硅胶负载硅钨酸催化剂上金刚烷的制备  

Preparation of adamantane over SiW/SiO_2 catalyst

作　　者：火焱 武文良[1] 李超[1] 周志伟[1] 赵彦平[1] 

机构地区：[1]南京工业大学化学化工学院,江苏南京210009

出　　处：《南京工业大学学报（自然科学版）》2010年第3期72-77,共6页Journal of Nanjing Tech University(Natural Science Edition)

基　　金：江苏省自然科学基金资助项目(BK2008376)

摘　　要：采用过量浸渍法制备一系列硅胶(SiO2)负载12-硅钨酸(SiW)催化剂,利用X线衍射(XRD)、傅里叶变换红外光谱(FT-IR)和氨程序升温脱附法(NH3-TPD)对催化剂的物化性质进行表征.并在100 mL间歇式不锈钢高压反应釜中考察其在桥式四氢双环戊二烯(endo-TCD)异构化制备金刚烷反应中的催化性能.实验结果表明:SiW在SiO2上最适宜的负载量为40%.在适宜的反应条件下,即催化剂的活化温度250℃,反应温度240℃,反应时间3 h,初始压力1.1 MPa.当催化剂与原料的质量比值为0.9、溶剂环己烷与原料的摩尔比值为5时,endo-TCD的转化率达到96.9%,金刚烷的收率达到17.8%.12-Silicotungstic acid（SiW） was immobilized on silica dioxide at room temperature to form SiW/SiO2 catalysts.The physical and chemical properties of catalysts SiW/SiO2 were characterized by X-ray diffraction（XRD）,Fourier transform infrared spectroscopy（FT-IR） and ammonia program temperature desorption（NH3-TPD）,and the catalytic performance of SiW/SiO2 catalysts was investigated on the isomerization reaction of endo-tetrahydrodicyclopentadiene（endo-TCD） to form adamantane（ADH） in a 100 mL stainless steel batch reactor equipped with a stirrer.The relations between the physical and chemical properties of the catalysts and their activity were discussed.The experimental results showed that the suitable SiW loading was 40% in weight.When the activation temperature of the catalyst was 250℃,the reaction temperature was 240℃,the reaction time was 3 hours,the initial pressure was 1.1MPa,the mass ratio of catalyst and material was 0.9 and the molar ratio of cyclohexane and endo-TCD was 5,the endo-TCD conversion reached 96.9%,and the maximum yield of ADH was up to 17.8%.

关 键 词：金刚烷 12-硅钨酸 硅胶 异构化 

分 类 号：TQ032.41[化学工程]