热塑性聚合物（PVC, PPS）纳米复合材料的制备及其性能研究
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摘要
我国聚氯乙烯(PVC)产量占通用塑料的30%以上,PVC的阻燃、抑烟为国家强制性标准,但现有的阻燃抑烟添加剂很难达到要求。特种工程塑料之首的聚苯硫醚(PPS)是目前唯一可以熔融纺丝的高性能纤维,但其紫外光(UV)稳定性很差,在室外使用时纤维、薄膜等制品的外观和使用性能显著下降,但目前尚无合适的抗UV添加剂。PVC、PPS等热塑性聚合物分子结构上存在的弱键,导致在高温或UV作用下发生降解,严重影响了材料的加工和使用性能。
本文通过热塑性聚合物(PVC、PPS)纳米复合材料的制备改进PVC材料的阻燃、抑烟性能和PPS材料的UV稳定性。
首次采用层状纳米水滑石(HT)和纳米氧化锌(ZnO)作为复合添加剂(HT-ZnO),制备了PVC纳米复合阻燃抑烟材料。通过TEM、TGA和裂解-气-质色谱(Py-GC-MS)等方法系统研究了纳米HT-ZnO复合添加剂的组成、含量对PVC材料阻燃、抑烟和力学性能的影响。同时以纳米氧化铈(CeO_2)、氧化钛(TiO_2)为紫外光稳定剂制备了PPS纳米复合材料,通过SEM、FTIR、DSC、DMA等方法研究了纯PPS及其纳米复合材料UV老化过程中分子结构、结晶结构和力学性能的变化规律,探讨了纳米CeO_2、TiO_2对PPS UV老化和结晶动力学的影响。
PVC纳米复合材料的阻燃、抑烟研究结果表明:当HT/ZnO为3:2时,复合添加剂在阻燃和抑烟性能上具有明显的协同效应。当HT/ZnO为3:2、HT-ZnO加入量为5%时,其在PVC中具有较好的分散性,软质PVC和建筑硬质PVC纳米复合材料均具有优异的阻燃、抑烟综合性能,极限氧指数比对照样提高了28-49%,烟密度等级比对照样下降了27-29%。软质PVC纳米复合材料的极限氧指数达到32.5%,烟密度等级达到70.1,这两项指标均达到GB8624-1997热塑性塑料难燃级材料(B_1)的要求;建筑硬质PVC纳米复合材料的开始发烟时间比对照样推近了15秒,最大烟密度下降了16%,极限氧指数达到64.0%,烟密度等级达到63.2,两项指标均明显优于国标。
纳米HT-ZnO复合添加剂的抑烟机理为能量移除和可燃物减少两方面的协同效果。在能量移除方面包括两部分:一是纳米HT结构自身脱去层间水吸收的能量和羟基、碳酸根分解生成大量的水和二氧化碳吸收的能量;二是纳米HT受热分解后生成的金属氧化物参与PVC分解过程中的反应,吸收体系中的能量。在可燃物减少方面主要是ZnO加速了PVC脱去HCl的反应,并控制形成反式多烯结构,进而发生交联反应形成焦炭层,从而阻止苯等芳香族化合物的生成,降低可燃物的释放。能量移除和可燃物减少两方面的协同作用,使纳米HT-ZnO复合组分具有显著的阻燃抑烟效果。本阻燃抑烟机理对阻燃聚合物材料的研究具有重要的参考价值。
PPS及其纳米复合材料的UV老化研究表明:PPS薄膜经过200小时光照后,薄膜表面的分子链明显降解,但交联反应不明显,薄膜的相对结晶度下降;纳米CeO_2对PPS的UV降解具有长效的抑制作用,在8%含量范围内抑制作用与纳米CeO_2含量成正比;纳米CeO_2也明显阻止了PPS因UV老化引起的结晶结构的变化。纳米TiO_2在200h的光照时间内可以很好地阻止PPS分子链的紫外光降解,但随着UV老化时间的增加,其作用明显下降。通过PPS材料UV老化过程中IR吸收峰与老化时间的变化关系曲线,确定了老化过程中新的吸收峰1418cm~(-1)是PPS光老化降解生成的低聚物的特征吸收峰。随着UV光照时间的延长,PPS及其纳米复合材料薄膜的储能模量均出现先增后减的趋势,纳米CeO_2、TiO_2对PPS材料UV老化后的力学性能影响不大。研究结果为PPS抗紫外添加剂的开发开辟了新的研究方向。
PPS/纳米(CeO_2、TiO_2)复合材料的等温和非等温结晶动力学研究结果表明:PPS纳米复合材料在不同结晶温度的结晶过程均为异相成核,纳米CeO_2、TiO_2起到了明显的异相成核作用;PPS纳米复合材料的结晶活化能均小于纯PPS,随着纳米CeO_2、TiO_2含量的增加,结晶活化能降低。莫志深方程较好地描述了PPS纳米复合材料的非等温结晶过程,纳米CeO_2、TiO_2的加入粒子改变了PPS的结晶方式,加速了PPS的结晶速度,使PPS达到相同的相对结晶度所需的冷却速率较小。研究结果对制备PPS工程塑料和高性能纤维加工过程中的结构和性能控制具有重要的作用。
The yield of PVC occupies more than 30% market of general plastics. The flame retardance and smoke suppression of PVC are important assessed values in the state compulsory standard. However, it is difficult to reach the standard. Poly (phenylene sulfide) (PPS) is one of the most important engineering polymers. It is the only high performance fiber which can be made by melt spinning as well. The appearance and usage property of PPS fiber, film, etc. will be deteriorated in natural weather, during the UV irradiation period. There is any suitable UV-resistant additive as yet. For the weak bond in the molecular chain, some thermoplastic polymers such as PVC, PPS, etc. will be degraded in high temperature or UV radiation, which will lead to decline in proceeding and performance.
The flame retardance and smoke suppression of PVC and UV stability of PPS were modified by thermoplastic polymer (PVC, PPS) nanocomposites prepared in this thesis.
Layer nano-Hydrotalcite (HT) and nano-zinc dioxide (ZnO) (HT-ZnO) were used to improve flame retardant and smoke suppressant properties for PVC material for the first time. Flame retardant, smoke suppressant and mechanical properties of PVC were investigated by TEM, TGA and Py-GC-MS. PPS/nano-CeO_2 and PPS/nano-TiO_2 composites were prepared. The changes of molecular structure, crystallization and mechanical properties by UV radiation for PPS nanocomposites were investigated by SEM, FTIR, DSC, DMA. Isothermal crystallization kinetics and non-isothermal crystallization kinetics of PPS nanocomposites were described as well.
The results indicated that nano-HT and nano-ZnO had an effective synergistic effect on the flame retardance and smoke suppression of PVC as their ratio is 3:2. As the ratio of HT/ZnO is 3:2, the nanocomposite loading 5% HT-ZnO, nano-particles are dispersed considerably, which makes slightly influence for mechanical property of PVC. Flexible PVC nanocomposite and structural rigid PVC nanocomposite exhibit good combination properties of flame retardance and smoke suppression, the limited oxygen index (LOI) increases 28-49%, and smoke density rank (SDR) decreases 27-29%, comparing with PVC. The LOI and SDR of flexible PVC nanocomposite are 32.5% and 70.1, respectively. The LOI and SDR of structural rigid PVC nanocomposite are 64.0% and 63.2, respectably. Smoke generating time of structural rigid is postponed 15s; the most smoke density decreases 16% as well. Flexible PVC and structural rigid PVC nanocomposites reach the flame retardence and smoke suppression standard.
The mechanism of smoke suppression for nano HT-ZnO is the synergistic effect on the energy removal and combustible reduce. The energy removal contains two parts: one is that the nano-HT can release water as well as CO_2 during its thermal decomposition, which undergoes high heat absorption; the other is that the metal oxide (MO) from degraded nano-HT reacts with the compounds from decomposed PVC, which absorbs the heat. ZnO can effectively accelerate the decomposition of PVC to release HCl and control the spatial structures of the decomposed products to trans-conjugated polyene sequences, which form cross-linked structures by Diels-Alder reaction and Friedel-Crafts reaction. Combustible aromatic compounds cannot easily be released. This mechanism has significant reference value for flame retardant polymer materials.
PPS has been degraded obviously in the film surface after 200h UV radiation, relative crystallinity decreases as well, but cross-link reaction can't be observed clearly. Nano-CeO_2 evidently retards the degradation of PPS by UV irradiation in whole time. The higher nano-CeO_2 content, the lower oligomers produced. Nano-CeO_2 prevents the crystal change of PPS caused by UV irradiation effectively. Nano-TiO_2 can effectively retards the degradation of PPS by UV irradiation within 200h UV radiation, but the retarded function decreases rapidly with the UV radiation time increasing. The peak of 1418cm~(-1) is made sure to be the absorbance of oligomer of PPS by the relationship of IR relative intensity and UV radiation time. The storages of PPS and nanocomposites film increases at first and decreases later as the UV radiation time increasing. The mechanical property is influenced slightly by nano-CeO_2 and nano-TiO_2. The results create a new field of PPS UV-resistant additives.
Results showed that the crystallization of all nanocomposites is heterogeneous nucleation. Nano-CeO_2 and nano-TiO_2 are the effective nucleating agents. Crystallization activation energy of nanocomposites is lower than that of PPS. The crystallization activation energy decreases as the nano-particle content increasing. Non-isothermal crystallization processes of nanocomposites are properly described by Mo equation. The crystallization style of PPS is changed by nano-particle. The crystallization rate needed to get the relative crystallinity is lower for nanocomposite. compared to PPS. The results have important function in controlling crystallization and property of PPS engineering plastic and high performance fiber in the processing.
Author Zhang Zhonghou(Materials Science and Engineering) Supervised by Prof. Zhu Meifang
本文通过热塑性聚合物(PVC、PPS)纳米复合材料的制备改进PVC材料的阻燃、抑烟性能和PPS材料的UV稳定性。
首次采用层状纳米水滑石(HT)和纳米氧化锌(ZnO)作为复合添加剂(HT-ZnO),制备了PVC纳米复合阻燃抑烟材料。通过TEM、TGA和裂解-气-质色谱(Py-GC-MS)等方法系统研究了纳米HT-ZnO复合添加剂的组成、含量对PVC材料阻燃、抑烟和力学性能的影响。同时以纳米氧化铈(CeO_2)、氧化钛(TiO_2)为紫外光稳定剂制备了PPS纳米复合材料,通过SEM、FTIR、DSC、DMA等方法研究了纯PPS及其纳米复合材料UV老化过程中分子结构、结晶结构和力学性能的变化规律,探讨了纳米CeO_2、TiO_2对PPS UV老化和结晶动力学的影响。
PVC纳米复合材料的阻燃、抑烟研究结果表明:当HT/ZnO为3:2时,复合添加剂在阻燃和抑烟性能上具有明显的协同效应。当HT/ZnO为3:2、HT-ZnO加入量为5%时,其在PVC中具有较好的分散性,软质PVC和建筑硬质PVC纳米复合材料均具有优异的阻燃、抑烟综合性能,极限氧指数比对照样提高了28-49%,烟密度等级比对照样下降了27-29%。软质PVC纳米复合材料的极限氧指数达到32.5%,烟密度等级达到70.1,这两项指标均达到GB8624-1997热塑性塑料难燃级材料(B_1)的要求;建筑硬质PVC纳米复合材料的开始发烟时间比对照样推近了15秒,最大烟密度下降了16%,极限氧指数达到64.0%,烟密度等级达到63.2,两项指标均明显优于国标。
纳米HT-ZnO复合添加剂的抑烟机理为能量移除和可燃物减少两方面的协同效果。在能量移除方面包括两部分:一是纳米HT结构自身脱去层间水吸收的能量和羟基、碳酸根分解生成大量的水和二氧化碳吸收的能量;二是纳米HT受热分解后生成的金属氧化物参与PVC分解过程中的反应,吸收体系中的能量。在可燃物减少方面主要是ZnO加速了PVC脱去HCl的反应,并控制形成反式多烯结构,进而发生交联反应形成焦炭层,从而阻止苯等芳香族化合物的生成,降低可燃物的释放。能量移除和可燃物减少两方面的协同作用,使纳米HT-ZnO复合组分具有显著的阻燃抑烟效果。本阻燃抑烟机理对阻燃聚合物材料的研究具有重要的参考价值。
PPS及其纳米复合材料的UV老化研究表明:PPS薄膜经过200小时光照后,薄膜表面的分子链明显降解,但交联反应不明显,薄膜的相对结晶度下降;纳米CeO_2对PPS的UV降解具有长效的抑制作用,在8%含量范围内抑制作用与纳米CeO_2含量成正比;纳米CeO_2也明显阻止了PPS因UV老化引起的结晶结构的变化。纳米TiO_2在200h的光照时间内可以很好地阻止PPS分子链的紫外光降解,但随着UV老化时间的增加,其作用明显下降。通过PPS材料UV老化过程中IR吸收峰与老化时间的变化关系曲线,确定了老化过程中新的吸收峰1418cm~(-1)是PPS光老化降解生成的低聚物的特征吸收峰。随着UV光照时间的延长,PPS及其纳米复合材料薄膜的储能模量均出现先增后减的趋势,纳米CeO_2、TiO_2对PPS材料UV老化后的力学性能影响不大。研究结果为PPS抗紫外添加剂的开发开辟了新的研究方向。
PPS/纳米(CeO_2、TiO_2)复合材料的等温和非等温结晶动力学研究结果表明:PPS纳米复合材料在不同结晶温度的结晶过程均为异相成核,纳米CeO_2、TiO_2起到了明显的异相成核作用;PPS纳米复合材料的结晶活化能均小于纯PPS,随着纳米CeO_2、TiO_2含量的增加,结晶活化能降低。莫志深方程较好地描述了PPS纳米复合材料的非等温结晶过程,纳米CeO_2、TiO_2的加入粒子改变了PPS的结晶方式,加速了PPS的结晶速度,使PPS达到相同的相对结晶度所需的冷却速率较小。研究结果对制备PPS工程塑料和高性能纤维加工过程中的结构和性能控制具有重要的作用。
The yield of PVC occupies more than 30% market of general plastics. The flame retardance and smoke suppression of PVC are important assessed values in the state compulsory standard. However, it is difficult to reach the standard. Poly (phenylene sulfide) (PPS) is one of the most important engineering polymers. It is the only high performance fiber which can be made by melt spinning as well. The appearance and usage property of PPS fiber, film, etc. will be deteriorated in natural weather, during the UV irradiation period. There is any suitable UV-resistant additive as yet. For the weak bond in the molecular chain, some thermoplastic polymers such as PVC, PPS, etc. will be degraded in high temperature or UV radiation, which will lead to decline in proceeding and performance.
The flame retardance and smoke suppression of PVC and UV stability of PPS were modified by thermoplastic polymer (PVC, PPS) nanocomposites prepared in this thesis.
Layer nano-Hydrotalcite (HT) and nano-zinc dioxide (ZnO) (HT-ZnO) were used to improve flame retardant and smoke suppressant properties for PVC material for the first time. Flame retardant, smoke suppressant and mechanical properties of PVC were investigated by TEM, TGA and Py-GC-MS. PPS/nano-CeO_2 and PPS/nano-TiO_2 composites were prepared. The changes of molecular structure, crystallization and mechanical properties by UV radiation for PPS nanocomposites were investigated by SEM, FTIR, DSC, DMA. Isothermal crystallization kinetics and non-isothermal crystallization kinetics of PPS nanocomposites were described as well.
The results indicated that nano-HT and nano-ZnO had an effective synergistic effect on the flame retardance and smoke suppression of PVC as their ratio is 3:2. As the ratio of HT/ZnO is 3:2, the nanocomposite loading 5% HT-ZnO, nano-particles are dispersed considerably, which makes slightly influence for mechanical property of PVC. Flexible PVC nanocomposite and structural rigid PVC nanocomposite exhibit good combination properties of flame retardance and smoke suppression, the limited oxygen index (LOI) increases 28-49%, and smoke density rank (SDR) decreases 27-29%, comparing with PVC. The LOI and SDR of flexible PVC nanocomposite are 32.5% and 70.1, respectively. The LOI and SDR of structural rigid PVC nanocomposite are 64.0% and 63.2, respectably. Smoke generating time of structural rigid is postponed 15s; the most smoke density decreases 16% as well. Flexible PVC and structural rigid PVC nanocomposites reach the flame retardence and smoke suppression standard.
The mechanism of smoke suppression for nano HT-ZnO is the synergistic effect on the energy removal and combustible reduce. The energy removal contains two parts: one is that the nano-HT can release water as well as CO_2 during its thermal decomposition, which undergoes high heat absorption; the other is that the metal oxide (MO) from degraded nano-HT reacts with the compounds from decomposed PVC, which absorbs the heat. ZnO can effectively accelerate the decomposition of PVC to release HCl and control the spatial structures of the decomposed products to trans-conjugated polyene sequences, which form cross-linked structures by Diels-Alder reaction and Friedel-Crafts reaction. Combustible aromatic compounds cannot easily be released. This mechanism has significant reference value for flame retardant polymer materials.
PPS has been degraded obviously in the film surface after 200h UV radiation, relative crystallinity decreases as well, but cross-link reaction can't be observed clearly. Nano-CeO_2 evidently retards the degradation of PPS by UV irradiation in whole time. The higher nano-CeO_2 content, the lower oligomers produced. Nano-CeO_2 prevents the crystal change of PPS caused by UV irradiation effectively. Nano-TiO_2 can effectively retards the degradation of PPS by UV irradiation within 200h UV radiation, but the retarded function decreases rapidly with the UV radiation time increasing. The peak of 1418cm~(-1) is made sure to be the absorbance of oligomer of PPS by the relationship of IR relative intensity and UV radiation time. The storages of PPS and nanocomposites film increases at first and decreases later as the UV radiation time increasing. The mechanical property is influenced slightly by nano-CeO_2 and nano-TiO_2. The results create a new field of PPS UV-resistant additives.
Results showed that the crystallization of all nanocomposites is heterogeneous nucleation. Nano-CeO_2 and nano-TiO_2 are the effective nucleating agents. Crystallization activation energy of nanocomposites is lower than that of PPS. The crystallization activation energy decreases as the nano-particle content increasing. Non-isothermal crystallization processes of nanocomposites are properly described by Mo equation. The crystallization style of PPS is changed by nano-particle. The crystallization rate needed to get the relative crystallinity is lower for nanocomposite. compared to PPS. The results have important function in controlling crystallization and property of PPS engineering plastic and high performance fiber in the processing.
Author Zhang Zhonghou(Materials Science and Engineering) Supervised by Prof. Zhu Meifang
引文
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