磷氮接枝木质素磺酸盐的合成及成炭阻燃热塑性聚烯烃弹性体  

Synthesis of a Flame Retardant-Lignosulfonate by Grafting Phosphorus-Nitrogen and Its Application in Thermoplastic Polyolefin Elastomers

作　　者：张红[1] 冯钠[1] 张桂霞[1] 曲敏杰[1] 朱云[1] 霍阳[1] 

机构地区：[1]大连工业大学纺织与材料工程学院,辽宁大连116034

出　　处：《高分子材料科学与工程》2015年第9期11-16,共6页Polymer Materials Science & Engineering

基　　金：国家自然科学基金资助项目(21276034)

摘　　要：以木质素磺酸盐(LS)、三氯氧磷和咪唑为原料,采用两步法合成制备"三源一体"的高分子膨胀型阻燃剂——磷氮接枝木质素磺酸盐(PNLS),并采用红外光谱(FT-IR)、核磁共振(1 H-NMR)、X射线能谱(EDS)及热重分析(TGA)对其结构和热性能进行分析表征;探讨了PNLS对热塑性聚烯烃弹性体(TPO)阻燃性能的影响。结果表明,PNLS的FT-IR和1 H-NMR谱图中出现明显的特征峰,与目标产物结构一致;磷、氮元素的含量分别达到21.03%和5.63%;TPO/PNLS初始分解温度为213℃,700℃的残炭量为33.79%。阻燃性能测试表明,TPO/PNLS体系的氧指数达29.4%,且体系能够通过UL94V-0级。SEM分析显示体系残炭炭层完整致密。FT-IR表明PNLS中的磷酸酯键使炭源脱水成炭。The intumescent flame retardant which combines acid source, blowing agent and char-forming agent within an individual molecule, lignosulfonate by grafting phosphorus-nitrogen（PNLS）, was synthesized by two-step reaction using lignosulfonate, phosphorus oxychloride and imidazole. The structure of PNLS was characterized by FT-IR, 1H-NMR and EDS. Thermal property of PNLS was investigated by thermo gravimetric analyzer （TGA）. And the impact of PNLS on flame retardant properties of thermoplastic polyolefin elastomers （TPO） was discussed. The result shows that some characteristic absorption peaks appear in the FT-IR and 1H-NMR spectra of PNLS. EDS results indicate that the PNLS has 21.03 % of P and 5.63 % of N. From the TG analysis, the initial decomposition temperature of TPO/PNLS is 213 ℃ , the residual carbon content at 700 ℃ is 33.79 %. The limiting oxygen index （LOI） of TPO/PNLS composite rises up to 29.4 % and the composites reach UL 94 V-0 rating. SEM analysis reveals that the residual carbon is dense and intact. And the phosphate key of PNLS can make carbon dehydration and form char layer from FT-IR.

关 键 词：膨胀型阻燃剂 合成 木质素磺酸盐 热塑性聚烯烃弹性体 

分 类 号：TQ334.2[化学工程—橡胶工业]