Zn-MpolyP阻燃玻纤增强尼龙66的界面相容性与热降解研究
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摘要
复合材料在当今经济飞速发展的时代,已经成为国民经济和人们日常生活中必不可少的重要材料,其中以玻璃纤维增强复合材料的研究最为完善,其应用领域也最为广泛。由于玻璃纤维增强尼龙复合材料的高机械性能和在汽车、电子电器等行业的广泛的应用,所以其阻燃性就被人们所重视。但是由于玻璃纤维产生的“烛芯效应”使得玻纤增强尼龙的阻燃变得很困难。传统的卤素阻燃玻纤增强尼龙虽然很好,但是在燃烧时释放出有毒的烟和气体,对环境造成了很大危害,所以玻纤增强尼龙的无卤阻燃的研究就变得非常的重要,而要获得高性能的无卤阻燃玻纤增强尼龙复合材料,其材料中各组分之间的界面相容性等情况就成为其关键。
本文以实验室合成的多聚磷酸蜜铵盐(MpolyP)和锌离子改性的的多聚磷酸蜜铵盐(Zn-MpolyP)为阻燃剂,用玻璃纤维为增强体来制备阻燃玻璃纤维增强尼龙66的复合材料(PA66/GF/FR)。然后对复合材料的结构形态、力学性能、热降解行为、结晶行为,以及复合材料中各组分的表面性质分别进行了表征,通过这些手段来对阻燃玻璃纤维增强尼龙66的复合材料(PA66/GF/FR)的界面相容性进行研究。
采用反相气相色谱(IGC)技术表征复合材料中各组分的表面色散自由能和Lewis酸碱性,实验数据表明:各组分表面色散自由能大小关系为:Zn-MpolyP＞MpolyP＞PA66＞Glass fiber。相对Lewis碱性(K_b/K_a)大小关系为:PA66(7.17)＞Glass fiber(5.61)＞MpolyP(4.00)＞Zn-MpolyP(2.32)。说明Zn-MpolyP与PA66和Glass fiber比MpolyP与PA66和Glass fiber有更强的路易斯酸碱吸附作用,导致Zn-MpolyP与PA66和Glass fiber之间的界面粘结强度也要更强,主要是由于Zn-MpolyP中的Zn~(2+)与尼龙66(PA66)和玻璃纤维中的O和N的孤对电子之间有强烈的络合作用。
阻燃剂能显著提高复合材料的拉伸强度和弯曲强度,特别是Zn-MpolyP阻燃剂,但它们都能降低缺口冲击强度。Zn-MpolyP阻燃的玻纤增强尼龙66的复合材料拉伸强度、弯曲强度和缺口冲击强度都高于MpolyP阻燃的玻纤增强尼龙66的复合材料,说明了Zn-MpolyP阻燃的玻纤增强尼龙66的复合材料的界面相容性要更好。Zn-MpolyP阻燃的玻纤增强尼龙66的复合材料在阻燃剂含量为15%的时候拉伸强度、弯曲强度和缺口冲击强度达到最大,分别为180.73MPa、257.84MPa和7.79 kJ·m~(-2)。
扫描电镜(SEM)结果证明了阻燃剂Zn-MpolyP和MpolyP在阻燃玻纤增强尼龙66体系中有很好的分散性,并且提高了尼龙66与玻璃纤维之间界面的相互作用,使界面的粘结强度增加。而且Zn-MpolyP阻燃的玻纤增强尼龙66复合材料(PA66/GF/Zn-MpolyP)要比MpolyP阻燃的玻纤增强尼龙66复合材料(PA66/GF/MpolyP)的界面的粘结强度要好,界面相容性要好。
利用DSC研究了阻燃剂和阻燃剂的含量对尼龙66的结晶焓和结晶温度的影响。阻燃剂Zn-MpolyP和MpolyP作为成核剂都起到了成核的作用,都可以提高尼龙66的结晶度和结晶温度。阻燃剂Zn-MpolyP对提高尼龙66的结晶度和结晶温度更加明显,这说明Zn-MpolyP起到的成核效果要比MpolyP好。
利用热重分析研究了阻燃的玻纤增强尼龙66复合材料(PA66/GF/FR)的热降解行为,结果表明:阻燃剂的加入改变了PA66的降解过程,使之成炭化学反应提前,提高残炭量。复合材料(PA66/GF/Zn-MpolyP)的初始分解温度,第一和第二失重速率峰值温度要比复合材料(PA66/GF/MpolyP)的要高,但残炭量却降低
Nowadays, composites already are indispensable material in national economy and daily life, and the research of glass fiber reinforced composites is the most perfect, at the same time the application of composites reinforced glass fiber is also most broad. Glass fiber reinforced PA66 has more practical applications, such as automobile, electric, electronic etc, due to enhanced softening point and mechanical performance. But the glass fiber reinforced nylon was quite difficult to flame retardanted because of the "candlewick effect" of the glass fibers. Traditional halogen-containing flame retardant and glass fiber reinforced nylon is very important, but it was bad for environment, and released noxious air at burning. Therefore, the research of halogen-free flame retardant glass fiber reinforced nylon is very important. In order to improve the high-performance of halogen-free flame retardant glass fiber reinforced nylon, the interfacial interaction and compatibility are most important, issues that researchers have been paied attention to.
In the paper, the flame retarded and glass fiber reinforced PA66 composites(PA66/GF/FR) were prepared with glass fiber and the flame retardant of (MpolyP) or Zn-MpolyP. The Morphological structures, mechanical properties, crystallization and melting behavior, thermal degradation behavior, and Surface properties of the components of the composites were studied. According to the results, the interfacial interaction and compatibility of PA66/GF/FR were discussed
Surface properties of the components of the composites were analyzed by inverse gas chromatography (IGC).The results show that the sorption of Lewis acid-base is stronger between Zn-MpolyP and nylon 66 or Glass fiber than MpolyP and nylon 66 or Glass fiber. This result is probably due to the strong complex between Zn~(2+) in Zn-MpolyP and lone pair electrons at O and N atoms of PA66 and Glass fiber.
The mechanical properties of flame retarded and glass fiber reinforced PA66 composites were investigated. The results show that the tensile strength, flexural strength and Notched Izod impact strength of Zn-MpolyP flame retarded and glass fiber reinforced PA66 composites (PA66/GF/Zn-MpolyP) were much higher than these of MpolyP flame retarded and glass fiber reinforced PA66 composites(PA66/GF/MpolyP).
Morphological structures of the flame retarded and glass fiber reinforced PA66 composites were observed by SEM. The results show the interfacial interaction and compatibility between PA66 and glass fiber were not good. However the flame retardants, MpolyP and Zn-MpolyP, could obviously improve the interfacial interaction and compatibility between PA66 and glass fiber. The effect of Zn-MpolyP was much better than that of MpolyP.
The non-isothermal crystallization of PA66/GF/FR were investigated by DSC. The results show that MpolyP and Zn-MpolyP could clearly enhance the enthalpy (△H_c) and temperature(T_C) of PA66 crystallization in the composites, because the flame retardants present the good nucleation function in PA66. The enthalpy (△AH_c) of PA66 crystallization in PA66/GF/Zn-MpolyP was higher than that in PA66/GF/MpolyP. It further proved that the flame retardants, especially Zn-MpolyP, could improve the interfacial interaction and compatibility among components in the composites.
The thermal degradation behavior of PA66/GF/FR composites was studied by thermal gravimetric analysis (TGA). The results show that the flame retardants of MpolyP and Zn-MpolyP changed the thermal degradation behavior of PA66, and improved the char residue formation. The T_(initial) , T_(1peak) and T_(2peak) of Zn-MpolyP flame retarded and glass fiber reinforced PA66 composites(PA66/GF/ Zn-MpolyP) were higher than MpolyP flame retarded and glass fiber reinforced PA66 composites(PA66/GF/ Zn-MpolyP).
本文以实验室合成的多聚磷酸蜜铵盐(MpolyP)和锌离子改性的的多聚磷酸蜜铵盐(Zn-MpolyP)为阻燃剂,用玻璃纤维为增强体来制备阻燃玻璃纤维增强尼龙66的复合材料(PA66/GF/FR)。然后对复合材料的结构形态、力学性能、热降解行为、结晶行为,以及复合材料中各组分的表面性质分别进行了表征,通过这些手段来对阻燃玻璃纤维增强尼龙66的复合材料(PA66/GF/FR)的界面相容性进行研究。
采用反相气相色谱(IGC)技术表征复合材料中各组分的表面色散自由能和Lewis酸碱性,实验数据表明:各组分表面色散自由能大小关系为:Zn-MpolyP＞MpolyP＞PA66＞Glass fiber。相对Lewis碱性(K_b/K_a)大小关系为:PA66(7.17)＞Glass fiber(5.61)＞MpolyP(4.00)＞Zn-MpolyP(2.32)。说明Zn-MpolyP与PA66和Glass fiber比MpolyP与PA66和Glass fiber有更强的路易斯酸碱吸附作用,导致Zn-MpolyP与PA66和Glass fiber之间的界面粘结强度也要更强,主要是由于Zn-MpolyP中的Zn~(2+)与尼龙66(PA66)和玻璃纤维中的O和N的孤对电子之间有强烈的络合作用。
阻燃剂能显著提高复合材料的拉伸强度和弯曲强度,特别是Zn-MpolyP阻燃剂,但它们都能降低缺口冲击强度。Zn-MpolyP阻燃的玻纤增强尼龙66的复合材料拉伸强度、弯曲强度和缺口冲击强度都高于MpolyP阻燃的玻纤增强尼龙66的复合材料,说明了Zn-MpolyP阻燃的玻纤增强尼龙66的复合材料的界面相容性要更好。Zn-MpolyP阻燃的玻纤增强尼龙66的复合材料在阻燃剂含量为15%的时候拉伸强度、弯曲强度和缺口冲击强度达到最大,分别为180.73MPa、257.84MPa和7.79 kJ·m~(-2)。
扫描电镜(SEM)结果证明了阻燃剂Zn-MpolyP和MpolyP在阻燃玻纤增强尼龙66体系中有很好的分散性,并且提高了尼龙66与玻璃纤维之间界面的相互作用,使界面的粘结强度增加。而且Zn-MpolyP阻燃的玻纤增强尼龙66复合材料(PA66/GF/Zn-MpolyP)要比MpolyP阻燃的玻纤增强尼龙66复合材料(PA66/GF/MpolyP)的界面的粘结强度要好,界面相容性要好。
利用DSC研究了阻燃剂和阻燃剂的含量对尼龙66的结晶焓和结晶温度的影响。阻燃剂Zn-MpolyP和MpolyP作为成核剂都起到了成核的作用,都可以提高尼龙66的结晶度和结晶温度。阻燃剂Zn-MpolyP对提高尼龙66的结晶度和结晶温度更加明显,这说明Zn-MpolyP起到的成核效果要比MpolyP好。
利用热重分析研究了阻燃的玻纤增强尼龙66复合材料(PA66/GF/FR)的热降解行为,结果表明:阻燃剂的加入改变了PA66的降解过程,使之成炭化学反应提前,提高残炭量。复合材料(PA66/GF/Zn-MpolyP)的初始分解温度,第一和第二失重速率峰值温度要比复合材料(PA66/GF/MpolyP)的要高,但残炭量却降低
Nowadays, composites already are indispensable material in national economy and daily life, and the research of glass fiber reinforced composites is the most perfect, at the same time the application of composites reinforced glass fiber is also most broad. Glass fiber reinforced PA66 has more practical applications, such as automobile, electric, electronic etc, due to enhanced softening point and mechanical performance. But the glass fiber reinforced nylon was quite difficult to flame retardanted because of the "candlewick effect" of the glass fibers. Traditional halogen-containing flame retardant and glass fiber reinforced nylon is very important, but it was bad for environment, and released noxious air at burning. Therefore, the research of halogen-free flame retardant glass fiber reinforced nylon is very important. In order to improve the high-performance of halogen-free flame retardant glass fiber reinforced nylon, the interfacial interaction and compatibility are most important, issues that researchers have been paied attention to.
In the paper, the flame retarded and glass fiber reinforced PA66 composites(PA66/GF/FR) were prepared with glass fiber and the flame retardant of (MpolyP) or Zn-MpolyP. The Morphological structures, mechanical properties, crystallization and melting behavior, thermal degradation behavior, and Surface properties of the components of the composites were studied. According to the results, the interfacial interaction and compatibility of PA66/GF/FR were discussed
Surface properties of the components of the composites were analyzed by inverse gas chromatography (IGC).The results show that the sorption of Lewis acid-base is stronger between Zn-MpolyP and nylon 66 or Glass fiber than MpolyP and nylon 66 or Glass fiber. This result is probably due to the strong complex between Zn~(2+) in Zn-MpolyP and lone pair electrons at O and N atoms of PA66 and Glass fiber.
The mechanical properties of flame retarded and glass fiber reinforced PA66 composites were investigated. The results show that the tensile strength, flexural strength and Notched Izod impact strength of Zn-MpolyP flame retarded and glass fiber reinforced PA66 composites (PA66/GF/Zn-MpolyP) were much higher than these of MpolyP flame retarded and glass fiber reinforced PA66 composites(PA66/GF/MpolyP).
Morphological structures of the flame retarded and glass fiber reinforced PA66 composites were observed by SEM. The results show the interfacial interaction and compatibility between PA66 and glass fiber were not good. However the flame retardants, MpolyP and Zn-MpolyP, could obviously improve the interfacial interaction and compatibility between PA66 and glass fiber. The effect of Zn-MpolyP was much better than that of MpolyP.
The non-isothermal crystallization of PA66/GF/FR were investigated by DSC. The results show that MpolyP and Zn-MpolyP could clearly enhance the enthalpy (△H_c) and temperature(T_C) of PA66 crystallization in the composites, because the flame retardants present the good nucleation function in PA66. The enthalpy (△AH_c) of PA66 crystallization in PA66/GF/Zn-MpolyP was higher than that in PA66/GF/MpolyP. It further proved that the flame retardants, especially Zn-MpolyP, could improve the interfacial interaction and compatibility among components in the composites.
The thermal degradation behavior of PA66/GF/FR composites was studied by thermal gravimetric analysis (TGA). The results show that the flame retardants of MpolyP and Zn-MpolyP changed the thermal degradation behavior of PA66, and improved the char residue formation. The T_(initial) , T_(1peak) and T_(2peak) of Zn-MpolyP flame retarded and glass fiber reinforced PA66 composites(PA66/GF/ Zn-MpolyP) were higher than MpolyP flame retarded and glass fiber reinforced PA66 composites(PA66/GF/ Zn-MpolyP).
引文
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