光固化膨胀阻燃涂层的制备及交联聚乙烯的热老化与机理的研究
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摘要
本论文针对用于电线电缆的聚乙烯树脂高耐热高阻燃的要求,一方面研究了抗氧剂的种类和分子量对XLPE热老化进程的影响,揭示了抗氧剂的分子量和分子结构对延缓XLPE老化的重要性；另一方面研究了高膨胀阻燃涂层的阻燃特性和热解特性的影响因素,揭示涂层组成、结构与性能内在本质关系；同时优化阻燃体系,初步探讨其用于XLPE防火保护的可行性。主要研究工作如下：
(1)从膨胀阻燃体系的要素出发,首先用两种光活性单体三(丙烯酰氧基乙基)磷酸酯(TAEP)和三聚氰胺丙烯酸酯(MAAR)制备了磷氮体系的高膨胀阻燃涂层。通过对燃烧性能以及碳渣形貌的表征发现当TAEP与MAAR的质量比为2/1时,燃烧时可以形成表面致密、内部有许多大尺寸的薄壁泡孔结构的高膨胀炭层。通过对阻燃涂层的热解过程的研究发现固化膜的热解有着自己的独特性：含磷部分对气源部分的降解有着明显的催化作用；多种可燃气体甚至毒性气体cO的生成量比两者单独生成的都低。但所形成的高膨胀炭层在高温下仍有不少被氧化降解。为此,我们又制备了含磷氮硅和磷氮硼的燃涂层。通过对燃烧性能研究发现当涂层有合适的磷氮硅比或者磷氮硼比时,燃烧时既能形成高膨胀的蜂窝状炭层,义能够有效提高炭层的机械强度。对它们热解过程的研究发现含硅和含硼陶瓷前驱体的加入均对膨胀阻燃涂层的热解性能造成显著影响：炭渣在高温下的耐氧化性显著提高；多种气体的释放量显著降低；均可以有效抑制有毒气体cO的释放。
(2)基于延缓抗氧剂的物理损失以及化学消耗的理念,首先研究了不同分子量的受阻酚类抗氧剂对XLPE老化进程的影响,发现受阻酚类抗氧剂分子量越高,XLPE的老化进程越缓慢。其次研究了不同辅助抗氧剂与主抗氧剂1010复配稳定的XLPE的老化进程,发现硫醚类与受阻酚类抗氧剂的协同抗氧效果远比亚磷酸酯类与受阻酚类之间的协同效果好。第三,合成了一种高分子量的含硫受阻酚抗氧剂,并将其对XLPE的稳定效果与工业上两种同类抗氧剂进行比较,发现对于该类抗氧剂,硫原子的化学环境十分关键,不直接键接在受阻酚的对位上的或者直接与两个受阻酚相连的抗氧剂有较好的耐辐照性,其稳定的XLPE也体现出较高耐老化性。
(3)基于前面对高膨胀阻燃涂层的研究,将TAEP/MAAR/SiMA体系用于XLPE的防火保护中。锥形量热仪结果表明TAEP/MAAR/SiMA体系对XLPE有一定的防火保护作用,受热时可以有效生成高膨胀蜂窝状的炭层,对质量和热量的传递有较好的延迟效应。但由于XLPE与涂层或者膨胀炭层在受热时变形程度差异较大,导致了涂层或者炭层破裂,引发了其保护的XLPE燃烧,结果是总热释放量和质量损失程度相差无几。
(4)为了说明本论文所制备的阻燃耐热XLPE电缆料的优点,我们将高膨胀阻燃涂层涂覆的高耐热XLPE的性能与氢氧化铝阻燃的XLPE的性能进行比较,发现氢氧化铝阻燃的XLPE的力学性能、体积电阻率、耐热老化性明显恶化,原因在于大量无机粉体的加入导致了界面问题的产生。另外,虽然膨胀阻燃涂层处理的XLPE的总惹释放量与纯XLPE相差无几,但其热释放和质量损失更为缓和。
Polyethylene resin, when applied in the wire and cable materials, often has to reach the excellent flame retardance and high resistance to thermal aging. On the one hand, the effects of the kinds and molecular weight of various antioxidants on the thermal aging progress of cross-linking polyethylene (XLPE) were studied and the results revealed that the molecular weight and structure of antioxidants were of great importance to lengthen the lifetime of XLPE. On the other hand, the influence of the coating composition and structure on its thermal stability, combustion performance and fire resistance was investigated. The flame retardant systems were optimized for the protection of XLPE with high resistance to thermal aging. This dissertation consists of the following parts:
(1) Based on the intumescent flame retardant mechanism, the ratios of tri(acryloyloxyethyl) phosphate (TAEP) to melamine-based acrylate resin (MAAR) were adjusted to prepare a series of flame-retarded coatings containing phosphorus and nitrogen by UV-cured technology. The characterization of the flammability and the char morphologies of these coatings displayed that the highly intumescent char with compact outer layer and lots of thin-walled large pore structure in the inner layer for the PN-2which containing2/1mass ratio of TAEP to MAAR. The investigation for the thermal degradation process of the coatings showed that the decomposition of the blowing agents could be catalyzed by the acid source. Moreover, the amount of many evolved gas products, even extremely toxic carbon oxide, decreased obviously. The intumescent char layer, however, still presented large weight loss at high temperature due to the oxidative-degradation. So a series of the coatings containing phosphorus-nitrogen-silicon or phosphorus-nitrogen-boron were prepared. It can be found from the results of their flammability that the coatings with suitable amount of silicon or boron elements can produce the char layer with higher mechanical strength, but also exhibited little negative effect on the formation of dramatically intumescent char layer. Furthermore, the study of their thermal degradation gave the clear results that the addition of silicon-or boron-bearing monomers could endow the char layer with high tolerance of the oxidative-degradation at high temperature. Besides, to our surprise, the release of carbon oxide for these coatings could effectively be suppressed.
(2) It is relied that the improving efficiency of antioxidants on the stabilization of XLPE can be attained by retarding the physical loss and chemical exhaustion of antioxidants. To begin with, the influence of several hindered phenolic antioxidants with different molecular weight on the aging progress of XLPE was studied and it was found that the higher the molecular weight of antioxidant, the slower the aging development of XLPE. Then the primary antioxidant1010was combined with various second antioxidants to stabilize XLPE and the results showed that sulfur-bearing second antioxidants presented a better synergistic effect with antioxidant1010than phosphorus-containing ones. Finally, a novel sulfur-containing hindered phenolic antioxidant with a high molecular weight was prepared and its effect on protecting XLPE was compared with that of two antioxidants with similar structure. It was shown that the chemical circumstance of sulfur atom is the key point to determine the stability of antioxidants and the effect on the protection of XLPE. In other words, the antioxidants, in which sulfur atom is not bonded directly onto or have two direct chemical linkages with the hindered phenolic group, displayed better resistance to the electron-beam irradiation and better protection of XLPE from thermal aging.
(3) On the basement of the above study, the optimized flame retardant systems (TAEP/MAAR/SiMA) were used to protect XLPE. The flammability analysis by cone calorimeter showed that the extremely intumescent flame retardant coatings could effectively reduce the HRR and PHRR and postpone the mass loss and heat transfer, but had difficulties in avoid the combustion of XLPE due to the crack of the cured coating or the rigid char layer led by the large deformation of XLPE exposed to heat flux.
(4) In order to show the good points of XLPE wire and cable materials prepared in this dissertation, several significant properties of XLPE flame-retarded by the coating and ATH, respectively, were compared. It was shown that ATH worsened the mechanical properties, volume resistivity and tolerance of thermal aging of XLPE, which was ascribed to the poor compatibility of ATH with XLPE. In addition, it is noteworthy that XLPE flame-retarded by the coating presented the slower heat release rate and more moderate mass loss than XLPE flame-retarded by ATH, despite the lower THR for the latter.
(1)从膨胀阻燃体系的要素出发,首先用两种光活性单体三(丙烯酰氧基乙基)磷酸酯(TAEP)和三聚氰胺丙烯酸酯(MAAR)制备了磷氮体系的高膨胀阻燃涂层。通过对燃烧性能以及碳渣形貌的表征发现当TAEP与MAAR的质量比为2/1时,燃烧时可以形成表面致密、内部有许多大尺寸的薄壁泡孔结构的高膨胀炭层。通过对阻燃涂层的热解过程的研究发现固化膜的热解有着自己的独特性：含磷部分对气源部分的降解有着明显的催化作用；多种可燃气体甚至毒性气体cO的生成量比两者单独生成的都低。但所形成的高膨胀炭层在高温下仍有不少被氧化降解。为此,我们又制备了含磷氮硅和磷氮硼的燃涂层。通过对燃烧性能研究发现当涂层有合适的磷氮硅比或者磷氮硼比时,燃烧时既能形成高膨胀的蜂窝状炭层,义能够有效提高炭层的机械强度。对它们热解过程的研究发现含硅和含硼陶瓷前驱体的加入均对膨胀阻燃涂层的热解性能造成显著影响：炭渣在高温下的耐氧化性显著提高；多种气体的释放量显著降低；均可以有效抑制有毒气体cO的释放。
(2)基于延缓抗氧剂的物理损失以及化学消耗的理念,首先研究了不同分子量的受阻酚类抗氧剂对XLPE老化进程的影响,发现受阻酚类抗氧剂分子量越高,XLPE的老化进程越缓慢。其次研究了不同辅助抗氧剂与主抗氧剂1010复配稳定的XLPE的老化进程,发现硫醚类与受阻酚类抗氧剂的协同抗氧效果远比亚磷酸酯类与受阻酚类之间的协同效果好。第三,合成了一种高分子量的含硫受阻酚抗氧剂,并将其对XLPE的稳定效果与工业上两种同类抗氧剂进行比较,发现对于该类抗氧剂,硫原子的化学环境十分关键,不直接键接在受阻酚的对位上的或者直接与两个受阻酚相连的抗氧剂有较好的耐辐照性,其稳定的XLPE也体现出较高耐老化性。
(3)基于前面对高膨胀阻燃涂层的研究,将TAEP/MAAR/SiMA体系用于XLPE的防火保护中。锥形量热仪结果表明TAEP/MAAR/SiMA体系对XLPE有一定的防火保护作用,受热时可以有效生成高膨胀蜂窝状的炭层,对质量和热量的传递有较好的延迟效应。但由于XLPE与涂层或者膨胀炭层在受热时变形程度差异较大,导致了涂层或者炭层破裂,引发了其保护的XLPE燃烧,结果是总热释放量和质量损失程度相差无几。
(4)为了说明本论文所制备的阻燃耐热XLPE电缆料的优点,我们将高膨胀阻燃涂层涂覆的高耐热XLPE的性能与氢氧化铝阻燃的XLPE的性能进行比较,发现氢氧化铝阻燃的XLPE的力学性能、体积电阻率、耐热老化性明显恶化,原因在于大量无机粉体的加入导致了界面问题的产生。另外,虽然膨胀阻燃涂层处理的XLPE的总惹释放量与纯XLPE相差无几,但其热释放和质量损失更为缓和。
Polyethylene resin, when applied in the wire and cable materials, often has to reach the excellent flame retardance and high resistance to thermal aging. On the one hand, the effects of the kinds and molecular weight of various antioxidants on the thermal aging progress of cross-linking polyethylene (XLPE) were studied and the results revealed that the molecular weight and structure of antioxidants were of great importance to lengthen the lifetime of XLPE. On the other hand, the influence of the coating composition and structure on its thermal stability, combustion performance and fire resistance was investigated. The flame retardant systems were optimized for the protection of XLPE with high resistance to thermal aging. This dissertation consists of the following parts:
(1) Based on the intumescent flame retardant mechanism, the ratios of tri(acryloyloxyethyl) phosphate (TAEP) to melamine-based acrylate resin (MAAR) were adjusted to prepare a series of flame-retarded coatings containing phosphorus and nitrogen by UV-cured technology. The characterization of the flammability and the char morphologies of these coatings displayed that the highly intumescent char with compact outer layer and lots of thin-walled large pore structure in the inner layer for the PN-2which containing2/1mass ratio of TAEP to MAAR. The investigation for the thermal degradation process of the coatings showed that the decomposition of the blowing agents could be catalyzed by the acid source. Moreover, the amount of many evolved gas products, even extremely toxic carbon oxide, decreased obviously. The intumescent char layer, however, still presented large weight loss at high temperature due to the oxidative-degradation. So a series of the coatings containing phosphorus-nitrogen-silicon or phosphorus-nitrogen-boron were prepared. It can be found from the results of their flammability that the coatings with suitable amount of silicon or boron elements can produce the char layer with higher mechanical strength, but also exhibited little negative effect on the formation of dramatically intumescent char layer. Furthermore, the study of their thermal degradation gave the clear results that the addition of silicon-or boron-bearing monomers could endow the char layer with high tolerance of the oxidative-degradation at high temperature. Besides, to our surprise, the release of carbon oxide for these coatings could effectively be suppressed.
(2) It is relied that the improving efficiency of antioxidants on the stabilization of XLPE can be attained by retarding the physical loss and chemical exhaustion of antioxidants. To begin with, the influence of several hindered phenolic antioxidants with different molecular weight on the aging progress of XLPE was studied and it was found that the higher the molecular weight of antioxidant, the slower the aging development of XLPE. Then the primary antioxidant1010was combined with various second antioxidants to stabilize XLPE and the results showed that sulfur-bearing second antioxidants presented a better synergistic effect with antioxidant1010than phosphorus-containing ones. Finally, a novel sulfur-containing hindered phenolic antioxidant with a high molecular weight was prepared and its effect on protecting XLPE was compared with that of two antioxidants with similar structure. It was shown that the chemical circumstance of sulfur atom is the key point to determine the stability of antioxidants and the effect on the protection of XLPE. In other words, the antioxidants, in which sulfur atom is not bonded directly onto or have two direct chemical linkages with the hindered phenolic group, displayed better resistance to the electron-beam irradiation and better protection of XLPE from thermal aging.
(3) On the basement of the above study, the optimized flame retardant systems (TAEP/MAAR/SiMA) were used to protect XLPE. The flammability analysis by cone calorimeter showed that the extremely intumescent flame retardant coatings could effectively reduce the HRR and PHRR and postpone the mass loss and heat transfer, but had difficulties in avoid the combustion of XLPE due to the crack of the cured coating or the rigid char layer led by the large deformation of XLPE exposed to heat flux.
(4) In order to show the good points of XLPE wire and cable materials prepared in this dissertation, several significant properties of XLPE flame-retarded by the coating and ATH, respectively, were compared. It was shown that ATH worsened the mechanical properties, volume resistivity and tolerance of thermal aging of XLPE, which was ascribed to the poor compatibility of ATH with XLPE. In addition, it is noteworthy that XLPE flame-retarded by the coating presented the slower heat release rate and more moderate mass loss than XLPE flame-retarded by ATH, despite the lower THR for the latter.
引文
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