三(2-乙基己基)氧膦与二(2-乙基己基)次膦酸的一步合成及表征  

Simultaneous Synthesis and Characterization of Tri(2-ethyl hexyl)phosphine Oxide and Bis(2-ethyl hexyl)phosphinic Acid

作　　者：黄华林[1] 李林艳[2] 黎铉海[1] 王学军[2] 刘欣[2] 

机构地区：[1]广西大学化学化工学院,广西南宁530004 [2]清华大学核能与新能源技术研究院,北京100084

出　　处：《湿法冶金》2015年第6期450-453,465,共5页Hydrometallurgy of China

基　　金：国家重点基础研究发展计划资助项目(2012CBA01201)

摘　　要：三(2-乙基己基)氧膦(a)和二(2-乙基己基)次膦酸(b)是性能优良的湿法冶金萃取剂。采用PCl_3与格氏试剂在常温下反应,一步合成a与b。初始产物中水溶性较大的单烷基次膦酸及其他杂质用碱液洗涤去除,采用改进的铜盐结晶沉淀法分离a与b,即在无其他溶剂条件下,用硫酸铜、氢氧化钠调节体系pH至二(2-乙基己基)次膦酸铜的等电点,得到絮状易过滤沉淀物,可使a与b分离。通过优化物料配比,a与b的总产率可达75.6%(以P计)。采用NMR、IR、MS对目标化合物的结构进行表征。Tri （2-ethyl hexyl）phosphine oxide（a） and bis （2-ethyl hexyl）phosphinic acid （b） are extractants with high performance in hydrometallurgy. A and b were synthesized in the same step through the reaction of PC13 and Grignard reagent at room temperature. The monoalkylphosphinic acid byproduct and other undesirable impurities were removed from the crude product by alkali washing. A and b were separated by copper-salt-precipitation method under solvent-free condition. CuSO4 and NaOH solution were used to adjust the pH of the mixture of a and b to the isoelectric point of the copper salt of b in order to obtain easy filtration floccule. The overall yields of a and b can reach 75.6%（based on P）. The structures of the title compounds are confirmed by NMR,MS and IR.

关 键 词：有机磷萃取剂 三(2-乙基己基)氧膦 二(2-乙基己基)次膦酸 合成 

分 类 号：O627.51[理学—有机化学]