用PPA制备4,6-二氨基间苯二酚磷酸盐及其稳定化

为改进4,6-二氨基间苯二酚磷酸盐的合成工艺,采用多聚磷酸(PPA)法制备磷酸盐,并对其结构进行表征。结果表明:PPA法制磷酸盐的合成工艺,可以使反应时间从几天缩短到几个小时,反应产率从79.46%提高到91.12%。以次亚磷酸为还原剂对磷酸盐单体进行稳定化的研究表明:稳定后的磷酸盐在室温条件下储藏一个月后,基本不发生氧化。将稳定化后的单体和对苯二甲酸(TA)在PPA的介质中进行缩聚反应可以得到具有高聚合度(特性粘数η]=17 dL/g)的聚亚苯基苯并二噁唑(PBO)。

Preparation of 4,6- Diaminoresorcinol Diphosphate Salt by PPA and Its Stabilization

In order to improve the synthesis of 4,6-diaminoresorcinol diphosphate,we prepared 4,6-(diaminoresorcinol) diphosphate by polyphosphoric acid and characterized its structure.The preparation of(4,6-)diaminoresorcinol diphosphate by PPA method reduce reaction time from two or three days to some hours and enhance the yield from 79.46% to 91.12%.To enhance the stability of 4,6-diaminoresorcinol diphosphate,H_3PO_2 was used for the stabilization of 4,6-diaminoresorcinol diphosphate.The study manifests that 4,6-diaminoresorcinol diphosphate is stable for oxidization after being placed one month.PBO spinning solution was prepared from 4,6-diaminoresorcinol diphosphate in polyphosphoric acid by solution poly-condensation.The polymerization degree of obtained PBO is high and the inherent viscosity is(17 dL/g.)