磷钨酸原位改性HMS催化苯甲醚乙酰化反应

Catalytic Synthesis of p-Methoxy Acetophenone with Modification Catalyst HMS by Phosphotungstic Acid

以正十二胺(DDA)为模板剂、正硅酸四乙酯(TEOS)为硅源、磷钨酸(HPW)为活性组分,经原位合成法制备了HPW改性的介孔材料HMS(HPW-HMS),并以此催化剂催化苯甲醚与乙酸酐发生傅-克(Friedel-Crafts)酰基化反应合成对甲氧基苯乙酮,对催化剂进行了XRD和IR表征,研究了催化剂制备方法、脱除模板剂的方式以及催化反应条件,考察反应温度、反应时间、催化剂质量、反应物的物质的量等对苯甲醚转化率和主产物对甲氧基苯乙酮选择性的影响。实验结果表明,固体催化剂HPW-HMS在此反应中具有较高的催化活性,当反应温度100℃,反应时间4h,催化剂质量0.15g,原料物质的量比n(苯甲醚)∶n(乙酸酐)=1∶1.5时,苯甲醚转化率达到83.1%,对甲氧基苯乙酮选择性达97.3%。

The modification solid catalyst HMS by phosphotungstic acid was prepared by in-situ synthesis from DDA, TEOS, and phosphotungstic acid, and applied in p-Methoxy acetophenone production with the Friedel-Crafts acylation reaction of phenyl methyl ether and Acetic anhydride. The factors including reaction temperature, reaction time, catalyst amount, reactants molar ratio phenyl methyl ether to Acetic anhydride on the Friedel-Crafts acylation reaction were investigated. The experimental effects show that solid acid catalyst HMS has high catalytic activity. The acylation reaction conversion can reach 83.1% and the selectivity of p-Methoxy acetophenone production is 97. 3% under the following optimal conditions： reaction temperature of 100 ℃, reaction time of 4 h, amount catalyst of 0.15 g, molar ratio of n（anisole） ： n（acetic anhydride） ：1 ： 1.5.