CN108117379A - 一种高孔隙率多孔陶瓷膜支撑体及其制备方法 - Google Patents

一种高孔隙率多孔陶瓷膜支撑体及其制备方法 Download PDF

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CN108117379A
CN108117379A CN201711252766.9A CN201711252766A CN108117379A CN 108117379 A CN108117379 A CN 108117379A CN 201711252766 A CN201711252766 A CN 201711252766A CN 108117379 A CN108117379 A CN 108117379A
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high porosity
preparation
film support
alumina powder
porous ceramics
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陈赞
贾志伟
王楚宁
于海斌
刘宗园
臧毅华
盛春光
鞠云鹏
罗超
李阳
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CNOOC Energy Technology and Services Ltd
CNOOC Tianjin Chemical Research and Design Institute Co Ltd
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CNOOC Tianjin Chemical Research and Design Institute Co Ltd
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Abstract

本发明涉及一种高孔隙率多孔陶瓷膜支撑体及其制备方法。该支撑体由氧化铝和助剂组成，其中以陶瓷膜支撑体总质量计，氧化铝含量为85wt％‑97wt％；外形为板状或管状，孔隙率为45％～50％。其制备方法包括：将水与粘结剂、琼脂混合后静置形成胶体后，将其与平均孔径为0.01～10μm的氧化铝粉、造孔剂及烧结助剂混合后经炼泥、老化、挤出成型和干燥后得到陶瓷支撑体干燥胚体，然后升温1200℃～1600℃烧结，自然降温到常温后制得高强度高孔隙率多孔陶瓷支撑体。本发明高孔隙率多孔陶瓷支撑体具有孔隙率高、抗弯强度及抗压强度高、抗化学腐蚀性能强，以及渗透性能好的优点。

Description

一种高孔隙率多孔陶瓷膜支撑体及其制备方法
技术领域
本发明涉及膜支撑体材料，具体涉及一种高孔隙率多孔陶瓷膜支撑体及其制备方法。
背景技术
自从多孔陶瓷膜技术工业化应用以来，其作为一种新型的分离技术已经被广泛应用于医药、食品、化工、生物、染料以及水处理等领域。与有机膜相比，陶瓷膜具有耐高温、耐溶剂、耐酸碱腐蚀和机械强度高、对环境友好等一系列独特的优点。目前，随着世界范围内对工业节能技术及环保技术需求的不断提高，陶瓷膜已经引起人们的广泛关注，并逐步实现了大规模应用。
多孔陶瓷膜在工业应用过程中要求膜有较高的渗透通量和较低的阻力，同时要求膜具有较小的孔径及较均匀的孔径分布，以达到较高的分离性能。由于对膜性能的影响因素较多，所以要制备出性能优良的多孔陶瓷膜支撑体并不容易。因此对多孔陶瓷膜支撑体的研究越来越受到重视。陶瓷膜支撑体的各项性能之间有些是一致的，而有些却是互相矛盾的。例如，孔隙率大，则通量、吸水率大，但抗弯和抗压强度等性能会相应降低。影响支撑体这些性能的因素较多，并且各个因素之间也相互联系。探讨出规律性试验方法，对制备支撑体就显得非常重要。
发明内容
本发明所要解决的技术问题是克服现有技术存在的问题，提供了一种高孔隙率多孔陶瓷膜支撑体及其制备方法。这种高孔隙率多孔陶瓷膜支撑体能够解决支撑体在耐腐蚀、高强度的前提下提高孔隙率的技术问题。
本发明提供了一种高孔隙率多孔陶瓷膜支撑体，该陶瓷膜支撑体由氧化铝和助剂组成，其中以陶瓷膜支撑体总质量计，氧化铝含量为85wt％-97wt％；外形为板状或管状，孔隙率为45％～50％。
本发明还进一步提供了上述高孔隙率多孔陶瓷膜支撑体的制备方法，该方法使粘结剂和增塑剂与水充分混合为胶体后再与氧化铝粉混合，所选用的粘结剂的大分子中含有大量羟基，可以与水分子形成配位键，增强粘结剂效果，具体步骤为：
1)将水与粘结剂、琼脂混合后静置，形成胶体；
2)将步骤1)形成的胶体与中位粒径为0.01～10μm的氧化铝粉、造孔剂及烧结助剂混合，混合后经炼泥、老化、挤出成型、干燥，待干燥到含水量小于10wt％得到高孔隙率多孔陶瓷膜支撑体干燥胚体；所述的烧结助剂的中位粒径为0.01～10μm；所述的造孔剂的中位粒径为10～20μm；
3)将步骤2)得到的胚体以1～5℃/min的升温速率升温到1200～1600℃，保温烧结2-6小时后，自然降温到常温后制得高孔隙率多孔陶瓷支撑体。
上述技术方案中，本发明所述的造孔剂优选为碳粉或碳酸氢铵中的一种或多种；所述的粘结剂优选为羟丙基纤维素、羧甲基纤维素或甲基纤维素中的一种或多种；所述的烧结助剂优选为钛白粉、氧化锆或氧化硅中的一种或多种。
上述技术方案，可进一步优选水的加入量为氧化铝粉质量的25～30％，造孔剂的加入量为氧化铝粉质量的1～5％，粘结剂的加入量为氧化铝粉质量的3～8％，琼脂的加入量为氧化铝粉质量的1～3％，烧结助剂的加入量为氧化铝粉质量的3～15％。
在所述的胚体干燥过程中，优选干燥时间为24～48h，干燥温度为15～25℃。
本发明通过加入烧结助剂、提高原料纯度和优化制备工艺，使粘结剂和琼脂与水充分混合为胶体后再与氧化铝粉体混合，所选用的粘结剂的大分子中含有大量羟基，可以与水分子形成配位键，增强粘结剂效果，并使用了适量的造孔剂，故制备的高孔隙率多孔陶瓷膜支撑体相对于现有陶瓷膜支撑体具有孔隙率高、抗弯强度及抗压强度高、以及渗透性能好的优点，优选方案采用高纯度氧化铝粉及特定粘结剂、特定制备工艺使得陶瓷膜支撑体还具有抗化学腐蚀性能强的特点。
附图说明
图1为本发明高孔隙率多孔陶瓷膜支撑体的制备方法流程图。
图2为本发明实施例4制备得到的高孔隙率多孔陶瓷膜支撑体的表层的扫描(SEM)照片。
具体实施方案
下面结合具体实施例及说明书附图对本发明技术方案作进一步说明。
实施例1：
将550g水、110g羧甲基纤维素、44g琼脂混合后静置至成为均匀胶体后，加入88g中位粒径为10～20μm的碳粉、220g中位粒径为0.01～10μm的钛白粉和2200g中位粒径为0.01～10μm的纯度为95wt％的氧化铝粉，进行搅拌、炼泥、老化和挤出成型，经15℃干燥24小时，再升温至1250℃煅烧2小时即得产品A。
实施例2：
将840g水、90g羟丙基纤维素、30g琼脂混合后静置至成为均匀胶体后，加入120g中位粒径为10～20μm的碳粉、150g中位粒径为0.01～10μm的钛白粉和3000g中位粒径为0.01～10μm的纯度为95wt％的氧化铝粉，进行搅拌、炼泥、老化和挤出成型，经20℃干燥30小时，再升温至1300℃煅烧2.5小时即得产品B。
实施例3：
将650g水、100g羧甲基纤维素、75g琼脂混合后静置至成为均匀胶体后，加入100g中位粒径为10～20μm的碳酸氢铵、175g中位粒径为0.01～10μm的氧化锆粉和2500g中位粒径为0.01～10μm的纯度为99wt％以上的氧化铝粉，进行搅拌、炼泥、老化和挤出成型，经20℃干燥40小时，再升温至1350℃煅烧4小时即得产品C。
实施例4：
将840g水、224g羧甲基纤维素、28g琼脂混合后静置至成为均匀胶体后，加入70g中位粒径为10～20μm的碳粉、252g中位粒径为0.01～10μm的氧化硅粉和2800g中位粒径为0.01～10μm的纯度为99wt％以上的氧化铝粉，进行搅拌、炼泥、老化和挤出成型，经15℃干燥48小时，再升温至1400℃煅烧5小时即得产品D。
性能测定
根据《GBT1966-1996多孔陶瓷显气孔率、容重试验方法》对实施例1-4制得的陶瓷膜支撑体产品A、B、C、D，以及陶瓷膜支撑体产品E(市场上购得的以常规方法制备的多孔氧化铝陶瓷膜支撑体)进行孔隙率测定，测试结果列于表1中；根据《GBT 1965-1996多孔陶瓷弯曲强度试验方法》对陶瓷膜支撑体产品A、B、C、D、E进行抗弯强度测定，测试结果列于表1中；根据《GBT 1970-1996多孔陶瓷耐酸、碱腐蚀性能试验方法》对陶瓷膜支撑体产品A、B、C、D、E进行耐酸碱腐蚀性能测定，测试结果列于表1中。
表1多孔陶瓷膜支撑体性能测定结果

Claims (6)

1.一种高孔隙率多孔陶瓷膜支撑体，其特征在于：所述的多孔陶瓷膜支撑体由氧化铝和助剂组成，其中以陶瓷膜支撑体总质量计，氧化铝含量为85wt％-97wt％；外形为板状或管状，孔隙率为45％～50％。
2.一种高孔隙率多孔陶瓷膜支撑体的制备方法，其特征在于，包括步骤为：
1)将水与粘结剂、琼脂混合后静置，形成胶体；
2)将步骤1)形成的胶体与中位粒径为0.01～10μm的氧化铝粉、造孔剂及烧结助剂混合，混合后经炼泥、老化、挤出成型、干燥，待干燥到含水量小于10wt％得到高孔隙率多孔陶瓷膜支撑体干燥胚体；所述的烧结助剂的中位粒径为0.01～10μm；所述的造孔剂的中位粒径为10～20μm；
3)将步骤2)得到的胚体以1～5℃/min的升温速率升温到1200～1600℃，保温烧结2-6小时后，自然降温到常温后制得高孔隙率多孔陶瓷支撑体。
3.根据权利要求2所述的制备方法，其特征在于，所述的造孔剂为碳粉或碳酸氢铵中的一种或多种；所述的粘结剂为羟丙基纤维素、羧甲基纤维素或甲基纤维素中的一种或多种；所述的烧结助剂为钛白粉、氧化锆或氧化硅中的一种或多种。
4.根据权利要求2所述的制备方法，其特征在于，水的加入量为氧化铝粉质量的25～30％，造孔剂的加入量为氧化铝粉质量的1～5％，粘结剂的加入量为氧化铝粉质量的3～8％，增塑剂的加入量为氧化铝粉质量的1～3％，烧结助剂的加入量为氧化铝粉质量的3～15％。
5.根据权利要求2所述的制备方法，其特征在于所述的胚体干燥过程中，干燥时间为24～48h，干燥温度为15～25℃。
6.根据权利要求3所述的制备方法，其特征在于所述的氧化铝粉体的氧化铝含量为99wt％以上。
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CN110885237A (zh) * 2019-12-08 2020-03-17 浙江理工大学 一种低温烧结氧化铝陶瓷支撑体的制备方法
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CN113381047B (zh) * 2021-05-25 2023-12-15 湖北赛傲氢能科技有限公司 一种高温氧化物离子导体电池及其制备方法
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