催化剂循环使用合成聚甲基膦酸乙二醇酯

Synthesis of PEMP with Recycled Catalyst

膦酸酯是一类优秀的阻燃剂,被广泛地应用在各种阻燃材料中。聚甲基膦酸乙二醇酯(PEMP)是其中的一种。对催化剂循环使用合成PEMP进行了研究,用傅里叶红外光谱(FTIR)和磷核磁共振光谱(31PNMR)跟踪了循环使用催化剂的合成过程。结果表明,催化剂可以循环使用三次,继续循环,由于产品黏度增高,催化剂与产品分离困难。根据31PNMR计算PEMP的聚合度发现,催化剂循环使用,可以提高产品的聚合度。催化剂第一次使用所得PEMP产品的聚合度为6.64,循环使用三次,产品聚合度能提高到19.62。循环使用催化剂,PEMP收率基本不变,维持在60%左右。

The phosphonate is a kind of excellent flame retardant which is widely applied in all kinds of flame retardant materials, and the poly(oxy-1,2-ethanediyl)methylphosphonate(PEMP)is one of them. The synthesis of PEMP with recycled catalyst is studied. The FTIR and31 PNMR is used to trace the process of synthesis with recycled catalyst. The results show that the catalyst can be reused for 3 times. If continue using, it will be too difficult to separate the catalyst with the product due to the viscosity enhanced with increasing recycling times. By calculating the degree of poly-merization of PEMP according to the31 PNMR, it is found that the recycling of catalyst can improve the degree of polymerization of PEMP. When the catalyst is first used, the degree of polymerization of PEMP is 6.64;and after 3 times of recycling of catalyst, the degree of polymerization of product can reach 19.62. The yield of PEMP essentially unchanged by the recycling of catalyst, remains about 60%.