新型磷系阻燃剂合成及其在聚丙烯中的应用  

Synthesis of a Novel Phosphorus Flame Retardant and Application for Polypropylene

作　　者：辛海亮 梁兵 XIN Hailiang;LIANG Bing(School of Material Science and Technology,Shenyang University of Chemical Technology,Shenyang,Liaoning 110142 ,China)

机构地区：[1]沈阳化工大学材料科学与工程学院

出　　处：《塑料》2019年第4期6-10,共5页Plastics

基　　金：中国辽宁省技术计划(2015304002)

摘　　要：以甲醛、DOPO、三氯氧磷为原料,制备了1种新型磷系阻燃剂三((6-氧代二苯并[c,e][1,2]氧杂膦嗪-6-基)甲基)磷酸酯(TOPMP),对反应的物料配比、溶剂用量、温度和时间进行了考察,TOPMP的最佳合成条件为:n(POCl3)∶n(DOPO-CH2OH)=1. 0∶3. 1,溶剂用量为DOPO-CH2OH质量的5倍,反应温度为80℃,反应时间为20 h。通过FT-IR、1HNMR与TG对阻燃剂的结构及热性能进行了测试表征;将TOPMP用于阻燃聚丙烯,并用TG、SEM分析了聚丙烯复合材料的阻燃性能、热性能及残炭形貌。TG结果表明:在800℃下,PP-3残炭率为20. 63%;扫描电镜结果表明:阻燃剂能够明显改善复合材料燃烧后的残炭形貌;当TOPMP加入量为30%时,聚丙烯复合材料的阻燃性能明显提高。A novel phosphorus flame-retardant,tris(( 6-oxodibenzo[c,e][1,2]oxaphosphazin-6-yl) methyl) phosphate( TOPMP) was synthesized by formaldehyde,DOPO and phosphorus oxychloride. The material ratio,solvent amount,temperature and time of the reaction were investigated. The results revealed that the optimum synthesis conditions were: n( POCl3) ∶ n( DOPO-CH2OH) = 1. 0 ∶ 3. 1,the solvent amount was 5 times by the mass of DOPO-CH2OH,the reaction temperature was 80 ℃,and the reaction time was 20 h. The chemical structure of the obtained compound was identified by FTIR and1 HNMR,and the thermal stability of TOPMP was tested by TG. The TOPMP was used in polypropylene,the thermal properties and carbon residue structure of the composite were characterized by TG and SEM,and the flame retardancy had been researched. TG results showed that residual carbon rate of PP-3 was 20. 63% at 800 ℃ . SEM results showed that the addition of flame retardancy could improve the carbon residue morphology after polypropylene combustion,and TOPMP could improve the flame resistance of polypropylene when TOPMP was 30%.

关 键 词：磷系阻燃剂 聚丙烯 复合材料 功能材料 力学性能 

分 类 号：TQ325.14[化学工程—合成树脂塑料工业]