两类层状硅酸盐/聚合物纳米复合材料
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摘要
本文分别以蒙脱土和滑石粉两类层状硅酸盐为填料,制备了具有纳米结构的层状硅酸盐/聚合物复合材料。首先采用环氧树脂(EP)改性尼龙6(N6)与有机蒙脱土(MMT)熔融共混、N6/EP/MMT一步法熔融共混、EP预处理MMT与N6熔融共混工艺制得了N6/MMT复合材料,研究了EP的添加量和混料顺序对N6基体的结晶、熔融行为、复合材料力学性能等的影响。其次,采用原位乙酰化和熔体插层缩聚,制备了剥离型热致液晶共聚酯/蒙脱土(LCP/MMT)纳米复合材料。最后分别采用原位聚合改性滑石粉(talc)、以甲基丙烯酸缩水甘油酯和苯乙烯固相接枝聚丙烯(GSP)为增容剂,通过熔融共混和注塑成型的方法制备了滑石粉/聚丙烯(talc/PP)复合材料。研究了原位聚合改性和增容剂对talc/PP复合材料的微观结构、结晶、熔融行为、聚丙烯基体的晶型结构以及复合材料力学性能等的影响,并探讨了talc对PP的增韧机理。得出如下结论:
(1)N6/MMT复合材料具有插层型纳米结构,三种混料顺序对N6/MMT复合材料的力学性能和热行为影响不大。环氧树脂的引入降低了N6/MMT复合材料中N6相的熔点、结晶温度和结晶度。同时环氧树脂对N6/MMT复合材料起到增塑作用,有效地提高了N6/MMT复合材料的断裂伸长率和缺口冲击强度。
(2)LCP/MMT纳米复合材料表现出向列相液晶行为,剥离的蒙脱土片层分散在整个基体中,破坏了LCP分子链的有序性,使其液晶微区细化、纹影结构的向错点变得模糊。由于LCP基体中富PBT相区和富PHB相区在分子链柔顺性和结构上的差异,剥离的蒙脱土片层对LCP/MMT复合材料中富PBT相区和富PHB相区的玻璃化行为的影响不同。随着MMT含量的增加,LCP/MMT复合材料中富PBT相区链段的Tg1呈上升趋势,而富PHB相区链段的Tg2呈下降趋势。在液晶高分子链取向的诱导作用下,均匀分散的、剥离的蒙脱土片层沿剪切力场取向排列。
(3)甲基丙烯酸甲酯(MMA)或丙烯酸丁酯(BA)原位聚合改性的滑石粉(talc)与聚丙烯(PP)复合制得了具有插层结构的talc/PP复合材料。用MMA原位聚合改性后,滑石粉以80 nm～240 nm的片层厚度分布在PP基体中。由于PBA与PP有更好的相容性,PBA改性的talc在PP基体中剥离为更薄的片层。滑石粉的原位聚合改性,增强了PP与talc之间的界面相互作用力,降低了talc对PP相的结晶成核作用及PP的结晶度。流动取向的talc片层诱导了PP晶体的取向,但PMMA或PBA的改性减弱了talc对PP晶体的取向程度。
(4)在PP/GSP/talc复合材料中,滑石粉片层在高剪切力作用下剥离成厚度在微纳米尺度的多尺度结构。增容剂GSP促进了PP与talc之间的相互作用,使talc更易于剥离,片层厚度进一步减小。PP/GSP/talc复合材料的弯曲模量、冲击强度和拉伸强度均存在一个最佳的talc含量。随着GSP含量增加,PP/GSP/talc复合材料的拉伸强度明显提高,而弯曲模量影响较小。PP/GSP/talc复合材料的冲击强度比PP高,且存在一个最佳的GSP添加量。
(5)在原位聚合改性talc/PP复合材料中,剥离的talc片状结构对复合材料银纹的形成有抑制作用,其二维几何结构不利于片层周围基体的屈服与界面脱粘、空化,因而导致talc/PP复合材料抗冲击强度降低。而在PP/GSP/talc复合材料中,滑石粉片层呈现的微、纳米多尺度结构、增容剂对talc/PP界面粘接的改善,使复合材料受到破坏时能够吸收更多的冲击能,提高了复合材料的韧性。
In this dissertation, polymer/layered silicate composites were prepared with two types of layered silicates, such as montmorillonite and talc, respectively. Firstly, nylon 6/montmorillonite (N6/MMT) composites were prepared via melt compounding with the following three different blending sequences: (1) Nylon 6 (N6) was modified by epoxy (EP), then mixed with MMT. (2) Nylon 6, EP and MMT were blended simultaneously. (3) Nylon 6 was compounded with MMT pretreated by EP. The effects of EP contents and blending sequence on melting, crystallization, and mechanical properties of composites were investigated. Secondly, the fully exfoliated thermotropic liquid crystalline copolyester/ montmorillonite (LCP/MMT) nanocomposites were synthesized by in-situ acetylation and melting intercaction condensation polymerization. Finally, the talc/isotactic polypropylene (PP) composites were prepared by melt extrusion with PP and talc modified by in-situ monomer/talc polymerization or adding glycidyl methacrylate/styrene solid-phase-grafted polypropylene (GSP) as compatibilizer. The effects of in-situ monomer/talc polymerization or compatibilizer on crystal structure, melting and crystallization properties of PP matrix, the micro-structure and mechanical properties of talc/PP composites were inverstigatied. And the toughening mechanism of talc on PP was also discussed. Based on experiment results, the conclusions were drawn as following:
(1) The intercalated structure nylon 6/montmorillonite (N6/MMT) nanocomposites were prepared; the blending sequences have few effects on the mechanical properties and thermal behavior of N6/MMT nanocomposites. The addition of epoxy decreases the melting temperature (Tm), crystallization temperature (Tc) and relative crystallinity (Xc) of N6 phase in N6/MMT nanocomposites. Due to its plasticizing effect, the epoxy enhances the elongation at break and Izod impact strength of N6/MMT nanocomposites.
(2) LCP/MMT nanocomposites exhibit nematic liquid crystalline behavior, and the incorporation of the exfoliated MMT layers throughout the LCP matrix results in very fine but imperfect schlieren texture, and the disinclination becomes blurred. The exfoliated MMT layers have different effects on the glass transitions of the PBT-rich and PHB-rich domains in LCP macromolecules due to their different chain flexibility and structure. With increasing MMT contents, the glass transition temperature (Tg1) of PBT-rich phase in LCP tends to increase, while the Tg2 of PHB-rich phase tends to decrease. Under the induction of LCP, the exfoliated MMT layers are oriented along the force field.
(3) After talc was modified with methyl methacrylate (MMA) or butyl acrylate (BA) via in-situ polymerization, the talc/PP composites is intercalated in nano-sized level. The thickness of the PMMA-modified talc layers in the PP matrix is in the range 80 nm to 240 nm, while the PBA-modified talc is even thinner. The modified talc enhances the interfacial action between PP and talc, weakens the nucleation effect of talc on crystallization of PP, and decreases the crystallinity of PP. The oriented talc layers induce orientation of PP crystals during molding process, while the degree of PP crystal orientation decreases after talc is modified with PMMA or PBA.
(4) During the processing of PP/talc composites, the talc particle is delaminated to platelets with multi-scale structure ranged from micro- and nano-size in thickness by high shearing force. The compati1izer (GSP) enhances the interfacial interaction between talc and PP matrix, which makes the thickness of talc platelets decrease further. There is an optimal talc contents for the flexural modulus, tensile strength and izod impact strength of PP/GSP/talc composites. With increasing GSP contents, the tensile strengths of PP/GS-PP/talc composites increase obviously, while the flexural modula of composites change little. The Izod impact strength of PP/GS-PP/talc composites is higher than that of PP. Moreover, there is an optimal GSP contents for the Izod impact strength of PP/GS-PP/talc composites.
(5) In in-situ polymerization modified talc/PP composites, the delaminated talc layers restrict the formation of crazes in composites. Their two-dimension structure is not beneficial to yielding polymer matrix around talc layers, debonding and cavitating of PP/talc interface, so that the impact strength of talc/PP composites decreases. For PP/GSP/talc composites, two factors, i. e. the multi-scale structure ranged from micro- and nano-size in thickness of talc layers, and enhanced interfacial adhesion between PP and talc due to compati1izer, lead to absorbing more impact energy during fracture, and increasing the toughness of PP/talc composites.
(1)N6/MMT复合材料具有插层型纳米结构,三种混料顺序对N6/MMT复合材料的力学性能和热行为影响不大。环氧树脂的引入降低了N6/MMT复合材料中N6相的熔点、结晶温度和结晶度。同时环氧树脂对N6/MMT复合材料起到增塑作用,有效地提高了N6/MMT复合材料的断裂伸长率和缺口冲击强度。
(2)LCP/MMT纳米复合材料表现出向列相液晶行为,剥离的蒙脱土片层分散在整个基体中,破坏了LCP分子链的有序性,使其液晶微区细化、纹影结构的向错点变得模糊。由于LCP基体中富PBT相区和富PHB相区在分子链柔顺性和结构上的差异,剥离的蒙脱土片层对LCP/MMT复合材料中富PBT相区和富PHB相区的玻璃化行为的影响不同。随着MMT含量的增加,LCP/MMT复合材料中富PBT相区链段的Tg1呈上升趋势,而富PHB相区链段的Tg2呈下降趋势。在液晶高分子链取向的诱导作用下,均匀分散的、剥离的蒙脱土片层沿剪切力场取向排列。
(3)甲基丙烯酸甲酯(MMA)或丙烯酸丁酯(BA)原位聚合改性的滑石粉(talc)与聚丙烯(PP)复合制得了具有插层结构的talc/PP复合材料。用MMA原位聚合改性后,滑石粉以80 nm～240 nm的片层厚度分布在PP基体中。由于PBA与PP有更好的相容性,PBA改性的talc在PP基体中剥离为更薄的片层。滑石粉的原位聚合改性,增强了PP与talc之间的界面相互作用力,降低了talc对PP相的结晶成核作用及PP的结晶度。流动取向的talc片层诱导了PP晶体的取向,但PMMA或PBA的改性减弱了talc对PP晶体的取向程度。
(4)在PP/GSP/talc复合材料中,滑石粉片层在高剪切力作用下剥离成厚度在微纳米尺度的多尺度结构。增容剂GSP促进了PP与talc之间的相互作用,使talc更易于剥离,片层厚度进一步减小。PP/GSP/talc复合材料的弯曲模量、冲击强度和拉伸强度均存在一个最佳的talc含量。随着GSP含量增加,PP/GSP/talc复合材料的拉伸强度明显提高,而弯曲模量影响较小。PP/GSP/talc复合材料的冲击强度比PP高,且存在一个最佳的GSP添加量。
(5)在原位聚合改性talc/PP复合材料中,剥离的talc片状结构对复合材料银纹的形成有抑制作用,其二维几何结构不利于片层周围基体的屈服与界面脱粘、空化,因而导致talc/PP复合材料抗冲击强度降低。而在PP/GSP/talc复合材料中,滑石粉片层呈现的微、纳米多尺度结构、增容剂对talc/PP界面粘接的改善,使复合材料受到破坏时能够吸收更多的冲击能,提高了复合材料的韧性。
In this dissertation, polymer/layered silicate composites were prepared with two types of layered silicates, such as montmorillonite and talc, respectively. Firstly, nylon 6/montmorillonite (N6/MMT) composites were prepared via melt compounding with the following three different blending sequences: (1) Nylon 6 (N6) was modified by epoxy (EP), then mixed with MMT. (2) Nylon 6, EP and MMT were blended simultaneously. (3) Nylon 6 was compounded with MMT pretreated by EP. The effects of EP contents and blending sequence on melting, crystallization, and mechanical properties of composites were investigated. Secondly, the fully exfoliated thermotropic liquid crystalline copolyester/ montmorillonite (LCP/MMT) nanocomposites were synthesized by in-situ acetylation and melting intercaction condensation polymerization. Finally, the talc/isotactic polypropylene (PP) composites were prepared by melt extrusion with PP and talc modified by in-situ monomer/talc polymerization or adding glycidyl methacrylate/styrene solid-phase-grafted polypropylene (GSP) as compatibilizer. The effects of in-situ monomer/talc polymerization or compatibilizer on crystal structure, melting and crystallization properties of PP matrix, the micro-structure and mechanical properties of talc/PP composites were inverstigatied. And the toughening mechanism of talc on PP was also discussed. Based on experiment results, the conclusions were drawn as following:
(1) The intercalated structure nylon 6/montmorillonite (N6/MMT) nanocomposites were prepared; the blending sequences have few effects on the mechanical properties and thermal behavior of N6/MMT nanocomposites. The addition of epoxy decreases the melting temperature (Tm), crystallization temperature (Tc) and relative crystallinity (Xc) of N6 phase in N6/MMT nanocomposites. Due to its plasticizing effect, the epoxy enhances the elongation at break and Izod impact strength of N6/MMT nanocomposites.
(2) LCP/MMT nanocomposites exhibit nematic liquid crystalline behavior, and the incorporation of the exfoliated MMT layers throughout the LCP matrix results in very fine but imperfect schlieren texture, and the disinclination becomes blurred. The exfoliated MMT layers have different effects on the glass transitions of the PBT-rich and PHB-rich domains in LCP macromolecules due to their different chain flexibility and structure. With increasing MMT contents, the glass transition temperature (Tg1) of PBT-rich phase in LCP tends to increase, while the Tg2 of PHB-rich phase tends to decrease. Under the induction of LCP, the exfoliated MMT layers are oriented along the force field.
(3) After talc was modified with methyl methacrylate (MMA) or butyl acrylate (BA) via in-situ polymerization, the talc/PP composites is intercalated in nano-sized level. The thickness of the PMMA-modified talc layers in the PP matrix is in the range 80 nm to 240 nm, while the PBA-modified talc is even thinner. The modified talc enhances the interfacial action between PP and talc, weakens the nucleation effect of talc on crystallization of PP, and decreases the crystallinity of PP. The oriented talc layers induce orientation of PP crystals during molding process, while the degree of PP crystal orientation decreases after talc is modified with PMMA or PBA.
(4) During the processing of PP/talc composites, the talc particle is delaminated to platelets with multi-scale structure ranged from micro- and nano-size in thickness by high shearing force. The compati1izer (GSP) enhances the interfacial interaction between talc and PP matrix, which makes the thickness of talc platelets decrease further. There is an optimal talc contents for the flexural modulus, tensile strength and izod impact strength of PP/GSP/talc composites. With increasing GSP contents, the tensile strengths of PP/GS-PP/talc composites increase obviously, while the flexural modula of composites change little. The Izod impact strength of PP/GS-PP/talc composites is higher than that of PP. Moreover, there is an optimal GSP contents for the Izod impact strength of PP/GS-PP/talc composites.
(5) In in-situ polymerization modified talc/PP composites, the delaminated talc layers restrict the formation of crazes in composites. Their two-dimension structure is not beneficial to yielding polymer matrix around talc layers, debonding and cavitating of PP/talc interface, so that the impact strength of talc/PP composites decreases. For PP/GSP/talc composites, two factors, i. e. the multi-scale structure ranged from micro- and nano-size in thickness of talc layers, and enhanced interfacial adhesion between PP and talc due to compati1izer, lead to absorbing more impact energy during fracture, and increasing the toughness of PP/talc composites.
引文
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