双季戊四醇二亚磷酸酯阻燃剂的合成  

Synthesis of Fire Retardants of Dipentaerythritol Diphosphonate Ester

作　　者：周浩[1] 王丹[1] 张士磊[1] 职慧珍[1] 杨锦飞[1] 

机构地区：[1]南京师范大学化学与环境科学学院,江苏南京210097

出　　处：《南京师范大学学报（工程技术版）》2010年第2期48-52,共5页Journal of Nanjing Normal University(Engineering and Technology Edition)

基　　金：江苏省科技厅科技攻关项目(BE2007050)

摘　　要：以双季戊四醇(DPE)、亚磷酸三苯酯(TPP)为原料,氢氧化钠为催化剂,通过酯交换反应得到双季戊四醇二亚磷酸酯阻燃剂.用正交法讨论了原料物质的量之比、反应温度、反应时间、催化剂种类和用量对反应的影响,确定了反应的最佳条件:催化剂为氢氧化钠,其用量为反应物总质量的1%,n(P(OPh)3)∶n(C10H22O7)为2.06∶1,反应温度为100℃～110℃,反应时间为10 h,双季戊四醇二亚磷酸酯收率为86.3%.采用红外吸收光谱和元素分析初步证实了产品的结构.Dipentaerythritol cyclic phosphonate ester was synthesized from dipentaerythritol（TPE） and triphenylphosphite（TPP） in the presence of sodium hydroxide catalyst by a step of ester exchange reaction.The effects of process parameters,such as molar ratio,reaction temperature,reaction time and catalyst on the yield were studied respectively from orthogonal experiments.The suitable synthesis conditions were defined as follows： sodium hydroxide is the suitable catalyst,its dosage is 1% of the amount of all reactant,the molar ratio of triphenylphosphite and dipentaerythritol is 2.06∶1,the reaction temperature is 100℃～110℃,and the reaction time is 10 hours.On the above conditions,the synthesis productivity is 86.3%.The structure of the product was confirmed by IR and EA respectively.

关 键 词：双季戊四醇 亚磷酸三苯酯 酯交换 二亚磷酸酯 阻燃剂 

分 类 号：TQ265.1[化学工程—有机化工]