甲撑双(2,4-二叔丁基苯氧基)磷酸铝的合成

Synthesis of Methylene Bis (2, 4-di-tert-butyl-benzyloxy) Phosphonate Aluminum

以2,4-二叔丁基苯酚和甲醛为原料、甲苯为溶剂,经缩合、磷酸酯化、水解、中和等反应合成了PP成核剂甲撑双(2,4-二叔丁基苯氧基)磷酸铝。通过正交实验确定了最佳工艺条件,即n(酚):n(醛)为2:1,催化剂用量 (质量分数)为5％,缩合反应时间为4 h,三氯氧磷过量3％,酯化时间为2 h．酯化温度为40℃,最优条件下的实验总收率近55％。对各步产品进行了IR光谱分析及熔点测定。

Methylene bis （2, 4-di-tert-butyl-benzyloxy） phosphonate aluminum nucleating agent for PP was prepared with 2, 4-bis-tert-butyl phenol and formaldehyde as raw materials and toluene as solvent, by means of condensation, estification, hydrolysis and neutralization. The optimum technological conditions were determined by means of orthogonal experiment： the molar ratio of n （phenol） ： n （foraldehyde） = 2：1 ; catalyst 3% ; condensation time 4 h ; phosphorus oxychloride 3 %, estification time 2 h at room temperature. Under the above mentioned conditions the total excellent yield was about 55 %. The products were characterized by IR and melting point test.