聚丙烯阻燃协效、成炭机理和新型膨胀阻燃体系的研究
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摘要
聚丙烯(PP)具有易加工、耐化学药品等优良特性,广泛应用于家电、建筑和汽车等领域,然而聚丙烯极易燃烧,使其应用领域受到极大限制。本论文在大量文献调研的基础上,综述聚丙烯膨胀阻燃技术以及聚丙烯纳米复合阻燃技术研究进展,在聚丙烯阻燃新技术和阻燃机理等方面开展了大量探索性工作,取得一系列原创性研究成果。采用水热合成的方法制备多种多孔金属磷酸盐,并将其与膨胀阻燃剂组成新型聚丙烯协效阻燃体系。研究多孔金属磷酸盐与膨胀阻燃剂的协效作用,并深入探讨该膨胀体系的协效阻燃机理：此外还制备膨胀阻燃聚丙烯／双氢氧化物(LDH)纳米复合材料,部分生物可降解聚丙烯阻燃复合材料以及具有耐水性好、阻燃效率优异的新型膨胀阻燃聚丙烯材料等。主要研究工作如下：
1.采用水热合成的方法制备具有多孔结构的磷酸镍(VSB-1),研究其在PP基体中与膨胀阻燃剂(IFR, APP/PER=2:1)的协效作用。极限氧指数(LOI)、UL94测试和锥型量热计(Cone)研究结果表明添加适量VSB-1的膨胀阻燃PP的阻燃性能比未添加VSB-1时显著增加,材料具有更高的火灾安全性。与硼酸锌(ZB)、4A分子筛、蒙脱土这些阻燃协效剂相比,在相同的添加量时VSB-1体系表现出最好的协效作用,添加VSB-1的阻燃PP能够以最低的阻燃剂添加量达到UL94 V-0级。同时,利用实时红外研究该膨胀体系的热氧化分解行为,表明VSB-1的加入能够提高材料的热稳定性。利用扫描电镜(SEM)对复合材料燃烧后残余炭层形貌进行表征,结果显示含有VSB-1的膨胀炭层更加致密。力学测试表明在保持阻燃性能相同的情况下,添加VSB-1能够明显减少阻燃剂的添加量,从而显著改善阻燃材料的力学性能。上述研究表明,在PP的基体中VSB-1对于膨胀阻燃剂具有明显协效作用,添加适量的VSB-1大幅度提高阻燃PP的热稳定性和阻燃性能。VSB-1的添加是设计新型高效膨胀阻燃材料的有效途径之一。
2.将过渡金属离子(Fe, Zn)引入到VSB-1结构中,通过水热法合成两种过渡金属离子掺杂的磷酸镍盐(TMIVSB-1),并研究TMIVSB-1在PP基体中与IFR的协效作用。同时选择另一种磷酸盐-焦磷酸铁(FePP),研究其与膨胀阻燃剂的协效作用及作用机理。LOI和UL94研究结果表明,TMIVSB-1和FePP均能明显提高IFR体系的阻燃性能。利用XPS分析受热相同时间取得的样品,研究表明,添加FePP可延迟基体的氧化分解,提高材料的耐热性能。此外,通过热重红外联用(TG-IR)研究发现PP/IFR/FePP复配体系的阻燃机理是凝聚相阻燃机理。
3.采用一步法制备十二烷基硫酸钠改性的锌铝双氢氧化物ZnAl (SDS)-LDH,并对其结构进行表征。通过熔融共混法制备膨胀阻燃PP/ZnAl(SDS)-LDH纳米复合材料。采用LOI、热重分析仪(TGA)和差热扫描分析仪(DSC)等表征手段研究有机改性的LDH对膨胀阻燃PP的阻燃性能、热稳定性和结晶性能的影响,并且研究阻燃材料的制备工艺对阻燃性能的影响。
4.利用同步辐射真空紫外单光子电离和飞行时间质谱相结合的技术研究PP真空热裂解产物,并分析PP裂解机理；通过熔融共混制备PP/OMT/Ni2O3复合材料,研究不同因素如气氛、温度、组分等对该复合材料成炭机制的影响,结合上述同步辐射技术的研究结果阐述催化成炭机理,并研究材料的燃烧性能,为深入研究新型阻燃聚合物复合材料的理论研究和工程应用提供帮助。
5.采用熔融共混法制备淀粉(starch)基的部分生物可降解PP阻燃复合材料。选用微胶囊化包裹聚磷酸铵(MCAPP)作为阻燃剂,同时由于微胶囊的外表保护壳层的存在,MCAPP可阻止复合材料加工过程中聚磷酸铵(APP)与淀粉中的羟基之间的反应,提高阻燃复合材料的加工稳定性。LOI、UL94、Cone和TGA结果表明将MCAPP加入淀粉基的PP复合材料后,材料的阻燃性和热性能显著提高。研究结果表明：将MCAPP加入到淀粉基的PP复合材料,MCAPP与starch可形成膨胀阻燃体系,在高温下能够在材料表面形成膨胀炭层,起到隔热、隔氧以及减缓可燃性气体逸出的作用,从而提高材料的阻燃性能。
6.将MCAPP与大分子三嗪类衍生物成炭剂(CFA)复配为新型膨胀阻燃体系,制备新型膨胀阻燃PP材料。研究表明CFA/MCAPP之间存在协效效应,CFA/MCAPP的复配比例对材料热稳定性和阻燃性能具有重要影响。PP/MCAPP和PP/CFA均易燃烧,然而当二者以适当比例复配后体系的阻燃性能显著提高。只有CFA与合适比例复配,体系才能形成致密的膨胀炭层。耐水性研究表明CFA/MCAPP=1:2时,材料的耐水性最好,在70℃热水中浸泡168h后仍能达到UL94 V-0级。
Polypropylene (PP) has broad applications in electronics, architectural materials, cars and so on, due to its easy processing, chemical resistance and other excellent properties. However, PP is flammable, so it is necessary to improve the flame retardancy of PP in order to expand its application. In this dissertation, a lot of literatures have been reviewed on the basis of intumescent flame retardant PP and flame retardant PP nanocomposites. Some porous metal phosphates were prepared by hydrothermal synthesis, and were used in the intumescent flame retardant PP. We also prepared flame retardant PP/layer double hydroxide (LDH) nanocomposites, some semi-biodegradable flame retardant PP composites, and new high efficiency intumescent flame retardant PP materials with good water resistant property. Main research works are as follows:
1. A novel synergist-nanoporous nickel phosphates VSB-1 was prepared by hydrothermal synthesis. Then we investigated the synergistic effect of the VSB-1 with intumescent flame retardants (IFR, APP/PER=2:1) in PP matrix. From the results of LOI, UL94 and Cone test, it can be found that flame retardant PP material with the suitable content of VSB-1 has a better flame retardant properties and a higher fire safety. Compared with ZB,4A zeolite and OMT which are very effective synergists with intumescent flame retardants, VSB-1 shows the best synergistic effect at the same loading. In addition, real-time infrared studies thermo-oxidative degradation mechanism of the intumescent system, and the addition of VSB-1 is found to increase the thermal stability. Scanning electron microscopy (SEM) is used to characterize the morphology of char layer after the oxygen index test, and the result shows that the VSB-1 containing char layer is more compact. Mechanical testing shows that keeping the flame retardant properties unchange, the addtion of VSB-1 can significantly improve the mechanical properties of flame retardant PP. Through the research we want to provide a more promising way for design new efficient intumescent material that can further reduce the addition of flame retardants.
2. We continue further study of previous work by the isomorphous substitution of transition metal ions (Fe, Zn) into the nickel phosphates VSB-1 framework. Then, the two kinds of transition metal ion-incorporated nickel phosphates (TMIVSB-1) materials were synthesized using a hydrothermal method. Meanwhile, a low cost synergist-ferric pyrophosphate (FePP) was used in intumescent flame retardant PP. The synergistic effects of TMIVSB-1 or FePP with intumescent flame retardants (IFR, APP/PER=2:1) in PP matrix were investigated. According to their flammability tests (LOI, UL94 test), TMIVSB-1 or FePP can obviously improve the flame retardant properties of PP composites. The results of XPS show that the addition of FePP can greatly improve the high temperature performance of flame retardant PP.TG-IR results also demonstrate that the flame retardant mechanism of PP/IFR/FePP system is in the condensed phase rather than in the gas phase.
3. Sodium dodecyl sulfate modified zinc-aluminum layered double hydroxide ZnAl(SDS)-LDH was prepared via one-step method, and its structure was characterized. Intumescent flame retardant PP/ZnAl(SDS)-LDH nanocomposites were prepared by melt blending. The effects of organic modified LDH on the flame retardant properties, thermal stability and crystal properties of the intumescent flame retardant PP composites have been studied by limiting oxygen index (LOI), thermal gravimetric analysis (TGA) and differential scanning analyzer (DSC). The influence of preparation method on flame retardant performance of materials has been studied as well.
4. Combining synchrotron radiation vacuum ultraviolet single-photon ionization and reflection time of flight mass spectrometry technology to characterize vacuum pyrolysis products of PP in order to study the mechanism of PP pyrolysis; PP/organically modified montmorillonite (OMT)/Ni2O3 composite were prepared by melted blending, and then investigated the influence of different factors such as atmosphere, temperature, composition on the carbonization of PP composites. In this work a detailed mechanism for the formation and the growth of MWCNTs is proposed based on the experimental analysis. Furthermore, the flame retardancy of PP composites was also investigated. From this work, we hope to help theoretical research and engineering applications of novel flame retardant polymer composites.
5. Starch containing polypropylene (SCP) semi-biocomposites were prepared by melted blend method. Microencapsulated ammonium polyphosphate (MCAPP) was added to the SCP not only to improve its flame retardant properties but also to restrain the reaction between ammonium polyphosphate (APP) and starch during processing. The flame retardant properties of the flame retardant SCP composites have been investigated by limited oxygen index (LOI), UL94 test and cone calorimeter test. The results show that flame retardant properites of SCP improve substantially compared with that of pure PP. MCAPP and starch can form an intumescent system to protect the matrix from further burning, so the flame retardant properties of SCP semi-biocomposites improve.
6. A novel flame retardant PP materials were prepared by the addtion of the intumescent flame retardants (IFR) consisting of a novel char forming agent (CFA) and MCAPP. With the loading 30wt% IFR(CFA/MCAPP=1/2), PP composites present the most effective flame retardancy ability with the value of LOI to 36.5. Even with 25wt% IFR (CFA/MCAPP=1/2), PP composites can still pass V-0 rating. The results of cone calorimeter show that heat release rate peak (pHRR), total heat release (THR), and the mass loss rate (MLR) of PP/30wt% IFR(CFA/MCAPP=1/2) decrease substantially when compared with those of pure PP, the pHRR decreasing from 1140 to 100 kW/m2, the THR decreaing from 96 to 16.8 MJ/m2and the MLR decreasing from 100% to 40%. SEM demonstrates the quality of char layers of PP/MCAPP/CFA systems are superior to those of PP/MCAPP and PP/CFA systems. From water resistant test, it shows that the sample of PP/30wt% IFR(CFA/MCAPP=1/2) also has excellent water resistant property, after 168h the sample can still obtain a UL94 V-0 rating.
1.采用水热合成的方法制备具有多孔结构的磷酸镍(VSB-1),研究其在PP基体中与膨胀阻燃剂(IFR, APP/PER=2:1)的协效作用。极限氧指数(LOI)、UL94测试和锥型量热计(Cone)研究结果表明添加适量VSB-1的膨胀阻燃PP的阻燃性能比未添加VSB-1时显著增加,材料具有更高的火灾安全性。与硼酸锌(ZB)、4A分子筛、蒙脱土这些阻燃协效剂相比,在相同的添加量时VSB-1体系表现出最好的协效作用,添加VSB-1的阻燃PP能够以最低的阻燃剂添加量达到UL94 V-0级。同时,利用实时红外研究该膨胀体系的热氧化分解行为,表明VSB-1的加入能够提高材料的热稳定性。利用扫描电镜(SEM)对复合材料燃烧后残余炭层形貌进行表征,结果显示含有VSB-1的膨胀炭层更加致密。力学测试表明在保持阻燃性能相同的情况下,添加VSB-1能够明显减少阻燃剂的添加量,从而显著改善阻燃材料的力学性能。上述研究表明,在PP的基体中VSB-1对于膨胀阻燃剂具有明显协效作用,添加适量的VSB-1大幅度提高阻燃PP的热稳定性和阻燃性能。VSB-1的添加是设计新型高效膨胀阻燃材料的有效途径之一。
2.将过渡金属离子(Fe, Zn)引入到VSB-1结构中,通过水热法合成两种过渡金属离子掺杂的磷酸镍盐(TMIVSB-1),并研究TMIVSB-1在PP基体中与IFR的协效作用。同时选择另一种磷酸盐-焦磷酸铁(FePP),研究其与膨胀阻燃剂的协效作用及作用机理。LOI和UL94研究结果表明,TMIVSB-1和FePP均能明显提高IFR体系的阻燃性能。利用XPS分析受热相同时间取得的样品,研究表明,添加FePP可延迟基体的氧化分解,提高材料的耐热性能。此外,通过热重红外联用(TG-IR)研究发现PP/IFR/FePP复配体系的阻燃机理是凝聚相阻燃机理。
3.采用一步法制备十二烷基硫酸钠改性的锌铝双氢氧化物ZnAl (SDS)-LDH,并对其结构进行表征。通过熔融共混法制备膨胀阻燃PP/ZnAl(SDS)-LDH纳米复合材料。采用LOI、热重分析仪(TGA)和差热扫描分析仪(DSC)等表征手段研究有机改性的LDH对膨胀阻燃PP的阻燃性能、热稳定性和结晶性能的影响,并且研究阻燃材料的制备工艺对阻燃性能的影响。
4.利用同步辐射真空紫外单光子电离和飞行时间质谱相结合的技术研究PP真空热裂解产物,并分析PP裂解机理；通过熔融共混制备PP/OMT/Ni2O3复合材料,研究不同因素如气氛、温度、组分等对该复合材料成炭机制的影响,结合上述同步辐射技术的研究结果阐述催化成炭机理,并研究材料的燃烧性能,为深入研究新型阻燃聚合物复合材料的理论研究和工程应用提供帮助。
5.采用熔融共混法制备淀粉(starch)基的部分生物可降解PP阻燃复合材料。选用微胶囊化包裹聚磷酸铵(MCAPP)作为阻燃剂,同时由于微胶囊的外表保护壳层的存在,MCAPP可阻止复合材料加工过程中聚磷酸铵(APP)与淀粉中的羟基之间的反应,提高阻燃复合材料的加工稳定性。LOI、UL94、Cone和TGA结果表明将MCAPP加入淀粉基的PP复合材料后,材料的阻燃性和热性能显著提高。研究结果表明：将MCAPP加入到淀粉基的PP复合材料,MCAPP与starch可形成膨胀阻燃体系,在高温下能够在材料表面形成膨胀炭层,起到隔热、隔氧以及减缓可燃性气体逸出的作用,从而提高材料的阻燃性能。
6.将MCAPP与大分子三嗪类衍生物成炭剂(CFA)复配为新型膨胀阻燃体系,制备新型膨胀阻燃PP材料。研究表明CFA/MCAPP之间存在协效效应,CFA/MCAPP的复配比例对材料热稳定性和阻燃性能具有重要影响。PP/MCAPP和PP/CFA均易燃烧,然而当二者以适当比例复配后体系的阻燃性能显著提高。只有CFA与合适比例复配,体系才能形成致密的膨胀炭层。耐水性研究表明CFA/MCAPP=1:2时,材料的耐水性最好,在70℃热水中浸泡168h后仍能达到UL94 V-0级。
Polypropylene (PP) has broad applications in electronics, architectural materials, cars and so on, due to its easy processing, chemical resistance and other excellent properties. However, PP is flammable, so it is necessary to improve the flame retardancy of PP in order to expand its application. In this dissertation, a lot of literatures have been reviewed on the basis of intumescent flame retardant PP and flame retardant PP nanocomposites. Some porous metal phosphates were prepared by hydrothermal synthesis, and were used in the intumescent flame retardant PP. We also prepared flame retardant PP/layer double hydroxide (LDH) nanocomposites, some semi-biodegradable flame retardant PP composites, and new high efficiency intumescent flame retardant PP materials with good water resistant property. Main research works are as follows:
1. A novel synergist-nanoporous nickel phosphates VSB-1 was prepared by hydrothermal synthesis. Then we investigated the synergistic effect of the VSB-1 with intumescent flame retardants (IFR, APP/PER=2:1) in PP matrix. From the results of LOI, UL94 and Cone test, it can be found that flame retardant PP material with the suitable content of VSB-1 has a better flame retardant properties and a higher fire safety. Compared with ZB,4A zeolite and OMT which are very effective synergists with intumescent flame retardants, VSB-1 shows the best synergistic effect at the same loading. In addition, real-time infrared studies thermo-oxidative degradation mechanism of the intumescent system, and the addition of VSB-1 is found to increase the thermal stability. Scanning electron microscopy (SEM) is used to characterize the morphology of char layer after the oxygen index test, and the result shows that the VSB-1 containing char layer is more compact. Mechanical testing shows that keeping the flame retardant properties unchange, the addtion of VSB-1 can significantly improve the mechanical properties of flame retardant PP. Through the research we want to provide a more promising way for design new efficient intumescent material that can further reduce the addition of flame retardants.
2. We continue further study of previous work by the isomorphous substitution of transition metal ions (Fe, Zn) into the nickel phosphates VSB-1 framework. Then, the two kinds of transition metal ion-incorporated nickel phosphates (TMIVSB-1) materials were synthesized using a hydrothermal method. Meanwhile, a low cost synergist-ferric pyrophosphate (FePP) was used in intumescent flame retardant PP. The synergistic effects of TMIVSB-1 or FePP with intumescent flame retardants (IFR, APP/PER=2:1) in PP matrix were investigated. According to their flammability tests (LOI, UL94 test), TMIVSB-1 or FePP can obviously improve the flame retardant properties of PP composites. The results of XPS show that the addition of FePP can greatly improve the high temperature performance of flame retardant PP.TG-IR results also demonstrate that the flame retardant mechanism of PP/IFR/FePP system is in the condensed phase rather than in the gas phase.
3. Sodium dodecyl sulfate modified zinc-aluminum layered double hydroxide ZnAl(SDS)-LDH was prepared via one-step method, and its structure was characterized. Intumescent flame retardant PP/ZnAl(SDS)-LDH nanocomposites were prepared by melt blending. The effects of organic modified LDH on the flame retardant properties, thermal stability and crystal properties of the intumescent flame retardant PP composites have been studied by limiting oxygen index (LOI), thermal gravimetric analysis (TGA) and differential scanning analyzer (DSC). The influence of preparation method on flame retardant performance of materials has been studied as well.
4. Combining synchrotron radiation vacuum ultraviolet single-photon ionization and reflection time of flight mass spectrometry technology to characterize vacuum pyrolysis products of PP in order to study the mechanism of PP pyrolysis; PP/organically modified montmorillonite (OMT)/Ni2O3 composite were prepared by melted blending, and then investigated the influence of different factors such as atmosphere, temperature, composition on the carbonization of PP composites. In this work a detailed mechanism for the formation and the growth of MWCNTs is proposed based on the experimental analysis. Furthermore, the flame retardancy of PP composites was also investigated. From this work, we hope to help theoretical research and engineering applications of novel flame retardant polymer composites.
5. Starch containing polypropylene (SCP) semi-biocomposites were prepared by melted blend method. Microencapsulated ammonium polyphosphate (MCAPP) was added to the SCP not only to improve its flame retardant properties but also to restrain the reaction between ammonium polyphosphate (APP) and starch during processing. The flame retardant properties of the flame retardant SCP composites have been investigated by limited oxygen index (LOI), UL94 test and cone calorimeter test. The results show that flame retardant properites of SCP improve substantially compared with that of pure PP. MCAPP and starch can form an intumescent system to protect the matrix from further burning, so the flame retardant properties of SCP semi-biocomposites improve.
6. A novel flame retardant PP materials were prepared by the addtion of the intumescent flame retardants (IFR) consisting of a novel char forming agent (CFA) and MCAPP. With the loading 30wt% IFR(CFA/MCAPP=1/2), PP composites present the most effective flame retardancy ability with the value of LOI to 36.5. Even with 25wt% IFR (CFA/MCAPP=1/2), PP composites can still pass V-0 rating. The results of cone calorimeter show that heat release rate peak (pHRR), total heat release (THR), and the mass loss rate (MLR) of PP/30wt% IFR(CFA/MCAPP=1/2) decrease substantially when compared with those of pure PP, the pHRR decreasing from 1140 to 100 kW/m2, the THR decreaing from 96 to 16.8 MJ/m2and the MLR decreasing from 100% to 40%. SEM demonstrates the quality of char layers of PP/MCAPP/CFA systems are superior to those of PP/MCAPP and PP/CFA systems. From water resistant test, it shows that the sample of PP/30wt% IFR(CFA/MCAPP=1/2) also has excellent water resistant property, after 168h the sample can still obtain a UL94 V-0 rating.
引文
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