机结合剂10-30份，润湿剂1-15份，分散剂1-15份，增稠剂1-15份、去离子水60-100份放入搅拌釜中并搅拌，直至混合均匀并冷却至室温，制成陶瓷纤维气凝胶浆料；c. 将步骤b中陶瓷纤维气凝胶浆料通过压板控制厚度为0.2-20mm，在30-150℃的烘干隧道中烘0.5-2h，收卷或切片后得到陶瓷纤维气凝胶复合材料。
6.根据权利要求4所述的陶瓷纤维气凝胶复合材料的制备方法，其特征在于：所述步骤a中烘箱的温度为150-600℃，在烘箱中烘烤0.5-4h。
7.根据权利要求4所述的陶瓷纤维气凝胶复合材料的制备方法，其特征在于：所述步骤b中的搅拌釜的温度为25-85℃时，搅拌速率为1000-5000r/min，在搅拌釜中搅拌时间为0.5-2h。
8.根据权利要求4所述的陶瓷纤维气凝胶复合材料的制备方法，其特征在于：所述有机结合剂为丙烯酸乳液、EVA乳液，聚氨酯乳液等可以作为结合剂的有机树脂乳液中的一种或几种；所述润湿剂包括氨水、聚乙二醇、三乙醇胺、多元醇中的一种或几种。
9.根据权利要求4所述的陶瓷纤维气凝胶复合材料的制备方法，其特征在于：所述分散剂为5040分散剂、六偏磷酸钠、十二烷基苯磺酸钠、聚丙烯酸、聚丙烯酸钠、聚丙烯酸钙、十二烷基硫酸钠、聚乙烯醇等中的一种或几种。
10.根据权利要求4所述的陶瓷纤维气凝胶复合材料的制备方法，其特征在于：所述增稠剂为的羟乙基纤维素、羧甲基纤维素钠、锂基膨润土中的一种或多种。
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