低熔点高阻燃含磷共聚酯的制备及性能

Preparation and Properties of Low Melting Point and High Flame Retardant Phosphorus-Containing Copolyester

随着无纺布应用的日益增加需要开发一种低熔点阻燃聚酯。以对苯二甲酸、间苯二甲酸、乙二醇为主要原料,添加第四单体新戊二醇和第五单体3-羟基苯基膦酰丙酸(CEPPA)合成了一系列不同CEPPA质量分数的阻燃共聚酯(PIENT)。通过红外光谱分析仪及核磁共振波谱仪对其结构进行了表征。通过极限氧指数(LOI)、热重分析、差示扫描量热分析、扫描电镜(SEM)、万能力学试验机、显微熔点测定仪、乌氏黏度计、拉曼光谱仪对PIENT的阻燃性能、热性能、炭层形貌、力学性能、特性黏度及残炭率进行了研究。结果表明,随着CEPPA质量分数的增加,PIENT共聚酯的特性黏度、玻璃化转变温度和熔点会有降低,当CEPPA的质量分数为3%时,阻燃PIENT聚酯的力学性能较好,LOI值提高到31%,垂直燃烧等级可通过V-0级。当CEPPA质量分数为6%时,熔点从134℃下降到105℃,LOI从21%提高到33%,700℃残炭率高达21.54%。通过炭层SEM分析和拉曼分析,证明了CEPPA的加入对PIENT的阻燃性能有了较大的改善。

With the increasing application of non-woven fabrics,a low melting point flame retardant polyester was needed to develop.A series of flame retardant polyester with different 3-hydroxyphenylphosphinyl-propanoic acid(CEPPA)content was successfully synthesized,using terephthalic acid,isophthalic acid,ethylene glycol as the main raw materials.The structure of polymers was analyzed by infrared spectrum and hydrogen nuclear magnetic resonance(1 H NMR).The flame retardant properties,thermal properties,carbon layer morphology,mechanical properties,intrinsic viscosity and carbon residue of PIENT were studied by limiting oxygen index(LOI),thermogravimetric analysis,differential scanning calorimetry,scanning electron microscopy(SEM),universal mechanical testing machine,micro melting point tester,Ubbelohde viscometer and Raman spectrometer.The results show that the intrinsic viscosity,glass transition temperature and melting point of PIENT copolyester decrease with the increase of CEPPA mass fraction.When the mass fraction of CEPPA is 3%,the mechanical properties are better,and the LOI value of flame retardant PIENT polyester increases to 31%,and the vertical combustion grade can pass V-0 grade.When the mass fraction of CEPPA is 6%,melting point decreases from 134℃to 105℃,LOI increases from 21%to 33%,and the char residue at 700℃is as high as 21.54%.Through SEM analysis and Raman analysis of the carbon layer,it is proved that the addition of CEPPA has greatly improved the flame retardancy of PIENT.