新戊二醇二硫代焦磷酸酯的合成与表征  

Synthesis and Characterization of Bisneopentyl Glycol Dithiocarboxyphosphate

作　　者：马君志 刘欢 宋焱 张帅[1] 王冬 MA Junzhi;LIU Huan;SONG Yan;ZHANG Shuai;WANG Dong(Shandong Engineering Research Center of Novel Functional Bio-based Fibers and Textiles,Dezhou University,Dezhou 253000,China;College of Information Engineering,Shandong Huayu Institute of Technology,Dezhou 253034,China;College of Textile Science and Engineering,Jiangnan University,Wuxi 214122,China)

机构地区：[1]德州学院新型功能生物基纤维与纺织品山东省工程研究中心,山东德州253000 [2]山东华宇工学院信息工程学院,山东德州253034 [3]江南大学纺织科学与工程学院,江苏无锡214122

出　　处：《山东化工》2024年第24期1-4,共4页Shandong Chemical Industry

基　　金：德州学院人才基金项目(2023xjrc125);山东省自然科学基金青年项目(ZR2023QE022)。

摘　　要：为提高新戊二醇二硫代焦磷酸酯合成效率与得率,选用4-二甲氨基吡啶为催化剂,采用一步法反应工艺合成新戊二醇二硫代焦磷酸酯。阐述了合成工艺选择及催化剂的催化作用机理,并对合成产物进行表征。结果表明:该一步法反应合成新戊二醇二硫代焦磷酸酯的总反应时间缩短至12 h以内,得率提高至85.30%。通过对新戊二醇二硫代焦磷酸酯FTIR、^(1)H NMR和XPS等测试结果进行分析,确定了合成产物的化学结构以及合成反应机理。表征了合成产物的微观表面形貌和结晶情况,并利用TGA热分析方法研究了新戊二醇二硫代焦磷酸酯在空气和氮气氛围下的热稳定性及热降解行为。结果表明:新戊二醇二硫代焦磷酸酯阻燃剂呈棒状,结晶度较高,具有良好的成炭性和热阻隔性能。In order to improve the synthesis efficiency and yield of bisneopentyl glycol dithiocarboxyphosphate,4-dimethylaminopyridine was selected as the catalyst.And a one-step reaction was adopted to synthesize the bisneopentyl glycol dithiocarboxyphosphate.The process selection and catalytic mechanism of the catalyst were explained,and the synthesized products were characterized.The results showed that the total reaction time for the one-step synthesis of bisneopentyl glycol dithiocarboxyphosphate was shortened to within 12 h,and the yield increased to 85.30%.By analyzing the results of FTIR,^(1)H NMR,and XPS of the synthesized product,the chemical structure formula and synthesis reaction mechanism of the synthesized product were determined.Then,the microstructure and crystallization of the synthesized product were characterized,and the thermal stability and degradation behavior of bisneopentyl glycol dithiocarboxyphosphate under air and nitrogen atmosphere were studied using TGA thermal analysis method.The results show that bisneopentyl glycol dithiocarboxyphosphate flame retardant is rod-shaped with high crystallinity,and has good carbonization and thermal barrier properties.

关 键 词：新戊二醇二硫代焦磷酸酯 合成 表征 热性能 

分 类 号：TQ314.248[化学工程—高聚物工业]