双羟基氨基磷酸酯的合成及其在棉织物上的应用

Synthesis of Di-hydroxyl Phosphoramidate and Application on Cotton Fabric

以亚磷酸二甲酯和二乙醇胺为原料,通过Atherton-Todd反应合成了双羟基氨基磷酸酯(DMHPA),并通过红外、核磁共振对DMHPA的结构进行表征。以丁烷四羧酸(BTCA)为交联剂,采用轧烘焙对棉织物进行阻燃整理,利用红外、电镜、能谱仪(EDS)对棉织物表面化学构成和形貌进行分析,利用极限氧指数(LOI)、垂直燃烧性能测试(VFT)、热重(TG)对整理棉织物的阻燃性能、热性能进行表征。结果表明:阻燃剂成功整理至棉织物上,整理后棉织物增重22.3%,极限氧指数可达到30.5%,损毁长度从300 mm下降到80 mm,在氮气条件下的残炭率提高到46.4%增加了30.5%,最大热分解速率下降了72.6%,经水洗15次极限氧指数下降到25.1%。结果表明,整理后棉织物有着良好的阻燃性和耐洗性。

To develop a durable non-formaldehyde flame retardant cotton fabrics,a novel phophoramidate compound,dimethyl-N,N′-bis(2-hydroxyethyl)phosphoramide(DMHPA)was synthesized by Atherton-Todd reaction using dimethyl phosphite and diethanolamine as raw materials.The product was then characterized by fourier transform infrared(FTIR)and nuclear magnetic resonance(NMR).Pad-dry-cure method was utilized to prepare flame retardant cotton fabrics.DMHPA was treated onto the cotton fabric in the presence of butane tetracarboxylic(BTCA)as a binder,and FTIR,scanning electron microscope(SEM)and energy dispersive spectrometer(EDS)were then used to investigated the chemical structure and surface morphology of the treated sample.To further investigate the flame retardant and thermal degradation of treated samples,limiting oxygen index(LOI),vertical flammability test and thermogravimetry(TG)were employed.Investigations show that DMHPA is successfully synthesized and treated onto cotton fabric.After treatment,the weight gain of the cotton fabric was 22.3%,and the limiting oxygen index could reach 30.5%,which could remain 25.1%after 15 washing cycles.As compared with control sample,the damage length decreases from 300 mm to 80 mm,carbon residue rate increases by 30.9%reaching 46.4%in nitrogen atmosphere.Moreover,the maximum thermal decomposition rate decreases by 72.6%.All these results show that the treated cotton fabric has good flame retardancy and washability.