3,3'-二乙基-1,1'-一缩二乙二醇二羰基双硫脲的合成、表征与性能  

Synthesis, characterization and properties of 3,3'-diethyl-1,1'-oxydiethylenedicarbonylbis(thiourea)

作　　者：刘广义[1] 任恒[1] 詹金华[1] 钟宏[1] 

机构地区：[1]中南大学化学化工学院有色金属资源化学教育部重点实验室,长沙410083

出　　处：《中国有色金属学报》2013年第1期290-296,共7页The Chinese Journal of Nonferrous Metals

基　　金：国家高技术研究发展计划资助项目(2007AA06Z122);国家重点基础研究发展计划资助项目(2007CB613602);国家"十一五"支撑计划资助项目(2007BAB22B01);国家自然科学基金资助项目(51074183;50604016);全国优秀博士论文作者专项基金资助项目(2007B52);新世纪优秀人才支持计划资助项目(NCET-08-0568)

摘　　要：以一缩二乙二醇双氯甲酸酯与硫氰酸钾为原料,以N,N-二甲基苯胺为催化剂,经相转移催化反应,合成一缩二乙二醇二羰基双异硫氰酸酯中间体;该中间体再与乙胺发生加成反应,合成了一种未见报道的3,3'-二乙基-1,1'-一缩二乙二醇二羰基双硫脲(DEOECTU)。经元素分析、红外光谱和核磁共振氢谱分析,证实所合成的化合物即为目标产物。DEOECTU与金属离子的作用结果表明:在实验条件下,DEOECTU与Zn2+、Pb2+、Fe3+或Fe2+的之间可能不存在化学作用,而与Cu2+之间存在化学作用,其可通过分子中的S和N原子与Cu2+作用而生成螯合环。吸附实验结果表明:DEOECTU能以化学作用方式吸附在黄铜矿表面,其在黄铜矿表面的吸附量远远高于在黄铁矿、闪锌矿和方铅矿表面的吸附量。纯矿物浮选实验进一步表明,DEOECTU对黄铜矿具有优良的捕收能力,而对黄铁矿、闪锌矿和方铅矿的捕收能力弱。The synthesis and characterization of novel thiourea compounds containing two alkoxycarbonyl and two thiourea groups were reported. Using oxydiethylene bis（chloroformate） and KSCN as reactants, N,N-dimethylaniline as catalyst, an oxydiethylenedicarbonyl bis（isothiocyanate） intermediate was synthesized by a phase transfer catalytic reaction. Then, through a nucleophilic addition reaction, this intermediate reacts with ethylamine to produce 3,3＇-diethyl-l,l＇-oxydiethylenedicarbonyl bis（thiourea） （DEOECTU）. The compound DEOECTU was characterized by UV-visible spectra, elemental analysis, infrared spectra and 1H NMR. The results of the interation of DEOECTU with metal ions indicate that DEOECTU can react with Cu2~ in solution to form a chelated complex through bonding of its S and N atoms with Cu atom, but no reaction of DEOECTU with Zn2＋, Pb2＋, Fe3＋ or Fe2＋ is observed under the experimental conditions. The results of adsorption measurement demonstrate that DEOECTU can be chemically adsorbed on chalcopyrite surface, and the adsorption amount of DEOECTU on chalcopyrite surfaces is fiarther greater than on pyrite, spbalerite or galena surfaces. The flotation results of pure minerals were further confirmed that DEOECTU exhibits superior collecting power to chalcopyrite and good selectivity against pyrite, sphalerite and galena.

关 键 词：二乙氧羰基双硫脲 合成 金属离子 吸附 浮选 

分 类 号：TQ311[化学工程—高聚物工业] O63[理学—高分子化学]