Keggin型配合物[(CH_2)_5NH_2]_5BW_(12)O_(40)的合成及其催化氧化合成苯甲酸的研究  被引量:1

Study on catalytic oxidation of benzaldehyde to benzoic acid with Keggin compound [(CH_2)_5NH_2]_5BW_(12)O_(40)

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作  者:庄志军[1] 丁元生[2] 

机构地区:[1]吉林化工学院教务处,吉林吉林132022 [2]吉林化工学院化学与制药工程学院,吉林吉林132022

出  处:《弹性体》2012年第6期28-31,共4页China Elastomerics

基  金:吉林省教育厅自然科学基金资助项目(2008174)

摘  要:以钨酸钠、硼酸为原料合成母体酸,以六氢吡啶为有机配体合成了有机/无机杂化电荷转移配合物[(CH2)5NH2]5BW12O40。通过红外光谱、X-射线衍射和热重分析表征,确认所合成的化合物中多酸阴离子仍保留Keggin结构。将新合成的[(CH2)5NH2]5BW12O40杂多酸哌啶盐应用到苯甲醛氧化合成苯甲酸反应中,考察了催化剂用量、氧化剂H2O2(质量分数为30%)的用量、反应温度、反应时间等对苯甲酸收率的影响。确定最佳工艺条件为:n(催化剂)∶n(苯甲醛)=1.880×10-3∶1;n(H2O2)∶n(苯甲醛)=4.760∶1;反应温度80℃;反应时间4h,此条件下苯甲酸的收率可达到80%。Organic/inorganic hybrid compound [(CH2) 5 NH2 ] 5BW12O40 was synthesized from ma- trix acid and piperidine,matrix acid was synthesized from sodium molybdate and phosphate. The struc- ture analysis suggusted that heteropoly anion in this compound was reserved its Keggin structure by IR , XRD, TG-DTA. By using [(CH2) 5 NH2 ] 5BW12O40 as the catalyst and 30 % H2O2 as the oxidation, the effects of catalyst dosage,oxidant dosage, reaction time and reaction temperature ect. , on the oxi- dation of benzaldehyde to benzoic acid were examined. The optimal tea ction conditions were identi- fied. Under the conditions as molar ratio of n(catalyst) : n(benzaldehyde) = 1. 880 × 10-3 : 1, molar ratio of n(H2O2): n(benzaldehyde)=4. 760 : 1, reaction time of 4 h, reaction temperature 80 ℃. The yield of benzoic acid achieves 80% and higher.

关 键 词:[(CH2)5NH2]5BW12O40 KEGGIN结构 催化 苯甲酸 

分 类 号:TQ426.94[化学工程]

 

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