万莉莎^1,2,李 菲^1,2,赵申远²,张建辉²,王玉琪¹,王玉军²

（1.西北大学 化工学院,陕西 西安 710069;2.清华大学 化学工程联合国家重点实验室,北京 100084）

DOI：10.13732/j.issn.1008-5548.2021.01.003

收稿日期：2020-08-12，修回日期：2020-10-08，在线出版时间：2020-11-02 10:31。

基金项目：国家重点研发计划项目，编号:2019YFA0905100；国家自然科学基金项目，编号:21878169,21991102；清华大学自主科研计划项目，编号:2018Z05JZY010。

第一作者简介：万莉莎(1995—)，女,硕士研究生，研究方向为膜分散微反应器制备纳米材料。E-mail:785064909@qq.com。

通信作者简介：

王玉琪(1974—)，男，博士，教授，博士生导师，研究方向为材料与能源化工、分离技术与反应工程。E-mail:wangyuqi@nwu.edu.cn。

王玉军(1973—)，男，博士，教授，博士生导师，研究方向为膜分离及膜反应分离一体化技术、高效分离材料制备。E-mail:wangyujun@mail.tsinghua.edu.cn。

摘要：以偏铝酸钠为分散相、硫酸铝为连续相，采用共沉淀方法在膜分散微反应器中进行纤维状γ-氧化铝制备工艺的千克级放大试验;研究不同膜分散微反应器的尺寸、NaAlO₂流量、Al₂(SO₄)₃质量浓度、反应时间、老化时间、洗涤方式和干燥温度对γ-氧化铝性质的影响，确定千克级放大制备工艺的最佳参数;通过TEM和XRD表征γ-氧化铝的性质和微观结构，验证放大试验的有效性。结果表明:千克级放大制备工艺的一组最佳参数为:膜分散微反应器的半径和高度分别为8 mm，偏铝酸钠流量为36 L/h，硫酸铝质量浓度为30 g/L，反应时间为1 h，老化时间为0～1 h，洗涤方式为碳酸钠-磷酸洗涤方式，干燥温度为120℃，制得的γ-氧化铝孔容为1.40 mL/g，平均孔径为13.1 nm，比表面积高达429.9 m₂/g。

关键词：膜分散微反应器；γ-氧化铝；放大试验

Abstract：Kilogram-scale test for preparation of fibrous γ-Al₂O₃ in membrane microreactor with co-precipitation method was carried out by using NaAlO2 as the dispersed phase and Al₂(SO₄)₃ as the continuous phase. The effects of different membrane dispersion microreactor size,NaAlO₂ flow rate,Al₂(SO₄)₃ mass concentration,reaction time,aging time,washing method and drying temperature on the properties of γ-Al₂O₃ were studied. The properties and microstructure of γ-Al₂O₃ were characterized by TEM and XRD to verify the effectiveness of the amplification test. The results show that the optimum parameters of kilogram-scale amplification process are as follows: the radius and height of membrane dispersion microreactor are 8 mm,flow rate of NaAlO2 is36 L/h,mass concentration of Al₂(SO₄)₃ is 30 g/L,reaction time is 1 h,aging time is from 0 to 1 h,washing method is sodium carbonate-phosphoric acid washing method and drying temperature is 120 ℃ ． The pore volume of prepared γ-Al₂O₃ is 1. 40 m L/g,average pore diameter is 13. 1 nm and specific surface area is up to 429. 9 m²/g.

Keywords：membrane dispersion microreactor; γ-Al₂O₃; scale-up test

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