N,N-二甲基胺乙基膦酸-磷酸氢锆为载体的新型固体碱研究

Study on Solid Base Supported on Zirconium Dimethyl Aminoethylphosphonate-phosphate

以 N,N-二甲基胺乙基膦酸 -磷酸氢锆为载体 ,用 5% Na OH溶液处理制得固体碱 ,用元素分析、IR、TG、DTG、DTA、BET表面积、碱强度、碱量测定对固体碱进行了表征 .指示剂法测得其碱强度为 9.3～ 15.0 ,与常用固体碳酸钠碱强度相当 .苯甲酸滴定法测得固体碱的碱量 ,讨论了载体中有机膦酸的相对含量、保温时间对碱性的影响 ,固体碱用于催化 Knoevenagel缩合反应 ,有很高的催化活性 ,产物的收率高 ,副反应少 ,可重复使用 6～ 7次 ,且易于再生 ,是一种环境友好的新型绿色催化剂 .

Some solid bases Zr(HPO 4) 2- x [O 3PCH 2CH 2N(CH 3) 2] x ·H 2O NaOH were prepared by treating zirconium dimethylaminoethyl phosphonate phosphate supporter with 5%NaOH solution and characterized by elemental analysis, IR, TG DTG, DTA and BET surface area measurements. The base strengths of the solid bases were of 9 3~15 0, which corresponded to that of solid sodium carbonate. Their base numbers were measured by benzoic acid titration method to be in dependence with x value. The influences of the x value, temperature keeping time in the preparation of the supporter were studied. The solid bases showed high catalytic activity in typical Knoevenagel condensation reaction in high product yields and little side reactions. The solid base catalysts can be reused for 6 to 7 times and easily regenerated.