粒度可调纳米CuO的制备及其表面硫化研究

Synthesis of Size Tunable Nano Copper Oxide and Its Surface Sulphidization

用Cu(NO3)2.3H2O为原料,25%氨水为配位剂,用NaOH做沉淀剂,在不同醇-氨水体系中用配位沉淀法制备粒径可调的纳米CuO。通过热重差热分析法(TG-DTA)分析前驱体的组成并得到煅烧最佳温度。在制备前驱体过程中,探究了反应体系溶剂分别为乙醇、正丁醇、正辛醇时对产物粒径的影响,实验结果表明:随着醇溶剂中碳链的增长,得到纳米CuO的比表面积依次增大,粒度依次减小。将纳米CuO与硫单质混合,在通入氮气的管式炉中以200℃加热90 min,可以得到表面硫化的CuO(CuO/CuS),利用X-射线粉末衍射(XRD)和红外吸收光谱(FT-IR)对纳米CuO和CuO/CuS进行表征。最后将纳米CuO和CuO/CuS分别对乙基黄原酸钾进行吸附,结果表明CuO/CuS对乙基黄原酸钾吸附能力明显增强,进而证明氧化铜表面发生了硫化。

Using Cu（NO3）2·3H2O as raw materials, 25% ammonia as eomplexing agent and NaOH as precipitant, the size tunable nano CuO was synthesized in variable alcohol-water systems. The eomponent and the optimized calcination temperature of the precursor were determined through TG-DTA analysis. The solvent used in ammonia -water system was ethanol, butanol and oetanol respectively and their effect on the product particle size was discussed. The results showed that the specific surface areas of CuO nanopartieles increased and their sizes decreased with increasing the carbon chain length of alcohol used. The surface sulphidization of CuO （CuO/CuS） was obtained by heat treatment of CuO and elemental sulfur mixture in a tube type furnace under nitrogen atmosphere at 200 ℃ for 90 minutes. Powder X-ray diffraction and infrared absorption spectroscopy analysis methods were used to characterize the physical and chemical properties of nano CuO and CuO/CuS. The adsorption of potassium ethyl xanthate at the surfaces of nano CuO and CuO/CuS was studied. The result revealed that the capability of CuO/CuS adsorbing potassium ethyl xanthate was markedly enhanced, further proving the surface sulphidization occurred on the surface of nano CuO.