CN107805064A - 一种纤维增强耐高温镁铝尖晶石气凝胶的制备方法 - Google Patents
一种纤维增强耐高温镁铝尖晶石气凝胶的制备方法 Download PDFInfo
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Abstract
本发明属于纳米多孔隔热材料的制备工艺领域，涉及一种纤维增强耐高温镁铝尖晶石气凝胶的制备方法。本发明使用纤维浸渍法，将气凝胶和纤维充分复合，克服了气凝胶力学强度弱的缺点，所制得的产品具有柔性。制备方法是将镁源溶解制得镁源溶液，将铝源溶解制得铝源溶液，将镁源溶液和铝源溶液充分混合，借助环氧化物催化剂，搅拌得到镁铝溶胶，将纤维浸渍在镁铝溶胶中，经溶胶‑凝胶、老化以及干燥得到纤维增强的尖晶石气凝胶前驱体，在马弗炉中进行空气氛热处理，最终制得一种耐高温纤维增强镁铝尖晶石气凝胶。该制备方法用料成本低廉，工艺稳定，易于实现批量生产。
Description
技术领域
本发明属于纳米多孔隔热材料的制备工艺领域，涉及一种纤维增强耐高温镁铝尖晶石气凝胶复合材料的制备方法。
背景技术
气凝胶是一种由纳米粒子或高聚物分子相互聚集而成的纳米多孔网络结构，具有低热导、高孔隙率、高比表面积等特点，在隔热、吸附、光催化等领域有着广阔的应用前景。镁铝尖晶石是一种性能优异的耐火材料，具有良好的抗侵蚀，腐蚀、剥落能力强，抗渣性能好，抗磨蚀能力，热震稳定性好，耐高温等性能特点。将其做成气凝胶，可在维持以上优点的基础上提高其比表面积、孔隙率及隔热性能。
发明内容
本发明的目的是为了改进现有技术的不足而提供一种纤维增强耐高温镁铝尖晶石气凝胶复合材料的制备方法。本发明使用纤维毡作为基体，结合纤维浸渍工艺，制备出纤维增强耐高温镁铝尖晶石气凝胶。镁铝尖晶石气凝胶充分填充于纤维骨架中，有效提升了基体材料隔热效果，同时使气凝胶具备抗压折能力，力学强度大大提升。该材料可进行机械加工，以适应不同使用环境要求被加工成各种异形件。
本发明的技术方案为：纤维增强耐高温镁铝尖晶石气凝胶的制备方法，具体步骤如下：
(1)溶胶的制备
将镁源、乙醇、去离子水按照一定比例放入容器，搅拌均匀，制得镁源溶液；将铝源、乙醇、去离子水按照一定比例放入容器，搅拌均匀，制得铝源溶液；将镁源溶液和铝源溶液按比例混合，加入催化剂环氧化物，搅拌均匀，制得水解的镁铝二元溶胶；
(2)浸渍法复合纤维毡
将纤维毡基体放在容器中，将步骤(1)中的镁铝二元溶胶倾倒入容器中，以没过纤维毡基体为准，待其凝胶；
(3)凝胶的老化
待步骤(2)中样品凝胶后，将纤维毡基体外的湿凝胶剥离后浸泡在老化液中，放入烘箱，进行老化和溶剂置换过程；
(4)干燥处理
将步骤(3)老化过后的纤维毡复合湿凝胶进行干燥处理，从而得到纤维增强耐高温镁铝尖晶石气凝胶前驱体材料；
(5)热处理
将步骤(4)制得的气凝胶前驱体材料放入马弗炉中，在空气氛围下进行热处理，最终制得纤维增强耐高温镁铝尖晶石气凝胶；
其中：步骤(1)中的镁源、乙醇、去离子水的摩尔比为1：(7～25)：(35～60)，铝源、乙醇、去离子水的摩尔比为1：(3～20)：(20～40)；镁源与铝源的摩尔比为1:(1～5)；催化剂环氧丙烷与镁源的摩尔比为(8～16)：1。
优选步骤(1)中所述的镁源为氯化镁、硝酸镁或硫酸镁中的一种或几种。
优选步骤(1)中所述的铝源为氯化铝、硝酸铝、仲丁醇铝或异丙醇铝中的一种或几种。
优选步骤(1)中制备镁源溶液和铝源溶液的搅拌速度为200～500rpm，搅拌时间0.5～1h；镁源溶液与铝源溶液混合后搅拌速度为300～450rpm，搅拌时间0.1～0.2h；搅拌温度均为20～50℃。
优选步骤(2)中所使用的纤维毡基材为石英纤维、氧化铝纤维或玻璃纤维中的一种。
优选步骤(3)中的老化液为乙醇、甲醇或丙酮中的一种或几种。
优选步骤(3)中老化温度为20～40℃；浸泡时间为48～72h，期间每10～12h更换一次老化液。
优选步骤(4)中的干燥方法为常压干燥、冷冻干燥、CO2超临界干燥或乙醇超临界干燥中的一种。
优选步骤(5)中的热处理温度为400～1200℃，升温速度为2～8℃/min，热处理时间为2～6h。
本发明所制得的纤维增强耐高温镁铝尖晶石气凝胶密度为0.13-0.32g/cm2，常温热导率在0.028～0.045W·m-1·K-1之间。
本发明使用纤维浸渍工艺，将气凝胶与纤维毡充分复合，经过空气氛围内热处理制得纤维增强耐高温镁铝尖晶石气凝胶。既克服气凝胶材料质脆地缺点，又使纤维毡的隔热性能和耐温性能有了进一步提升，可用于钢铁冶炼、水泥回转窑和玻璃工业窑炉保温结构中。
有益效果：
(1)相比较于传统的纤维毡增强SiO2气凝胶样品，本发明制备得到的镁铝尖晶石气凝胶具有更好的耐温性能。
(2)相比较于尖晶石材料，本发明所制备的镁铝尖晶石气凝胶具有更高的气孔率，隔热性能好，导热系数更低。
附图说明
图1是实例1所制备的纤维增强耐高温镁铝尖晶石气凝胶的实物图。
具体实施方式
下面结合实例对本发明作进一步说明，但保护范围并不限于此。
实例1
在烧杯中加入20.33g六水合氯化镁(0.1mol)、40.9mL乙醇(0.7mol)、63mL水(3.5mol)，在20℃下以200rpm的转速搅拌0.5h；在烧杯中加入24.14g六水合氯化铝(0.1mol)、17.5mL乙醇(0.3mol)、36mL水(2mol)，在20℃下以200rpm的转速搅拌0.5h，。将上述两份溶液倒入同一烧杯，加入56mL环氧丙烷(0.8mol)，在20℃下以300rpm的转速搅拌0.1h制得镁铝二元溶胶。将石英纤维针刺毡放入容器，将镁铝二元溶胶倒入容器中，以没过基材为准。待其凝胶后，将纤维毡基体外的湿凝胶剥离后浸泡在乙醇老化液中，放入烘箱，进行老化和溶剂置换过程，老化温度20℃，浸泡时间为48小时，期间每10h换一次乙醇老化液。将复合凝胶放入反应釜中进行乙醇超临界干燥，干燥温度设置为260℃，温度升上去后，压力维持在10MPa，恒温恒压下状态下维持3h，然后保持匀速在30min内将气体放出，等反应釜温度降下之后取出容器，得到纤维增强镁铝尖晶石气凝胶前驱体。将该前驱体放入马弗炉进行空气热处理，其中煅烧温度为400℃，升温速度为2℃/min，热处理时间为2h，最终制得纤维增强耐高温镁铝尖晶石气凝胶。所制备的材料密度为0.13g/cm3，常温热导率0.030W·m-1·K-1。所制备的纤维增强耐高温镁铝尖晶石气凝胶的实物图如图1所示。
实例2
在烧杯中加入2.56g六水合硝酸镁(0.01mol)、14.6mL乙醇(0.25mol)、10.8mL水(0.6mol)，在50℃下以500rpm的转速搅拌1h；在烧杯中加入18.76g九水合硝酸铝(0.05mol)、58.4mL乙醇(1mol)、36mL水(2mol)，在50℃下以500rpm的转速搅拌2h，。将上述两份溶液倒入同一烧杯，加入11.96mL环氧丙烷(0.16mol)，在50℃下以450rpm的转速搅拌0.2h制得镁铝二元溶胶。将氧化铝纤维毡放入容器，将镁铝二元溶胶倒入容器中，以没过基材为准。待其凝胶后，将纤维毡基体外的湿凝胶剥离后浸泡在甲醇老化液中，放入烘箱，进行老化和溶剂置换过程，老化温度40℃，浸泡时间为72小时，期间每12h换一次甲醇老化液。将复合凝胶放入反应釜中进行CO2超临界干燥，干燥温度设置为50℃，温度升上去后，压力维持在10MPa，恒温恒压下状态下维持8h，关闭进气并将反应釜内压力释放后，得到纤维增强镁铝尖晶石气凝胶前驱体。将该前驱体放入马弗炉进行空气热处理，其中煅烧温度为1200℃，升温速度为8℃/min，热处理时间为6h，最终制得纤维增强耐高温镁铝尖晶石气凝胶。所制备的材料密度为0.21g/cm3，常温热导率0.028W·m-1·K-1。
实例3
在烧杯中加入13.84g一水合硫酸镁(0.1mol)、116.8mL乙醇(2mol)、72mL水(4mol)，在50℃下以400rpm的转速搅拌0.6h；在烧杯中加入49.26g仲丁醇铝(0.2mol)、116.8mL乙醇(2mol)、108mL水(6mol)，在50℃下以400rpm的转速搅拌0.6h，。将上述两份溶液倒入同一烧杯，加入70mL环氧丙烷(1mol)，在50℃下以400rpm的转速搅拌0.15h制得镁铝二元溶胶。将玻璃纤维毡放入容器，将镁铝二元溶胶倒入容器中，以没过基材为准。待其凝胶后，将纤维毡基体外的湿凝胶剥离后浸泡在丙酮老化液中，放入烘箱，进行老化和溶剂置换过程，老化温度30℃，浸泡时间为60小时，期间每11h换一次丙酮老化液。使用乙醇洗涤后在常温下自然干燥24h，最后在60℃烘箱中干燥12h，得到纤维增强镁铝尖晶石气凝胶前驱体。将该前驱体放入马弗炉进行空气热处理，其中煅烧温度为1000℃，升温速度为4℃/min，热处理时间为4h，最终制得纤维增强耐高温镁铝尖晶石气凝胶。所制备的材料密度为0.32g/cm3，常温热导率0.045W·m-1·K-1。
实例4
在烧杯中加入20.33g六水合氯化镁(0.1mol)、58.4mL乙醇(1mol)、90mL水(5mol)，在40℃下以350rpm的转速搅拌1h；在烧杯中加入61.27g异丙醇铝(0.3mol)、175.2mL乙醇(3mol)、162mL水(9mol)，在40℃下以350rpm的转速搅拌1h，。将上述两份溶液倒入同一烧杯，加入56mL环氧丙烷(0.8mol)，在40℃下以450rpm的转速搅拌0.12h制得镁铝二元溶胶。将石英纤维针刺毡放入容器，将镁铝二元溶胶倒入容器中，以没过基材为准。待其凝胶后，将纤维毡基体外的湿凝胶剥离后浸泡在乙醇丙酮混合液中，放入烘箱，进行老化和溶剂置换过程，老化温度25℃，浸泡时间为64小时，期间每12h换一次乙醇丙酮混合液。使用液氮将复合湿凝胶进行急冷处理，然后在50Pa的冷冻干燥机中干燥24h，得到纤维增强镁铝尖晶石气凝胶前驱体。将该前驱体放入马弗炉进行空气热处理，其中煅烧温度为800℃，升温速度为6℃/min，热处理时间为5h，最终制得纤维增强耐高温镁铝尖晶石气凝胶。所制备的材料密度为0.28g/cm3，常温热导率0.035W·m-1·K-1。
Claims (9)
1.纤维增强耐高温镁铝尖晶石气凝胶的制备方法，具体步骤如下：
(1)溶胶的制备
将镁源、乙醇、去离子水按照一定比例放入容器，搅拌均匀，制得镁源溶液；将铝源、乙醇、去离子水按照一定比例放入容器，搅拌均匀，制得铝源溶液；将镁源溶液和铝源溶液按比例混合，加入催化剂环氧化物，搅拌均匀，制得水解的镁铝二元溶胶；
(2)浸渍法复合纤维毡
将纤维毡基体放在容器中，将步骤(1)中的镁铝二元溶胶倾倒入容器中，以没过纤维毡基体为准，待其凝胶；
(3)凝胶的老化
待步骤(2)中样品凝胶后，将纤维毡基体外的湿凝胶剥离后浸泡在老化液中，放入烘箱，进行老化和溶剂置换过程；
(4)干燥处理
将步骤(3)老化过后的纤维毡复合湿凝胶进行干燥处理，从而得到纤维增强耐高温镁铝尖晶石气凝胶前驱体材料；
(5)热处理
将步骤(4)制得的气凝胶前驱体材料放入马弗炉中，在空气氛围下进行热处理，最终制得纤维增强耐高温镁铝尖晶石气凝胶；
其中：步骤(1)中的镁源、乙醇、去离子水的摩尔比为1：(7～25)：(35～60)，铝源、乙醇、去离子水的摩尔比为1：(3～20)：(20～40)；镁源与铝源的摩尔比为1:(1～5)；催化剂环氧丙烷与镁源的摩尔比为(8～16)：1。
2.根据权利要求1所述的制备方法，其特征在于步骤(1)中所述的镁源为氯化镁、硝酸镁或硫酸镁中的一种或几种。
3.根据权利要求1所述的制备方法，其特征在于步骤(1)中所述的铝源为氯化铝、硝酸铝、仲丁醇铝或异丙醇铝中的一种或几种。
4.根据权利要求1所述的制备方法，其特征在于步骤(1)中制备镁源溶液和铝源溶液的搅拌速度为200～500rpm，搅拌时间0.5～1h；镁源溶液与铝源溶液混合后搅拌速度为300～450rpm，搅拌时间0.1～0.2h；搅拌温度均为20～50℃。
5.根据权利要求1所述的制备方法，其特征在于步骤(2)中所使用的纤维毡基材为石英纤维、氧化铝纤维或玻璃纤维中的一种。
6.根据权利要求1所述的制备方法，其特征在于步骤(3)中的老化液为乙醇、甲醇或丙酮中的一种或几种。
7.根据权利要求1所述的制备方法，其特征在于步骤(3)中老化温度为20～40℃；浸泡时间为48～72h，期间每10～12h更换一次老化液。
8.根据权利要求1所述的制备方法，其特征在于步骤(4)中的干燥方法为常压干燥、冷冻干燥、CO2超临界干燥或乙醇超临界干燥中的一种。
9.根据权利要求1所述的制备方法，其特征在于步骤(5)中的热处理温度为400～1200℃，升温速度为2～8℃/min，热处理时间为2～6h。
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