季铵盐型聚丙烯接枝物的制备及其在PP/PVC共混体系中的应用
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摘要
聚丙烯(PP)具有力学性能优良,耐化学腐蚀等优点,但分子链规整性高,极性低,导致染色性、粘接性、抗静电性、亲水性以及与其它极性高聚物和无机填料的相容性差。聚氯乙烯(PVC)具有强度高、阻燃和价格低廉等优点,为极性聚合物。若PP与PVC共混合金化,可使性能互补,而两者极性的显著差异导致其相容性很差。因此,制备性能优良的PP/PVC共混物,提高两者的相容性一直是该领域的研究热点。
本文探索了季铵盐型PP接枝物PP-g-(St-co-DMC)的制备、结晶动力学以及对PP/PVC共混体系的增容作用,并探讨了PP-g-(St-co-DMC)与超支化聚合物(HBP)共同对PP/PVC共混体系的增容效应,取得了重要成果,对于相关材料的制备和应用具有重要理论指导意义。
以季铵盐型烯类单体DMC为原料,采用悬浮固相接枝方法,制备了一种季铵盐型PP接枝物PP-g-(St-co-DMC)。FT-IR、DSC和TGA测试表明DMC单体成功接枝到PP链上;考察了引发剂用量、单体浓度、第二单体用量、反应温度、溶胀时间和反应时间等因素对接枝率的影响。此外,对该反应的接枝机理进行了初步探讨。
用Avrami方程(改进的Avrami方程和莫志深法)对PP-g-(St-co-DMC)接枝物的等温结晶动力学(非等温结晶动力学)进行了探讨。研究表明,等温和非等温条件下,DMC链的引入,均改变其结晶模式,加速PP的结晶。低接枝率的样品中,DMC链起到异相成核作用,加速结晶;接枝率的提高,降低结晶速率,以上结果可能源于季铵盐阳离子基团两方面的作用:一方面离子的静电吸引作用加速了成核,促进结晶;另一方面,离子间相互作用的增强阻碍了结晶链的迁移,使结晶时PP链扩散到晶核表面的活化能增加,降低结晶速度。此外,探讨了PP-g-(St-co-DMC)/PP(10/90)共混体系的结晶动力学。
研究了季铵盐型PP接枝物PP-g-(St-co-DMC)对PP/PVC共混体系的增容作用。扫描电子显微镜(SEM)和拉伸及抗冲强度测试表明,PP-g-(St-co-DMC)使PP/PVC(80/20)共混体系相容性提高。当PP-g-(St-co-DMC)加入量为4%时,拉伸强度和抗冲强度分别提高19.15%和74.48%;但继续增大添加量,力学性能反而急剧下降。PP-g-(St-co-DMC)使PP/PVC(80/20)共混体系的熔体表观粘度增大,加入量为4%(wt)时,达到最大值。另外,接枝率对体系增容情况的研究表明,PP-g-(St-co-DMC)接枝率为16.78%时对PP/PVC共混体系的增容效果最好。
为探索HBP对PP/PVC/PP-g-(St-co-DMC)共混体系的增容效应,研究了HBP对PP结晶行为的影响。等温及非等温条件下的结晶动力学表明,超支化聚合物的引入,改变了其结晶模式,极大提高了PP的结晶速度,使Avrami指数明显增大,可能的原因为,具有分形结构的超支化聚合物影响了晶体的生长及结晶链段的扩散模式。在所研究的含量范围(1-5%)内,低含量时,HBP明显加速PP结晶;HBP含量的提高,结晶速率有所降低。此外,HBP的分子量对PP结晶动力学的影响研究表明,在共混样品中,分子量的增加使结晶速度降低。
在研究了HBP对PP结晶行为影响的基础上,进一步探讨了AB3HBP对PP/PVC/ PP-g-(St-co-DMC)(80/20/4)共混体系的增容效应。扫描电子显微镜(SEM)和拉伸及抗冲强度测试表明,季铵盐型PP接枝物PP-g-(St-co-DMC)与AB3HBP对PP/PVC(80/20)共混体系具有共同增容效应。AB3HBP和PP-g-(St-co-DMC)同时加入PP/PVC(80/20)共混体系中,使PP/PVC共混物熔体表观粘度发生了改变,拉伸及抗冲强度增大。在PP/PVC/PP-g-(St-co-DMC)(80/20/4)共混体系中加入1%AB3型HBP时,共混物的拉伸和抗冲强度达到最大值,较未加AB3HBP增容剂时分别提高8.16%、53.41%。同时,熔体表观粘度达到较小值。此外,探讨了不同分子量超支化聚合物对PP/PVC/PP-g-(St-co-DMC)共混体系的增容效果。
Polypropylene (PP) had advantages such as excellent mechanical properties and chemical erosion resistance. However, its high molecular integrity and low polarity led to poor properties of dyeing, adherence, antistatic and hydrophilicity, and low compatibility with other polar polymers or inorganic additives. Polyvinylchloride (PVC), an inexpensive polar polymer, was of high strength and fireproof. The striking difference between polarity of PP and PVC resulted in the low compatibility, and the inferiorities originated from it could be counteracted by blending. Recently, the preparation of PP/PVC blends with excellent properties and the enhancement of their compatibilization by additives had been the focus of research interests all around the world.
In this paper, preparation, crystallization kinetics and compatibility PP/PVC blends of a quaternary ammonium bearing graft copolymer, PP-g-(St-co-DMC), had been investigated. In addition, compatibilization of PP-g-(St-co-DMC)/HBP on PP/PVC had been studied in detail. This work was of fundamental and technological importance in the theoretical investigation and the application of those polymers.
A quaternary ammonium bearing graft copolymer, PP-g-(St-co-DMC) had been prepared by a suspension solid-state grafting process using a cationic monomer with quaternary ammonium groups, methacryloxyethyltrimethyl ammonium chloride (DMC), as a material. The grafted PP was systematically characterized using FT-IR, TGA and DSC. It was then suggested that DMC was successfully grafted onto the PP backbone. The effects of monomer concentration, swelling time, initiator concentration, the second monomer dosage, reaction time, and reaction temperature on the grafting yield were examined. In addition, the grafting mechanism of this reaction was proposed.
The isothermal (non-isothermal) crystallization kinetics of PP-g- (St-co-DMC) sample was investigated using Avrami equation (modified Avrami equation and Mo’s method). It was indicated that the induction of DMC chain could result in the modification of the crystallization mode and hence the acceleration of the crystallization under both the isothermal and the non-isothermal conditions. In the samples with low grafting yield, DMC chain led to the heterogeneous nucleation and acceleration of crystallization, and whereas, the rate of crystallization decreased. The aforementioned results might originate from the effects of quaternary ammonium groups bearing DMC. On the one hand, electrostatic attraction promoted nucleation and enhanced the crystallization. On the other hand, the increased intermolecular interaction between ions could hinder the migration of the crystallization chain, and therefore increase the diffusion activation energy of PP chain, which decreased the rate of crystallization. Furthermore, the crystallization kinetics of PP-g-(St-co-DMC) /PP(10/90) blends was discussed.
The effect of compatibility of quaternary ammonium bearing PP-g- (St-co-DMC) on PP/PVC (80/20) blends was investigated systematically. The measurements of SEM, tensile strength and impact strength indicated that the PP-g- (St-co-DMC) could enhance compatibility of PP/PVC blend remarkably. The tensile strength and the impact strength of PP/PVC blends with a concentration of PP-g-(St-co-DMC) at 4%(wt) increased up to19.15% and 74.48%, respectively. The subsequent increase in the concentration of PP-g-(St-co-DMC) decreased the mechanical properties remarkably. The apparent melt viscosity of PP/PVC blends increased by the addition of PP-g-(St-co-DMC) and reached its maximum at a concentration of 4%. Study on the effect of the degree of grafting (DG) of PP-g- (St-co-DMC) on the compatibility of PP/PVC blends suggested that it should reach a peak at DG of 16.78%.
For clarifying the compatibility capacity of hyperbranched polymer (HBP) on PP/PVC/PP-g-(St-co-DMC)/ blend, the effect of AB2 typed HBP on the crystallization kinetics of polypropylene (PP) was investigated. The crystallization kinetics under isothermal and non-isothermal conditions indicated that the introduction of HBP could modify its crystallization mode, and therefore accelerate the crystallization process of PP, and increase the Avrami exponent. This might be because the HBP with fractal structure had an effect on the crystal growth and diffusion mode of the crystal chain. It was indicated that, in the examined range of concentration (1-5%) of HBP, this additive with low concentration could accelerate the crystallization remarkably, and whereas, the rate of crystallization decreased. In addition, the study of molecular weight of HBP on PP crystallization kinetics indicated that, in blend samples, the increase in molecular weight reduced the rate of crystallization.
The compatibility of the HBP on PP/PVC/PP-g- (St-co-DMC) (80/20/4) was further studied on the basis of effect of HBP on the crystallization behavior of PP. The measurement of SEM, tensile strength and impact strength indicated that PP-g-(St-co-DMC)/HBP could enhance the compatibility of PP/PVC blends. The addition of the mixture of PP-g-(St-co-DMC) and HBP into PP/PVC blends facilitated the modification of melt apparent viscosity of the latter. With comparison to those of the blend free of HBP, the tensile strength and the impact strength of the PP/PVC/PP-g- (St-co-DMC) (80/20/4) blends could reach up to 8.16% and 53.41% at the most, respectively, and meanwhile the apparent melt viscosity of blends reached the less value when the content of HBP was 1%. Furthermore, the influence of the molecular weight of HBP on the compatibility of PP/PVC/PP-g-(St-co-DMC) blend was discussed.
本文探索了季铵盐型PP接枝物PP-g-(St-co-DMC)的制备、结晶动力学以及对PP/PVC共混体系的增容作用,并探讨了PP-g-(St-co-DMC)与超支化聚合物(HBP)共同对PP/PVC共混体系的增容效应,取得了重要成果,对于相关材料的制备和应用具有重要理论指导意义。
以季铵盐型烯类单体DMC为原料,采用悬浮固相接枝方法,制备了一种季铵盐型PP接枝物PP-g-(St-co-DMC)。FT-IR、DSC和TGA测试表明DMC单体成功接枝到PP链上;考察了引发剂用量、单体浓度、第二单体用量、反应温度、溶胀时间和反应时间等因素对接枝率的影响。此外,对该反应的接枝机理进行了初步探讨。
用Avrami方程(改进的Avrami方程和莫志深法)对PP-g-(St-co-DMC)接枝物的等温结晶动力学(非等温结晶动力学)进行了探讨。研究表明,等温和非等温条件下,DMC链的引入,均改变其结晶模式,加速PP的结晶。低接枝率的样品中,DMC链起到异相成核作用,加速结晶;接枝率的提高,降低结晶速率,以上结果可能源于季铵盐阳离子基团两方面的作用:一方面离子的静电吸引作用加速了成核,促进结晶;另一方面,离子间相互作用的增强阻碍了结晶链的迁移,使结晶时PP链扩散到晶核表面的活化能增加,降低结晶速度。此外,探讨了PP-g-(St-co-DMC)/PP(10/90)共混体系的结晶动力学。
研究了季铵盐型PP接枝物PP-g-(St-co-DMC)对PP/PVC共混体系的增容作用。扫描电子显微镜(SEM)和拉伸及抗冲强度测试表明,PP-g-(St-co-DMC)使PP/PVC(80/20)共混体系相容性提高。当PP-g-(St-co-DMC)加入量为4%时,拉伸强度和抗冲强度分别提高19.15%和74.48%;但继续增大添加量,力学性能反而急剧下降。PP-g-(St-co-DMC)使PP/PVC(80/20)共混体系的熔体表观粘度增大,加入量为4%(wt)时,达到最大值。另外,接枝率对体系增容情况的研究表明,PP-g-(St-co-DMC)接枝率为16.78%时对PP/PVC共混体系的增容效果最好。
为探索HBP对PP/PVC/PP-g-(St-co-DMC)共混体系的增容效应,研究了HBP对PP结晶行为的影响。等温及非等温条件下的结晶动力学表明,超支化聚合物的引入,改变了其结晶模式,极大提高了PP的结晶速度,使Avrami指数明显增大,可能的原因为,具有分形结构的超支化聚合物影响了晶体的生长及结晶链段的扩散模式。在所研究的含量范围(1-5%)内,低含量时,HBP明显加速PP结晶;HBP含量的提高,结晶速率有所降低。此外,HBP的分子量对PP结晶动力学的影响研究表明,在共混样品中,分子量的增加使结晶速度降低。
在研究了HBP对PP结晶行为影响的基础上,进一步探讨了AB3HBP对PP/PVC/ PP-g-(St-co-DMC)(80/20/4)共混体系的增容效应。扫描电子显微镜(SEM)和拉伸及抗冲强度测试表明,季铵盐型PP接枝物PP-g-(St-co-DMC)与AB3HBP对PP/PVC(80/20)共混体系具有共同增容效应。AB3HBP和PP-g-(St-co-DMC)同时加入PP/PVC(80/20)共混体系中,使PP/PVC共混物熔体表观粘度发生了改变,拉伸及抗冲强度增大。在PP/PVC/PP-g-(St-co-DMC)(80/20/4)共混体系中加入1%AB3型HBP时,共混物的拉伸和抗冲强度达到最大值,较未加AB3HBP增容剂时分别提高8.16%、53.41%。同时,熔体表观粘度达到较小值。此外,探讨了不同分子量超支化聚合物对PP/PVC/PP-g-(St-co-DMC)共混体系的增容效果。
Polypropylene (PP) had advantages such as excellent mechanical properties and chemical erosion resistance. However, its high molecular integrity and low polarity led to poor properties of dyeing, adherence, antistatic and hydrophilicity, and low compatibility with other polar polymers or inorganic additives. Polyvinylchloride (PVC), an inexpensive polar polymer, was of high strength and fireproof. The striking difference between polarity of PP and PVC resulted in the low compatibility, and the inferiorities originated from it could be counteracted by blending. Recently, the preparation of PP/PVC blends with excellent properties and the enhancement of their compatibilization by additives had been the focus of research interests all around the world.
In this paper, preparation, crystallization kinetics and compatibility PP/PVC blends of a quaternary ammonium bearing graft copolymer, PP-g-(St-co-DMC), had been investigated. In addition, compatibilization of PP-g-(St-co-DMC)/HBP on PP/PVC had been studied in detail. This work was of fundamental and technological importance in the theoretical investigation and the application of those polymers.
A quaternary ammonium bearing graft copolymer, PP-g-(St-co-DMC) had been prepared by a suspension solid-state grafting process using a cationic monomer with quaternary ammonium groups, methacryloxyethyltrimethyl ammonium chloride (DMC), as a material. The grafted PP was systematically characterized using FT-IR, TGA and DSC. It was then suggested that DMC was successfully grafted onto the PP backbone. The effects of monomer concentration, swelling time, initiator concentration, the second monomer dosage, reaction time, and reaction temperature on the grafting yield were examined. In addition, the grafting mechanism of this reaction was proposed.
The isothermal (non-isothermal) crystallization kinetics of PP-g- (St-co-DMC) sample was investigated using Avrami equation (modified Avrami equation and Mo’s method). It was indicated that the induction of DMC chain could result in the modification of the crystallization mode and hence the acceleration of the crystallization under both the isothermal and the non-isothermal conditions. In the samples with low grafting yield, DMC chain led to the heterogeneous nucleation and acceleration of crystallization, and whereas, the rate of crystallization decreased. The aforementioned results might originate from the effects of quaternary ammonium groups bearing DMC. On the one hand, electrostatic attraction promoted nucleation and enhanced the crystallization. On the other hand, the increased intermolecular interaction between ions could hinder the migration of the crystallization chain, and therefore increase the diffusion activation energy of PP chain, which decreased the rate of crystallization. Furthermore, the crystallization kinetics of PP-g-(St-co-DMC) /PP(10/90) blends was discussed.
The effect of compatibility of quaternary ammonium bearing PP-g- (St-co-DMC) on PP/PVC (80/20) blends was investigated systematically. The measurements of SEM, tensile strength and impact strength indicated that the PP-g- (St-co-DMC) could enhance compatibility of PP/PVC blend remarkably. The tensile strength and the impact strength of PP/PVC blends with a concentration of PP-g-(St-co-DMC) at 4%(wt) increased up to19.15% and 74.48%, respectively. The subsequent increase in the concentration of PP-g-(St-co-DMC) decreased the mechanical properties remarkably. The apparent melt viscosity of PP/PVC blends increased by the addition of PP-g-(St-co-DMC) and reached its maximum at a concentration of 4%. Study on the effect of the degree of grafting (DG) of PP-g- (St-co-DMC) on the compatibility of PP/PVC blends suggested that it should reach a peak at DG of 16.78%.
For clarifying the compatibility capacity of hyperbranched polymer (HBP) on PP/PVC/PP-g-(St-co-DMC)/ blend, the effect of AB2 typed HBP on the crystallization kinetics of polypropylene (PP) was investigated. The crystallization kinetics under isothermal and non-isothermal conditions indicated that the introduction of HBP could modify its crystallization mode, and therefore accelerate the crystallization process of PP, and increase the Avrami exponent. This might be because the HBP with fractal structure had an effect on the crystal growth and diffusion mode of the crystal chain. It was indicated that, in the examined range of concentration (1-5%) of HBP, this additive with low concentration could accelerate the crystallization remarkably, and whereas, the rate of crystallization decreased. In addition, the study of molecular weight of HBP on PP crystallization kinetics indicated that, in blend samples, the increase in molecular weight reduced the rate of crystallization.
The compatibility of the HBP on PP/PVC/PP-g- (St-co-DMC) (80/20/4) was further studied on the basis of effect of HBP on the crystallization behavior of PP. The measurement of SEM, tensile strength and impact strength indicated that PP-g-(St-co-DMC)/HBP could enhance the compatibility of PP/PVC blends. The addition of the mixture of PP-g-(St-co-DMC) and HBP into PP/PVC blends facilitated the modification of melt apparent viscosity of the latter. With comparison to those of the blend free of HBP, the tensile strength and the impact strength of the PP/PVC/PP-g- (St-co-DMC) (80/20/4) blends could reach up to 8.16% and 53.41% at the most, respectively, and meanwhile the apparent melt viscosity of blends reached the less value when the content of HBP was 1%. Furthermore, the influence of the molecular weight of HBP on the compatibility of PP/PVC/PP-g-(St-co-DMC) blend was discussed.
引文
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