聚乳酸/次磷酸盐复合材料的制备、阻燃机理以及烟气毒性研究
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摘要
聚乳酸(PLA)是一种以可再生资源为原料制备的可降解聚合物。由于其优良的力学性能和生物相容性,聚乳酸公被认为是最具有发展潜质的非石油基聚合物。但是,其易燃性、燃烧过程中出现的大量有毒烟气以及熔融滴落严重制约了聚乳酸在相关领域的发展,因此,为了扩大聚乳酸材料的使用范围,研究和发展阻燃性聚乳酸材料显得非常重要。本文首先系统性综述了近几十年所开发出的无卤阻燃技术,探讨这些无卤阻燃技术在在聚乳酸中应用的可行性。其次,研究了几种次磷酸盐在聚乳酸复合材料中的热解以及阻燃机理。最后,采用稳态管式炉烟气毒性试验平台(SSTF)研究了几种聚乳酸复合材料在不同条件下的燃烧烟气毒性。
1.采用新型阻燃剂次磷酸铝(AHP),将其应用于聚乳酸的阻燃,制备出一系列PLA/AHP复合材料。热重测试表明,复合材料的成炭有明显提高,质量损失速率有明显降低。极限氧指数测试和垂直燃烧测试表明次磷酸铝可以提高复合材料的阻燃性能,20%次磷酸铝添加量即可使得次磷酸铝/次磷酸铝(PLA/AHP)复合材料达到UL-94VO级别,燃烧过程中的熔融滴落现象完全消失,极限氧指数达到27.5vol%;MCC测试和锥形量热测试表明次磷酸铝的加入可以有效降低热释放速率峰值；对燃烧后的炭渣进行SEM测试,燃烧形成的炭层更加致密。与此同时,DSC和DMA测试表明,次磷酸铝的加入有效提高了复合材料的结晶性能和储能模量。
2.借鉴次磷酸铝(AHP)在聚乳酸复合材料的优异表现,将次磷酸钙(CaHP)作为一种潜在的阻燃剂应用聚乳酸,制备出一系列聚乳酸/次磷酸钙阻燃复合材料。研究表明,次磷酸钙的加入亦有效提高聚乳酸/次磷酸钙(PLA/CaHP)复合材料的极限氧指数,30%次磷酸钙添加量可以使得复合材料达到UL94VO级别,滴落完全消失,极限氧指数为26.5vol%。MCC测试结果表明,次磷酸钙的加入可以降低复合材料的PHRR;TGA测试表明次磷酸钙的加入虽然使得复合材料的热稳定性和成炭量都有了明显的提高；对炭渣的测试研究表明,随着次磷酸钙的加入,复合材料的炭渣更加致密稳定.
3.将膨胀石墨(EG)作为阻燃协效剂与次磷酸铝复配用于聚乳酸复合材料阻燃,制备出聚乳酸/次磷酸铝/膨胀石墨(PLA/AHP/EG)三元阻燃复合材料。将次磷酸铝和膨胀石墨以3：1的比例按照进行复配在20%添加量条件下可以明显提高复合材料的极限氧指数和垂直燃烧级别。MCC和锥形量热测试表明,次磷酸铝和膨胀石墨复配可以明显降低复合材料的热释放塑料峰值(pHRR)和总热释放量(THR)。TGA测试表明,复合材料中的次磷酸铝成分在空气条件下能有效抑制复合材料在高温段的降解。TG-IR测试表明,在次磷酸铝/膨胀石墨的复配能有效降低挥发性气体的产生；同时,SEM研究表明,膨胀石墨燃烧过程中出现剥离膨胀覆盖在多孔炭渣的表面,从而有利于致密炭渣的形成,有效抑制燃烧区域物质和能量的交换。在此基础上,提出次磷酸铝膨胀石墨复配体系阻燃机理：膨胀石墨作为成炭剂在燃烧初期迅速膨胀,次磷酸铝降解成分复合形成致密的膨胀炭层,有效阻止燃烧区物质、能量以及氧气的交换,延缓了燃烧的进行；同时膨胀石墨膨胀形成的蠕虫状结构中的微小空间可以作为微反应器有利于聚乳酸降解产物以及有毒气体的相互反应,有效降低上述成分的产量,同时也利于成炭量的提高,从而有效提高复合材料的阻燃性能。
4.合成了两种稀土次磷酸盐次磷酸镧(LaHP)和次磷酸铈(CeHP)。SEM研究表明,两种稀土次磷酸盐均呈微米尺度的棒状结构。TGA测试表明：这两种次磷酸盐在不同燃烧氛围下呈现完全不同的降解机制。以LaHP和CeHP为阻燃添加剂,制备出一系列聚乳酸阻燃复合材料(FR-PLA)。TGA测试表明,两种稀土次磷酸盐的加入均提高了聚乳酸阻燃复合材料的热稳定性。30%添加量的次磷酸镧和次磷酸铈使得复合材料达到UL-94VO级别,氧指数为28.5vo1%.TG-IR测试表明,两种稀土次磷酸盐的加入可以有效降低挥发性气体的产生。MCC和锥形量热测试均表明LaHP和CeHP的加入能有效降低热释放塑料峰值(pHRR)。同时,采用SEM研究炭渣,表明不同稀土次磷酸盐添加量对炭渣形貌有很大的影响；采用XPS对炭渣进行元素分析,表明复合材料的燃烧产物主要为次磷酸盐降解产物和催化成炭产物。
5.按照国际标准,搭建中国首台稳态管式炉烟气毒性试验平台(SSTF)。在此基础上研究了聚乳酸,聚乳酸/次磷酸铝,聚乳酸/次磷酸钙,聚乳酸/次磷酸镧和聚乳酸/次磷酸铈复合材料的烟气毒性。研究表明：聚乳酸燃烧过程中,其氧气消耗与二氧化碳生成存在高度关联,燃烧过程中消耗的氧气主要进入二氧化碳中；不同氧气供应条件下,聚乳酸以及聚乳酸复合材料的烟气产生迥异,其在等值比附近氧气最大限度转化为二氧化碳,一氧化碳浓度最低,此时烟气毒性最小；不同金属阳离子的次磷酸盐对复合材料烟气毒性影响显著,其中,聚乳酸/稀土次磷酸盐复合材料燃烧烟气毒性最低。
Polylactic acid (PLA) was a degradable polymer which was derived from renewable resource. PLA present excellent mechanical properties and biocompatibility, it was considered to replace polyolefins to some extent. However, the development and application of PLA was limited due to its poor fire resistance and serious dripping when subjected to elevated temperatures or combustion. So, it was important to research and develop flame retarded PLA. Firstly, this thesis systematically reviewing previous studies on halogen-free flame retardant technology, discussing the application feasibility of several these technologies in PLA. Secondly, several PLA/hypophosphite salts composites were prepared, and also, the degradation and flame retardant mechanism of these composites were investigated. Thirdly, the author successfully constructed first static state tube furnace toxicity test platform (SSTF); furthermore, the fire effluent toxicity of the PLA/hypophosphite salt composites in different conditions were investigated by this platform.
1. Aluminum hypophosphite (AHP) was firstly used as a novel flame retardant and composed with PLA, a series of PLA/AHP composites were prepared. TGA test indicated that the addition of AHP could significantly increase the char residue and reduce mass loss rate. LOI and UL-94test indicated that the flame retardancy of the composites was significantly improved. FR-PLA composites with20wt%AHP loading could pass UL-94V-0rating without dripping, and the LOI value was27.5vol%. MCC and Cone test indicated that the peak of heat release rate (PHRR) was significantly reduced. The char residue of PLA/AHP composites after LOI test was tested by SEM, indicating condensed char structure was formed. Furthermore, DSC and DMA test indicate that the addition of AHP could significantly improve crystallization property and storage modulus of PLA/AHP composites.
2. Inspired by the high performance of AHP, another calcium hypophosphite was used as a potential flame retardant for PLA, and a series of PLA/CaHP composites were prepared. The addition of CaHP could significantly improve the flame retardancy of PLA/CaHP composites. PLA/CaHP could pass UL-94V-0rating without dripping, and the LOI value was26.5vol%. MCC test indicated that the PHRR value was significantly reduced. TGA test indicated that the addition of CaHP could significantly increase the char residue and reduce the mass loss rate. The char after LOI test was investigated by SEM, revealing that the char residue of PLA/CaHP was condensed, which could improve the fire safety of the composites.
3. Expanded graphite was used as flame retardant synergist and combined with AHP, a series of PLA/AHP/EG composites were prepared. The composite containing20wt%could pass UL-94VO rating with a high LOI value of34vol%(AHP:EG=3:1). MCC and Cone testing revealed that, the combination of AHP with EG could significantly reduce the PHRR and the total heart release (THR) of the composites. TGA test indicated that AHP could inhibit the degradation of the composites in high temperature. TG-IR revealed that the combination of AHP and EG resulted in significant decrease of gas products. SEM test showed that EG expanded and lamellar structure covered on the porous char residue which benefited to the formation of condensed char layer. Based on the experimental datum, the possible mechanism of PLA/AHP/EG composites was put forward:The EG particle rapidly expands and form vermicular structure which combined with decomposition products of AHP to form condensed char layer, which could further prohibit the transportation of mass and fuel. Further-more, the space of vermicular structure could act as a "micro-reactor", which is approximately seemed as a closed room in which toxicity gas can adequately react with the decomposition products of PLA. The sufficient reaction significantly inhibits the combustible and toxic gas, result in the improvement of char residue, and also, the flame reatrdancy of the composites was significantly improved.
4. Two kinds of rare earth metal hypophosphite (REHP), lanthanum (Ⅲ) hypophosphite and cerium (Ⅲ) hypophosphite, were successfully synthesized and characterized. SEM analysis illustrated both of these two REHP presented rod-like structure with micron sizes. TGA test illustrated that REHP showed different degradation process in nitrogen and air atmosphere. A series of PLA/REHP composites were prepared by addition of LaHP and CeHP. TGA test showed that both the incorporation of LaHP and CeHP could significantly improve the thermal stability of PLA/REHP composites. For the composites containing30wt%LaHP and CeHP, it could reach UL-94V-0rating with a LOI value of28.5vol%. TG-IR test illustrated that the all the volatilized products were reduced by the addition of REHP. MCC and Cone testing showed that the addition of REHP could significantly reduce the PHRR value of PLA/PRHP composites. Char residue after Cone testing were investigated by SEM, illustrating that the morphology of the char residue were significantly effect by PEHP loading. Furthermore, the char was investigated by XPS, which showed that the main component was the degradation products of REHP and carbon-containing materials.
5. First static state tube furnace toxicity test platform (SSTF) in China were constructed according to ISO19700. The fire effluents of PLA, PLA/AHP, PLA/CaHP, PLA/LaHP and PLA/CeHP composites in different conditions were investigated by SSTF. The research illustrated that, the oxygen consumption and CO2concentration presented high correlation, the oxygen mostly consumed by the formation of CO2. The composition of fire effluent was highly effected by oxygen supply condition; in equivalence ratio condition, the oxygen was transformed into CO2to the maximum content, the CO concentration was lowest, the fire effluent presented lowest toxicity. The kinds of cation in hypoposphite salts shows high effect on the fire effluent, in which, the composites containing rare earth hypophosphite shows the lowest fire toxicity.
1.采用新型阻燃剂次磷酸铝(AHP),将其应用于聚乳酸的阻燃,制备出一系列PLA/AHP复合材料。热重测试表明,复合材料的成炭有明显提高,质量损失速率有明显降低。极限氧指数测试和垂直燃烧测试表明次磷酸铝可以提高复合材料的阻燃性能,20%次磷酸铝添加量即可使得次磷酸铝/次磷酸铝(PLA/AHP)复合材料达到UL-94VO级别,燃烧过程中的熔融滴落现象完全消失,极限氧指数达到27.5vol%;MCC测试和锥形量热测试表明次磷酸铝的加入可以有效降低热释放速率峰值；对燃烧后的炭渣进行SEM测试,燃烧形成的炭层更加致密。与此同时,DSC和DMA测试表明,次磷酸铝的加入有效提高了复合材料的结晶性能和储能模量。
2.借鉴次磷酸铝(AHP)在聚乳酸复合材料的优异表现,将次磷酸钙(CaHP)作为一种潜在的阻燃剂应用聚乳酸,制备出一系列聚乳酸/次磷酸钙阻燃复合材料。研究表明,次磷酸钙的加入亦有效提高聚乳酸/次磷酸钙(PLA/CaHP)复合材料的极限氧指数,30%次磷酸钙添加量可以使得复合材料达到UL94VO级别,滴落完全消失,极限氧指数为26.5vol%。MCC测试结果表明,次磷酸钙的加入可以降低复合材料的PHRR;TGA测试表明次磷酸钙的加入虽然使得复合材料的热稳定性和成炭量都有了明显的提高；对炭渣的测试研究表明,随着次磷酸钙的加入,复合材料的炭渣更加致密稳定.
3.将膨胀石墨(EG)作为阻燃协效剂与次磷酸铝复配用于聚乳酸复合材料阻燃,制备出聚乳酸/次磷酸铝/膨胀石墨(PLA/AHP/EG)三元阻燃复合材料。将次磷酸铝和膨胀石墨以3：1的比例按照进行复配在20%添加量条件下可以明显提高复合材料的极限氧指数和垂直燃烧级别。MCC和锥形量热测试表明,次磷酸铝和膨胀石墨复配可以明显降低复合材料的热释放塑料峰值(pHRR)和总热释放量(THR)。TGA测试表明,复合材料中的次磷酸铝成分在空气条件下能有效抑制复合材料在高温段的降解。TG-IR测试表明,在次磷酸铝/膨胀石墨的复配能有效降低挥发性气体的产生；同时,SEM研究表明,膨胀石墨燃烧过程中出现剥离膨胀覆盖在多孔炭渣的表面,从而有利于致密炭渣的形成,有效抑制燃烧区域物质和能量的交换。在此基础上,提出次磷酸铝膨胀石墨复配体系阻燃机理：膨胀石墨作为成炭剂在燃烧初期迅速膨胀,次磷酸铝降解成分复合形成致密的膨胀炭层,有效阻止燃烧区物质、能量以及氧气的交换,延缓了燃烧的进行；同时膨胀石墨膨胀形成的蠕虫状结构中的微小空间可以作为微反应器有利于聚乳酸降解产物以及有毒气体的相互反应,有效降低上述成分的产量,同时也利于成炭量的提高,从而有效提高复合材料的阻燃性能。
4.合成了两种稀土次磷酸盐次磷酸镧(LaHP)和次磷酸铈(CeHP)。SEM研究表明,两种稀土次磷酸盐均呈微米尺度的棒状结构。TGA测试表明：这两种次磷酸盐在不同燃烧氛围下呈现完全不同的降解机制。以LaHP和CeHP为阻燃添加剂,制备出一系列聚乳酸阻燃复合材料(FR-PLA)。TGA测试表明,两种稀土次磷酸盐的加入均提高了聚乳酸阻燃复合材料的热稳定性。30%添加量的次磷酸镧和次磷酸铈使得复合材料达到UL-94VO级别,氧指数为28.5vo1%.TG-IR测试表明,两种稀土次磷酸盐的加入可以有效降低挥发性气体的产生。MCC和锥形量热测试均表明LaHP和CeHP的加入能有效降低热释放塑料峰值(pHRR)。同时,采用SEM研究炭渣,表明不同稀土次磷酸盐添加量对炭渣形貌有很大的影响；采用XPS对炭渣进行元素分析,表明复合材料的燃烧产物主要为次磷酸盐降解产物和催化成炭产物。
5.按照国际标准,搭建中国首台稳态管式炉烟气毒性试验平台(SSTF)。在此基础上研究了聚乳酸,聚乳酸/次磷酸铝,聚乳酸/次磷酸钙,聚乳酸/次磷酸镧和聚乳酸/次磷酸铈复合材料的烟气毒性。研究表明：聚乳酸燃烧过程中,其氧气消耗与二氧化碳生成存在高度关联,燃烧过程中消耗的氧气主要进入二氧化碳中；不同氧气供应条件下,聚乳酸以及聚乳酸复合材料的烟气产生迥异,其在等值比附近氧气最大限度转化为二氧化碳,一氧化碳浓度最低,此时烟气毒性最小；不同金属阳离子的次磷酸盐对复合材料烟气毒性影响显著,其中,聚乳酸/稀土次磷酸盐复合材料燃烧烟气毒性最低。
Polylactic acid (PLA) was a degradable polymer which was derived from renewable resource. PLA present excellent mechanical properties and biocompatibility, it was considered to replace polyolefins to some extent. However, the development and application of PLA was limited due to its poor fire resistance and serious dripping when subjected to elevated temperatures or combustion. So, it was important to research and develop flame retarded PLA. Firstly, this thesis systematically reviewing previous studies on halogen-free flame retardant technology, discussing the application feasibility of several these technologies in PLA. Secondly, several PLA/hypophosphite salts composites were prepared, and also, the degradation and flame retardant mechanism of these composites were investigated. Thirdly, the author successfully constructed first static state tube furnace toxicity test platform (SSTF); furthermore, the fire effluent toxicity of the PLA/hypophosphite salt composites in different conditions were investigated by this platform.
1. Aluminum hypophosphite (AHP) was firstly used as a novel flame retardant and composed with PLA, a series of PLA/AHP composites were prepared. TGA test indicated that the addition of AHP could significantly increase the char residue and reduce mass loss rate. LOI and UL-94test indicated that the flame retardancy of the composites was significantly improved. FR-PLA composites with20wt%AHP loading could pass UL-94V-0rating without dripping, and the LOI value was27.5vol%. MCC and Cone test indicated that the peak of heat release rate (PHRR) was significantly reduced. The char residue of PLA/AHP composites after LOI test was tested by SEM, indicating condensed char structure was formed. Furthermore, DSC and DMA test indicate that the addition of AHP could significantly improve crystallization property and storage modulus of PLA/AHP composites.
2. Inspired by the high performance of AHP, another calcium hypophosphite was used as a potential flame retardant for PLA, and a series of PLA/CaHP composites were prepared. The addition of CaHP could significantly improve the flame retardancy of PLA/CaHP composites. PLA/CaHP could pass UL-94V-0rating without dripping, and the LOI value was26.5vol%. MCC test indicated that the PHRR value was significantly reduced. TGA test indicated that the addition of CaHP could significantly increase the char residue and reduce the mass loss rate. The char after LOI test was investigated by SEM, revealing that the char residue of PLA/CaHP was condensed, which could improve the fire safety of the composites.
3. Expanded graphite was used as flame retardant synergist and combined with AHP, a series of PLA/AHP/EG composites were prepared. The composite containing20wt%could pass UL-94VO rating with a high LOI value of34vol%(AHP:EG=3:1). MCC and Cone testing revealed that, the combination of AHP with EG could significantly reduce the PHRR and the total heart release (THR) of the composites. TGA test indicated that AHP could inhibit the degradation of the composites in high temperature. TG-IR revealed that the combination of AHP and EG resulted in significant decrease of gas products. SEM test showed that EG expanded and lamellar structure covered on the porous char residue which benefited to the formation of condensed char layer. Based on the experimental datum, the possible mechanism of PLA/AHP/EG composites was put forward:The EG particle rapidly expands and form vermicular structure which combined with decomposition products of AHP to form condensed char layer, which could further prohibit the transportation of mass and fuel. Further-more, the space of vermicular structure could act as a "micro-reactor", which is approximately seemed as a closed room in which toxicity gas can adequately react with the decomposition products of PLA. The sufficient reaction significantly inhibits the combustible and toxic gas, result in the improvement of char residue, and also, the flame reatrdancy of the composites was significantly improved.
4. Two kinds of rare earth metal hypophosphite (REHP), lanthanum (Ⅲ) hypophosphite and cerium (Ⅲ) hypophosphite, were successfully synthesized and characterized. SEM analysis illustrated both of these two REHP presented rod-like structure with micron sizes. TGA test illustrated that REHP showed different degradation process in nitrogen and air atmosphere. A series of PLA/REHP composites were prepared by addition of LaHP and CeHP. TGA test showed that both the incorporation of LaHP and CeHP could significantly improve the thermal stability of PLA/REHP composites. For the composites containing30wt%LaHP and CeHP, it could reach UL-94V-0rating with a LOI value of28.5vol%. TG-IR test illustrated that the all the volatilized products were reduced by the addition of REHP. MCC and Cone testing showed that the addition of REHP could significantly reduce the PHRR value of PLA/PRHP composites. Char residue after Cone testing were investigated by SEM, illustrating that the morphology of the char residue were significantly effect by PEHP loading. Furthermore, the char was investigated by XPS, which showed that the main component was the degradation products of REHP and carbon-containing materials.
5. First static state tube furnace toxicity test platform (SSTF) in China were constructed according to ISO19700. The fire effluents of PLA, PLA/AHP, PLA/CaHP, PLA/LaHP and PLA/CeHP composites in different conditions were investigated by SSTF. The research illustrated that, the oxygen consumption and CO2concentration presented high correlation, the oxygen mostly consumed by the formation of CO2. The composition of fire effluent was highly effected by oxygen supply condition; in equivalence ratio condition, the oxygen was transformed into CO2to the maximum content, the CO concentration was lowest, the fire effluent presented lowest toxicity. The kinds of cation in hypoposphite salts shows high effect on the fire effluent, in which, the composites containing rare earth hypophosphite shows the lowest fire toxicity.
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[15]Yuan, X. Y., Wang, D. Y., Chen, L., Wang, X. L., Wang, Y.Z. Inherent flame retardation of bio-based poly(lactic acid) by incorporating phosphorus linked pendent group into the backbone. Polymer Degradation and Stability 2011; 96:1669-1675.
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[6]Yuan, X. Y., Wang, D. Y., Chen, L., Wang, X. L., Wang, Y.Z. Inherent flame retardation of bio-based poly(lactic acid) by incorporating phosphorus linked pendent group into the backbone. Polymer Degradation and Stability 2011; 96:1669-1675.
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[8]Yang, W., Song, L., Hu Y., Lu, H.D. Yuen, R. K. K. Enhancement of fire retardancy performance of glass-fibre reinforced poly(ethylene terephthalate) composites with the incorporation of aluminum hypophosphite and melamine cyanurate. Composites Part B:Engineering.2011;42:1057-1065.
[9]Yang, W.,Hu, Y., Tai, Q. L., Lu, H. D., Song, L., Yuen, R. K. K. Fire and mechanical performance of nanoclay reinforced glass-fiber/PBT composites containing aluminum hypophosphite particles. Composites Part A:Applied Science and Manufacturing.2011; 42:794-800.
[10]Braun, U., Schartel, B., Fichera, M. A., Jager. C. Flame retardancy mechanisms of aluminium phosphinate in combination with melamine polyphosphate and zinc borate in glass-fiber reinforced polyamide 6,6. Polymer Degradation and Stability. 2007; 92:1528-1545.
[11]Tang, G., Wang, X., Xing, W.Y., Zhang, P., Wang, B.B., Hong, N.N., Yang, W., Hu, Y., Song, L. Thermal Degradation and Flame Retardance of Biobased Polylactide Composites Based on Aluminum Hypophosphite. Industrial & Engineering Chemistry Research.2012; 51:12009-12016.
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[17]Zhu, H.F., Zhu, Q. L., Li. J., Tao, K., Xue, L. X., Yan, Q. Synergistic effect between expandable graphite and ammonium polyphosphate on flame retarded polylactide. Polymer Degradation and Stability.2011;96:183-189.
[18]Lyon, R. E., Walters, R. N., Stoliarov, S. I. Screening flame retardants for plastics using microscale combustion calorimetry. Polymer Engineering and Science. 2007; 47:1501-1510.
[19]Cheng, K. C., Yu, C. B.. Guo. W. J., Wang, S. F., Chuang, T. C., Lin, Y. H. Thermal properties and flammability of polylactide nanocomposites with aluminum trihydrate and organoclay. Carbohydrate Polymer.2012; 87:1119-1123.
[20]Yoshida, Y., Inoue, K., Kyritsakas, N., Kurmoo, M. Syntheses, structures and magnetic properties of zig-zag chains of transition metals with O-P-O bridges. Inorganica Chimica Acta.2009; 362:1428-1434.
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[10]Wei, L. L., Wang, D. Y., Chen, H. B., Chen, Li., Wang, X. L., Wang, Y. Z. Effect of a phosphorus-containing flame retardant on the thermal properties and ease of ignition of poly(lactic acid). Polymer Degradation and Stability 2011;96: 1557-1561.
[11]Yuan, X. Y., Wang, D. Y., Chen, L., Wang, X. L., Wang, Y.Z. Inherent flame retardation of bio-based poly(lactic acid) by incorporating phosphorus linked pendent group into the backbone. Polymer Degradation and Stability 2011; 96:1669-1675.
[12]Wang, D. Y., Song, Y.P., Lin, L., Wang, X. L., Wang, Y. Z. A novel phosphorus-containing poly(lactic acid) toward its flame retardation. A novel phosphorus-containing poly(lactic acid) toward its flame retardation. Polymer.2011; 52:233-238.
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[15]Braun, U., Schartel, B., Fichera, M. A., Jager, C. Flame retardancy mechanisms of aluminium phosphinate in combination with melamine polyphosphate and zinc borate in glass-fiber reinforced polyamide 6,6. Polymer Degradation and Stability. 2007;92:1528-1545.
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