固相法合成螺环磷酰哌嗪酯阻燃剂

Spirocyclic Piperazine Phosphate Synthesized in Solid Phase

摘要:

本文将螺环磷酰二氯(SPDPC)与哌嗪按一定比例混合，在没有任何溶剂和催化剂的存在下，用高速万能粉碎机，在粉碎混合的同时，通过转刀高速旋转的剪切力所产生的热能，使体系加热，反应发生，合成了螺环磷酰哌嗪酯。分析了原料摩尔比以及混合时间对产品得率的影响，得出了较优的反应条件：螺环磷酰二氯与哌嗪的摩尔比1:2，混合350s。暗白色粉末状固体产品得率达到95%以上。产品用红外光谱和核磁共振谱进行了表征。

Abstract:

From spirocyclic phosphate, 3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphasprio [5.5]undecane-3,9-dioxide (SPDPC) and piperazine mixed in appropriate ratio in high speed universal grinder, no solvent and catalyst, spirocyclic piperazine phosphate was synthesized under the heat energy produced from the grinder rotating knife high-speed shear strength. The mole ratio of raw material and the mixing time were researched and the suitable reaction condition was identified. The result is SPDPC and piperazine were mixed 350 s in 1:2(n/n) and the fuzzy white powder yielded over 95%. The product’s structure was characterized by IR and NMR.