摘要
为了找寻一种在无硫酸的介入下制备膨胀石墨的工艺,达到无有害硫残余的目的,以钾-四氢呋喃-萘的络合物溶液为介质,用电化学法合成了钾-四氢呋喃-石墨插层化合物,并对其进行微波膨化,制备膨胀石墨。通过正交实验优化了影响石墨膨胀率的因素,得出了各因素对膨化率由强到弱的影响次序:电解电压、反应时间、电解液浓度、微波功率。确定出最佳影响因素水平:电解电压2 V、反应时间2 h、电解液浓度8:3、微波功率700 W。并用ESEM,XRD技术对膨胀后的石墨的表面形貌和结构进行了表征分析。
In order to find an effective process for fabricating graphite intercalation compound without sulfur, a ternary potassium-tetrabydrofuran-graphite intercalation compound was prepared successfully in potassium - tetrahydrofuran solutions by electrochemical method and was bulked in Micro-Wave oven. Reaction conditions was optimized by using orthogonal design,and the sequence of factors influencing the ratio of expansion was obtained, which was, from strong to weak, the electric voltage of electrolysis, the reaction time,the molar ratio of tetrahydrofuran to potassium and the power of micro - wave. The optimum technical parameters were determined, namely, the electric voltage of electrolysis 2V, the reaction time 2h, the molar ratio of tetrabydrofuran to potassium 8:3 and the power of Micro - Wave 700w. The microcosmic performance and structure of the expanded graphite were characterized and analyzed by ESEM and XRD techniques.
基金
山东省科技计划(2006GG2203027)
山东省教育厅科技计划(J06I06)
关键词
石墨层间化合物
电化学合成
钾
四氢呋喃
微波
graphite intercalation compound
electrochemical synthesis
potassium
tetrahydrofuran
micro - wave