(1. 清華大學 核能與新能源技術研究院，北京100084; 2. 北京分子科學國家實驗室，北京 100080;
3. 北京礦冶研究總院，北京100044)
摘 要: 以混合癸烯為原料，采用自由基加成法合成二癸基次膦酸(DDPA)，并研究自由基引發(fā)劑的種類、反應溫度和反應時間對DDPA產(chǎn)率的影響，獲得DDPA的最佳合成條件；通過堿洗和離心分離等手段除去產(chǎn)物中的單烷基次膦酸和烯烴聚合物等雜質(zhì)，得到較純的DDPA，并用核磁、質(zhì)譜等方法對產(chǎn)物進行表征。研究產(chǎn)物在硫酸介質(zhì)中對二價鈷、鎳、銅、鎂、鋅及錳等多種離子的萃取性能，并著重研究鈷鎳分離性能。結果表明：用10%DDPA(溶劑為環(huán)己烷)作萃取劑，經(jīng)過二級萃取，二級洗滌，鈷鎳分離系數(shù)可達1.20×105。
關鍵字: 自由基加成；二癸基次膦酸；萃取劑；鎳鈷分離
（1. Institute of Nuclear and New Energy Technology, Tsinghua University, Beijing 100084, China;
2. Beijing National Laboratory for Molecular Sciences (BNLMS), Beijing 100080, China;
3. Beijing General Research Institute of Mining and Metallurgy, Beijing 100044, China）
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.
Key words: free radical addition；di-decylphosphinic acid；extractant; separation for cobalt and nickel
