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CN109400132A - 一种低成本高强度氧化铝陶瓷膜支撑体及其制备方法 - Google Patents

一种低成本高强度氧化铝陶瓷膜支撑体及其制备方法 Download PDF

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CN109400132A
CN109400132A CN201811275869.1A CN201811275869A CN109400132A CN 109400132 A CN109400132 A CN 109400132A CN 201811275869 A CN201811275869 A CN 201811275869A CN 109400132 A CN109400132 A CN 109400132A
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aluminium oxide
film support
oxide ceramics
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powder
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余阳
何文龙
胡鹏飞
和丞
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Donghua University
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Abstract

本发明公开了一种低成本高强度氧化铝陶瓷膜支撑体，其特征在于，其原料为两种α‑Al2O3粉末的混合粉末，其中一种α‑Al2O3粉末的中位径为10～30μm，另一种α‑Al2O3粉末的中位径为1～5μm。制备方法为：将混合粉末与溶剂、粘结剂、造孔剂、烧结助剂、消泡剂混合形成浆料；将浆料脱除部分溶剂后形成泥料，泥料通过模具挤压成型形成生坯；生坯经过干燥固化形成煅烧胚品；煅烧胚品在氧气气氛中烧结成为氧化铝陶瓷膜支撑体。本发明所制得的氧化铝陶瓷膜支撑体拥有比传统商品化的氧化铝陶瓷膜支撑体更低的制备成本和更高的抗压强度。

Description

一种低成本高强度氧化铝陶瓷膜支撑体及其制备方法
技术领域
本发明涉及一种陶瓷膜支撑体及其制备方法，具体涉及一种低成本高强度氧 化铝陶瓷膜支撑体及其制备方法。
背景技术
膜分离技术是一门经济高效的分离技术。由于其具备分离、浓缩、纯化和精 制的功能，又兼具高效、节能、环保、使用简便、耗能低等一系列优点，被广泛 应用于食品、医药、生物、环保、化工、能源、水处理等领域，已成为当今分离 科学中最重要的手段之一。其中，陶瓷膜技术始于二战时期的原子弹计划，随 着材料技术的发展及其自身优势的普及，陶瓷膜的制备技术正在成为各国科技发 展的热点和重点。陶瓷膜是一类以无机材料经特殊工艺制备而形成的非对称膜， 相较于有机膜具有更好的化学稳定性、耐酸耐碱、耐有机溶剂、耐菌、耐高温、 机械强度高、分离过程简单、操作维护简便、使用寿命长等众多优势，得到了广 泛的重视与应用。
在现有的技术中，商品化的氧化铝陶瓷膜支撑体通常需要在高温条件 (1700℃以上)下长时间(在烧结温度下保温时间通常≥2h)烧结而成，这大大 增加了氧化铝陶瓷膜支撑体的制备成本，实现陶瓷膜的低成本化生产，结合构建 面向应用过程的膜材料设计与制备方法，解决陶瓷膜推广应用的瓶颈问题，这是 未来的一大发展趋势。同时因为强度不足，支撑体需要较厚的厚度，因此其通道 内的膜面积较小，导致陶瓷膜过滤设备的集成度低，设备造价贵，运行费用高， 限制了陶瓷膜在水处理、油水分离等领域的应用。
发明内容
本发明所要解决的问题是：提供一种具有高强度、高纯水通量、低的制备成 本的氧化铝陶瓷膜支撑体及其制造方法。
为了解决上述问题，本发明的技术方案如下：
一种低成本高强度氧化铝陶瓷膜支撑体，其特征在于，其原料为两种α -Al2O3粉末的混合粉末，其中一种α-Al2O3粉末的中位径为10～30μm，另一种 α-Al2O3粉末的中位径为1～5μm。
优选地，两种所述α-Al2O3粉末的质量比为1:1。
本发明还提供了一种上述低成本高强度氧化铝陶瓷膜支撑体的制备方法，其 特征在于，包括以下步骤：
步骤1)：将混合粉末与溶剂、粘结剂、造孔剂、烧结助剂、消泡剂混合形 成浆料；
步骤2)：将浆料脱除部分溶剂后形成泥料，泥料通过模具挤压成型形成生 坯；
步骤3)：生坯经过干燥固化形成煅烧胚品；
步骤4)：煅烧胚品在氧气气氛中烧结成为氧化铝陶瓷膜支撑体。
优选地，所述步骤1)中溶剂的用量为混合粉末重量的20％-30％；溶剂采用 水。
优选地，所述步骤1)中的粘结剂采用聚合度1750±50的聚乙烯醇，造孔 剂采用可溶性淀粉，烧结助剂采用二氧化钛、氧化镁、二氧化锰、氧化铜和硅酸 钠中的一种或几种，三者的总用量为混合粉末重量的10-15％。
更优选地，当所述烧结助剂为二氧化钛、氧化镁、二氧化锰、氧化铜或硅酸 钠时，其对应的用量依次分别为混合粉体重量的2％、0.5％、1.5％、1.5％、4％。 优选采用四元烧结助剂(0.5％MgO+2％TiO2+1.5％MnO2+1.5％CuO)来降低烧结 温度，增大抗压强度。其中MgO可在较低的温度下形成液相，液相在颗粒间流 动，浸润并包围粉体颗粒，使粉体颗粒产生竞相连接，使传质机理由固相扩散转 变为液相扩散，形成玻璃相从而降低烧结温度。TiO2、MnO2、CuO利用粒子半 径与Al3+的差异，加上本身是变价离子，活化了Al2O3晶体的晶格，产生中间固 溶体，从而降低烧结温度，提高支撑体的抗压强度。所制备的陶瓷膜支撑体直径 在7.8-8.2cm，厚度在5-7mm，纯水通量在8000-9000L·m-2·h-1·bar-1，孔隙率 在30％-38％，抗压强度在20-50MPa。
优选地，所述步骤1)中的消泡剂为有机硅消泡剂，其用量为混合粉末重量 的1％-5％，优选为5％。
优选地，所述步骤3)中的干燥固化方式采用自然干燥法，在室温下干燥固 化不少于1天。
优选地，所述步骤4)中烧结的温度为1450℃，保温时间为0.5-2h。本发明 制备的氧化铝陶瓷膜支撑体采用特定粒度级配的α-Al2O3搭配而成，在1450℃ 的低温中短时间(≤2h)烧结，综合考虑烧结成本及支撑的整体性能，优选烧结 保温时间为1h，制成陶瓷膜支撑体。
本发明所制得的氧化铝陶瓷膜支撑体拥有比传统商品化的氧化铝陶瓷膜支 撑体更低的制备成本和更高的抗压强度。
具体实施方式
为使本发明更明显易懂，兹以优选实施例，并作详细说明如下。
实施例1
一种低成本高强度氧化铝陶瓷膜支撑体的制备方法：
1)将中位径为10μm的α-Al2O3粉末100g、中位径为3μm的α-Al2O3粉 末100g、硅酸钠8g，取适量水溶解，形成硅酸钠溶液；
2)可溶性淀粉12g，在80℃水中溶解形成溶胶；
3)PVA(聚合度1750±50)1.2g，在85℃水中溶解完全；
4)将上述各物质与MgO 1g，TiO2 8g混合后，加入45mL的水，用均质搅 拌机以1800r/min的速度搅拌30min，使浆料混合均匀，再在浆料中加入10g有 机硅消泡剂并在超声+抽滤装置中放置30min脱除气泡；
5)将脱泡后的浆料在100℃烘箱中脱水1h，形成泥料，将泥料以每份100g 用挤压式圆形模具中挤压形成生坯，在室温条件下干燥1天；
6)在空气气氛下，放于马弗炉中以3℃/min的速率从50℃升高至200℃， 并保温30min；以5℃/min的速率从200℃升高至1000℃，保温30min；以3℃/min 的速率从1000℃升高至1450℃，并保温2h。
得到的氧化铝陶瓷膜支撑体直径为8cm，厚度为4mm，纯水通量为8482 L·m-2·h-1·bar-1，孔隙率为31.3％，抗压强度为27.3MPa。
实施例2
本实施例与实施例1的不同之处在于，步骤4)中TiO2用CuO 3g代替。
得到的氧化铝陶瓷膜支撑体直径为7.8cm，厚度为5mm，纯水通量为8342 L·m-2·h-1·bar-1，孔隙率为35.2％，抗压强度为20.1MPa。
实施例3
本实施例与实施例1的不同之处在于，步骤4)中TiO2用MnO2 3g代替。
得到的氧化铝陶瓷膜支撑体直径为8.3cm，厚度为4mm，纯水通量为8791 L·m-2·h-1·bar-1，孔隙率为30.0％，抗压强度为15.3MPa。
实施例4
本实施例与实施例1的不同之处在于，步骤4)中烧结助剂增加了CuO 3g。
得到的氧化铝陶瓷膜支撑体直径为8.1cm，厚度为5mm，纯水通量为8123 L·m-2·h-1·bar-1，孔隙率为33.4％，抗压强度为35.6MPa。
实施例5
本实施例与实施例1的不同之处在于，步骤4)中烧结助剂增加了MnO2 3g。
得到的氧化铝陶瓷膜支撑体直径为7.9cm，厚度为4mm，纯水通量为8319 L·m-2·h-1·bar-1，孔隙率为38.3％，抗压强度为30.1MPa。
实施例6
本实施例与实施例1的不同之处在于，步骤4)中烧结助剂增加了CuO 3g、 MnO23g。
得到的氧化铝陶瓷膜支撑体直径为8.0cm，厚度为5mm，纯水通量为8521 L·m-2·h-1·bar-1，孔隙率为35.8％，抗压强度为45.9MPa。
实施例7
本实施例与实施例6的不同之处在于，所述步骤6)中升至1450℃后保温 0.5h。
得到的氧化铝陶瓷膜支撑体直径为8.0cm，厚度为5mm，纯水通量为9146 L·m-2·h-1·bar-1，孔隙率为38.5％，抗压强度为25.2MPa。
实施例8
本实施例与实施例6的不同之处在于，所述步骤6)中升至1450℃后保温1h。
得到的氧化铝陶瓷膜支撑体直径为8.3cm，厚度为4mm，纯水通量为8945 L·m-2·h-1·bar-1，孔隙率为36.9％，抗压强度为38.4MPa。
实施例9
本实施例与实施例6的不同之处在于，所述步骤6)中升至1450℃后保温 1.5h。
得到的氧化铝陶瓷膜支撑体直径为7.8cm，厚度为5mm，纯水通量为8672 L·m-2·h-1·bar-1，孔隙率为37.1％，抗压强度为42.3MPa。

Claims (9)

1.一种低成本高强度氧化铝陶瓷膜支撑体，其特征在于，其原料为两种α-Al2O3粉末的混合粉末，其中一种α-Al2O3粉末的中位径为10～30μm，另一种α-Al2O3粉末的中位径为1～5μm。
2.如权利要求1所述的低成本高强度氧化铝陶瓷膜支撑体，其特征在于，两种所述α-Al2O3粉末的质量比为1:1。
3.一种权利要求1或2所述的低成本高强度氧化铝陶瓷膜支撑体的制备方法，其特征在于，包括以下步骤：
步骤1)：将混合粉末与溶剂、粘结剂、造孔剂、烧结助剂、消泡剂混合形成浆料；
步骤2)：将浆料脱除部分溶剂后形成泥料，泥料通过模具挤压成型形成生坯；
步骤3)：生坯经过干燥固化形成煅烧胚品；
步骤4)：煅烧胚品在氧气气氛中烧结成为氧化铝陶瓷膜支撑体。
4.如权利要求3所述的低成本高强度氧化铝陶瓷膜支撑体的制备方法，其特征在于，所述步骤1)中溶剂的用量为混合粉末重量的20％-30％；溶剂采用水。
5.如权利要求3所述的低成本高强度氧化铝陶瓷膜支撑体的制备方法，其特征在于，所述步骤1)中的粘结剂采用聚合度1750±50的聚乙烯醇，造孔剂采用可溶性淀粉，烧结助剂采用二氧化钛、氧化镁、二氧化锰、氧化铜和硅酸钠中的一种或几种，三者的总用量为混合粉末重量的10-15％。
6.如权利要求5所述的低成本高强度氧化铝陶瓷膜支撑体的制备方法，其特征在于，当所述烧结助剂为二氧化钛、氧化镁、二氧化锰、氧化铜或硅酸钠时，其对应的用量依次分别为混合粉体重量的2％、0.5％、1.5％、1.5％、4％。
7.如权利要求3所述的低成本高强度氧化铝陶瓷膜支撑体的制备方法，其特征在于，所述步骤1)中的消泡剂为有机硅消泡剂，其用量为混合粉末重量的1％-5％。
8.如权利要求3所述的低成本高强度氧化铝陶瓷膜支撑体的制备方法，其特征在于，所述步骤3)中的干燥固化方式采用自然干燥法，在室温下干燥固化不少于1天。
9.如权利要求3所述的低成本高强度氧化铝陶瓷膜支撑体的制备方法，其特征在于，所述步骤4)中烧结的温度为1450℃，保温时间为0.5-2h。
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