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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。
The Cu2 + ions in the organic phase composed of CCl4-TOA-CuCl2 were stripped by H2C2O4-ethanol aqueous solution using stripping precipitation method. The ultrafine CuC2O4 powder was obtained by phase-transfer reaction. The effects of copper concentration in the organic phase, concentration of ethanol in the stripping solution, stripping temperature and stripping time were investigated by X-ray diffraction, electron microscopy (SEM and TEM) and laser particle size analysis. Effect of particle size and morphology of ultrafine powder. The results showed that the copper concentration in the organic phase, the ethanol concentration in the stripping solution and the stripping temperature had a significant effect on the particle size and particle size distribution of precipitated copper oxalate particles during stripping and precipitation. The suitable conditions (the volume fraction of TOA in the organic phase and the concentration of Cu2 + in the organic phase was 0.1mol / L, the concentration of oxalic acid in the stripping solution was 0.1mol / L and the concentration of ethanol was 80%, the stripping temperature was 15 ℃ and the stripping time was 2h ), The ultrafine powder of oxalic acid with a particle size of about 100 nm can be prepared, and the powder is a spherical particle with a blue-cyan monoclinic structure.