中国有色金属学报
中國有色金屬學報
중국유색금속학보
THE CHINESE JOURNAL OF NONFERROUS METALS
2013年
1期
290-296
,共7页
刘广义%任恒%詹金华%钟宏
劉廣義%任恆%詹金華%鐘宏
류엄의%임항%첨금화%종굉
二乙氧羰基双硫脲%合成%金属离子%吸附%浮选
二乙氧羰基雙硫脲%閤成%金屬離子%吸附%浮選
이을양탄기쌍류뇨%합성%금속리자%흡부%부선
diethoxycarbonybis(thiourea)%synthesis%metal ion%adsorption%flotation
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.
以一縮二乙二醇雙氯甲痠酯與硫氰痠鉀為原料,以N, N?二甲基苯胺為催化劑,經相轉移催化反應,閤成一縮二乙二醇二羰基雙異硫氰痠酯中間體;該中間體再與乙胺髮生加成反應,閤成瞭一種未見報道的3,3'?二乙基?1,1'?一縮二乙二醇二羰基雙硫脲(DEOECTU).經元素分析、紅外光譜和覈磁共振氫譜分析,證實所閤成的化閤物即為目標產物.DEOECTU 與金屬離子的作用結果錶明:在實驗條件下,DEOECTU 與 Zn2+、Pb2+、Fe3+或Fe2+的之間可能不存在化學作用,而與Cu2+之間存在化學作用,其可通過分子中的S和N原子與Cu2+作用而生成螯閤環.吸附實驗結果錶明:DEOECTU能以化學作用方式吸附在黃銅礦錶麵,其在黃銅礦錶麵的吸附量遠遠高于在黃鐵礦、閃鋅礦和方鉛礦錶麵的吸附量.純礦物浮選實驗進一步錶明,DEOECTU對黃銅礦具有優良的捕收能力,而對黃鐵礦、閃鋅礦和方鉛礦的捕收能力弱.
이일축이을이순쌍록갑산지여류청산갑위원료,이N, N?이갑기분알위최화제,경상전이최화반응,합성일축이을이순이탄기쌍이류청산지중간체;해중간체재여을알발생가성반응,합성료일충미견보도적3,3'?이을기?1,1'?일축이을이순이탄기쌍류뇨(DEOECTU).경원소분석、홍외광보화핵자공진경보분석,증실소합성적화합물즉위목표산물.DEOECTU 여금속리자적작용결과표명:재실험조건하,DEOECTU 여 Zn2+、Pb2+、Fe3+혹Fe2+적지간가능불존재화학작용,이여Cu2+지간존재화학작용,기가통과분자중적S화N원자여Cu2+작용이생성오합배.흡부실험결과표명:DEOECTU능이화학작용방식흡부재황동광표면,기재황동광표면적흡부량원원고우재황철광、섬자광화방연광표면적흡부량.순광물부선실험진일보표명,DEOECTU대황동광구유우량적포수능력,이대황철광、섬자광화방연광적포수능력약.
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?1,1'?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 further greater than on pyrite, sphalerite 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.