报道了一种新型双磷酸酯阻燃剂——新戊二醇双磷酸二苯酯(NDP)的合成方法.采用氯化磷酸二苯酯(DPCP)和新戊二醇(NPG)为原料,以4-二甲氨基吡啶(DMAP)为催化剂,成功合成了NDP,并考察了溶剂、原料配比、反应温度、反应时间、催化剂用量等因素对反应收率的影响.反应的最佳条件为:以正己烷为溶剂,DPCP和NPG的摩尔比为2:1,在0-5℃下反应12h,DMAP与DPCP的质量比为5.3％,反应收率可达89.1％.经核磁、红外表征证明产品结构正确.热分析表明产品的热稳定性好,其分解可分为2个阶段:第1阶段在290℃左右,此时分解速度最快,在400℃仍有18.03％的质量残余；第2阶段热分解出现在717℃左右.%A novel halogen-free bis-phosphate flame retardant, namely neopentyl glycol bis-( diphenylphosphate) (NDP) , was reported. NDP was synthesized by using chlorodiphenylphosphate (DPCP) and neopentyl glycol (NGP) as raw materials, and 4-diaminopyridine (DMAP) as catalyst. The factors that affect the yield were investigated, including solvent, molar ratio, reaction temperature, reaction time, and catalyst dosage. The optimum reaction conditions were obtained as follows; hexane as solvent, the molar ratio of DPCP to NGP is 2 :1, reaction time is 12 h at 0-5℃ , the mass ratio of DMAP to DPCP is 5. 3% , and the yield is as high as 89. 1%. The structure of NDP respectively determined by NMR and FTIR is correct. The thermal analysis of NDP shows that the product possesses high thermal stability. A two-stage process is involved during the thermal decomposition of NDP; the first appears at near 290 ℃ , where NDP is decomposed the fastest, and 18. 03 % mass residue still remains after 400 ℃ ; the last occurs at near 717 ℃ , which may be the decomposition of the char layer.
展开▼
