聚酯复合材料无卤协效阻燃研究及机理的研究
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摘要
聚对苯二甲酸乙二醇酯(PET)和聚对苯二甲酸丁二醇酯(PBT)是聚酯家族中应用最为广泛的两种工程塑料。由于它们具有良好的尺寸稳定性和热稳定性,PET和PBT已广泛应用于纺织、汽车、电子电器等领域。然而,PET和PBT均是十分容易燃烧的聚合物,在它们的燃烧过程中还会产生大量的烟气以及较为严重的滴落现象。因此,为了扩大PET和PBT的应用范围,研究和发展阻燃型聚酯材料已显得非常重要。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,探讨这些技术或阻燃体系在聚酯和玻纤增强聚酯中应用的可行性。其次,研究了现有阻燃剂或阻燃体系在聚酯和玻纤增强聚酯中的热解和阻燃机制。最后,针对聚酯和玻纤增强聚酯热解和燃烧的机理,合成出几种新型阻燃剂,并研究它们对聚酯和玻纤增强聚酯的阻燃作用。主要研究工作如下：
1.首先比较研究了两种不同微胶囊化聚磷酸铵：硅凝胶包裹聚磷酸铵(MAPP(Si))和聚氨酯包裹聚磷酸铵(MAPP(PU))对PBT阻燃性能的影响。调控MAPP和三聚氰胺氰尿酸盐(MC)之间的比例关系,制备了几种无卤阻燃PBT复合材料,研究了其热分解行为和阻燃性能,探讨了其阻燃和热解机理。研究结果显示：MAPP(Si)和MAPP (PU)分别与三聚氰胺氰尿酸盐按相同比例复配,均能使得PBT材料获得优异的阻燃性能。其次,以有机改性蒙脱土(OMMT)为纳米添加剂,制备了PBT/IFR/OMMT纳米复合材料,研究了OMMT和IFR之间的协同阻燃作用。燃烧性能测试表明低含量的OMMT可以有效的提高材料的阻燃性能。在PBT/IFR/OMMT的炭层研究中首次在扫描电子显微镜(SEM)下观察到了微米结构的颗粒,这些颗粒的存在保护了PBT基体,使其在500℃的马弗炉中灼烧10分钟后仍有α相存在。
2.以无机次磷酸铝(AHP)为主要阻燃添加剂,通过与三聚氰胺衍生物(MD)、聚碳酸酯(PC)进行复配,并调控其比例关系,组成新的阻燃体系,并成功应用于PBT和玻纤增强PBT中。微型燃烧量热仪(MCC)和热重-红外联用(TGA-FTIR)分析结果表明：AHP和三聚氰胺衍生物的复配使得PBT具有较低的火灾危险性。同时,总量为20wt%的复配阻燃剂可以使得PBT获得较高的极限氧指数,且能通过垂直燃烧V-O级别测试。对于阻燃玻纤增强PBT复合材料的研究结果表明：AHP,MC和PC所组成的阻燃体系可以使得0.8mm厚的玻纤增强PBT(GRPBT)样条通过垂直燃烧V-O级别测试,且材料的热释放速率得到了极大的降低。TGA和炭渣研究表明：PC的加入有效提高了材料的成炭量,并显著增强了材料的阻燃性能,降低了材料的火灾危险性。
3.研究了纳米粘土(Clay)和AHP对GRPBT阻燃性能和力学性能的影响,分析了其阻燃作用机制。X射线衍射(XRD)和透射电子显微镜(TEM)分析结果表明：Clay主要以剥离结构存在于GRPBT中。TGA-FTIR分析结果表明：在材料热分解过程中,AHP与Clay的引入极大的抑制了酯类物质的释放。阻燃性能测试结果表明：AHP能够有效的提高GRPBT的阻燃性能,而Clay的引入进一步提高了GRPBT的阻燃性能,这是因为均匀分散在PBT基体中的Clay片层在GRPBT-AHP复合材料燃烧过程中起到了“微反应器”的作用。力学性能测试结果表明：单独添加Clay可以提高GRPBT的拉伸强度和模量,而单独添加AHP使得GRPBT的拉伸强度和模量急剧降低,Clay替代部分AHP恢复材料的拉伸强度和模量。
4.采用氯化镧、氯化铈和次磷酸钠为原料,合成了次磷酸镧(LHP)和次磷酸铈(CHP)。通过SEM分析看出,两种次磷酸盐均为棒状结构,尺寸均为微米级；TGA结果显示两种次磷酸盐均有良好的热稳定性。以LHP和CHP为阻燃添加剂,设计制备了一系列阻燃型GRPBT复合材料。TGA结果表明低含量的LHP和CHP均提高了GRPBT的热稳定性,降低GRPBT的质量损失速率。燃烧性能测试表明LHP和CHP的加入大幅提高了GRPBT的阻燃性能。动态力学性能和拉伸性能测试表明LHP和CHP均增强了GRPBT的力学性能。调控LHP或CHP和MC之间的比例关系,设计制备了另一组阻燃型GRPBT复合材料。阻燃性能测试结果发现材料的氧指数和垂直燃烧测试级别得到进一步提高。
5.比较研究了AHP和CHP对GRPET复合材料热解和阻燃性能的影响。TGA分析表明：AHP和CHP的引入均降低了GRPET的热稳定性,而CHP对GRPET热稳定性的影响较小。燃烧性能测试表明AHP和CHP的加入大幅提高了GRPET的阻燃性能,与CHP相比,AHP对GRPET阻燃性能的促进作用更为显著。调控AHP和MC之间的比例关系,设计制备了另一组无卤阻燃型GRPET复合材料。TGA分析表明二者的加入大幅降低了GRPET复合材料的热稳定性,但减少了PET基体在热分解过程所释放出的挥发性物质。阻燃性能测试结果表明AHP和MC产生了明显的协同阻燃效应,显著提高了GRPET复合材料的阻燃性能。
Represented by poly(ethylene terephthalate)(PET) and poly(1,4-butylene terephthalate)(PBT), partly aromatic polyesters are widely applied as engineering plastics in textile, high volume automotive, electrical, and other fields, owing to their good dimensional stability and thermal resistance. However, the development and application of polyesters are limited due to its flammability and serious dripping when subjected to elevated temperatures or combustion. Based on systematically reviewing previous studies on flame retardant techniques used in halogen-free flame retarded polymeric materials including polyesters, several flame retardant techniques or systems which are suitable for polyesters were firstly introduced into polyesters in this study. The thermal decomposition and flame retardancy mechanisms were then studied. Finally, novel compounds used as flame retardants in polyesters were synthesized, and the flame retardancy mechanisms were investigated. The following work was completed.
1. The effect of microencapsulated APP with silica gel shell (MAPP(Si)) and polyurethane shell (MAPP(PU)) in combination with MC on flame retardancy of PBT was firstly studied. The experimental results showed that both MAPP(Si) and MAPP(PU) significantly improved the flame retardancy of PBT in the presence of MC compared with APP. Based on the excellent fire retardancy of the intumescent flame retardant (IFR) system containing MAPP(PU) and MC, organo-modified montmorillonite (OMMT) was then introduced to the PBT/IFR system. The synergistic effect between OMMT and IFR was also found that the addition of OMMT further improved the flame retardancy of PBT/IFR composites. A mass of microcomposite structure particles formed in the heating or combustion process of PBT/IFR/OMMT nanocomposites were the first time to be found in the SEM images. It was a strong evidence to confirm the migration or accumulation of montmorillonite and carbonaceous-silicate materials during the heating or combustion process.
2. A novel halogen-free flame retardant system was established, composed of aluminum hypophosphite (AHP) and melamine derivatives (MD) to develop halogen-free fire retarded PBT and GRPBT composites. For the PBT composites with the incorporation of AHP and melamine derivatives, the heat release capacity (HRC) which is an indicator of a material fire hazard from microscale combustion calorimeter (MCC) testing was significantly reduced. The intensities of a variety of combustible or toxic gases detected by Thermogravimetric analysis/Fourier transform infrared spectrometry (TGA-FTIR) technique were remarkably decreased. Moreover, a loading of20wt%flame retardant mixture fulfilled the PBT composites high limiting oxygen index (LOI) and V-0classification in Underwriters Laboratories94(UL-94) testing. The flame retarded GRPBT composite containing AHP, MD and PC can achieve a V-0classification in UL-94testing (the thickness of testing bar is0.8mm). In MCC and cone calorimeter testing, both of the two different PHRRs (peak of heat release rate) for GRPBT composites are significantly reduced by the incorporation of the novel system. Thermogravimetric analysis and residue characterization revealed that the addition of PC promotes the formation of char residues leading the reduction of mass loss rate, which results in the improvement of fire retardancy.
3. Nanoclay and AHP were used to develop halogen-free fire retardant GRPBT composites with enhanced fire retarded performance. Exfoliated clay nanocomposites of flame retarded/GRPBT were fabricated through melt blending process. TGA-FTIR analysis showed that the incorporation of AHP and nanoclay remarkably reduced the release of esters decomposed from PBT. MCC results indicated that the HRC was reduced by51%. Moreover, significant improvements were obtained in LOI along with maintained UL-94ratings. Thermogravimetric analysis and residue characterization revealed the flame retardancy mechanism in which the well dispersed layered silicates in polymer matrix probably play an important role of "microreactor" during the combustion. In addition, the substitution of a certain fraction of AHP by nanoclay could recover the interface between glass fiber and polymer matrix leading to the improvement of tensile strength.
4. Inspired by the flame retardant effects provided by AHP, another metal hypophosphite was taken into account to improve the fire retardancy performance of GRPs. Two kinds of rare earth metal hypophosphite, lanthanum (Ⅲ) hypophosphite and cerium (Ⅲ) hypophosphite, were successfully synthesized and characterized. Thermogravimetric analysis illustrated that both the incorporation of LHP and CHP could improve the thermal stability of GRPBT. TGA-FTIR analysis showed that all the volatilized products were reduced by the addition of LHP or CHP. For the composite containing20wt%of LHP or CHP, it could achieve a V-0classification with a high LOI (about28%). Additionally, both the PHRR and total heat release (THR) values of GRPBT composites were significantly reduced by the addition of LHP and CHP. The incorporation of the flame retardant mixture containing LHP or CHP with MC can further improve the flame retardancy of GRPBT.
5. Comparative study on the thermal decomposition and combustion behavior of CHP and AHP in GRPET composites was completed. TGA results showed that both the introduction of CHP and AHP reduced the thermal stability of GRPET, and improved the char residues. LOI and UL-94testing indicated that both the addition of CHP and AHP could enhance the flame retardancy of GRPET. GRPET containing10wt%of AHP achieved V-0classification with a high LOI of30%, while only V-1classification was obtained for GRPET with10wt%of CHP. Cone calorimeter testing results showed that CHP and AHP can both reduce the PHRR and THR of GRPET, and GRPET/AHP showed lower THR. For the PET/GF composites with a low loading of the flame retardant mixture containing AHP and MC, the HRC value was reduced by47%, meanwhile, the intensities of a variety of combustible or toxic gases detected by TGA-FTIR technique were remarkably decreased. Thermal decomposition and residue analysis revealed that the flame retardancy of GRPET composites was enhanced by the condensed-phase action of AHP and the gas-phase dilution effect of MC.
1.首先比较研究了两种不同微胶囊化聚磷酸铵：硅凝胶包裹聚磷酸铵(MAPP(Si))和聚氨酯包裹聚磷酸铵(MAPP(PU))对PBT阻燃性能的影响。调控MAPP和三聚氰胺氰尿酸盐(MC)之间的比例关系,制备了几种无卤阻燃PBT复合材料,研究了其热分解行为和阻燃性能,探讨了其阻燃和热解机理。研究结果显示：MAPP(Si)和MAPP (PU)分别与三聚氰胺氰尿酸盐按相同比例复配,均能使得PBT材料获得优异的阻燃性能。其次,以有机改性蒙脱土(OMMT)为纳米添加剂,制备了PBT/IFR/OMMT纳米复合材料,研究了OMMT和IFR之间的协同阻燃作用。燃烧性能测试表明低含量的OMMT可以有效的提高材料的阻燃性能。在PBT/IFR/OMMT的炭层研究中首次在扫描电子显微镜(SEM)下观察到了微米结构的颗粒,这些颗粒的存在保护了PBT基体,使其在500℃的马弗炉中灼烧10分钟后仍有α相存在。
2.以无机次磷酸铝(AHP)为主要阻燃添加剂,通过与三聚氰胺衍生物(MD)、聚碳酸酯(PC)进行复配,并调控其比例关系,组成新的阻燃体系,并成功应用于PBT和玻纤增强PBT中。微型燃烧量热仪(MCC)和热重-红外联用(TGA-FTIR)分析结果表明：AHP和三聚氰胺衍生物的复配使得PBT具有较低的火灾危险性。同时,总量为20wt%的复配阻燃剂可以使得PBT获得较高的极限氧指数,且能通过垂直燃烧V-O级别测试。对于阻燃玻纤增强PBT复合材料的研究结果表明：AHP,MC和PC所组成的阻燃体系可以使得0.8mm厚的玻纤增强PBT(GRPBT)样条通过垂直燃烧V-O级别测试,且材料的热释放速率得到了极大的降低。TGA和炭渣研究表明：PC的加入有效提高了材料的成炭量,并显著增强了材料的阻燃性能,降低了材料的火灾危险性。
3.研究了纳米粘土(Clay)和AHP对GRPBT阻燃性能和力学性能的影响,分析了其阻燃作用机制。X射线衍射(XRD)和透射电子显微镜(TEM)分析结果表明：Clay主要以剥离结构存在于GRPBT中。TGA-FTIR分析结果表明：在材料热分解过程中,AHP与Clay的引入极大的抑制了酯类物质的释放。阻燃性能测试结果表明：AHP能够有效的提高GRPBT的阻燃性能,而Clay的引入进一步提高了GRPBT的阻燃性能,这是因为均匀分散在PBT基体中的Clay片层在GRPBT-AHP复合材料燃烧过程中起到了“微反应器”的作用。力学性能测试结果表明：单独添加Clay可以提高GRPBT的拉伸强度和模量,而单独添加AHP使得GRPBT的拉伸强度和模量急剧降低,Clay替代部分AHP恢复材料的拉伸强度和模量。
4.采用氯化镧、氯化铈和次磷酸钠为原料,合成了次磷酸镧(LHP)和次磷酸铈(CHP)。通过SEM分析看出,两种次磷酸盐均为棒状结构,尺寸均为微米级；TGA结果显示两种次磷酸盐均有良好的热稳定性。以LHP和CHP为阻燃添加剂,设计制备了一系列阻燃型GRPBT复合材料。TGA结果表明低含量的LHP和CHP均提高了GRPBT的热稳定性,降低GRPBT的质量损失速率。燃烧性能测试表明LHP和CHP的加入大幅提高了GRPBT的阻燃性能。动态力学性能和拉伸性能测试表明LHP和CHP均增强了GRPBT的力学性能。调控LHP或CHP和MC之间的比例关系,设计制备了另一组阻燃型GRPBT复合材料。阻燃性能测试结果发现材料的氧指数和垂直燃烧测试级别得到进一步提高。
5.比较研究了AHP和CHP对GRPET复合材料热解和阻燃性能的影响。TGA分析表明：AHP和CHP的引入均降低了GRPET的热稳定性,而CHP对GRPET热稳定性的影响较小。燃烧性能测试表明AHP和CHP的加入大幅提高了GRPET的阻燃性能,与CHP相比,AHP对GRPET阻燃性能的促进作用更为显著。调控AHP和MC之间的比例关系,设计制备了另一组无卤阻燃型GRPET复合材料。TGA分析表明二者的加入大幅降低了GRPET复合材料的热稳定性,但减少了PET基体在热分解过程所释放出的挥发性物质。阻燃性能测试结果表明AHP和MC产生了明显的协同阻燃效应,显著提高了GRPET复合材料的阻燃性能。
Represented by poly(ethylene terephthalate)(PET) and poly(1,4-butylene terephthalate)(PBT), partly aromatic polyesters are widely applied as engineering plastics in textile, high volume automotive, electrical, and other fields, owing to their good dimensional stability and thermal resistance. However, the development and application of polyesters are limited due to its flammability and serious dripping when subjected to elevated temperatures or combustion. Based on systematically reviewing previous studies on flame retardant techniques used in halogen-free flame retarded polymeric materials including polyesters, several flame retardant techniques or systems which are suitable for polyesters were firstly introduced into polyesters in this study. The thermal decomposition and flame retardancy mechanisms were then studied. Finally, novel compounds used as flame retardants in polyesters were synthesized, and the flame retardancy mechanisms were investigated. The following work was completed.
1. The effect of microencapsulated APP with silica gel shell (MAPP(Si)) and polyurethane shell (MAPP(PU)) in combination with MC on flame retardancy of PBT was firstly studied. The experimental results showed that both MAPP(Si) and MAPP(PU) significantly improved the flame retardancy of PBT in the presence of MC compared with APP. Based on the excellent fire retardancy of the intumescent flame retardant (IFR) system containing MAPP(PU) and MC, organo-modified montmorillonite (OMMT) was then introduced to the PBT/IFR system. The synergistic effect between OMMT and IFR was also found that the addition of OMMT further improved the flame retardancy of PBT/IFR composites. A mass of microcomposite structure particles formed in the heating or combustion process of PBT/IFR/OMMT nanocomposites were the first time to be found in the SEM images. It was a strong evidence to confirm the migration or accumulation of montmorillonite and carbonaceous-silicate materials during the heating or combustion process.
2. A novel halogen-free flame retardant system was established, composed of aluminum hypophosphite (AHP) and melamine derivatives (MD) to develop halogen-free fire retarded PBT and GRPBT composites. For the PBT composites with the incorporation of AHP and melamine derivatives, the heat release capacity (HRC) which is an indicator of a material fire hazard from microscale combustion calorimeter (MCC) testing was significantly reduced. The intensities of a variety of combustible or toxic gases detected by Thermogravimetric analysis/Fourier transform infrared spectrometry (TGA-FTIR) technique were remarkably decreased. Moreover, a loading of20wt%flame retardant mixture fulfilled the PBT composites high limiting oxygen index (LOI) and V-0classification in Underwriters Laboratories94(UL-94) testing. The flame retarded GRPBT composite containing AHP, MD and PC can achieve a V-0classification in UL-94testing (the thickness of testing bar is0.8mm). In MCC and cone calorimeter testing, both of the two different PHRRs (peak of heat release rate) for GRPBT composites are significantly reduced by the incorporation of the novel system. Thermogravimetric analysis and residue characterization revealed that the addition of PC promotes the formation of char residues leading the reduction of mass loss rate, which results in the improvement of fire retardancy.
3. Nanoclay and AHP were used to develop halogen-free fire retardant GRPBT composites with enhanced fire retarded performance. Exfoliated clay nanocomposites of flame retarded/GRPBT were fabricated through melt blending process. TGA-FTIR analysis showed that the incorporation of AHP and nanoclay remarkably reduced the release of esters decomposed from PBT. MCC results indicated that the HRC was reduced by51%. Moreover, significant improvements were obtained in LOI along with maintained UL-94ratings. Thermogravimetric analysis and residue characterization revealed the flame retardancy mechanism in which the well dispersed layered silicates in polymer matrix probably play an important role of "microreactor" during the combustion. In addition, the substitution of a certain fraction of AHP by nanoclay could recover the interface between glass fiber and polymer matrix leading to the improvement of tensile strength.
4. Inspired by the flame retardant effects provided by AHP, another metal hypophosphite was taken into account to improve the fire retardancy performance of GRPs. Two kinds of rare earth metal hypophosphite, lanthanum (Ⅲ) hypophosphite and cerium (Ⅲ) hypophosphite, were successfully synthesized and characterized. Thermogravimetric analysis illustrated that both the incorporation of LHP and CHP could improve the thermal stability of GRPBT. TGA-FTIR analysis showed that all the volatilized products were reduced by the addition of LHP or CHP. For the composite containing20wt%of LHP or CHP, it could achieve a V-0classification with a high LOI (about28%). Additionally, both the PHRR and total heat release (THR) values of GRPBT composites were significantly reduced by the addition of LHP and CHP. The incorporation of the flame retardant mixture containing LHP or CHP with MC can further improve the flame retardancy of GRPBT.
5. Comparative study on the thermal decomposition and combustion behavior of CHP and AHP in GRPET composites was completed. TGA results showed that both the introduction of CHP and AHP reduced the thermal stability of GRPET, and improved the char residues. LOI and UL-94testing indicated that both the addition of CHP and AHP could enhance the flame retardancy of GRPET. GRPET containing10wt%of AHP achieved V-0classification with a high LOI of30%, while only V-1classification was obtained for GRPET with10wt%of CHP. Cone calorimeter testing results showed that CHP and AHP can both reduce the PHRR and THR of GRPET, and GRPET/AHP showed lower THR. For the PET/GF composites with a low loading of the flame retardant mixture containing AHP and MC, the HRC value was reduced by47%, meanwhile, the intensities of a variety of combustible or toxic gases detected by TGA-FTIR technique were remarkably decreased. Thermal decomposition and residue analysis revealed that the flame retardancy of GRPET composites was enhanced by the condensed-phase action of AHP and the gas-phase dilution effect of MC.
引文
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