摘要
以氯化磷酸二苯酯(DPCP)和1-氧代-4-羟甲基-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷(PEPA)为原料、4-(N,N-二甲氨基)吡啶(DMAP)为催化剂,合成了一种新型高效无卤阻燃剂(1-氧代-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷-4-基)甲基二苯基磷酸酯(OMDP),考察了溶剂种类、反应温度、催化剂用量和原料配比对产品收率的影响;并采用FTIR,NMR,MS,TG等手段对OMDP的结构进行了表征。实验结果表明,当以乙腈为溶剂、反应温度80℃、催化剂DMAP用量(基于PEPA的质量)1.85%(w)、n(DPCP)∶n(PEPA)=1.10∶1.00、反应24 h时,OMDP收率可达80.60%。热分析结果表明,所制备的OMDP具有很高的热稳定性。
A novel efficient halogen-free flame retardant,namely（1-oxido-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octan-4-yl）methyl diphenylphosphate（OMDP） was synthesized from diphenylchlorophosphate（DPCP） and 4-（hydroxymethyl）-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane 1-oxide（PEPA） with 4-（N,N-dimethyamino）pyridine（DMAP） as the catalyst. The influences of solvents,reaction temperature,catalyst dosage and feed ratio on the yield of OMDP were investigated. The structure of OMDP was characterized by means of FTIR,NMR,MS and TGDTA. The results showed that,the yield could reach 80.60% under the conditions of acetonitrile as the solvent,reaction temperature 80 ℃,the catalyst DMAP dosage 1.85%（based on the mass of PEPA）,n（DPCP）∶n（PEPA） 1.10∶1.00 and reaction time 24 h. The thermal analysis of the product OMDP indicated that its thermal stability was high.
出处
《石油化工》
CAS
CSCD
北大核心
2014年第8期934-937,共4页
Petrochemical Technology
基金
河南省科技厅基础前沿项目(13230041033)
河南省国际科技合作项目(134300510072)
河南省教育厅重点攻关项目(13B530916)
关键词
氯化磷酸二苯酯
无卤阻燃剂
磷酸酯
diphenylchlorophosphate
halogen-free flame retardant
phosphate
