双DOPO结构化合物的合成及对PET织物阻燃性能与机理  

Synthesis of double DOPO structure compound and its flame retardancy and mechanism on PET fabrics

作　　者：闫鑫 沈勇[1] 徐丽慧[1] 王黎明[1] 徐鸿涛 王飞翔 潘虹 YAN Xin;SHEN Yong;XU Lihui;WANG Liming;XU Hongtao;WANG Feixiang;PAN Hong(School of Textile and Fashion,Shanghai University of Engineering Science,Shanghai 201620,China)

机构地区：[1]上海工程技术大学纺织服装学院,上海201620

出　　处：《材料科学与工艺》2024年第3期59-68,共10页Materials Science and Technology

基　　金：上海市自然科学基金面上项目(21ZR1426200);国家自然科学基金资助项目(51703123).

摘　　要：为提高对苯二甲酸乙二醇酯(PET)织物的阻燃抗熔滴性能,以9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)和对二甲醛(TDCA)合成了一种双DOPO结构的磷系阻燃剂(TDCA-DOPO),将其与三聚氰胺(MEL)复配,然后采用聚氨酯作为涂层剂,得到阻燃涂层剂用于PET织物阻燃。结果表明,当两种阻燃剂的质量比为2∶1,总添加量为20%时,极限氧指数提高到28.5%,在垂直燃烧试验中,阻燃涂层抑制了PET织物燃烧时熔滴滴落现象。SEM和EDS的结果显示,阻燃涂层在PET织物上均匀分布。从氮气气氛中的热重分析来看,阻燃PET织物在较高温度区的残炭率由6.5%增加到11.7%。残炭的SEM结果显示阻燃涂层促进PET织物形成膨胀性炭层。根据热裂解气相色谱、残炭的Raman和XPS数据分析结果,复合阻燃涂层在气相上生成含磷碎片与不可燃气体,并促进PET织物形成膨胀致密的炭层,同时具有气相与凝聚相阻燃效果。本研究内容可为PET阻燃抗熔滴剂的开发提供指导。In order to improve the flame retardant and drop-resistant properties of PET fabrics,a phosphor flame retardant with a DOPO structure was synthesized with 9,10-Dihydro-9-oxa-10-phosphazephenanthroline-10-oxide(DOPO)and p-diformaldehyde(TDCA).The TDCA-DOPO was mixed with melamine(MEL),and then polyurethane was used as coating agent.A flame retardant coating agent was obtained for PET fabric flame retardant.The results showed that when the mass ratio of the two flame retardants was 2∶1 and the total amount is 20%,the limiting oxygen index increased to 28.5%.In the vertical combustion test,the flame retardant coating inhibited the melting of PET fabric during combustion.Scanning electron microscopy and energy dispersion spectroscopy showed that the flame retardant coating was uniformly distributed on the PET fabric.According to the thermogravimetric analysis in nitrogen atmosphere,the carbon residue rate of flame retardant PET fabric increased from 6.5%to 11.7%at higher temperature.Scanning electron microscopy(SEM)of residual carbon showed that the flame retardant coating promoted the formation of an expansive carbon layer on PET fabric.The flame retardation mechanism was investigated by pyrolysis gas chromatography,Raman and X-ray photoelectron spectroscopy(XPS)data of residual carbon.

关 键 词：PET 阻燃整理 抗熔滴 DOPO衍生物 协同阻燃 

分 类 号：TQ323.41[化学工程—合成树脂塑料工业]