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作 者:田志茗[1] 邓启刚[1] 赵德丰[2] 刘美华[1]
机构地区:[1]齐齐哈尔大学化学与化工学院,黑龙江齐齐哈尔161006 [2]大连理工大学精细化工国家重点实验室,辽宁大连116012
出 处:《合成化学》2010年第6期686-690,共5页Chinese Journal of Synthetic Chemistry
基 金:齐齐哈尔市工业攻关项目(GYGG-08001-3)
摘 要:以介孔分子筛SBA-15为载体,采用固相研磨法将Ce和SO42-同时掺杂在SBA-15中,合成了Ce-SO42-/SBA-15负载型催化剂(Cat)。用IR,XRD,TEM,低温N2吸附-脱附,TG和NH3-TPD等方法对Cat的结构性质及其表面酸性进行了研究。结果表明,Cat保持高度有序的一维六方介孔结构,且具有弱酸中心和中强酸中心。用Hammett指示剂法测得其表面酸强度为0.99~1.80,表明Cat为固体酸。将Cat用于催化合成乙酸正丁酯,正交实验结果表明:在冰乙酸0.126 mol,n(冰乙酸)∶n(正丁醇)=1.0∶1.2,Cat 375 mg,回流反应140 min的较佳反应条件下,酯化率达97.45%。Supported Ce-SO2-4/SBA-15 catalyst(Cat) was synthesized by solid state grinding method incorporated with amount of cerium and SO2-4.The structure and surface acidity of Cat were investigated by IR,XRD,TEM,low temperature nitrogen adsorption-desorption,TG and NH3-TPD techniques.The results showed that Cat keep highly ordered mesoporous one-dimensional hexagonal structure,possesses weak acid sites and medium strong acid sites.Surface acidity of Cat were 0.99~1.80 by Hammett indication method determination.It is indicated that Cat are solid acid catalyst.Catalytic performance of Cat were investigated by catalytic synthesizing n-butyl acetate.The optimum conditions of esterification were as follows: acetic acid was 0.126 mol;n(acetic acid)∶n(n-butanol) was 1.0 ∶1.2;amount of Cat was 375 mg;reflux reaction time was 140 min.The yield of n-butyl acetate was 97.45% under the optimum conditions.
关 键 词:SBA-15介孔分子筛 铈改性 固相合成 催化剂 酯化反应
分 类 号:TQ316.33[化学工程—高聚物工业]
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