二(2,4,4-三甲基戊基)次膦酸(Cyanex272)的合成工艺改进  

Improvement of Synthesis Technology for Bis(2,4,4-triMethylpentyl)-phosphinic Acid

作　　者：李芹[1] 李林艳[2] 张瑛[1] 王学军[2] 刘欣[2] 

机构地区：[1]中国石油大学(北京)理学院,北京102249 [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》2016年第4期327-332,共6页Hydrometallurgy of China

基　　金：国家重点基础研究发展计划(973计划)项目(2012CBA01201)资助

摘　　要：根据Cyanex272自由基加成法合成工艺,直接以次磷酸、二异丁烯为原料,以过氧化二叔丁基为自由基引发剂,通过自由基加成反应合成Cyanex272。工艺中,次磷酸既是反应原料,又为反应体系提供强酸性条件,使主反应一步完成,简化了后处理步骤,同时大大提高了产物纯度。采用磁共振(1 H,31 P谱)、红外光谱及质谱对产物进行表征,结果表明,产物的结构与目标化合物Cyanex272吻合,纯度大于98%。The organophosphorus compounds are widely used as extractant in hydrometallurgy.Bis（2,4,4-trimethylpentyl）-phosphinic acid（commercial named as Cyanex272）shows excellent performance for extracting rare earths and Ni/Co.Since the intellectual property rights of the extractant still belongs to foreign countries,so Cyanex272 is very expensive in our country.Herein,an improved synthesis route for Cyanex272 is pointed out,in which hypophosphorous acid and diisobutene are used as raw material,and di-tert-butyl peroxide is used as free radical initiator.In this synthesis process,hypophosphorous acid served as both phosphorus source and a strong acid which could reduce the by-products greatly and simplified the post-processing.The structures of the as-synthesized products are characterized by 31P-NMR,1 H-NMR,gas chromatography,infrared spectrum（IR）,and MS.The purity of the title compound synthesized by the improved route can reach 98%.

关 键 词：二(2 4 4-三甲基戊基)次膦酸 自由基加成法 合成 改进 

分 类 号：TQ265.1[化学工程—有机化工]