新型单组分磷-氮膨胀型阻燃剂的合成及其阻燃性能  

Synthesis and Flame Retardant Properties of a Novel Monomolecular P-N Intumescent Flame Retardant

作　　者：毋登辉[1,2] 赵培华[1,2] 张美[1,2] 刘亚青[1,2] 李天凯[2] 廖登雄[2] 

机构地区：[1]中北大学山西省高分子复合材料工程技术研究中心,山西太原030051 [2]中北大学材料科学与工程学院,山西太原030051

出　　处：《合成化学》2013年第5期530-533,共4页Chinese Journal of Synthetic Chemistry

基　　金：教育部新世纪优秀人才支持计划(NCET-08-0889);山西省科技攻关项目(20100321082-02)

摘　　要：以氯化螺环磷酸酯(1)和对甲苯胺(2)为原料,经亲核取代反应合成了"三源"一体的新型单分子磷-氮膨胀型阻燃剂——季戊四醇螺环磷酰对甲苯胺(3),其结构经1H NMR和IR表征。考察了溶剂、原料配比、反应温度、反应时间和缚酸剂对3产率的影响。合成3的最佳反应条件为:乙腈为溶剂,三乙胺为缚酸剂,1 10mmol,n(1)∶n(2)=1∶3,于80℃反应4 h,产率79.3%。阻燃性能研究结果表明,3的初始分解温度为220℃,500℃成炭率达43.3%。A novel monomolecular P-N intumescent flame retardant,toluidine spirocyclic pentaerythritol bisphosphonate （3）,was synthesized by the nucleophilic substitution reaction of spirocyclic pentaerythritol bisphosphorate disphosphoryl chloride （1） and p-aminotoluene （2）.The structure was characterized by 1H NMR and IR.Effcets of solvent,reaction temperature,reaction time,mole ratio of raw materials and acid acceptor on the yield of 3 were investigated.The results showed that the optimum reaction conditions at 80 ℃ for 4 h were as follows：1 was 1 mmol,n （1） ∶ n （2） was 1 ∶ 3,acetonitrile was the solvent,and triethylamine was the acid acceptor,the yield of 3 was 79.3％.TGA study results showed that the initial decomposition temperature of 3 was 220 ℃,and the char yield is about 43.3 ％ at 500 ℃.

关 键 词：磷-氮膨胀型阻燃剂 氯化螺环磷酸酯 合成 阻燃性能 

分 类 号：O626.4[理学—有机化学] O625.6[理学—化学]