同心圆式反应器中精确调控和连续制备β-四钼酸铵  

Precise control and continuous production ofβ-ammonium tetramolybdate in concentric reactor

作　　者：李江涛 罗勇进[1] 李志超 赵中伟 刘旭恒 陈星宇[1] 何利华 孙丰龙 张宁 Jiang-tao LI;Yong-jin LUO;Zhi-chao LI;Zhong-wei ZHAO;Xu-heng LIU;Xing-yu CHEN;Li-hua HE;Feng-long SUN;Ning ZHANG(School of Metallurgy and Environment,Central South University,Changsha 410083,China;Key Laboratory of Hunan Province for Metallurgy and Material Processing of Rare Metals,Central South University,Changsha 410083,China;College of Science,Central South University of Forestry and Technology,Changsha 410004,China)

机构地区：[1]中南大学冶金与环境学院,长沙410083 [2]中南大学稀有金属冶金与材料制备湖南省重点实验室,长沙410083 [3]中南林业科技大学理学院,长沙410004

出　　处：《Transactions of Nonferrous Metals Society of China》2024年第1期309-321,共13页中国有色金属学报（英文版）

基　　金：financially supported by the National Natural Science Foundation of China (Nos. 52174340, 51704338);the Basic Science Center of the National Natural Science Foundation of China (No. 72088101);the National Key Research and Development Project of China (No. 2022YFC2904505)。

摘　　要：采用同心圆式反应器制备β-四钼酸铵,研究制备过程中Mo离子聚合形态和微观结构受溶液酸度影响的变化规律。结果表明,将溶液的pH值控制在2.5以下可以得到四钼酸铵晶体;采用NH_(3)·H_(2)O将溶液pH值调回至3.0有利于细粒钼酸铵结晶的溶解,并促进七钼酸铵向四钼酸铵结晶的转变;降低(NH_(4))_(4)Mo_(4)O_(12)(O_(2))2·2H_(2)O晶体与结晶母液的接触时间有利于获得β-(NH_(4))_(2)Mo_(4)O_(13)结晶。基于钼的聚合机理,设计多个格区的同心圆反应器,实现钼酸铵结晶的分区域调控。通过调控硝酸、氨水和含晶种的母液在各格区中加入的位置和时机,可制备出优质的β-(NH_(4))_(2)Mo_(4)O_(13)结晶。β-ammonium tetramolybdate[β-(NH_(4))_(2)Mo_(4)O_(13)]was prepared in a concentric structure reactor.The species and microstructure of Mo with the change of solution acidity in the preparation process were investigated.The results showed that the pH of the solution should be controlled below 2.5 to obtain ammonium tetramolybdate crystals.In the acidification process,NH3∙H2O was used to adjust the pH back to about 3.0 to dissolve the fine crystals produced and facilitate the conversion of ammonium heptadmolybdate to ammonium tetramolybdate.Decreasing the soaking time between the(NH_(4))_(4)Mo_(4)O_(12)(O_(2))2∙2H_(2)O crystals and the original liquor was beneficial to obtaining β-(NH_(4))_(2)Mo_(4)O_(13).Based on the polymerization mechanism of molybdenum,a multi-lattice concentric circle reactor was designed to realize the regional regulation of ammonium molybdate crystallization.High-quality β-(NH_(4))_(2)Mo_(4)O_(13) was prepared continually by periodically adding HNO_(3) solution,ammonia water,and product slurry under specified conditions.

关 键 词：β-四钼酸铵 酸化 离子聚合 同心圆式反应器 

分 类 号：TQ113.79[化学工程—无机化工]