六水合高氯酸镍的制备及工艺设计

发布时间：2018-10-14 11:18

【摘要】：本文的目的是找到一条经济、绿色、高效的方法合成六水合高氯酸镍,以期实现工业化进程。选择废旧的镍氢电池作为研究对象,采取破碎分离、酸浸、萃取和反萃取等手段从中提取硫酸镍,进而沉淀转化为碱式碳酸镍,并以此作为镍源合成高氯酸镍晶体。最终实现六水合高氯酸镍的经济、绿色、高效的工业化生产。针对废旧镍氢电池进行酸浸实验。选择废旧电池的负极材料,采取机械分离的手段得到负极的储氢材料,然后选用H2SO4酸浸。实验条件为:3mol/L的H2SO4溶液,固液比为1:5,浸出时间为4h,浸出温度为95℃。得到结果为稀土金属的沉淀率达到95%,而Ni与Co等元素浸出率高达99.5%,可以达到初步分离的效果。随后进行正负极活性金属粉末的整体浸出实验,得到最佳的浸出条件是:3mol/L的硫酸溶液,液固比为7.5:1,浸出温度为95℃,浸出时间为4h。在该条件下,可以实现稀土金属与其他金属的初步分离。用5mol/L的NaOH溶液调节浸出液的pH值,浸出液中的稀土金属以各自硫酸盐的形式从浸出液中沉淀析出,稀土金属的沉淀析出率可以达到98%,pH值控制在0.6～1.2之间。通过浸出和调节pH值,将废旧镍氢电池中99%以上的稀土金属以稀土金属硫酸盐沉淀的形式回收并加以利用,不需要再进行加热萃取等步骤。选用湖南宏邦提供的HBL110萃取剂,在萃原液中该萃取剂的萃取先后顺序为:NiCoZn。结论是:萃取剂浓度为50%,空载有机相萃取剂pH为3,萃原液pH为2,相比为7,萃取级数为5,大部分的镍进入有机相,其他干扰金属元素全都留在萃余液中。随后用硫酸进行镍离子的反萃,最佳反萃条件:室温、反萃时间为7min、硫酸浓度为100g/L、有机相和水相的比值为5、一级反萃,反萃率可以达到99.6%。硫酸镍合成碱式碳酸镍最佳条件:0.5mol/L硫酸镍溶液,滴入到盛有饱和碳酸钠的反应器中(反加法),控制终点pH值为8.5,反应温度为70℃,沉淀过滤、去离子水冲洗去杂质离子、干燥、得到碱式碳酸镍粉末。通过碱式碳酸镍和30%的高氯酸反应,得到纯度较高的六水合高氯酸镍。
[Abstract]:The purpose of this paper is to find an economical, green and efficient method for the synthesis of nickel perchlorate hexahydrate. The waste Ni-MH battery was selected as the research object. Nickel sulfate was extracted by crushing separation, acid leaching, extraction and back-extraction, and then precipitated into basic nickel carbonate, which was used as a nickel source to synthesize nickel perchlorate crystals. The final realization of nickel perchlorate hexahydrate economy, green, efficient industrial production. Acid leaching experiments were carried out for waste Ni-MH batteries. The negative electrode material of waste battery is selected, the hydrogen storage material of negative electrode is obtained by mechanical separation, and then H2SO4 acid leaching is selected. The experimental conditions are as follows: the H2SO4 solution of 3mol/L, the ratio of solid to liquid is 1: 5, the leaching time is 4 h, and the leaching temperature is 95 鈩，

本文编号：2270298