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作 者:张天永[1,2,3] 王梦颖[1] 李彬[1,3] 吴武斌[1] 刘茜[1]
机构地区:[1]天津大学化工学院,天津市应用催化科学与工程重点实验室,天津300354 [2]天津化学化工协同创新中心,天津300354 [3]天津市功能精细化学品技术工程中心,天津300354
出 处:《应用化学》2016年第10期1161-1167,共7页Chinese Journal of Applied Chemistry
基 金:国家自然科学基金(21276187);天津市自然科学基金(16JCYBJC20800);教育部博士点基金(20110032120011)资助项目~~
摘 要:以工业填料γ-Al_2O_3为催化剂,30%H_2O_2为氧化剂,冰醋酸为溶剂,一步法催化氧化偏三甲苯(TMB)合成2,3,5-三甲基苯醌(TMBQ)。考察了催化剂用量、反应温度、反应时间、氧化剂用量对该反应的影响。条件优化的结果为:m(γ-Al_2O_3)/m(TMB)=0.005,m(30%H_2O_2)/m(TMB)=2.5,反应时间2 h,反应温度80℃,得到TMB转化率为21.3%,TMBQ收率为16.0%,选择性为75.2%。通过XRD、FTIR、SEM、BET等技术手段,证明γ-Al_2O_3结晶度是影响氧化反应催化活性的关键因素。填料γ-Al_2O_3具有较大孔隙结构、比表面积较大、颗粒分布不均匀,为不规则片状,是廉价易得的工业品,具有较好的应用前景。2,3,5-Trimethylbenzoquinone (TMBQ) was synthesized by one-step catalytic oxidation of 1,2,4- trimethylbenzene (TMB) with industrial packing γ-alumina as catalyst, acetic acid as solvent, and 30% H202 as oxidant. The effects of catalyst amount, oxidant dosage, reaction temperature and reaction time were investigated. 21.3% conversion of TMB, 16. 0% yield of TMBQ, and 75.2% selectivity were obained under optimal conditions:m(γ-Al2O3)/m(TMB) =0. 005, m(30%H2O2)/m(TMB) =2. 5, reaction 2 h at 80 ℃. The catalyst's properties were characterized by SEM, XRD, FTIR and BET, indicating γ-Al2O3 's crystallinity is the key factor to catalytic activity. With pore structure, large specific surface area, uneven particle distribution, irregular lamellar structure, packing γ-Al2O3 is cheap, readily available and has bright prospects.
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