木粉/聚丙烯复合界面分子运动弛豫过程解析
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摘要
为进一步探明木塑复合界面特性和偶联剂作用机理及最佳用量问题,本文利用直接热压工艺和先造粒后热压工艺制备不同木粉含量和不同偶联剂种类及添加量的毛白杨木粉／聚丙烯复合材料,通过动态热机械分析(DMA)、介电弛豫和应力松弛方法从分子运动弛豫过程的角度对其界而特性进行了研究。
本研究得到如下结论：
(1)DMA研究结果表明,毛白杨木粉／聚丙烯复合材料的储存模量E′随温度的升高而减小,添加偶联剂后,储存模量E′显著升高,表明偶联剂与木粉发生反应并和聚丙烯分子链产生缠绕作用,界面结合强度增强。复合材料在温度0℃附近区域出现一个松弛峰,添加偶联剂后,松弛峰增大,表明偶联剂使复合材料内无定形分子链段运动受到更多的限制,木粉与聚丙烯产生新的结合,木塑界面结合更加紧密。
(2)对毛白杨木粉／聚丙烯复合材料的介电弛豫研究表明,未添加偶联剂以及添加马来酸酐接枝聚丙烯(MAPP)和硅烷偶联剂的复合材料在温度为0℃、频率为5MHz附近均出现一个介电弛豫过程,该过程基于木材细胞壁中无定形区中伯醇羟基(CH2OH)的回转取向运动,弛豫强度(εs-ε∞)与木粉含量以及偶联剂种类和添加量有关。弛豫强度随木粉含量增大而增大,随偶联剂添加量增加先逐渐降低,而后缓慢增大。MAPP和硅烷偶联剂均能与木材无定形区中纤维素分子链上的伯醇羟基发生反应,使产生回转取向运动的伯醇羟基数量减少,因此弛豫强度降低。偶联剂超过理想用量后,弛豫强度缓慢增大,有可能是未参与反应的偶联剂所致。
(3)根据Eyring绝对速度反应论计算得到毛白杨木粉／聚丙烯复合材料在介电弛豫过程中的表观活化能(AE),用以定量表征木塑两相界面的结合作用。对未添加偶联剂的复合材料,当木粉含量为40%时,表观活化能最大,表明木塑两相相容性最好,界面结合作用最强。对添加两种偶联剂制备的复合材料来说,ΔE总体的变化趋势基本一致,随偶联剂添加量的增加先增大后减小。在木研究条件下,添加MAPP和硅烷偶联剂的复合材料均在添加量为2%时出现ΔE最大值,分别为33.52kJ/mol和28.12kJ/mol,与未添加偶联剂的复合材料(13.86kJ/mol)相比增加至2倍以上,表明弛豫过程中伯醇羟基回转取向运动需要克服的能垒增加,复合材料的内部结合力增强,性能更加稳定。但当MAPP和硅烷偶联剂过量后,ΔE分别降至22.0kJ/mol和16.0kJ/mol以下。硅烷偶联剂过量后ΔE下降更为明显,接近未添加偶联剂的水平,表明弛豫过程中伯醇羟基回转取向运动需要克服的能垒降低,过量的偶联剂存在于木粉与聚丙烯之间,造成界面结构不均匀,内部结合力减弱。
(4)采用直接热压和先造粒后热压两种工艺制备添加MAPP的毛白杨木粉／聚丙烯复合材料并对其进行介电弛豫分析,结果表明：在相同的温度频率域都出现弛豫过程,弛豫损耗峰和弛豫强度的变化趋势一致。先造粒后热压制备的复合材料伯醇羟基的数量比直接热压制备的复合材料少,表明经过先造粒过程,复合材料分散性更好,有利于MAPP和伯醇羟基的反应。添加量2%时,直接热压法制备的复合材料ΔE为26.2kJ/mol,低于先造粒后热压法制备复合材料的ΔE值(33.5kJ/mol)。
(5)毛白杨木粉／聚丙烯复合材料的应力松弛结果与介电弛豫研究结果一致。即木粉含量40%时,木塑两相界面相容性最佳,内部结合作用最强。MAPP和硅烷偶联剂添加量2%时,应力松弛最缓慢,木塑两相结合紧密,结构最稳定。由两种工艺制备的复合材料应力松弛及其速率随偶联剂添加量的变化趋势是一致,但先造粒后热压工艺制备的复合材料,应力松弛较缓慢,应力松弛速率较小,性能优于直接热压制备的复合材料。
To further ascertain the interface characteristics, mechanism and the optimal loading of coupling agent of the wood plastic composite, which was one of the different wood flour content, type and content of coupling agents using direct hot-pressing process and hot pressing process after granulating respectively were prepared in this study. In the research with the dynamic thermal mechanical analysis (DMA), the dielectric approach and the stress relaxation methods, the interface characteristics were investigated from relaxation process of molecular movement.
The main conclusions are summarized as follows:
(1) The storage modulus (E') of Simon poplar wood flour/polypropylene composite increased with the rising of temperature and significantly increased after adding coupling agent, because coupling agent could make interface bonding strength increase by reacting with wood flour and producing entanglement with polypropylene molecular chain. The relaxation peak was observed around0℃and was higher after adding coupling agent, because coupling agent had maken more difficulty of molecular chain segments motion in amorphous region by a new combination between wood flour and polypropylene, therefore wood flour/polypropylene composite interface was more closely.
(2) There was relaxation process in Simon poplar wood flour/polypropylene composite without and with coupling agent which is based on reorientation of the methynol groups (CH2OH) in amorphous region of wood cell wall was related to the different wood flour content, type and content of coupling agents. The relaxation strength (εs-ε∞) was gradually increased with the wood flour content increasing and was first decreased then increased with loading levels of coupling agent, suggesting that the number of the motive methynol groups was deduced as a result of coupling agent reacting with methynol groups. But the relaxation strength was slowly increased above the optimal loading of coupling agent (2%), which may be caused by coupling agent that did not participate in the reaction.
(3) The apparent activation energy (△E) was calculated according to the Eyring's absolute rate reaction theory in relaxation process of Simon poplar wood flour/polypropylene composite and quantitatively characterized the combination on wood flour-polypropylene interface. The apparent activation energy of the samples without coupling agent reached a maximum when wood flour content is40%, suggesting the best compatibility and strongest internal bonding between wood flour and polypropylene. The apparent activation energy of the samples with maleic anhydride grafted polypropylene (MAPP) or silane as coupling agent was almost the same change trend and first increased then decreased with coupling agent increasing, and began to increase above that value:33.52k.l/mol and28.12kJ/mol respectively, more than twice as likely to samples without coupling agent, when the optimal loading of coupling agent (2%); that was due to the strong hindrance to the reorientation of methylol groups and, therefore, suggested the best compatibility and strongest internal bonding between wood flour and polypropylene; but the apparent activation energy of samples with two coupling agents fell to22.0kJ/mol and16.0kJ/mol respectively above the optimal loading of coupling agent, especially that of sample with silane dropped to that of sample without coupling agent and, therefore, suggested the energy barrier to the reorientation of the methynol groups was lower, too much coupling agent was present in wood flour and polypropylene, which resulted in uneven interface structure and weaker internal binding force.
(4) The same relaxation process of wood flour/polypropylene composites with MAPP by using hot-pressing process after granulating and using direct hot-pressing process was the same changed. It was compared with two processes that the relaxation strength of sample and the apparent activation energy of sample at MAPP loading of2%both were higher than those of the latter, because wood flour, polypropylene and coupling agent in granulating could be mixed more uniformly leading to improve dispersity and interfacial compatibility between wood flour and polypropylene.
(5) The stress relaxation behavior of wood flour/polypropylene composites appeared similar trends with that of dielectric relaxation. It was the best compatibility and the strongest internal bonding between wood and polypropylene that wood flour content is40%, the mechanical properties could be obviously increased by adding MAPP or silane as coupling agent, but the optimal loading of coupling agent was related to wood content and the type of coupling agent. The trendency of both stress relaxation and stress relaxation rate were consistent with loading of coupling agent, the stress relaxation and stress relaxation rate of wood flour/polypropylene composites by using hot-pressing process after granulating was slower to by using direct hot-pressing process, therefore performance of materials is superior to by using direct hot-pressing process.
本研究得到如下结论：
(1)DMA研究结果表明,毛白杨木粉／聚丙烯复合材料的储存模量E′随温度的升高而减小,添加偶联剂后,储存模量E′显著升高,表明偶联剂与木粉发生反应并和聚丙烯分子链产生缠绕作用,界面结合强度增强。复合材料在温度0℃附近区域出现一个松弛峰,添加偶联剂后,松弛峰增大,表明偶联剂使复合材料内无定形分子链段运动受到更多的限制,木粉与聚丙烯产生新的结合,木塑界面结合更加紧密。
(2)对毛白杨木粉／聚丙烯复合材料的介电弛豫研究表明,未添加偶联剂以及添加马来酸酐接枝聚丙烯(MAPP)和硅烷偶联剂的复合材料在温度为0℃、频率为5MHz附近均出现一个介电弛豫过程,该过程基于木材细胞壁中无定形区中伯醇羟基(CH2OH)的回转取向运动,弛豫强度(εs-ε∞)与木粉含量以及偶联剂种类和添加量有关。弛豫强度随木粉含量增大而增大,随偶联剂添加量增加先逐渐降低,而后缓慢增大。MAPP和硅烷偶联剂均能与木材无定形区中纤维素分子链上的伯醇羟基发生反应,使产生回转取向运动的伯醇羟基数量减少,因此弛豫强度降低。偶联剂超过理想用量后,弛豫强度缓慢增大,有可能是未参与反应的偶联剂所致。
(3)根据Eyring绝对速度反应论计算得到毛白杨木粉／聚丙烯复合材料在介电弛豫过程中的表观活化能(AE),用以定量表征木塑两相界面的结合作用。对未添加偶联剂的复合材料,当木粉含量为40%时,表观活化能最大,表明木塑两相相容性最好,界面结合作用最强。对添加两种偶联剂制备的复合材料来说,ΔE总体的变化趋势基本一致,随偶联剂添加量的增加先增大后减小。在木研究条件下,添加MAPP和硅烷偶联剂的复合材料均在添加量为2%时出现ΔE最大值,分别为33.52kJ/mol和28.12kJ/mol,与未添加偶联剂的复合材料(13.86kJ/mol)相比增加至2倍以上,表明弛豫过程中伯醇羟基回转取向运动需要克服的能垒增加,复合材料的内部结合力增强,性能更加稳定。但当MAPP和硅烷偶联剂过量后,ΔE分别降至22.0kJ/mol和16.0kJ/mol以下。硅烷偶联剂过量后ΔE下降更为明显,接近未添加偶联剂的水平,表明弛豫过程中伯醇羟基回转取向运动需要克服的能垒降低,过量的偶联剂存在于木粉与聚丙烯之间,造成界面结构不均匀,内部结合力减弱。
(4)采用直接热压和先造粒后热压两种工艺制备添加MAPP的毛白杨木粉／聚丙烯复合材料并对其进行介电弛豫分析,结果表明：在相同的温度频率域都出现弛豫过程,弛豫损耗峰和弛豫强度的变化趋势一致。先造粒后热压制备的复合材料伯醇羟基的数量比直接热压制备的复合材料少,表明经过先造粒过程,复合材料分散性更好,有利于MAPP和伯醇羟基的反应。添加量2%时,直接热压法制备的复合材料ΔE为26.2kJ/mol,低于先造粒后热压法制备复合材料的ΔE值(33.5kJ/mol)。
(5)毛白杨木粉／聚丙烯复合材料的应力松弛结果与介电弛豫研究结果一致。即木粉含量40%时,木塑两相界面相容性最佳,内部结合作用最强。MAPP和硅烷偶联剂添加量2%时,应力松弛最缓慢,木塑两相结合紧密,结构最稳定。由两种工艺制备的复合材料应力松弛及其速率随偶联剂添加量的变化趋势是一致,但先造粒后热压工艺制备的复合材料,应力松弛较缓慢,应力松弛速率较小,性能优于直接热压制备的复合材料。
To further ascertain the interface characteristics, mechanism and the optimal loading of coupling agent of the wood plastic composite, which was one of the different wood flour content, type and content of coupling agents using direct hot-pressing process and hot pressing process after granulating respectively were prepared in this study. In the research with the dynamic thermal mechanical analysis (DMA), the dielectric approach and the stress relaxation methods, the interface characteristics were investigated from relaxation process of molecular movement.
The main conclusions are summarized as follows:
(1) The storage modulus (E') of Simon poplar wood flour/polypropylene composite increased with the rising of temperature and significantly increased after adding coupling agent, because coupling agent could make interface bonding strength increase by reacting with wood flour and producing entanglement with polypropylene molecular chain. The relaxation peak was observed around0℃and was higher after adding coupling agent, because coupling agent had maken more difficulty of molecular chain segments motion in amorphous region by a new combination between wood flour and polypropylene, therefore wood flour/polypropylene composite interface was more closely.
(2) There was relaxation process in Simon poplar wood flour/polypropylene composite without and with coupling agent which is based on reorientation of the methynol groups (CH2OH) in amorphous region of wood cell wall was related to the different wood flour content, type and content of coupling agents. The relaxation strength (εs-ε∞) was gradually increased with the wood flour content increasing and was first decreased then increased with loading levels of coupling agent, suggesting that the number of the motive methynol groups was deduced as a result of coupling agent reacting with methynol groups. But the relaxation strength was slowly increased above the optimal loading of coupling agent (2%), which may be caused by coupling agent that did not participate in the reaction.
(3) The apparent activation energy (△E) was calculated according to the Eyring's absolute rate reaction theory in relaxation process of Simon poplar wood flour/polypropylene composite and quantitatively characterized the combination on wood flour-polypropylene interface. The apparent activation energy of the samples without coupling agent reached a maximum when wood flour content is40%, suggesting the best compatibility and strongest internal bonding between wood flour and polypropylene. The apparent activation energy of the samples with maleic anhydride grafted polypropylene (MAPP) or silane as coupling agent was almost the same change trend and first increased then decreased with coupling agent increasing, and began to increase above that value:33.52k.l/mol and28.12kJ/mol respectively, more than twice as likely to samples without coupling agent, when the optimal loading of coupling agent (2%); that was due to the strong hindrance to the reorientation of methylol groups and, therefore, suggested the best compatibility and strongest internal bonding between wood flour and polypropylene; but the apparent activation energy of samples with two coupling agents fell to22.0kJ/mol and16.0kJ/mol respectively above the optimal loading of coupling agent, especially that of sample with silane dropped to that of sample without coupling agent and, therefore, suggested the energy barrier to the reorientation of the methynol groups was lower, too much coupling agent was present in wood flour and polypropylene, which resulted in uneven interface structure and weaker internal binding force.
(4) The same relaxation process of wood flour/polypropylene composites with MAPP by using hot-pressing process after granulating and using direct hot-pressing process was the same changed. It was compared with two processes that the relaxation strength of sample and the apparent activation energy of sample at MAPP loading of2%both were higher than those of the latter, because wood flour, polypropylene and coupling agent in granulating could be mixed more uniformly leading to improve dispersity and interfacial compatibility between wood flour and polypropylene.
(5) The stress relaxation behavior of wood flour/polypropylene composites appeared similar trends with that of dielectric relaxation. It was the best compatibility and the strongest internal bonding between wood and polypropylene that wood flour content is40%, the mechanical properties could be obviously increased by adding MAPP or silane as coupling agent, but the optimal loading of coupling agent was related to wood content and the type of coupling agent. The trendency of both stress relaxation and stress relaxation rate were consistent with loading of coupling agent, the stress relaxation and stress relaxation rate of wood flour/polypropylene composites by using hot-pressing process after granulating was slower to by using direct hot-pressing process, therefore performance of materials is superior to by using direct hot-pressing process.
引文
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