膜分散微反应器制备γ-氧化铝千克级放大试验  

Kilogram-scale magnification test for preparation ofγ-Al2O3 in membrane dispersion microreactor

作　　者：万莉莎 李菲 赵申远 张建辉 王玉琪[1] 王玉军[2] WAN Lisha;LI Fei;ZHAO Shenyuan;ZHANG Jianhui;WANG Yuqi;WANG Yujun(School of Chemical Engineering,Northwest University,Xi'an 710069,China;State Key Laboratory of Chemical Engineering,Tsinghua University,Beijing 100084,China)

机构地区：[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

出　　处：《中国粉体技术》2021年第1期22-31,共10页China Powder Science and Technology

基　　金：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。

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。Kilogram-scale test for preparation of fibrousγ-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 ofγ-Al2O3 were studied.The properties and microstructure ofγ-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 preparedγ-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.

关 键 词：膜分散微反应器 Γ-氧化铝 放大试验 

分 类 号：TQ133.1[化学工程—无机化工]