含DOPO磷硅杂化阻燃剂的设计及其阻燃环氧与聚脲树脂性能的研究
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摘要
高分子材料被广泛应用于人们生活的各个领域,如塑料、橡胶、纤维、涂料和胶粘剂等高分子材料在世界各地需求量很大。尽管高分子材料相对于传统材料有很多优势,但其易燃性使其在某些特殊领域的应用受到限制。因此对高分子材料进行阻燃处理是扩展其应用的必然途径。含磷硅的阻燃剂是一种有广泛应用前景的有机无机杂化阻燃剂,但有机无机杂化阻燃剂的阻燃效率是其广泛应用的障碍。本文通过分子设计制备了一种含磷和硅的杂化阻燃剂。通过溶胶凝胶法将这种有机无机杂化阻燃剂以原位聚合的方式添加到高分子中以提升高分子基体的阻燃性能,对材料的阻燃机理进行了探讨。膨胀型阻燃技术、纳米复合技术和溶胶凝胶技术被用来进一步提升这种含磷和硅的有机无机杂化阻燃剂的阻燃效率。主要研究内容如下：
1.通过分子设计制备了一种含磷和硅的液态硅烷阻燃剂(DOPO-VTS),通过溶胶凝胶法将其添加到环氧树脂和环氧丙烯酸树脂中以制备阻燃复合材料。对阻燃环氧树脂和环氧丙烯酸树脂的阻燃性能和阻燃机理进行了探讨。极限氧指数和热释放表明高的磷和硅添加量对环氧树脂和环氧丙烯酸树脂具有很好的阻燃作用。相对于环氧丙烯酸树脂复合材料,环氧树脂复合材料在低杂化阻燃剂的添加量的情况下展现出较高的阻燃效率：15wt%添加量可使材料达到UL-94V0级。通过直接裂解-质谱分析可知,有机无机杂化阻燃剂在环氧丙烯酸树脂中的热降解主要集中在低温阶段,而在环氧树脂中的热降解伴随着整个复合材料的热降解过程。因此这种有机无机杂化阻燃剂对环氧树脂具有较高的阻燃效率,值得深入研究。
2.通过溶胶凝胶法制备了一种含磷氮硅三种阻燃元素的有机无机杂化阻燃剂,通过原位聚合法将其添加到环氧树脂中以制备膨胀型阻燃复合材料。对阻燃剂的耐水性及其对环氧树脂的阻燃性进行了研究。这种有机无机杂化阻燃剂相比于传统阻燃剂APP具有较高的耐水性。此外,由于磷氮的防同阻燃作用,这种膨胀型阻燃体系在一定的磷氮比例情况下具有较高的阻燃效率。微型燃烧量热仪(MCC)结果表明这种有机无机杂化阻燃剂的添加能够明显降低材料燃烧过程中的热释放峰值(pHRR)和总热释放量(THR)。此外极限氧指数、垂直燃烧试验和热重分析验证了总热释放量的结果。SEM、FTIR、XPS和TGA-FTIR结果表明这种含磷氮硅的有机无机杂化阻燃剂在阻燃过程中能够同时起到气相阻燃和和凝聚相阻燃的作同。
3.一种含层离石墨烯的有机无机杂化阻燃剂的制备方法(阻.燃剂母粒法)被提出并制备出含层离石墨烯的有机无机杂化阻燃剂(FRs-rGO)。通过原位聚合法将所合成的杂化阻燃剂添加到环氧树脂中。复合材料FRs-rGO/EP的阻燃性能及力学性能用热重(TGA)、垂直燃烧测试(UL-94)、极限氧指数测试(LOI)、热释放测试(HRR)和动态力学性能测试(DMA)来研究。FRs-rGO的添加能够显著提升复合材料的高温残炭量。由于石墨烯的炭层增强作用和片层阻隔作用,FRs-rGO/EP在阻燃剂添加量为5wt.%时能够达到UL-94V0级,展现出较高的阻燃效率。
4.通过分子设计制备了一种含基于DOPO-VTS的有机无机杂化阻燃粒子(FRs-nanoparticles)并通过原位聚合法将这种杂化阻燃粒子添加到聚脲弹性体中。研究了材料的阻燃性能并对其阻燃机理进行了探讨。热重分析(TGA)表明FRs-nanoparticles能够显著提升复合材料的热稳定性,燃烧性能(MCC)表明复合材料的热释放峰值(pHRR)由于FRs-nanoparticles的添加而得到显著降低。实时红外分析(RTIR)表明FRs-nanoparticles能够促进复合材料生成苯环结构或者能够提高苯环结构的热稳定性,而苯环结构有助于材料燃烧过程中的成炭。复合材料的力学结果表明FRs-nanoparticles不仅能够提升材料的阻燃性能也能够提升材料的力学性能。
5.通过溶胶凝胶法用DOPO-VTS来修饰石墨烯从而形成有机无机杂化粒子修饰的石墨烯(nanoparticles-rGO),通过改变DOPO-VTS的添加量实现了对nanoparticles-rGO厚度的控制。nanoparticles-rGO以不同的比例添加到聚脲弹性体中并研究了复合材料的热稳定性和火安全性。结果表明rGO的良好分散和rGO上功能基团对复合材料阻燃性能和热稳定性的提升起着决定性作用。热释放结果表明0.5wt.%的nanoparticles-rGO添加量与5wt.%的FRs-nanoparticles添加量的热释放峰值降低效果相同,这说明了层状材料和有机无机杂化材料的结合的对材料阻燃的高效性。
The polymeric materials are widely used in our life and the quantity demanded of polymer commodity polymer such as plastic, rubbers, fiber, coating and adhesive are large all over the world.Despite having a number of benefits in applications, those polymeric materials also have drawbacks; the main drawback is due to their flammability, which hinders their applications in some areas, especially for the places require the fire safety. In this dissertation, a novel organic-inorganic hybrid flame retardant containing phosphorus and silicon were synthesized by the way of molecular design. Meanwhile, the novel organic-inorganic flame retardant was incorporated into polymeric matrix through the sol-gel and thermal curing processes to improve the flame retardancy of polymeric materials. Novel technologies such as sol-gel technology and "nano" technology are adopted, with the aim of further improving the flame retardant efficiency of the polymeric materials. The research work of this dissertation is composed of the following parts:
1. A novel liquid monomer containing phosphorus and silicon was synthesized by the way of molecular design. The sol-gel, UV-curing and thermo-curing technologies are employed to incorporate the flame retardants into the structures of epoxy acrylates and epoxy resins, resulting in the formation of organic-inorganic hybrid materials. The flame retardant performances of the organic-inorganic FRs/EP and organic-inorganic FRs/EA are compared and the flame retardant mechanisms are also discussed. The high content of phosphorus and silicon contribute a good flame retardancy to epoxy acrylates and epoxy resinswhich can be confirmed by the LOI and heat release results. The FRs/EP composites exhibit high flame retardant efficiency compared with EA/FRs composites:the FRs/EP can reach the UL-94VO ratio at the loading of15wt.%and has higher char residues at high temperature. From the DP-MS analysis, it can be found that the degradation of FRs in the FRs/EA matrix only occurs at low temperature. However, as for the FRs/EP composites. DOPO and its derivates are released at low temperature as well as high temperature. As a result, it can be concluded that the organic-inorganic FRs can play its flame retardant roles during the thermal degradation process of EP. Thus, the organic-inorganic flame retardants could impart great flame retardant efficiency to EP. which is worth depthly study.
2. A novel organic-inorganic FRs containing phosphorus, nitrogen and silicon was prepared through the sol-gel process and incorporated the flame retardants into epoxy resins. The organic-inorganic networks were formed and the organic-inorganic FRs has good water resistance. The flame retardant properties of the composites are investigated. The heat release results showed that the inclusion of EP-N1can significantly decrease the pHRR and THR ofEP compared with other composites, exhibiting the synergistic effect between phosphorus and nitrogen. Interestingly, at the same addition level. EP-N1exhibited much better flame retardancy (LOI and UL-94) and thermal stability (TGA, air). The SEM. FTIR. XPS and the TGA-FTIR results indicates that the strategy of organic-inorganic FRs combines condensed phase and gases phase flame retardant strategies.
3. A novel flame retardant (FRs-rGO) containing exfoliated graphene via in suit sol-gel process and incorporated the flame retardants into epoxy resins. With the incorporation of FRs-rGO into EP. a significant improvement in thermal stability is achieved in both air atmosphere and nitrogen atmosphere. The results indicate that the FRs-rGO could significantly improve the char residues at high temperature. Thus, satisfactory flame retardant grade was obtained when5wt.%of FRs-rGO was incorporated into the epoxy resins, indicating the great improvement.
4. The organic-inorganic nanoparticles (FRs-nanoparticles) containing organophosphorus and silicon were synthesized through the sol-gel process by the way of molecular design. Then FRs-nanoparticles were incorporated into the polyurea in different ratio via in situ polymerizationand the flame retardant properties and the mechanism are investigated. The TGA results indicated that FRs-nanoparticles could significantly postpone the initial decomposition temperature of the nanocomposites in air atmosphere. The peakheat release rate (pHRR) of the materials was significantly reduced due to the incorporation of FRs-nanoparticles. The RTIR results indicated that FRs-nanoparticles could catalyze the formation of benzene and its derived structure or improve thermal stability of benzene in the polyurea matrix. Furthermore, the tensile testing demonstrated that FRs-nanoparticles could also enhance the mechanical properties of polyurea.
5. The rGO was decorated with organic-inorganic nanoparticles (DOPO-VTS) through sol-gel process and the thickness of the nanoparticles-rGO can be varied by changing the additive amount of DOPO-VTS. Then, the nanoparticles-rGO was incorporated into polyurea in different rations via in situ polymerization. The thermal stability and the fire safety of the composites are investigated. Compared with the untreated rGO. the nanoparticles-rGO could significantly improve the thermal stability of polyurea and combustion properties, implying that the good dispersion of nanoparticles-rGO and thefunctional groups on the surface of rGO had the significant effect on the thermal stability of polyurea in air atmosphere. Moreover, the tensile and dynamic mechanical properties showed that the tensile strength and storage modulus of the nanocomposites could be obviously improved by incorporation of nanoparticles-rGO at low contents. The heart release results indicate that the0.5wt.%loading of nanoparticles-rGO has the same effect with the5wt.%loading of nanoparticles. indicating the advancement of layered nanotechnology.
1.通过分子设计制备了一种含磷和硅的液态硅烷阻燃剂(DOPO-VTS),通过溶胶凝胶法将其添加到环氧树脂和环氧丙烯酸树脂中以制备阻燃复合材料。对阻燃环氧树脂和环氧丙烯酸树脂的阻燃性能和阻燃机理进行了探讨。极限氧指数和热释放表明高的磷和硅添加量对环氧树脂和环氧丙烯酸树脂具有很好的阻燃作用。相对于环氧丙烯酸树脂复合材料,环氧树脂复合材料在低杂化阻燃剂的添加量的情况下展现出较高的阻燃效率：15wt%添加量可使材料达到UL-94V0级。通过直接裂解-质谱分析可知,有机无机杂化阻燃剂在环氧丙烯酸树脂中的热降解主要集中在低温阶段,而在环氧树脂中的热降解伴随着整个复合材料的热降解过程。因此这种有机无机杂化阻燃剂对环氧树脂具有较高的阻燃效率,值得深入研究。
2.通过溶胶凝胶法制备了一种含磷氮硅三种阻燃元素的有机无机杂化阻燃剂,通过原位聚合法将其添加到环氧树脂中以制备膨胀型阻燃复合材料。对阻燃剂的耐水性及其对环氧树脂的阻燃性进行了研究。这种有机无机杂化阻燃剂相比于传统阻燃剂APP具有较高的耐水性。此外,由于磷氮的防同阻燃作用,这种膨胀型阻燃体系在一定的磷氮比例情况下具有较高的阻燃效率。微型燃烧量热仪(MCC)结果表明这种有机无机杂化阻燃剂的添加能够明显降低材料燃烧过程中的热释放峰值(pHRR)和总热释放量(THR)。此外极限氧指数、垂直燃烧试验和热重分析验证了总热释放量的结果。SEM、FTIR、XPS和TGA-FTIR结果表明这种含磷氮硅的有机无机杂化阻燃剂在阻燃过程中能够同时起到气相阻燃和和凝聚相阻燃的作同。
3.一种含层离石墨烯的有机无机杂化阻燃剂的制备方法(阻.燃剂母粒法)被提出并制备出含层离石墨烯的有机无机杂化阻燃剂(FRs-rGO)。通过原位聚合法将所合成的杂化阻燃剂添加到环氧树脂中。复合材料FRs-rGO/EP的阻燃性能及力学性能用热重(TGA)、垂直燃烧测试(UL-94)、极限氧指数测试(LOI)、热释放测试(HRR)和动态力学性能测试(DMA)来研究。FRs-rGO的添加能够显著提升复合材料的高温残炭量。由于石墨烯的炭层增强作用和片层阻隔作用,FRs-rGO/EP在阻燃剂添加量为5wt.%时能够达到UL-94V0级,展现出较高的阻燃效率。
4.通过分子设计制备了一种含基于DOPO-VTS的有机无机杂化阻燃粒子(FRs-nanoparticles)并通过原位聚合法将这种杂化阻燃粒子添加到聚脲弹性体中。研究了材料的阻燃性能并对其阻燃机理进行了探讨。热重分析(TGA)表明FRs-nanoparticles能够显著提升复合材料的热稳定性,燃烧性能(MCC)表明复合材料的热释放峰值(pHRR)由于FRs-nanoparticles的添加而得到显著降低。实时红外分析(RTIR)表明FRs-nanoparticles能够促进复合材料生成苯环结构或者能够提高苯环结构的热稳定性,而苯环结构有助于材料燃烧过程中的成炭。复合材料的力学结果表明FRs-nanoparticles不仅能够提升材料的阻燃性能也能够提升材料的力学性能。
5.通过溶胶凝胶法用DOPO-VTS来修饰石墨烯从而形成有机无机杂化粒子修饰的石墨烯(nanoparticles-rGO),通过改变DOPO-VTS的添加量实现了对nanoparticles-rGO厚度的控制。nanoparticles-rGO以不同的比例添加到聚脲弹性体中并研究了复合材料的热稳定性和火安全性。结果表明rGO的良好分散和rGO上功能基团对复合材料阻燃性能和热稳定性的提升起着决定性作用。热释放结果表明0.5wt.%的nanoparticles-rGO添加量与5wt.%的FRs-nanoparticles添加量的热释放峰值降低效果相同,这说明了层状材料和有机无机杂化材料的结合的对材料阻燃的高效性。
The polymeric materials are widely used in our life and the quantity demanded of polymer commodity polymer such as plastic, rubbers, fiber, coating and adhesive are large all over the world.Despite having a number of benefits in applications, those polymeric materials also have drawbacks; the main drawback is due to their flammability, which hinders their applications in some areas, especially for the places require the fire safety. In this dissertation, a novel organic-inorganic hybrid flame retardant containing phosphorus and silicon were synthesized by the way of molecular design. Meanwhile, the novel organic-inorganic flame retardant was incorporated into polymeric matrix through the sol-gel and thermal curing processes to improve the flame retardancy of polymeric materials. Novel technologies such as sol-gel technology and "nano" technology are adopted, with the aim of further improving the flame retardant efficiency of the polymeric materials. The research work of this dissertation is composed of the following parts:
1. A novel liquid monomer containing phosphorus and silicon was synthesized by the way of molecular design. The sol-gel, UV-curing and thermo-curing technologies are employed to incorporate the flame retardants into the structures of epoxy acrylates and epoxy resins, resulting in the formation of organic-inorganic hybrid materials. The flame retardant performances of the organic-inorganic FRs/EP and organic-inorganic FRs/EA are compared and the flame retardant mechanisms are also discussed. The high content of phosphorus and silicon contribute a good flame retardancy to epoxy acrylates and epoxy resinswhich can be confirmed by the LOI and heat release results. The FRs/EP composites exhibit high flame retardant efficiency compared with EA/FRs composites:the FRs/EP can reach the UL-94VO ratio at the loading of15wt.%and has higher char residues at high temperature. From the DP-MS analysis, it can be found that the degradation of FRs in the FRs/EA matrix only occurs at low temperature. However, as for the FRs/EP composites. DOPO and its derivates are released at low temperature as well as high temperature. As a result, it can be concluded that the organic-inorganic FRs can play its flame retardant roles during the thermal degradation process of EP. Thus, the organic-inorganic flame retardants could impart great flame retardant efficiency to EP. which is worth depthly study.
2. A novel organic-inorganic FRs containing phosphorus, nitrogen and silicon was prepared through the sol-gel process and incorporated the flame retardants into epoxy resins. The organic-inorganic networks were formed and the organic-inorganic FRs has good water resistance. The flame retardant properties of the composites are investigated. The heat release results showed that the inclusion of EP-N1can significantly decrease the pHRR and THR ofEP compared with other composites, exhibiting the synergistic effect between phosphorus and nitrogen. Interestingly, at the same addition level. EP-N1exhibited much better flame retardancy (LOI and UL-94) and thermal stability (TGA, air). The SEM. FTIR. XPS and the TGA-FTIR results indicates that the strategy of organic-inorganic FRs combines condensed phase and gases phase flame retardant strategies.
3. A novel flame retardant (FRs-rGO) containing exfoliated graphene via in suit sol-gel process and incorporated the flame retardants into epoxy resins. With the incorporation of FRs-rGO into EP. a significant improvement in thermal stability is achieved in both air atmosphere and nitrogen atmosphere. The results indicate that the FRs-rGO could significantly improve the char residues at high temperature. Thus, satisfactory flame retardant grade was obtained when5wt.%of FRs-rGO was incorporated into the epoxy resins, indicating the great improvement.
4. The organic-inorganic nanoparticles (FRs-nanoparticles) containing organophosphorus and silicon were synthesized through the sol-gel process by the way of molecular design. Then FRs-nanoparticles were incorporated into the polyurea in different ratio via in situ polymerizationand the flame retardant properties and the mechanism are investigated. The TGA results indicated that FRs-nanoparticles could significantly postpone the initial decomposition temperature of the nanocomposites in air atmosphere. The peakheat release rate (pHRR) of the materials was significantly reduced due to the incorporation of FRs-nanoparticles. The RTIR results indicated that FRs-nanoparticles could catalyze the formation of benzene and its derived structure or improve thermal stability of benzene in the polyurea matrix. Furthermore, the tensile testing demonstrated that FRs-nanoparticles could also enhance the mechanical properties of polyurea.
5. The rGO was decorated with organic-inorganic nanoparticles (DOPO-VTS) through sol-gel process and the thickness of the nanoparticles-rGO can be varied by changing the additive amount of DOPO-VTS. Then, the nanoparticles-rGO was incorporated into polyurea in different rations via in situ polymerization. The thermal stability and the fire safety of the composites are investigated. Compared with the untreated rGO. the nanoparticles-rGO could significantly improve the thermal stability of polyurea and combustion properties, implying that the good dispersion of nanoparticles-rGO and thefunctional groups on the surface of rGO had the significant effect on the thermal stability of polyurea in air atmosphere. Moreover, the tensile and dynamic mechanical properties showed that the tensile strength and storage modulus of the nanocomposites could be obviously improved by incorporation of nanoparticles-rGO at low contents. The heart release results indicate that the0.5wt.%loading of nanoparticles-rGO has the same effect with the5wt.%loading of nanoparticles. indicating the advancement of layered nanotechnology.
引文
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