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溶析结晶法制备高纯度亚微米硫酸钡粒子

王晓辉; 蒋斌波; 陈纪忠   

  1. 浙江大学化学工程与生物工程学系, 杭州 310027
  • 收稿日期:2004-05-28 修回日期:2004-07-07 出版日期:2005-07-20 网络出版日期:2005-07-20

Preparation of Barium Sulfate Submicro-particles with High Purity by Solventing-out Process

WANG Xiao-Hui; JIANG Bin-Bo; CHEN Ji-Zhong   

  1. Department of Chemical and Biochemical Engineering; Zhejiang University; Hangzhou 310027; China
  • Received:2004-05-28 Revised:2004-07-07 Published:2005-07-20 Online:2005-07-20

摘要: 采用溶析结晶法制备亚微米硫酸钡粒子,并运用TEM、SEM、XRD、激光粒度分析仪等分析方法对粒子的粒径、粒度分布、形貌和晶相进行了表征.结果表明溶析结晶法制备的粒子平均粒径160-750nm、粒度分布均匀、纯度高、晶相完整.考察了结晶温度、加料方式、搅拌速率和料液浓度等过程参数以及分散剂对硫酸钡粒子的影响,发现较低的结晶温度, 反向加料方式、较快的搅拌速率、一定的料液浓度等因素有利于制备亚微米硫酸钡粒子.

关键词: 硫酸钡, 溶析结晶, 亚微米, 晶相

Abstract: A novel micronization technique using solventing-out crystallization was described for the preparation of submicron BaSO4 particles. The submicron BaSO4 particles were characterized by transmission electron microscope (TEM),
scanning electron microscope (SEM), laser diffraction-based particle size analyzer and X-ray diffraction (XRD). The product was obtained as spherical particles with mean sizes from 160--750 nm. The effects of feed mode, feed
concentration, feed rate, agitation intensity and crystallization temperature in the solventing-out process were investigated. A well-efficiency dispersant was selected. The experimental results indicate that lower crystallization
temperature, reversed feed mode, higher feed rate, controlling solution concentration to a certain extent and faster agitation rate will lead to producing smaller BaSO4 particles. Furthermore, the purity of submicron BaSO4 particles
prepared by solventing-out crystallization is upon to 99.7%, and it indicates that the solventing-out crystallization is not only a micronization technique but also an excellent purification process.

Key words: barium sulfate, solventing-out, submicro-particles, crystalline

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