摘要
以高锰酸钾为氧化剂,硫酸、钛酸四丁酯作插入剂,经反应、水洗、干燥、高温膨胀,制备了负载氧化钛的膨胀石墨。通过正交实验确定了高锰酸钾、一定浓度硫酸、钛酸四丁酯与原料石墨的配比;单因素实验考察了高锰酸钾用量、反应时间、反应温度、钛酸四丁酯用量对产品膨胀容积的影响;对各种形式的石墨进行了XRD物相分析及能量散射(EDS)表征。实验确定制备负载氧化钛的膨胀石墨的最佳工艺条件为:液(硫酸)∶固=3.0∶1,KM nO4∶C=0.5∶1,硫酸浓度为75%,钛酸四丁酯∶C=0.2∶1,反应温度为45℃,反应时间为60分(均为质量比)。最佳条件下负载氧化钛的膨胀石墨的膨胀容积为260m l/g;EDS证实了钛的存在;XRD物相分析表明,可膨胀石墨中钛以T iO2形式存在,膨胀石墨中钛以T ixOy形式存在。
Expanded graphite（EG） loaded with titania was prepared with potassium permanganate as oxidant, sulfuric acid and tetra-- n-- butyl titanate as inserting substance, and then washing, drying, expanding rapidly at high temperature. The optimum mass ratio of C to KMnO4 C to HZSO4（75%）,C to tetra--n-- butyl titanate was obtained through orthogonal experiment. The influences of dosage of potassium permanganate,reaction time,reaction temperature,and dosage of tetra--n--butyl titanate on expanded volume of EG were discussed. Homemade products were evaluated by means of XRD and EDS. The results show that the optimum condition to prepare EG loaded with titania is C ： KMnO4 ： HZSO4（75） ： tetra--n--butyl; titanate=1 ： 0. 5 ： 3.0（75%） ： 0. 2,and the reaction temperature is 45℃ ,the reaction time is 60min. Under the optimum condition,EG with an expanded volume of 260 ml/g is obtained. The results of XRD and EDS testify the state of Ti is TiO2 in expandable graphite,and TixOy in EG.
出处
《炭素》
2008年第4期8-12,共5页
Carbon
关键词
膨胀石墨
石墨层间化合物
钛的氧化物
膨胀容积
正交试验
expanded graphite
graphite intercalation compound
Titania
expanded volume
orthogonal experiment
