CN110981453A - 一种轻质陶瓷过滤膜的制备方法 - Google Patents

一种轻质陶瓷过滤膜的制备方法 Download PDF

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CN110981453A
CN110981453A CN201910997317.XA CN201910997317A CN110981453A CN 110981453 A CN110981453 A CN 110981453A CN 201910997317 A CN201910997317 A CN 201910997317A CN 110981453 A CN110981453 A CN 110981453A
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丘助国
洪昱斌
方富林
蓝伟光
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Suntar Membrane Technology Xiamen Co Ltd
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Abstract

本发明公开了一种轻质陶瓷过滤膜的制备方法，采用中空的球形或者椭球行金属氧化物骨料颗粒，并辅助添加少量纳米烧结助剂和成型助剂，成型为陶瓷膜支撑体，烘干后再进行高温烧结而成支撑体，该支撑体孔隙率为40‑85％，纯水通量10000‑20000LMH，单根膜管重量相较于同等材质与粒径的实心颗粒制备的陶瓷膜管降低约30‑80％，以外径30mm，长度1200mm的陶瓷膜为例，本发明制备的单根支撑体的重量约1kg，由此大幅度降低了陶瓷膜在生产、运输及应用过程中的直接或者间接能耗及使用成本。

Description

一种轻质陶瓷过滤膜的制备方法
技术领域
本发明属于陶瓷膜制备技术领域，具体涉及一种轻质陶瓷过滤膜的制备方法。
背景技术
膜与膜过程是20世纪60年代开始快速发展起来的高新技术领域。世界各国都高度重视，将其放在科技创新和国民经济发展的重要地位。相较于传统聚合物分离膜材料，陶瓷膜具有化学稳定性好，能耐酸、耐碱、耐有机溶剂；机械强度大，可反向冲洗；抗微生物能力强；耐高温；孔径分布窄、分离效率高等优点，在食品工业、生物工程、环境工程、化学工业、石油化工、冶金工业等领域得到了广泛的应用。
陶瓷膜主要以不同规格的氧化铝、氧化锆、氧化钛和氧化硅等无机陶瓷材料作为支撑体，经表面涂膜、高温烧制而成。商品化的陶瓷膜通常具有三层结构(多孔支撑层、过渡层及分离层)，呈非对称分布，其孔径规格为0.8nm～1μm不等，过滤精度涵盖微滤、超滤、纳滤级别。
其中，陶瓷膜支撑体的制备采用实心氧化铝、碳化硅或者氧化硅等陶瓷颗粒作为骨架颗粒，并辅助添加少量金属氧化物细颗粒以及各种降低烧结温度的烧结助剂，混以成型胶体后通过各种成型方式和烧结工艺进行烧结，最终形成具有一定孔隙率和强度的陶瓷膜支撑体结构。由于金属氧化物的密度都比较大，为了实现比较好的支撑强度，陶瓷颗粒间也必须达到一定的密实度，所以目前市场上的陶瓷膜支撑体自重都比较大(以市场常见的外径30mm，长度1200mm的陶瓷膜为例，其单根支撑体的重量约2-3kg，100m2过滤面积的陶瓷膜，其膜管自身重量将近1吨)，远远超过相同过滤面积的有机膜材料。由于陶瓷膜较重，其生产过程中(尤其是烧结过程)能耗大，产品运输包装要求高，容易断裂，产品安装、使用、更换及回收等一系列与陶瓷膜相关的操作都会有成本较高，操作不便的问题。与陶瓷膜相关的配套组件等设备设施也需要因陶瓷膜自重较大而进行加强设计，无形中大幅增加了相应的设备设施成本。
发明内容
本发明的目的在于克服现有技术缺陷，提供一种轻质陶瓷过滤膜的制备方法。
本发明的技术方案如下：
一种轻质陶瓷过滤膜的制备方法，包括如下步骤：
(1)将圆形或椭圆形的中空金属氧化物骨料颗粒、纳米烧结助剂、成型助剂和水充分混合，制成陶瓷浆料，其中，中空金属氧化物骨料颗粒的粒径为10-100um，纳米烧结助剂的粒径为1-300nm，中空金属氧化物骨料颗粒、纳米烧结助剂和成型助剂的质量比为85-95∶3-5∶4-7；
(2)将上述陶瓷浆料经成型处理，制成支撑体湿坯；
(3)将上述支撑体湿坯依次经阴干、烘干和烧结，制成支撑体；
(4)在步骤(3)获得的支撑体上涂覆至少一层过滤膜，即得所述轻质陶瓷过滤膜。
在本发明的一个优选实施方案中，所述中空金属氧化物骨料颗粒的材质为氧化硅或氧化铝。
在本发明的一个优选实施方案中，所述纳米烧结助剂的材质为氧化钛。
在本发明的一个优选实施方案中，所述步骤(2)中的成型处理所用的方法为挤出成型法或者凝胶注模成型法。
在本发明的一个优选实施方案中，所述挤出成型法中的成型助剂包括玉米淀粉、PVA和甘油。
在本发明的一个优选实施方案中，所述凝胶注模成型法中的成型助剂包括活性炭粉、PVA粉末和明胶粉末。
在本发明的一个优选实施方案中，所述步骤(4)中的涂覆的方法为浸渍法或者喷涂法。
本发明的有益效果是：本发明采用中空的球形或者椭球行金属氧化物骨料颗粒，并辅助添加少量纳米烧结助剂和成型助剂，成型为陶瓷膜支撑体，烘干后再进行高温烧结而成支撑体，该支撑体孔隙率40-85％，纯水通量10000-20000LMH，单根膜管重量相较于同等材质与粒径的实心颗粒制备的陶瓷膜管降低约30-80％，以外径30mm，长度1200mm的陶瓷膜为例，本发明制备的单根支撑体的重量约1kg，由此大幅度降低了陶瓷膜在生产、运输及应用过程中的直接或者间接能耗及使用成本。
附图说明
图1为本发明实施例1所制得的轻质陶瓷膜支撑体的扫描电镜照片。
具体实施方式
以下通过具体实施方式结合附图对本发明的技术方案进行进一步的说明和描述。
实施例1：
将中空球状氧化铝(40um，75wt％)、氧化钛(100m，3wt％)、玉米淀粉(1um，3wt％)、PVA(1um，2wt％)用混料机混合4h，往混合好的粉料中加入RO水(15wt％)和甘油(2wt％)，再次混合4h后形成陶瓷泥料并陈腐48h。用真空练泥机对陈腐后的陶瓷泥料进行真空(-0.1MPa)练泥后，采用挤出成型的方式成型陶瓷膜支撑体湿坯。湿坯成型后室温阴干24h，然后用烘箱以1℃/min的速度升温至120℃烘干2h。最后采用高温烧结窑炉1500℃保温2h烧结成如图1所示的轻质陶瓷膜支撑体。该支撑体的平均孔径为15um，孔隙率为60％，在0.1Mpa压力下，支撑体纯水通量为15m3/m2h。后续在此支撑体上通过浸渍或者喷涂等陶瓷过滤膜制膜工艺涂覆一层或者多层过滤膜，最终制备成轻质陶瓷膜产品。以上配方制得外径30mm，长度1200mm的陶瓷膜，单根陶瓷膜管的重量0.85kg。
Figure BDA0002238957890000031
实施例2：
将中空球状氧化铝(60μm，90wt％)、氧化钛(100nm，5wt％)、活性炭粉(20μm，1wt％)、PVA粉末(分子量2000，1wt％)、明胶粉末(纯度98％，3wt％)球磨2h混合均匀，获得混合粉末。加入RO水(混合粉末与RO水溶液的体积比为2.2∶1)，85℃水浴加温的条件下球磨分散20h制成分散均匀的浆料。将浆料80℃保温状态下真空(-0.1MPa)除泡后立即浇注在模具中，物理降温至20℃后原位凝固为具有一定强度的湿坯。湿坯脱模后室温阴干48h，80℃烘干48h。在空气气氛中进行保温烧结，烧结温度为1650℃，保温时间为2h，制得轻质陶瓷膜支撑体。该轻质陶瓷膜支撑体平的均孔径为20μm，孔隙率为45％，在0.1MPa的压力下，支撑体纯水通量为16m3/m2h。后续在此支撑体上通过浸渍或者喷涂等陶瓷过滤膜制膜工艺涂覆一层或者多层过滤膜，最终制备成轻质陶瓷膜产品。以上配方制得外径30mm，长度1200mm的陶瓷膜，单根陶瓷膜管的重量0.95kg。
Figure BDA0002238957890000032
Figure BDA0002238957890000041
实施例3：
将中空球状氧化硅(10μm，90wt％)、氧化钛(100nm，3wt％)、活性炭粉(3μm，2wt％)、PVA粉末(分子量2000，2wt％)、明胶粉末(纯度98％，3wt％)球磨2h混合均匀，获得混合粉末。加入RO水(混合粉末与RO水溶液的体积比为2.2∶1)，85℃水浴加温的条件下球磨分散20h制成分散均匀的浆料。将浆料80℃保温状态下真空(-0.1MPa)除泡后立即浇注在模具中，物理降温至20℃后原位凝固为具有一定强度的湿坯。湿坯脱模后室温阴干72h，80℃烘干72h。在空气气氛中进行保温烧结，烧结温度为1350℃，保温时间为3h，制得轻质陶瓷膜支撑体。该轻质陶瓷膜支撑体平均孔径为3μm，孔隙率为65％，在0.1MPa的压力下，支撑体纯水通量为1m3/m2h。后续在此支撑体上通过浸渍或者喷涂等陶瓷过滤膜制膜工艺涂覆一层或者多层过滤膜，最终制备成轻质陶瓷膜产品。以上配方制得外径30mm，长度1200mm的陶瓷膜，单根陶瓷膜管的重量0.6kg。
Figure BDA0002238957890000042
以上所述，仅为本发明的较佳实施例而已，故不能依此限定本发明实施的范围，即依本发明专利范围及说明书内容所作的等效变化与修饰，皆应仍属本发明涵盖的范围内。

Claims (7)

1.一种轻质陶瓷过滤膜的制备方法，其特征在于：包括如下步骤：
(1)将圆形或椭圆形的中空金属氧化物骨料颗粒、纳米烧结助剂、成型助剂和水充分混合，制成陶瓷浆料，其中，中空金属氧化物骨料颗粒的粒径为10-100um，纳米烧结助剂的粒径为1-300nm，中空金属氧化物骨料颗粒、纳米烧结助剂和成型助剂的质量比为85-95∶3-5∶4-7；
(2)将上述陶瓷浆料经成型处理，制成支撑体湿坯；
(3)将上述支撑体湿坯依次经阴干、烘干和烧结，制成支撑体；
(4)在步骤(3)获得的支撑体上涂覆至少一层过滤膜，即得所述轻质陶瓷过滤膜。
2.如权利要求1所述的制备方法，其特征在于：所述中空金属氧化物骨料颗粒的材质为氧化硅或氧化铝。
3.如权利要求1所述的制备方法，其特征在于：所述纳米烧结助剂的材质为氧化钛。
4.如权利要求1所述的制备方法，其特征在于：所述步骤(2)中的成型处理所用的方法为挤出成型法或者凝胶注模成型法。
5.如权利要求1所述的制备方法，其特征在于：所述挤出成型法中的成型助剂包括玉米淀粉、PVA和甘油。
6.如权利要求1所述的制备方法，其特征在于：所述凝胶注模成型法中的成型助剂包括活性炭粉、PVA粉末和明胶粉末。
7.如权利要求1所述的制备方法，其特征在于：所述步骤(4)中的涂覆的方法为浸渍法或者喷涂法。
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