磷氮复合阻燃剂DMS的合成及其阻燃增韧PLA  

Synthesis of phosphorous-nitrogen compound flame retardant and its application in flame retardant toughened polylactic acid

作　　者：贺心怡 范家鑫 唐龙祥 HE Xinyi;FAN Jiaxin;TANG Longxiang(School of Chemistry and Chemical Engineering,Hefei University of Technology,Hefei 230009,China)

机构地区：[1]合肥工业大学化学与化工学院,安徽合肥230009

出　　处：《弹性体》2023年第6期21-27,共7页China Elastomerics

基　　金：省级大学生创新创业计划项目(S202210359130)。

摘　　要：利用9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、对苯二甲醛(TPA)和三聚氰胺(ME)合成了磷氮复合阻燃剂(DMS)。傅立叶变换红外光谱(FTIR)测试证明了DMS的成功制备。热重分析(TGA)结果表明,DMS具有较好的热稳定性与优秀的成炭能力。将聚乳酸(PLA)、DMS、热塑性聚酯弹性体(TPEE)与增容剂环氧大豆油(ESO)共混制备了阻燃增韧PLA复合材料。添加质量分数为1%DMS、5%TPEE、5%ESO的PLA复合材料,其极限氧指数(LOI)为30%,UL-94垂直燃烧测试中达到V-0等级。锥形量热(CCT)测试结果显示,峰值热释放速率(PHRR)和总热释放(THR)相比于纯PLA大幅度下降,表明DMS具有优异的阻燃能力;其冲击强度相比纯PLA提升了291%,表明TPEE对于PLA具有较好的增韧作用。扫描电子显微镜(SEM)和拉曼光谱(LRS)测试表明,DMS的添加可以促使PLA复合材料形成连续致密的炭层。The phosphorus-nitrogen compound flame retardant DMS was synthesized from 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide(DOPO),terephthalaldehyde(TPA)and melamine(ME).The successful synthesis of DMS was proved by Fourier infrared spectroscopy(FT-IR)measurement.The thermogravimetric analysis(TGA)results indicate that DMS has better thermal stability and excellent char formation ability.The flame retardant and toughened PLA composites were prepared by blending PLA with DMS and thermoplastic polyether ester elastomer(TPEE),epoxidized soybean oil(ESO)as compatibilizer.The PLA composite with 1%DMS,5%TPEE and 5%ESO of weight has a LOI value of 30%and passes the UL-94 test with a V-0 rating.The cone calorimeter(CCT)results show a significant decrease in peak heat release rate(PHRR)and total heat release(THR)compared to pure PLA,indicating that DMS has excellent flame retardancy performance.The impact strength of the PLA composite increases by 291%compared to neat PLA,indicating that TPEE possesses a good toughening effect for PLA.Moreover,scanning electron microscopy(SEM)and laser Raman spectroscopy(LRS)measurements show that the addition of DMS can promote the continuous and compact char formation of PLA composites.

关 键 词：聚乳酸 阻燃 增韧 磷氮复合阻燃剂 

分 类 号：TQ328.1[化学工程—合成树脂塑料工业]