合成了一种新的固体酸催化剂3-吡啶磺酸-磷钼酸(PSA-HPM),利用X-射线粉末衍射(XRD)、红外光谱(FT-IR)、热重(TG)以及电位滴定等方法对其进行分析,并以油酸与甲醇的酯化反应为探针反应,考察了该催化剂对酯化反应的催化性能,系统探讨了催化剂用量、醇酸物质的量比、反应时间、反应温度以及催化剂重复利用等对催化反应的影响。结果表明,PSA-HPM具有典型的Keggin结构,在T〈352℃时表现出较好的热稳定性,同时具有较高的酸度;PSA-HPM在催化酯化反应中表现出了高的催化活性。当醇酸物质的量比为7∶1、催化剂用量为油酸质量的10 wt%、在80℃反应5 h后油酸甲酯产率达96.5%。PSA-HPM同时表现出好的重复利用性,4次使用后,催化剂的物相以及Keggin结构没有明显变化。
A novel solid acid was synthesized by the reaction of 12-molybdophosphoric acid(HPM) with 3-pyridine sulfonic acid(PSA) and confirmed by X-ray powder diffraction,FT-IR,TG and potentiometric titration.Then the solid acid was employed for esterification to evaluate its acid-catalytic activity.Various reaction parameters,including methanol/oleic acid molar ratio,catalyst dosage,reaction temperature and time were systematically examined.These results indicated that the prepared catalyst maintained the Keggin structure of the raw HPM,exhibited good thermal stability and higher acidity.The catalyst exhibited excellent catalytic activity in esterification and good reusability.96.5% conversion of oleic acid was obtained under the following conditions:mole ratio of alcohol to acid 7∶ 1,the reaction temperature 80 ℃,catalyst amount 10 wt% of the weight of oleic acid and the reaction time5 h.After the fourth recycling,there was no obvious change in phase and Keggin structure for the catalysts.