Keggin型配合物[(CH_2)_5NH_2]_4SiMo_(12)O_(40)的合成及其催化氧化合成苯甲酸的研究  

STUDY ON SYNTHESIS OF Keggin COMPOUND[(CH_2)_5NH_2]_4SiMo_(12)O_(40) AND SYNTHESIS OF BENZOIC ACID BY CATALYTIC OXIDATIO WITH IT

作　　者：丁元生[1] 罗志臣[2] 周端文[1] 

机构地区：[1]吉林化工学院化学与制药工程学院,吉林吉林132022 [2]扬州工业职业技术学院化学工程系,江苏扬州225127

出　　处：《精细石油化工》2010年第3期19-22,共4页Speciality Petrochemicals

基　　金：吉林省教育厅自然科学基金资助项目(2008174)

摘　　要：实验以钼酸钠,硅酸钠为原料合成母体酸,以六氢吡啶为有机配体合成有机/无机电荷转移配合物[(CH2)5NH2]4Si Mo12O40。将合成的[(CH2)5NH2]4Si Mo12O40杂多酸哌啶盐应用于苯甲醛氧化合成苯甲酸反应,考察了催化剂用量、氧化剂30%H2O2的用量、反应温度、反应时间等对苯甲酸收率的影响。最佳工艺条件为:n(催化剂)∶n(苯甲醛)=0.003∶1,n(H2O2)∶n(苯甲醛)=7.2∶1,反应温度80℃,反应时间2.5h。苯甲酸收率达85%以上。The organic-inorganic hybrid catalyst [（CH2）5NH2-]4SiMo12O40 was prepared by matrix acid and piperidine as organic ligand. The matrix acid was synthesized by sodium molybdate and sodium silicate. The composition and structure of the catalyst were characterized by FT-IR, XRD, TG-DTA and elemental analysis. The results indicated that the heteropoly anions still reserved their Keggin structure in the compound. Its catalytic performance was evaluated in the oxidation of benzaldehyde to benzoic acid. The optimal reaction conditions were found as follows： n（catalyst） ： n（benzaldehyde）= 0. 003 ： 1; n（H2O2） ： n（benzaldehyde）=7.2 ： 1; reaction temperature 80℃ and reaction time 2.5 h. The yield of benzoic acid was above 85 %.

关 键 词：[(CH2)5NH2-]4SiMo12O40 KEGGIN结构 催化 苯甲酸 

分 类 号：TQ426.94[化学工程]