(中南大學(xué) 化學(xué)化工學(xué)院 有色金屬資源化學(xué)教育部重點(diǎn)實(shí)驗(yàn)室，長(zhǎng)沙410083)
摘 要: 以一縮二乙二醇雙氯甲酸酯與硫氰酸鉀為原料，以N, N-二甲基苯胺為催化劑，經(jīng)相轉(zhuǎn)移催化反應(yīng)，合成一縮二乙二醇二羰基雙異硫氰酸酯中間體；該中間體再與乙胺發(fā)生加成反應(yīng)，合成了一種未見報(bào)道的3,3'-二乙基-1,1'-一縮二乙二醇二羰基雙硫脲(DEOECTU)。經(jīng)元素分析、紅外光譜和核磁共振氫譜分析，證實(shí)所合成的化合物即為目標(biāo)產(chǎn)物。DEOECTU與金屬離子的作用結(jié)果表明：在實(shí)驗(yàn)條件下，DEOECTU與Zn2+、Pb2+、Fe3+或Fe2+的之間可能不存在化學(xué)作用，而與Cu2+之間存在化學(xué)作用，其可通過(guò)分子中的S和N原子與Cu2+作用而生成螯合環(huán)。吸附實(shí)驗(yàn)結(jié)果表明：DEOECTU能以化學(xué)作用方式吸附在黃銅礦表面，其在黃銅礦表面的吸附量遠(yuǎn)遠(yuǎn)高于在黃鐵礦、閃鋅礦和方鉛礦表面的吸附量。純礦物浮選實(shí)驗(yàn)進(jìn)一步表明，DEOECTU對(duì)黃銅礦具有優(yōu)良的捕收能力，而對(duì)黃鐵礦、閃鋅礦和方鉛礦的捕收能力弱。
關(guān)鍵字: 二乙氧羰基雙硫脲；合成；金屬離子；吸附；浮選
（Key Laboratory of Resources Chemistry of Nonferrous Metals, Ministry of Education,
School of Chemistry and Chemical Engineering, Central South University, Changsha 410083）
Abstract: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.
Key words: diethoxycarbonybis(thiourea), synthesis; metal ion; adsorption; flotation
