二癸基次膦酸的合成与萃取性能
来源期刊：中国有色金属学报2010年第11期
论文作者：居中军 李林艳 徐盛明 王成彦 廖复辉 李国宝
文章页码：2254 - 2259
关键词：自由基加成；二癸基次膦酸；萃取剂；镍钴分离
Key words：free radical addition；di-decylphosphinic acid；extractant; separation for cobalt and nickel
摘 要：以混合癸烯为原料，采用自由基加成法合成二癸基次膦酸(DDPA)，并研究自由基引发剂的种类、反应温度和反应时间对DDPA产率的影响，获得DDPA的最佳合成条件；通过碱洗和离心分离等手段除去产物中的单烷基次膦酸和烯烃聚合物等杂质，得到较纯的DDPA，并用核磁、质谱等方法对产物进行表征。研究产物在硫酸介质中对二价钴、镍、铜、镁、锌及锰等多种离子的萃取性能，并着重研究钴镍分离性能。结果表明：用10%DDPA(溶剂为环己烷)作萃取剂，经过二级萃取，二级洗涤，钴镍分离系数可达1.20×105。
Abstract: Di-decylphosphinic acid (DDPA) was synthesized by free radical addition method using mixed decylene as starting materials. The influence of initiator species, reaction temperature and time on the yield of DDPA was investigated. After post treatments, such as alkaline cleaning and centrifugation, the high-purte di-decylphosphinic acid was obtained. The product was characterized by nuclear magnetic resonance (NMR) and mass spectrum. The extraction properties of the as-synthesized product for cobalt, nickel, copper, magnesium, zinc and manganese in the medium of H2SO4 were studied, especially focused on the extractive separation for nickel and cobalt. With 10%DDPA in cyclohexane as extractant, the separation coefficient for Ni-Co could reach 1.20×105 through two-step extraction and two-step scrubbing.
