固相法合成螺环磷酰哌嗪酯阻燃剂

Synthesis of Flame Retardent Spirocyclic Piperazine Phosphate by Solid Phase Method

以螺环磷酰二氯(SPDPC)与哌嗪为原料,在未加溶剂和催化剂的条件下,用高速万能粉碎机粉碎混合原料的同时,借助转刀高速旋转的剪切力所产生的热能加热体系发生反应,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:n(螺环磷酰二氯)∶n(哌嗪)=1∶2,混合时间350s,在该条件下得到暗白色粉末状固体,产率达95%以上。产品用红外光谱和核磁共振波谱进行了表征。

With spirocyclic phosphate,3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphasprio undecane-3,9-dioxide（SPDPC） and piperazine as raw materials,which were mixed and ground in a high-speed multi-functional grinder,and with no solvent and catalyst in presence,spirocyclic piperazine phosphate was synthesized under the heat energy produced by the high-speed shear strength of the grinder′s rotating knife.The effect of the mole ratio of raw materials and the mixing time on the yield of the final product was studied and the optimum reaction conditions were identified.The yield of the final product in the shape of fuzzy white powder reached more than 95% when SPDPC and piperazine were mixed for 350 s in molar ratio 1∶2.The structure of the product was characterized by means of IR and NMR.