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以粗铜精炼富钴废渣为原料,通过硫酸氧化浸出,得到浸出液,然后采用草酸铵沉淀-固态盐热分解法合成Co3O4粉体。考察了草酸铵用量、沉淀反应温度、沉淀终点pH值等对钴沉淀率的影响,探索了草酸钴分解得到Co3O4的温度条件。采用X射线衍射对草酸钴和Co3O4粉体进行了分析。实验结果表明:沉钴反应温度40℃,草酸铵用量为理论量的1.1倍,反应终点pH值为1.8,钴的沉淀率可达99.7%,所得草酸钴含钴量达到30.2%。在草酸钴热分解为Co3O4的温度范围内(450～750℃,保温3 h),随着分解温度的升高,分解所得Co3O4逐步向活性Co3O4转化,晶形逐步变好。
Cobalt-rich waste slag is used as raw material, leaching solution is obtained by sulfuric acid oxidation, and then Co3O4 powder is synthesized by ammonium oxalate precipitation-solid salt thermal decomposition method. The effects of the amount of ammonium oxalate, the reaction temperature of precipitation and the pH of the final precipitate on the precipitation rate of cobalt were investigated. The temperature conditions for the decomposition of cobalt oxalate to obtain Co3O4 were investigated. The cobalt oxalate and Co3O4 powders were analyzed by X-ray diffraction. The experimental results show that the reaction temperature is 40 ℃, the dosage of ammonium oxalate is 1.1 times of the theoretical amount, the final pH value is 1.8, the precipitation rate of cobalt is up to 99.7% and the cobalt oxalate content is 30.2%. In the temperature range from 450 to 750 ℃ for 3 h, the decomposition of Co3O4 decomposed into Co3O4 gradually and the crystal form became better.