N-P-Si三元阻燃剂的合成及其在Lyocell纤维中的应用  

Synthesis of N-P-Si ternary flame retardant and its application in Lyocell fiber

作　　者：宋俊[1] 史开敏 SONG Jun;SHI Kai-min(School of Material Science and Engineering,Tiangong University,Tianjin 300387,China)

机构地区：[1]天津工业大学材料科学与工程学院,天津300387

出　　处：《天津工业大学学报》2022年第4期36-42,共7页Journal of Tiangong University

基　　金：国家基础研究计划项目(973计划)(2014CB660813);天津市自然科学基金资助项目(14JCQNJC03600)。

摘　　要：为提高Lyocell纤维的阻燃性能,将六氯环三磷腈与3-氨基丙基三乙氧基硅烷反应,合成一种新型绿色环保的三元一体P-N-Si无卤阻燃剂六(3-氨基丙基三乙氧基硅)环三磷腈,采用1H NMR、FTIR、XPS及TG/DTG对阻燃剂的结构与性能进行表征;将合成的阻燃剂六(3-氨基丙基三乙氧基硅)环三磷腈应用于Lyocell纤维,采用三浸三轧的后整理法制备了阻燃Lyocell纤维,对阻燃Lyocell纤维进行FTIR和XPS表征,并测试了阻燃Lyocell纤维的TG/DTG、极限氧指数(limiting oxygen index,LOI)、燃烧后形貌和热裂解-气相质谱,通过测试结果对阻燃Lyocell纤维的阻燃机理进行了分析。结果表明:阻燃剂初始分解温度为214℃,在798℃时炭残留量约为27.03%;LOI值显示合成的阻燃剂可赋予Lyocell较好的阻燃性能,当阻燃剂的质量分数为30%、水洗次数为20次时,整理后的Lyocell纤维LOI为26.4%;热重分析结果表明整理后的Lyocell纤维在798℃时的残炭量提高16.9%;热裂解-气相质谱及燃烧后纤维形貌表明,合成的阻燃剂对Lyocell纤维的阻燃改性,主要基于凝聚相和气相阻燃模式协同作用。In order to improve flame retardant performance of Lyocell fiber, hexachlorocyclotriphosphazene reacted with 3-aminopropyl triethoxysilane to synthesize a new green environmentally ternary P-N-Si halogen-free flame retardant. The structure of the synthetic flame retardant was characterized by1H NMR, FTIR and XPS, and its thermal properties were performed by TG/DTG. The flame retardant was applied to process Lyocell fiber, and the flameretardant Lyocell fiber was prepared by a finishing method. The flame-retardant Lyocell fiber was characterized by FTIR and XPS. Then, TG/DTG, LOI, surface morphology after combustion and thermal pyrolysis-gas-mass spectrometry were used to characterize the flame-retardant propery and analyze the flame retardant mechanism of the fiber. The results show that the initial decomposition temperature of the flame retardant is 214 ℃, and the carbon residue is about 27.03% at 798 ℃. The LOI value shows that flame retardant agent can give Lyocell better flame retardant performance. When the mass fraction of flame retardant is 30% and the value of washing times is 20, the LOI of the finished Lyocell fiber is 26.4%. The results of thermogravimetric analysis show that the residual carbon content at 798 ℃ increases by 16.9%. Pyrolysis-gas-phase mass spectrometry and the morphology of the fiber after combustion show that the flame retardant modification of Lyocell fiber by the synthesized flame retardant is mainly based on the condensed phase and gas phase flame retardant mode.

关 键 词：阻燃剂 LYOCELL纤维 阻燃性能 

分 类 号：TS195.17[轻工技术与工程—纺织化学与染整工程]