聚氯乙烯（PVC）/纳米SiO_2复合材料的制备及性能研究
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摘要
通用塑料的高性能化和多功能化是开发新型材料的一个重要趋势,而将纳米粒子作为填料来填充改性聚合物,是获得高强高韧复合材料有效方法之一。目前,有关PVC纳米复合材料结构与性能之间的关系方面缺乏系统深入的研究。本论文分别采用原位聚合和熔融共混方法,选用不同表面修饰的可分散型和可反应型纳米SiO2,制备得到了PVC/纳米SiO2复合材料,研究了不同类型的纳米SiO2对于PVC聚合过程、颗粒特性和复合材料结构与性能的影响。具体研究内容和主要研究结果如下所示:
1.不同纳米SiO2对与PVC聚合过程和颗粒特性的影响
利用原位聚合的方法,首先考察了可分散型DNS系列和可反应型RNS系列纳米SiO2对于氯乙烯(VC)单体聚合过程的影响,结果发现:RNS-A、RNS-SR、DNS-2对VC聚合过程产生不利的影响,使得聚合时釜内出现结块,最后出料为不合格的颗粒料,只有RNS-D和DNS-3在3份以下对聚合没有太大影响。然后,我们着重研究了RNS-D对与VC聚合过程的影响,主要包括对于聚合时间和颗粒的常规特性的影响。结果发现,RNS-D的加入使得聚合反应的时间延长;通过对PVC内部和外部形貌的观察,可知RNS-D使PVC的颗粒的外部的形态更加均匀,内部结构的更加疏松,孔隙明显的增多;常规性能的测试结果表明:RNS-D加入时树脂的粘数、吸油值明显增加,而表观密度略有下降;颗粒大小随着RNS-D加入量的增加略有变粗,但是在3%以下基本没有什么影响。
2. PVC/纳米SiO2复合材料的界面结构分析
为了考察不同纳米SiO2对于PVC性能造成影响的原因,我们采用多次超声洗涤从PVC纳米复合树脂中抽提出纳米SiO2:RNS-D和DNS-3,分别对他们进行了TGA,FTIR,XPS表面结构分析,结果是洗脱出RNS-D表面仍然有PVC存在,而DNS-3表面却没有,证明了可反应的RNS-D确实参与了VC的聚合,与PVC基体之间形成了化学的结合,无法通过洗涤除掉。
3. PVC/纳米SiO2复合材料力学性能研究
我们考察了原位聚合和熔融共混法制备的不同PVC纳米复合材料的力学性能,主要测试了不同纳米SiO2对于PVC拉伸性能和冲击性能的影响。实验结果表明:原位聚合法制备的PVC/RNS-D纳米复合材料的拉伸强度有10%的提高,断裂伸长率提高106%,弹性模量也有明显提高,而冲击强度却有明显下降;熔融共混法制备的PVC/RNS-D和PVC/DNS-2纳米复合材料的力学性能有大幅度的提高,RNS-D含量为4%使得PVC的冲击强度提高了约70%,拉伸性能稍有提高,DNS-2含量为6%时使得PVC的冲击强度提高了141%,拉伸强度没有明显下降。4. PVC/纳米SiO2复合材料的热性能及加工流变性能研究
通过对PVC/纳米SiO2热性能的研究,结果显示:原位聚合法PVC/RNS-D纳米复合材料的维卡软化点较纯PVC有明显上升;TG结果显示原位聚合PVC/RNS-D纳米树脂的HCl降解速率明显下降;且纳米树脂经加工过以后的热稳定性也有提高;熔融共混法PVC/纳米SiO2复合材料的热稳定性均有提高。加工流变性能的测试结果显示:原位聚合PVC/RNS-D纳米复合材料的加工流变性能变差,熔融时间(塑化时间)延长,加工扭矩没有太大变化;熔融共混法PVC/纳米SiO2复合材料的加工流变性能大幅度提高,熔融时间大大缩短,扭矩略有增加,最终的熔融因数明显提高,RNS-D改善流变性能的效果更加明显。
Research and development of general plastics with super properties and high additional values have been an important trend. But little attention has been paid on the relationships between the structure and mechanical properties of Polyvinyl chloride (PVC) nanocomposite. In this paper, with the different surface modified nano-SiO2, PVC /nano-SiO2 composites were prepared by in situ polymerization and melt-blending methods. The effects of different surface modified nano-SiO2 on the polymerization process, grains properties of PVC resins and the structure and properties of composites were investigated. The main results are summarized as follows:
1. The effects of different surface modified nano-SiO2 on the polymerization process, grains properties of PVC resins
The effects of the dispersible and the reactable nano-SiO2 on the polymerization process, grains properties of PVC resins were researched in the process of polymerization.The results showed that RNS-A, RNS-SR, DNS-2 were disadvantageous to the polymerization process, the agglomeration of PVC grains were found in polymerization process. But RNS-D and DNS-3 didn’t affect the polymerization when the content of nano-SiO2 was under 3%.
Afterwards, the effects of RNS-D on the polymerization time and PVC grains properties were established mainly. It was found that external morphology of PVC nano-resin grains was more symmetrical, inner structure was looser than the pure PVC. Viscidity number of PVC and absorption amount of DOP is increased obviously, apparent density was decreased in a way because of the introduction of RNS-D. The effect of RNS-D on the PVC grain size was unconspicuous.
2. The analysis of interface structure of PVC/nano-SiO2 composites
In order to investigate the reason of effect of nano-SiO2 on the properties of PVC, RNS-D and DNS-3 extracted from PVC nano-resins were analyzed by TGA, FT-IR and XPS technology. The results indicated that there were some PVC chains on the surface of the extracted RNS-D, but there was nothing on the surface of the extracted DNS-3, it was proved that nanosilica reacted with VC and was linked with PVC by covalent bond.
3. The mechanical performance of PVC/nano-SiO2 composites
The mechanical performance of different PVC/nano-SiO2 composites, which prepared by in situ polymerization and melt-blending methods, were established, especially the tensile and impact properties. It was found that tensile strength, elongation at break, Young’s modulus of PVC/RNS-D nanocomposites prepared by in situ polymerization method were improved obviously, but the notched impact strength was decreased heavy. The impact strength of PVC/DNS-2 nanocomposites prepared by melt-blending method increased by 141% when the content of DNS-2 was 6%, and the tensile strength dropped a little only. The impact strength of PVC/RNS-D nanocomposites prepared by melt-blending method increased by 70% when the content of RNS-D was 6%, and the tensile strength increased a little.
4. The thermal stabilization and rheology properties of PVC/nano-SiO2 composites
The heat-properties of PVC/nano-SiO2 composites were also investigated. It was indicated that the Vicat soften point of PVC/RNS-D nanocomposites prepared by in situ polymerization method was increased obviously, and the degradation speed of PVC nano-resin was slower than the pure PVC. The heat-stabilization of PVC nanocomposites prepared by the melt-blending method also was improved compared with the pure PVC.
The effect on PVC fusion properties of different surface-modified nano-SiO2 was investigated by HAKKE RHEOLOGY INSTRUMENT. It was found that the rheology properties of PVC/RNS-D nanocomposites prepared by the in situ polymerization method dropped a little and the fusion time was prolonged. But the rheology properties of PVC/nano-SiO2 composites prepared by the melt-blending method improved evidently. The fusion time of PVC/nano-SiO2 composites is decreased as the amount of nano-SiO2 increased, on the contrary, the torque (Tmax, Tmin, Teq) was dropped.
1.不同纳米SiO2对与PVC聚合过程和颗粒特性的影响
利用原位聚合的方法,首先考察了可分散型DNS系列和可反应型RNS系列纳米SiO2对于氯乙烯(VC)单体聚合过程的影响,结果发现:RNS-A、RNS-SR、DNS-2对VC聚合过程产生不利的影响,使得聚合时釜内出现结块,最后出料为不合格的颗粒料,只有RNS-D和DNS-3在3份以下对聚合没有太大影响。然后,我们着重研究了RNS-D对与VC聚合过程的影响,主要包括对于聚合时间和颗粒的常规特性的影响。结果发现,RNS-D的加入使得聚合反应的时间延长;通过对PVC内部和外部形貌的观察,可知RNS-D使PVC的颗粒的外部的形态更加均匀,内部结构的更加疏松,孔隙明显的增多;常规性能的测试结果表明:RNS-D加入时树脂的粘数、吸油值明显增加,而表观密度略有下降;颗粒大小随着RNS-D加入量的增加略有变粗,但是在3%以下基本没有什么影响。
2. PVC/纳米SiO2复合材料的界面结构分析
为了考察不同纳米SiO2对于PVC性能造成影响的原因,我们采用多次超声洗涤从PVC纳米复合树脂中抽提出纳米SiO2:RNS-D和DNS-3,分别对他们进行了TGA,FTIR,XPS表面结构分析,结果是洗脱出RNS-D表面仍然有PVC存在,而DNS-3表面却没有,证明了可反应的RNS-D确实参与了VC的聚合,与PVC基体之间形成了化学的结合,无法通过洗涤除掉。
3. PVC/纳米SiO2复合材料力学性能研究
我们考察了原位聚合和熔融共混法制备的不同PVC纳米复合材料的力学性能,主要测试了不同纳米SiO2对于PVC拉伸性能和冲击性能的影响。实验结果表明:原位聚合法制备的PVC/RNS-D纳米复合材料的拉伸强度有10%的提高,断裂伸长率提高106%,弹性模量也有明显提高,而冲击强度却有明显下降;熔融共混法制备的PVC/RNS-D和PVC/DNS-2纳米复合材料的力学性能有大幅度的提高,RNS-D含量为4%使得PVC的冲击强度提高了约70%,拉伸性能稍有提高,DNS-2含量为6%时使得PVC的冲击强度提高了141%,拉伸强度没有明显下降。4. PVC/纳米SiO2复合材料的热性能及加工流变性能研究
通过对PVC/纳米SiO2热性能的研究,结果显示:原位聚合法PVC/RNS-D纳米复合材料的维卡软化点较纯PVC有明显上升;TG结果显示原位聚合PVC/RNS-D纳米树脂的HCl降解速率明显下降;且纳米树脂经加工过以后的热稳定性也有提高;熔融共混法PVC/纳米SiO2复合材料的热稳定性均有提高。加工流变性能的测试结果显示:原位聚合PVC/RNS-D纳米复合材料的加工流变性能变差,熔融时间(塑化时间)延长,加工扭矩没有太大变化;熔融共混法PVC/纳米SiO2复合材料的加工流变性能大幅度提高,熔融时间大大缩短,扭矩略有增加,最终的熔融因数明显提高,RNS-D改善流变性能的效果更加明显。
Research and development of general plastics with super properties and high additional values have been an important trend. But little attention has been paid on the relationships between the structure and mechanical properties of Polyvinyl chloride (PVC) nanocomposite. In this paper, with the different surface modified nano-SiO2, PVC /nano-SiO2 composites were prepared by in situ polymerization and melt-blending methods. The effects of different surface modified nano-SiO2 on the polymerization process, grains properties of PVC resins and the structure and properties of composites were investigated. The main results are summarized as follows:
1. The effects of different surface modified nano-SiO2 on the polymerization process, grains properties of PVC resins
The effects of the dispersible and the reactable nano-SiO2 on the polymerization process, grains properties of PVC resins were researched in the process of polymerization.The results showed that RNS-A, RNS-SR, DNS-2 were disadvantageous to the polymerization process, the agglomeration of PVC grains were found in polymerization process. But RNS-D and DNS-3 didn’t affect the polymerization when the content of nano-SiO2 was under 3%.
Afterwards, the effects of RNS-D on the polymerization time and PVC grains properties were established mainly. It was found that external morphology of PVC nano-resin grains was more symmetrical, inner structure was looser than the pure PVC. Viscidity number of PVC and absorption amount of DOP is increased obviously, apparent density was decreased in a way because of the introduction of RNS-D. The effect of RNS-D on the PVC grain size was unconspicuous.
2. The analysis of interface structure of PVC/nano-SiO2 composites
In order to investigate the reason of effect of nano-SiO2 on the properties of PVC, RNS-D and DNS-3 extracted from PVC nano-resins were analyzed by TGA, FT-IR and XPS technology. The results indicated that there were some PVC chains on the surface of the extracted RNS-D, but there was nothing on the surface of the extracted DNS-3, it was proved that nanosilica reacted with VC and was linked with PVC by covalent bond.
3. The mechanical performance of PVC/nano-SiO2 composites
The mechanical performance of different PVC/nano-SiO2 composites, which prepared by in situ polymerization and melt-blending methods, were established, especially the tensile and impact properties. It was found that tensile strength, elongation at break, Young’s modulus of PVC/RNS-D nanocomposites prepared by in situ polymerization method were improved obviously, but the notched impact strength was decreased heavy. The impact strength of PVC/DNS-2 nanocomposites prepared by melt-blending method increased by 141% when the content of DNS-2 was 6%, and the tensile strength dropped a little only. The impact strength of PVC/RNS-D nanocomposites prepared by melt-blending method increased by 70% when the content of RNS-D was 6%, and the tensile strength increased a little.
4. The thermal stabilization and rheology properties of PVC/nano-SiO2 composites
The heat-properties of PVC/nano-SiO2 composites were also investigated. It was indicated that the Vicat soften point of PVC/RNS-D nanocomposites prepared by in situ polymerization method was increased obviously, and the degradation speed of PVC nano-resin was slower than the pure PVC. The heat-stabilization of PVC nanocomposites prepared by the melt-blending method also was improved compared with the pure PVC.
The effect on PVC fusion properties of different surface-modified nano-SiO2 was investigated by HAKKE RHEOLOGY INSTRUMENT. It was found that the rheology properties of PVC/RNS-D nanocomposites prepared by the in situ polymerization method dropped a little and the fusion time was prolonged. But the rheology properties of PVC/nano-SiO2 composites prepared by the melt-blending method improved evidently. The fusion time of PVC/nano-SiO2 composites is decreased as the amount of nano-SiO2 increased, on the contrary, the torque (Tmax, Tmin, Teq) was dropped.
引文
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