CN115521158A - 一种高透气性陶瓷纤维过滤管的制备方法 - Google Patents
一种高透气性陶瓷纤维过滤管的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高透气性陶瓷纤维过滤管的制备方法，以莫来石短纤维为骨料，添加玻璃纤维和硅溶胶作为烧结助剂，采用压滤成型工艺得到陶瓷纤维滤管生坯，依次通过冷冻干燥和热处理得到高透气性的陶瓷纤维过滤管。两种不同性质烧结助剂的结合使用能有效改善湿法成型技术制备的陶瓷纤维过滤管性能。同时，冷冻干燥处理能够阻断硅溶胶中的纳米颗粒由于毛细作用力向陶瓷纤维过滤管表面迁移的路径，从而使制备得的陶瓷纤维过滤管的性质更均匀。为制备高通量的陶瓷纤维膜提供了参考。
Description
技术领域
本发明涉及一种高透气性陶瓷纤维过滤管的制备方法，属于膜材料的制备领域。
背景技术
陶瓷纤维膜是以耐高温陶瓷纤维，如氧化铝纤维、硅酸铝纤维、莫来石纤维等为骨料制备的一类陶瓷过滤材料。陶瓷纤维之间通过相互桥连形成的三维网络状多孔结构，赋予了陶瓷纤维膜孔隙率高、热稳定性好、气体渗透性高的特点，使其成为最具发展前景的陶瓷膜材料之一。传统的陶瓷纤维过滤管通常是以湿法真空抽滤成型工艺制备的，然而由于负压的抽吸作用，容易造成纤维多孔陶瓷材料内部不均的问题，从而对陶瓷纤维膜的透气性产生不利影响。因此，如何改善陶瓷纤维过滤管的制备工艺，以制备高透气性的陶瓷纤维过滤管十分重要。
模具成型技术（包括干压成型、凝胶注模、压滤成型等）具备操作简单、高效的特点，在陶瓷纤维膜制备领域有广泛的应用前景。干压成型技术制备得到的陶瓷纤维过滤材料，虽然强度明显提高，但是由于成型压力较大，多孔纤维骨架结构会被压实而导致气体渗透性损失较大。Xu等人[Ceramics International, 2017, 43(1): 228-233]采用凝胶注模法，将莫来石纤维和烧结助剂添加到叔丁醇基的凝胶预混溶液中，在引发剂的作用下有机单体聚合使料浆凝固，从而得到高强度的生坯。王树海等人[现代陶瓷技术, 1995(04):19-25]介绍了压滤成型工艺的工艺原理以及浆料体系、工艺参数对成品性能的影响，指出在受到压力和摩擦阻力的影响下，固相颗粒的团聚性降低，增加了浆料的均匀性；分散度高的浆料成型的固化层因渗透系数低而成型缓慢，可能引起密度梯度导致整体均匀性不佳；较大的成型压力可以得到更均匀的陶瓷成品，然而压力过高往往会造成脱模及干燥过程中的开裂，比较理想的压力范围为1-4 MPa。
液相烧结助剂具有粒径小、分散性好的特点，可以均匀包裹在骨料表面和交叉点处，有助于促进低温烧结过程，溶胶以及陶瓷前驱体溶液均可以用于辅助多孔陶瓷烧结过程。Hai等人[Refractories and Industrial Ceramics, 2012, 53: 157-161]以聚碳硅烷为前驱体溶液，干燥后，在1000 ℃不添加任何烧结助剂的条件下烧结得到了纯质的碳化硅多孔陶瓷，平均孔隙率为33.4%，断裂强度~16 MPa，平均孔径为2.275 μm。依靠纤维连接点处少量无机溶胶形成的颈部连接强度较低，不利于陶瓷纤维膜的长时间使用，而低熔点的固体烧结助剂能够有效强化多孔材料的机械性能。Xu等人[Ceramics International,2017, 43(1): 228-233]考察了不同的固体烧结助剂（硅粉末、二氧化硅粉末以及硼硅混合物）对制备的纤维多孔陶瓷材料机械性能的影响。结果表明，在1500 °C烧结下，以硼硅混合物作为烧结助剂制备得到的多孔陶瓷纤维材料抗压强度最高，约为2.08 MPa。
发明内容
本发明的目的是为改进现有技术的缺陷而提出结合固态和液态两种不同性质的烧结助剂代替常见的液态烧结助剂制备陶瓷纤维过滤管，通过不同性质烧结助剂的使用，解决了纤维连接点处颈部连接弱的不足；同时以冷冻干燥技术处理生坯，有效提高陶瓷纤维管的均一性，制备出高透气性的陶瓷纤维过滤管。
本发明的技术方案为：一种高透气性陶瓷纤维过滤管的制备方法，其具体步骤如下：A首先将一定质量分数的硅溶胶与水按一定体积比混合并进行充分搅拌，随后加入莫来石短纤维、玻璃纤维，其中硅溶胶、莫来石短纤维和玻璃纤维的质量比为（30-45）：（1.5-9）：1，加入有机成型助剂并搅拌一定时间，搅拌一定时间后迅速注入压滤模具中，缓慢施加压力至水滤出后得到陶瓷纤维滤管生坯；B将脱模后的生坯放入冰箱冷冻12-24 h，再置于-60℃至-20 ℃环境中干燥12-24 h，随后经煅烧过程得到陶瓷纤维过滤管。
优选所述的硅溶胶的质量分数为20 wt%-40 wt%，其与水混合的体积比为1：（1.5-9）；莫来石短纤维的长径比为50-200；有机成型助剂为聚乙烯醇（PVA）溶液，浓度为8 wt%-12 wt%，添加量为莫来石短纤维和玻璃纤维总质量的60%-80%。
优选所述的制膜液搅拌时间为3-10 min。
优选所述的压滤成型过程中的压力为2-4 MPa。
优选所述的煅烧过程为：将生坯在800-1400 ℃下煅烧，升温速率和降温速率控制在0.5-3 ℃/min，保温时间为1-3 h。
本发明制得的陶瓷纤维过滤管平均孔径为34.1-35.2 μm，孔隙率为74-75.2％，气体渗透率为642-787 m3·m-2·h-1·kPa-1，抗弯强度为1.86-2.88 MPa。
有益效果：
本发明通过结合硅溶胶和玻璃纤维两种性质不同的烧结助剂，以及通过煅烧前对生坯进行冷冻干燥处理，提高陶瓷纤维过滤管的均匀性，成功制备出透气性良好的陶瓷纤维过滤管，烧结温度的降低也降低了制备陶瓷纤维过滤管的烧结能耗。两种不同性质烧结助剂的结合使用能有效改善湿法成型技术制备的陶瓷纤维过滤管性能。同时，冷冻干燥处理能够阻断硅溶胶中的纳米颗粒由于毛细作用力向陶瓷纤维过滤管表面迁移的路径，从而使制备得的陶瓷纤维过滤管的性质更均匀。为制备高通量的陶瓷纤维膜提供了参考。
附图说明
图1是实例3中所使用的玻璃纤维的微观形貌SEM图。
图2是实例3中制备的陶瓷纤维滤管的宏观形貌图。
图3是实例3中制备的陶瓷纤维过滤管断面形貌、外表面以及中间局部放大的SEM图。
图4是实例3中制备的陶瓷纤维过滤管断裂后表面和断面的SEM图。
图5是实例3中制备的陶瓷纤维过滤管的孔径分布图。
图6是实例3中制备的陶瓷纤维过滤管与其他研究工作制备的陶瓷纤维膜的达西渗透率与孔隙度以及孔径之间的关系对比图。
具体实施方式
实施例1
首先将团聚的莫来石短纤维置于水中进行搅拌分散，过滤掉多余的水分后置于120 °C烘箱内烘干，得到分散性良好的短纤维（长径比为50）。然后将40 wt%硅溶胶与水按一定体积比混合并充分搅拌，其中硅溶胶：水=1：9，随后加入莫来石短纤维和玻璃纤维，使硅溶胶、莫来石短纤维和玻璃纤维的质量比为30：1.5：1，继续添加质量为上述两种纤维总质量60%的12 wt%PVA溶液，搅拌10 min后迅速注入压滤模具中，缓慢施加压力至2 MPa，待水滤出后得到陶瓷纤维滤管生坯，将脱模后的生坯放入冰箱冷冻24 h，置于-60 ℃真空冷冻干燥机中干燥24 h，然后在空气气氛下以0.5 ℃/min的速率升温至800 ℃并保温3 h，制备出的陶瓷纤维过滤管平均孔径为34.1 μm，孔隙率约为74 %，气体渗透性为642 m3·m-2·h-1·kPa-1，平均抗弯强度约为1.86 MPa。
实施例2
首先将团聚的莫来石短纤维置于水中进行搅拌分散，过滤掉多余的水分后置于120 °C烘箱内烘干，得到分散性良好的短纤维（长径比为200）。然后将35 wt%硅溶胶与水按一定体积比混合并充分搅拌，其中硅溶胶：水=1：4，随后加入莫来石短纤维和玻璃纤维，使硅溶胶、莫来石短纤维和玻璃纤维的质量比为35：2.33：1，继续添加质量为上述两种纤维总质量70%的10 wt%PVA溶液，搅拌8 min后迅速注入压滤模具中，缓慢施加压力至3 MPa，待水滤出后得到陶瓷纤维滤管生坯，将脱模后的生坯放入冰箱冷冻12 h，置于-50 ℃真空冷冻干燥机中干燥24 h，然后在空气气氛下以2 ℃/min的速率升温至1000 ℃并保温2 h，制备出的陶瓷纤维过滤管平均孔径为34.6 μm，孔隙率约为74.6 %，气体渗透性为680 m3·m-2·h-1·kPa-1，平均抗弯强度约为2.34 MPa。
实施例3
首先将团聚的莫来石短纤维置于水中进行搅拌分散，过滤掉多余的水分后置于120 °C烘箱内烘干，得到分散性良好的短纤维（长径比为100）。然后将30 wt%硅溶胶与水按一定体积比混合并充分搅拌，其中硅溶胶：水=1：2.33，随后加入莫来石短纤维和玻璃纤维，使硅溶胶、莫来石短纤维和玻璃纤维的质量比为40：4：1，继续添加质量为上述两种纤维总质量75%的10wt %PVA溶液，搅拌5 min后迅速注入压滤模具中，缓慢施加压力至3 MPa，待水滤出后得到陶瓷纤维滤管生坯，将脱模后的生坯放入冰箱冷冻24 h，置于-40 ℃真空冷冻干燥机中干燥12 h，然后在空气气氛下以2 ℃/min的速率升温至1200 ℃并保温2 h，制备出的陶瓷纤维过滤管平均孔径为35.2 μm，孔隙率约为75 %，气体渗透性为787 m3·m-2·h-1·kPa-1，平均抗弯强度约为2.68 MPa。
表1是本实例中制备的莫来石纤维管与文献中碳化硅颗粒陶瓷管的性能对比，莫来石纤维管具有明显的高透气性优势。图1是本实例中使用的玻璃纤维的微观形貌SEM图，玻璃纤维直径约为10 μm，平均长度约为60 μm。图2是本实例中制备的陶瓷纤维滤管的宏观形貌图，纤维滤管的长度80 mm，外径为39 mm，壁厚为12 mm。图3是本实例中制备的陶瓷纤维过滤管断面形貌、外表面以及中间局部放大的SEM图，陶瓷纤维过滤管中烧结助剂分布均匀。图4是本实例中制备的陶瓷纤维过滤管断裂后表面和断面的SEM图，大量的纤维延伸到断裂面外侧，结合烧结助剂在陶瓷纤维材料内部分散的均匀性，证明了纤维的桥连机制在断裂过程中起一定作用。图5是本实例中制备的陶瓷纤维过滤管的孔径分布图，孔径分布集中，平均孔径约为35.2 μm。图6是本实例中制备的陶瓷纤维过滤管与其他研究工作制备的陶瓷纤维膜的达西渗透率与孔隙度以及孔径之间的关系，可见本工作制备的陶瓷纤维过滤管透气性优于平均水平。
实施例4
首先将团聚的莫来石短纤维置于水中进行搅拌分散，过滤掉多余的水分后置于120 °C烘箱内烘干，得到分散性良好的短纤维（长径比为150）。然后将20 wt%硅溶胶与水按一定体积比混合并充分搅拌，其中硅溶胶：水=1：1.5，随后加入莫来石短纤维和玻璃纤维，使硅溶胶、莫来石短纤维和玻璃纤维的质量比为45：9：1，继续添加质量为上述两种纤维总质量80%的8 wt%PVA溶液，搅拌3 min后迅速注入压滤模具中，缓慢施加压力至4 MPa，待水滤出后得到陶瓷纤维滤管生坯，将脱模后的生坯放入冰箱冷冻12 h，置于-20 ℃真空冷冻干燥机中干燥24 h，然后在空气气氛下以3 ℃/min的速率升温至1400 ℃并保温1 h，制备出的陶瓷纤维过滤管平均孔径为34.8 μm，孔隙率约为75.2 %，气体渗透性为740 m3·m-2·h-1·kPa-1，平均抗弯强度约为2.88 MPa。
表1 实例3中制备的莫来石纤维管与文献中碳化硅颗粒陶瓷管的性能对比
Claims (6)
1.一种高透气性陶瓷纤维过滤管的制备方法，其特征在于，具体操作步骤如下：
A、将一定质量分数的硅溶胶与水按体积比混合后加入莫来石短纤维与玻璃纤维，其中硅溶胶、莫来石短纤维和玻璃纤维的质量比为（30-45）：（1.5-9）：1，加入有机成型助剂并搅拌一定时间，随后通过压滤成型法得到陶瓷纤维滤管生坯；选用的莫来石短纤维长径比为50-200；
B、将脱模后的生坯放入冰箱冷冻12-24 h，再置于-60 ℃至-20 ℃环境中干燥12-24h，随后经煅烧过程得到陶瓷纤维过滤管。
2.根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：步骤A中所述硅溶胶的质量分数为20 wt%-40 wt%，其与水混合的体积比为1：（1.5-9）。
3.根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：步骤A中所述的有机成型剂为聚乙烯醇（PVA）溶液，浓度为8 wt%-12 wt%，添加量为莫来石短纤维和玻璃纤维总质量的60%-80%。
4.根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：制膜液搅拌时间为3-10 min。
5.根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：压滤成型过程中的压力为2-4 MPa。
6.根据权利要求1所述的一种高透气性陶瓷纤维过滤管的制备方法，其特征在于：煅烧过程为将生坯在800-1400 ℃下煅烧，升温速率和降温速率控制在0.5-3 ℃/min，保温时间为1-3 h。
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