反萃沉淀法制备草酸铜超细粉体

Preparation of Ultra-Fine Copper Oxalate Powder by Stripping Precipitation Method

采用反萃沉淀法,以H2C2O4-乙醇水溶液反萃CCl4-TOA-CuCl2组成的有机相中的铜离子,利用相界面传质反应过程获取CuC2O4超细粉体。采用X射线衍射分析、电子显微分析(SEM和TEM)、激光粒度分析等手段,考察了有机相铜浓度、反萃液中乙醇的浓度、反萃温度以及反萃时间等操作条件对草酸铜超细粉体的粒径和形貌的影响。结果表明,在反萃沉淀过程中,有机相中铜浓度、反萃液中乙醇浓度、反萃温度对草酸铜沉淀颗粒的粒径和粒径分布影响较大,反萃时间的影响小;在适宜条件(有机相中TOA40%(体积比)和Cu2+浓度0.1mol/L,反萃液中草酸浓度0.1mol/L和乙醇浓度80%(体积比),反萃温度15℃以及反萃时间2h)下,可制备粒径约100nm的草酸铜超细粉体,粉体为蓝青色单斜晶系结构的球形颗粒。

Based on the interfacial mass transfer process,the ultra-fine copper oxide powder was prepared from the CCl4-TOA-CuCl2organic phase by the stripping precipitation method with H2C2O4-C2H5OH aqueous solution as the stripping agent and precipitant.The effects of preparation conditions on the structure and size distribution of CuC2O4powders were studied by XRD,SEM,TEM and laser particle analysis.The results show that the TOA and Cu2＋concentrations in the organic phase,the H2C2O4 and C2H5OH concentrations in the water phase,stripping temperature have obviously influence on the structure and size distribution of CuC2O4powders,while the effect of stripping time is slight.At 40% TDA,0.1mol/L Cu2＋,0.10mol/L H2C2O4-80% C2H5OH,stripping temperature of 15℃and stripping time of 2h,black brown,welldispersed CuC2O4powders with the average size about 100nm and high purity of monoclinic crystal phase were obtained.