以四氯化钛为插层剂制备插钛膨胀石墨的实验研究  

Preparation of Expanded Graphite Loaded Titanium Oxide with Titanium Tetrachloride as Intercalation Reagent

作　　者：庞秀言[1] 游婷婷[1] 苏亚娟[1] 陈阳[1] 

机构地区：[1]河北大学化学与环境科学学院,河北保定071002

出　　处：《非金属矿》2009年第5期1-4,共4页Non-Metallic Mines

摘　　要：以高锰酸钾为氧化剂,硫酸、四氯化钛作插层剂,制备了插钛膨胀石墨。分别以石墨膨胀容积和插钛膨胀石墨对酸性桃红的脱色率为优化目标,通过正交实验确定了高锰酸钾、硫酸、四氯化钛与原料石墨的最佳配比以及反应温度;对各种形式的石墨进行了XRD表征。实验确定以膨胀容积为目标制备插钛膨胀石墨的适宜反应条件为:石墨∶KMnO4∶H2SO4(75%)∶TiCl4=1∶0.5∶3.0∶0.35,反应温度45℃,反应时间60min,膨胀石墨的膨胀容积为410mL/g;以脱色率为考察目标制备插钛膨胀石墨适宜条件为:质量比石墨∶KMnO4∶H2SO4(75%)∶TiCl4=1∶0.5∶4.0∶0.4,反应温度为45℃,反应时间60min,浓度为100mg/L酸性桃红12h脱色率为56.5%。XRD证实了石墨层间化合物的生成,可膨胀石墨中钛以Ti(SO4)2以及锐钛型TiO2形式存在,膨胀石墨中以钛氧化物形式存在。热重-质谱联用(TG-MS)分析证实了可膨胀石墨膨胀过程中SO2的产生。Expanded graphite （EG） loaded titanium oxide is prepared with potassium permanganate as oxidant, sulfuric acid and titanium tetrachloride as intercalation reagent. With expanded volume （EV）, decolouring rate of acid brilliant red regarded as optimum object, the mass ratio of graphite to KMnO4, graphite to H2SO4 （75%）, graphite to titanium tetrachloride and reaction temperature are gained through orthogonal experiment. Every kinds of graphite are evaluated with XRD. The following results are obtained： the feasible condition to gain EG with maximum EV is graphite ： KMnO4 ： H2SO4 （75%） ： TiCl4=1 ： 0.5 ： 3.0 ： 0.35, and the reaction temperature is 45℃, the reaction time is 60min. While, the feasible condition to gain EG with high decolouring rate for acid brilliant red is graphite ： KMnO4 ： H2SO4（75%） ： TiCl4=1 ： 0.5 ： 4.0 ： 0.4, and the reaction temperature is 45℃, reaction time is 60min. Under the feasible condition, an EV of 4 10mL/g and decolouring rate of 56.5% are obtained, respectively. As testified by XRD, Ti exists in the form of Ti（SO4）2 and anatase TiO2 in expandable graphite, titanium oxide in EG. The combination of TG and MS testifies the existence of SO2 during expansion of expandable graphite.

关 键 词：膨胀石墨 层间化合物TiO2 膨胀容积 脱色率 

分 类 号：TQ165[化学工程—高温制品工业]