2’-羟基联苯基-2-次膦酸的合成

SYNTHESIS OF 2'-HYDROXYBIPHENYL-2-YLPHOSPHINIC ACID

以2-羟基联苯(OPP)和三氯化磷为原料,采用两步法合成了新型阻燃剂中间体2’-羟基联苯基-2-次膦酸(HBP)。通过正交实验确定的适宜工艺条件为:m(催化剂):m(OPP)=0．006:1,n(PCl3):n(OPP)= 1．4:1;PCl2先在80℃滴加70％,剩余部分在180℃滴加,然后升温到220℃并维持反应2 h。在上述条件下,OPP的转化率达99％以上,HBP收率达93％以上,产物经熔点测定和红外表征确认。

A new flame retardant intermediate, 2-（2-hydroxyphenyl）-phenylphosphonic acid, was synthesized from o-phenylphenol （OPP） and phosphorus trichloride by two steps. By orthogonally designed experiments, the optimal synthetic conditions were obtained as follows, the amount of catalyst ZnCl2 was 0.6% based on OPP, n（PCl3） ： n（OPP）=1. 4 ： 1, after PCl3 was added in batches, reaction time 2 h at 220 ℃. Under these conditions, OPP conversion was above 99% and the yield of products was above 93 %.