Keggin型配合物[（CH2）5NH2]5BW12O40的合成及其催化氧化合成苯甲酸的研究

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袁征，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、氧化责4H2O2（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%。

Study on catalytic oxidation of benzaldehyde to benzoic acid with Keggin compound [(CH2)5NH2]5BW12O40

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.