膨胀阻燃丁苯橡胶及三元乙丙橡胶/聚丙烯材料的制备和性能研究
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摘要
膨胀型阻燃剂是近年来颇受大家关注的一类新型无卤的阻燃剂,这类阻燃剂阻燃效果好,在高分子材料阻燃研究领域的应用越来越广泛。它具有阻燃性能高、无熔滴行为,低烟、无毒和没有腐蚀气体生成的特点。本文通过对大量的国内外文献进行调研,并且结合本实验室的相关工作,分析研究了丁苯橡胶(SBR)和三元乙丙橡胶/聚丙烯(EPDM/PP)的阻燃技术以及稀土类化合物的作用等。本文以SBR和EPDM/PP为基体,用膨胀阻燃体系中的典型阻燃剂聚磷酸铵(APP)/季戊四醇(PER)组合,制备了膨胀阻燃材料,并对其热稳定性和阻燃性能进行测试,重点考察了稀土盐及铁基蒙脱土对膨胀阻燃剂的协同增效作用,对其热稳定性以及协效机理进行分析。
稀土元素的研究日益热门,其应用也日益广泛,尤其是在研制现代的一些新型功能性材料领域的应用,稀土元素已成为不可缺少的原料。本文研究了磷酸铈对SBR和EPDM/PP复合材料的协效阻燃性能、机械性能、以及碳层微观结构等的影响。研究结果表明,磷酸铈盐对改善膨胀性阻燃SBR和EPDM/PP材料的垂直燃烧等级、减少热释放和增强物理机械性能等发挥一定的积极作用,是一种比较好的阻燃协效剂。
本论文的主要研究工作有以下几方面:
1.为了能够有效缓和膨胀阻燃材料耐水性能差的缺点,本文用聚氨脂树脂包裹的APP(PUMAPP)和PER复配组成膨胀性体系用来阻燃SBR,制备了膨胀型阻燃SBR。其阻燃性能主要用氧指数法(LOI)和垂直燃烧(UL-94)表征。通过热重分析(TGA)结果发现,添加阻燃剂后,SBR在高温区的热稳定性得到提高,并且最后的碳残余量也有所增加。使用实时红外(FTIR)探测,结果显示,在高温条件下,材料会形成一种含大量磷元素的稳固炭层。文中对添加不同阻燃剂后材料燃烧性能、力学性能及水溶性等方面进行了对比。研究发现,在添加量相同的情况下,用PUMAPP的阻燃性能要优于APP,其主要原因可能与包裹后的APP的界面和在材料中分散性有关。
2.以SBR为基体,在APP和PER组成的阻燃体系加入四价的磷酸铈(CeP(IV)),考察了SBR在不同的CeP(IV)添加量下LOI以及UL-94等级的变化。同时,使用TGA考察了空气条件下CeP(IV)对膨胀型阻燃SBR的热失重的影响,并用FTIR对膨胀型阻燃SBR复合物进行实时监测和分析,对碳层的形貌进行了扫描电镜(SEM)分析。
3.在对EPDM/PP体系进行阻燃时,考察磷酸铈(CeP)以及铁基蒙脱土(Fe-MMT)对膨胀体系的协效作用。利用LOI、UL-94和TGA研究了EPDM/PP材料的阻燃性能和热稳定性,通过SEM观察了协效剂对材料燃烧后炭层的影响。本文研究加入协效剂对材料在阻燃性能、成炭机理和热稳定性等方面的影响。
Intumescent flame retardant(IFR) is a new type of halogen-free flame retardant and has played an important role in improving the flame retardancy. IFR are generally used in polymers because of their high efficiency, low dose levels, low smoke and non-toxic and so on. In this paper, the development of flame retardant styrene butadiene rubber(SBR) and EPDM/PP as well as the research progress of flame retardant were explored based on the related work in our laboratory and literatures. SBR and EPDM/PP were used as matrix and the typical IFR system which APP/PER were chosen as flame retardant to prepare intumescent flame retardant materials. The thermal stability and flame retardant properties of the materials were investigated. The study focused on the effect of some compounds used as the synergists and the synergistic mechanism as well as its thermal stability were discussed.
With the development of the application of rare earth elements, it has been widely used in the fields of electronics, energy, light industry, petrochemicals, machinery, environmental friendly, agriculture and other fields. Especially with the study and application of the modern functional materials, the rare earth elements have become essential raw materials. In this paper, the effect of cerium phosphate on combustion and mechnical properties of SBR and EPDM/PP composites was studied. The experimental results showed that the rare earth phosphate promoted the vertical flame rating improvement on SBR and EPDM/PP, lowered the heat release rate and improved the mechanical properties. The rare earth phosphate is a excellent synergistic agent.
The main research work in this paper as followed:
1. In order to solve the poor water resistance of IFR, the microencapsulated technology was used, which is wrapped APP in PU resin. In this paper, the mixture of APP (or PUMAPP) and PER was used to flame retard SBR. The SBR composites were prepared. And the flame retardant properties were measured by the LOI and UL94. From the result of TGA, it found that the addition of IFR improved the thermal stability of SBR at high temperature and greatly increase the amount of char residue. From FTIR results, it found that there is a stable carbon layer formed which contained mostly phosphorus at the high temperature. The combustion properties, mechanical properties and water-soluble were studied. It found that adding the same amount of APP and PUMAPP, the performance of SBR with PUMAPP is better than that with APP. The main reason may be related with the interface and dispersion of APP after microcapsuled.
2. The IFR system composed with APP and PER, which consisted of CeP(IV) were added into the SBR. The flame retardant propertis of SBR were investigated under different amounts of CeP(IV) using LOI and UL94. At the same time, the TGA was used to investigate the effect of synergistic agent to thermal decomposition of SBR under air atmosphere. The thermal degradation behavior of SBR composites is investigated using FTIR. To further analyze how the structure of intumescent charred layer determines flame retardancy of SBR, the morphologies of the charred layers were examined by SEM.
3. In the preparation of EPDM/PP system, the CeP and Fe-MMT were used. And their synergist effect was studied. The flame retardant properties and thermal stability of EPDM/PP was observed using the LOI, UL-94 and TGA. SEM was used to investigate the morphological structure of the char layer. It had been found that the addition of synergistic agent into the EPDM/PP/APP/PER composites has better flame retardancy. In this paper, the effect between synergistic agent and intumenscent flame retardant system was studied.
稀土元素的研究日益热门,其应用也日益广泛,尤其是在研制现代的一些新型功能性材料领域的应用,稀土元素已成为不可缺少的原料。本文研究了磷酸铈对SBR和EPDM/PP复合材料的协效阻燃性能、机械性能、以及碳层微观结构等的影响。研究结果表明,磷酸铈盐对改善膨胀性阻燃SBR和EPDM/PP材料的垂直燃烧等级、减少热释放和增强物理机械性能等发挥一定的积极作用,是一种比较好的阻燃协效剂。
本论文的主要研究工作有以下几方面:
1.为了能够有效缓和膨胀阻燃材料耐水性能差的缺点,本文用聚氨脂树脂包裹的APP(PUMAPP)和PER复配组成膨胀性体系用来阻燃SBR,制备了膨胀型阻燃SBR。其阻燃性能主要用氧指数法(LOI)和垂直燃烧(UL-94)表征。通过热重分析(TGA)结果发现,添加阻燃剂后,SBR在高温区的热稳定性得到提高,并且最后的碳残余量也有所增加。使用实时红外(FTIR)探测,结果显示,在高温条件下,材料会形成一种含大量磷元素的稳固炭层。文中对添加不同阻燃剂后材料燃烧性能、力学性能及水溶性等方面进行了对比。研究发现,在添加量相同的情况下,用PUMAPP的阻燃性能要优于APP,其主要原因可能与包裹后的APP的界面和在材料中分散性有关。
2.以SBR为基体,在APP和PER组成的阻燃体系加入四价的磷酸铈(CeP(IV)),考察了SBR在不同的CeP(IV)添加量下LOI以及UL-94等级的变化。同时,使用TGA考察了空气条件下CeP(IV)对膨胀型阻燃SBR的热失重的影响,并用FTIR对膨胀型阻燃SBR复合物进行实时监测和分析,对碳层的形貌进行了扫描电镜(SEM)分析。
3.在对EPDM/PP体系进行阻燃时,考察磷酸铈(CeP)以及铁基蒙脱土(Fe-MMT)对膨胀体系的协效作用。利用LOI、UL-94和TGA研究了EPDM/PP材料的阻燃性能和热稳定性,通过SEM观察了协效剂对材料燃烧后炭层的影响。本文研究加入协效剂对材料在阻燃性能、成炭机理和热稳定性等方面的影响。
Intumescent flame retardant(IFR) is a new type of halogen-free flame retardant and has played an important role in improving the flame retardancy. IFR are generally used in polymers because of their high efficiency, low dose levels, low smoke and non-toxic and so on. In this paper, the development of flame retardant styrene butadiene rubber(SBR) and EPDM/PP as well as the research progress of flame retardant were explored based on the related work in our laboratory and literatures. SBR and EPDM/PP were used as matrix and the typical IFR system which APP/PER were chosen as flame retardant to prepare intumescent flame retardant materials. The thermal stability and flame retardant properties of the materials were investigated. The study focused on the effect of some compounds used as the synergists and the synergistic mechanism as well as its thermal stability were discussed.
With the development of the application of rare earth elements, it has been widely used in the fields of electronics, energy, light industry, petrochemicals, machinery, environmental friendly, agriculture and other fields. Especially with the study and application of the modern functional materials, the rare earth elements have become essential raw materials. In this paper, the effect of cerium phosphate on combustion and mechnical properties of SBR and EPDM/PP composites was studied. The experimental results showed that the rare earth phosphate promoted the vertical flame rating improvement on SBR and EPDM/PP, lowered the heat release rate and improved the mechanical properties. The rare earth phosphate is a excellent synergistic agent.
The main research work in this paper as followed:
1. In order to solve the poor water resistance of IFR, the microencapsulated technology was used, which is wrapped APP in PU resin. In this paper, the mixture of APP (or PUMAPP) and PER was used to flame retard SBR. The SBR composites were prepared. And the flame retardant properties were measured by the LOI and UL94. From the result of TGA, it found that the addition of IFR improved the thermal stability of SBR at high temperature and greatly increase the amount of char residue. From FTIR results, it found that there is a stable carbon layer formed which contained mostly phosphorus at the high temperature. The combustion properties, mechanical properties and water-soluble were studied. It found that adding the same amount of APP and PUMAPP, the performance of SBR with PUMAPP is better than that with APP. The main reason may be related with the interface and dispersion of APP after microcapsuled.
2. The IFR system composed with APP and PER, which consisted of CeP(IV) were added into the SBR. The flame retardant propertis of SBR were investigated under different amounts of CeP(IV) using LOI and UL94. At the same time, the TGA was used to investigate the effect of synergistic agent to thermal decomposition of SBR under air atmosphere. The thermal degradation behavior of SBR composites is investigated using FTIR. To further analyze how the structure of intumescent charred layer determines flame retardancy of SBR, the morphologies of the charred layers were examined by SEM.
3. In the preparation of EPDM/PP system, the CeP and Fe-MMT were used. And their synergist effect was studied. The flame retardant properties and thermal stability of EPDM/PP was observed using the LOI, UL-94 and TGA. SEM was used to investigate the morphological structure of the char layer. It had been found that the addition of synergistic agent into the EPDM/PP/APP/PER composites has better flame retardancy. In this paper, the effect between synergistic agent and intumenscent flame retardant system was studied.
引文
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