室温离子液体改性橡胶/填料复合材料
摘要
室温离子液体(Room temperature ionic liquid, RTIL)是一种由有机阳离子与有机或无机阴离子组成的、熔点低于100℃的熔盐,具有近零蒸气压、强极性、高耐热、宽的电化学窗口、良好的溶解性、高导电和导离子性等优点,已经开始广泛应用于绿色溶剂、高效反应介质、电解质、催化剂等领域。RTIL可以与无机填料发生各种相互作用,因而,可以对高分子/填料复合材料的界面进行改性,并有效地提高复合材料的性能。
本文研究了以RTIL为界面改性剂制备具有新型界面和优良性能的橡胶/填料复合材料,研究了不同RTIL与多种橡胶填料之间的相互作用,研究了RTIL与橡胶之间的反应性,深入系统地研究了RTIL对橡胶/填料复合材料的微观结构与性能的影响。
研究了1-丁基-3-甲基咪唑六氟磷酸盐(BmimPF6)与炭黑(CB)之间的相互作用及辅助微波改性对CB结构与性质的影响。BmimPF6可以通过阳离子-π相互作用强烈地吸附于CB的表面,微波辐照下,发生分解,分解过程中CB的微观形貌发生很大改变。RTIL辅助微波改性后,CB比表面积变大,石墨化程度增高,石墨微晶尺寸明显降低,介孔含量增加。采用RTIL辅助微波改性的CB用于补强橡胶,优化了改性工艺。研究了改性炭黑(m-CB)对丁苯橡胶(SBR)、顺丁橡胶(BR)、丁腈橡胶(NBR)补强效果。在低用量填料时,m-CB可以大大改善CB对橡胶的补强效果；在高用量填料时,m-CB与CB对橡胶补强的效果无明显差别。这是m-CB与橡胶相互作用增强和界面区粘滞层(Sticky Layer)分子高度取向共同作用的结果。
设计和制备了两种具有可聚合基团的RTIL,1-甲基咪唑山梨酸盐(MimS)和1-甲基咪唑甲基丙烯酸盐(MimMa),并研究了其对SBR/白炭黑(silica)复合材料的改性效果及机理。MimS和MimMa可以与silica发生强烈的氢键相互作用。在自由基引发条件下,两者均可以与SBR分子发生接枝反应。MimS和MimMa的加入可以大大抑制silica在橡胶基体中的填料网络化,促进硫化,有效改善silica的分散,增强SBR-silica界面相互作用,有效提高SBR/silica硫化胶的力学性能。
制备了含有巯基官能团的RTIL—1-甲基咪唑巯基丙酸盐(MimMP),并研究了其对SBR/silica复合材料的改性效果。通过巯烯反应(thiol-ene reaction), MimMP上的巯基与SBR分子发生反应,且反应的位置主要是SBR中的端双键。MimMP因与silica之间的氢键相互作用,可以削弱填料之间的相互作用,降低填料网络化效应,改善填料分散。MimMP的巯基及咪唑阳离子可以有效促进混炼胶的硫化。MimMP/silica之间的氢键相互作用和MimMP/SBR之间的巯烯反应可以大大提高SBR-silica之间的界面相互作用,显著提高硫化胶的拉伸强度、撕裂强度及耐磨性等。
制备了具有含有巯基且具有双离子结构的RTIL—双(1-甲基咪唑)巯基琥珀酸盐(BMimMS),并研究了MimMP和BMimMS对SBR/埃洛石纳米管(HNTs)复合材料的改性。MimMP和BMimMS均可与HNTs发生氢键相互作用,但机理稍有不同。MimMP主要与HNTs上的A1OH、SiOH和A1OA1发生氢键相互作用,而BMimMS主要与HNTs上的A1OH、SiOH和SiOSi发生氢键相互作用。MimMP和BMimMS与SBR分子之间均可发生巯烯反应。不同之处在于,前者主要以高活性的端双键为主,而后者,在两个咪唑阳离子的催化下,BMimMS可以与SBR分子端双键和内双键均发生有效反应。MimMP和BMimMS的加入可有效促进硫化,改善HNTs在橡胶基体中的分散,可有效增强SBR-HNTs的界面相互作用,显著提高复合材料的力学性能。由于BMimMS可以与HNTs外表面的SiOSi发生氢键相互作用,故而其对HNTs分散、SBR-HNTs界面相互作用力以及材料的最终性能的改善均优于MimMP。
Room temperature ionic liquid (RTIL) was utilized as interfacial modifier for rubber/filler composites with novel interfacial structure and good performance. The affinities of RTIL towards various fillers and their reaction with SBR chains were studied. The influence of RTILs on the microstructure and performance was systemically investigated。
RTIL, comprised of an organic cation and an organic or inorganic anion, is molten salt with a molten temperature lower than 100℃. For their specific characteristics such as near vapor pressure, high polarity, good thermalstability, wide potential, excellent solubility, high electric and ionic conductivity, RTILs have been widely explored as green solvent, high efficient media, electrolyte and catalysis. RTIL can be interacted with various fillers via the widely reported interactions. So, they can be potentially utilized as interfacial modifiers for polymer/filler composites and greatly improve the performance of the composites.
One kind of common RTIL, 1-butyl-3-methylimidazolium hexafluorophosphate rate (BmimPF6) could be interacted with carbon black (CB) via cation-πinteraction. Together with microwave irradiation, CB was modified and the structure of CB was found to be substantially changed. BmimPF6 was decomposed on the CB surface. The modified carbon black was found to be with larger surface area, increased graphitization, obviously decreased microcrystalline size and higher content of mesopores. The reinforcement of m-CB towards styrene butadiene rubber (SBR), butadiene rubber (BR) and nitrile butadiene rubber (NBR) was studied. The preparing parameters were optimized. At a low loading of filler, m-CB could more effectively reinforce rubber matrix. While at a high loading of filler, there is no practical difference between m-CB and CB according to the performance of the vulcanizates. The increased interfacial interaction and the higher orientation of the segments in the sticky layer were both responsible.
Two kinds of RTILs with polymerizable groups,1-methylimidazolium sorbate (MimS) and 1-methylimidazolium methacrylate (MimMa) were designed and prepared. The performance of the modified SBR/silica composites was characterized and the related mechanism was studied. The incorporation of MimS and MimMa could effectively restrain the filler networking in the rubber matrix, accelerate the vulcanization, obviously improve the dispersion of silica, strengthen the SBR-silica interfacial interaction and largely improve the mechanical performance of SBR/silica vulcanizates.
RTIL containing thiol group,1-methylimidazolium propionate (MimMP), was prepared and investigated as interfacial modifier for SBR/silica composites. MimMP could be reacted with SBR chains via the thiol-ene reaction between the thiol group in MimMP and the double bond in SBR chains. The reactive sites in SBR were mainly the side double bonds. MimS and MimMa could be interacted with silica by hydrogen bonding, which could weaken the filler-filler interaction, restrain the filler networking of silica and improve the dispersion of silica in rubber matrix. Thiol and imidazolium cation in MimMP could accelerate the vulcanization. Both the thiol-ene reaction and the hydrogen bonding are responsible for the increased SBR-silica interfacial interaction and the improved mechanical performance of SBR/silica vulcanizates.
A kind of RTIL with thiol group and Gemini structure, bis(1-methylimidazolium) mercaptosuccinate (BMimMS), was synthesized. Both MimMP and BMimMS were utilized as interfacial modifiers for SBR/halloysite nanotubes (HNTs) composites. MimMP and BMimMS could be hydrogen bonded with HNTs but with a subtle difference on the mechanism. MimMP could be interacted with the aluminol (A1OH), silanol (SiOH) and aluminum oxide (A1OA1) of HNTs. BMimMS could be interacted with the A1OH, SiOH and silicon oxide (SiOSi). Both MimMP and BMimMS could be grafted onto SBR chains with thiol-ene reaction. MimMP could be mainly reacted with the side double bonds in SBR. While in that of BMimMS, the active sites were almost equally originated from the side double bonds and the inside double bonds possibly due to its Gemini structure. The incorporation of MimMP and BMimMS could effectively accelerate vulcanization, improve the HNTs dispersion, strengthen the SBR-HNTs interfacial bonding and enhance the mechanical performance of the vulcanizates. Because BMimMS could be interacted with the outward surface of HNTs, BMimMS could be more effective in improving the HNTs dispersion, the interfacial bonding and the final performance of the vulcanizates in comparison with that of MimMP.
本文研究了以RTIL为界面改性剂制备具有新型界面和优良性能的橡胶/填料复合材料,研究了不同RTIL与多种橡胶填料之间的相互作用,研究了RTIL与橡胶之间的反应性,深入系统地研究了RTIL对橡胶/填料复合材料的微观结构与性能的影响。
研究了1-丁基-3-甲基咪唑六氟磷酸盐(BmimPF6)与炭黑(CB)之间的相互作用及辅助微波改性对CB结构与性质的影响。BmimPF6可以通过阳离子-π相互作用强烈地吸附于CB的表面,微波辐照下,发生分解,分解过程中CB的微观形貌发生很大改变。RTIL辅助微波改性后,CB比表面积变大,石墨化程度增高,石墨微晶尺寸明显降低,介孔含量增加。采用RTIL辅助微波改性的CB用于补强橡胶,优化了改性工艺。研究了改性炭黑(m-CB)对丁苯橡胶(SBR)、顺丁橡胶(BR)、丁腈橡胶(NBR)补强效果。在低用量填料时,m-CB可以大大改善CB对橡胶的补强效果；在高用量填料时,m-CB与CB对橡胶补强的效果无明显差别。这是m-CB与橡胶相互作用增强和界面区粘滞层(Sticky Layer)分子高度取向共同作用的结果。
设计和制备了两种具有可聚合基团的RTIL,1-甲基咪唑山梨酸盐(MimS)和1-甲基咪唑甲基丙烯酸盐(MimMa),并研究了其对SBR/白炭黑(silica)复合材料的改性效果及机理。MimS和MimMa可以与silica发生强烈的氢键相互作用。在自由基引发条件下,两者均可以与SBR分子发生接枝反应。MimS和MimMa的加入可以大大抑制silica在橡胶基体中的填料网络化,促进硫化,有效改善silica的分散,增强SBR-silica界面相互作用,有效提高SBR/silica硫化胶的力学性能。
制备了含有巯基官能团的RTIL—1-甲基咪唑巯基丙酸盐(MimMP),并研究了其对SBR/silica复合材料的改性效果。通过巯烯反应(thiol-ene reaction), MimMP上的巯基与SBR分子发生反应,且反应的位置主要是SBR中的端双键。MimMP因与silica之间的氢键相互作用,可以削弱填料之间的相互作用,降低填料网络化效应,改善填料分散。MimMP的巯基及咪唑阳离子可以有效促进混炼胶的硫化。MimMP/silica之间的氢键相互作用和MimMP/SBR之间的巯烯反应可以大大提高SBR-silica之间的界面相互作用,显著提高硫化胶的拉伸强度、撕裂强度及耐磨性等。
制备了具有含有巯基且具有双离子结构的RTIL—双(1-甲基咪唑)巯基琥珀酸盐(BMimMS),并研究了MimMP和BMimMS对SBR/埃洛石纳米管(HNTs)复合材料的改性。MimMP和BMimMS均可与HNTs发生氢键相互作用,但机理稍有不同。MimMP主要与HNTs上的A1OH、SiOH和A1OA1发生氢键相互作用,而BMimMS主要与HNTs上的A1OH、SiOH和SiOSi发生氢键相互作用。MimMP和BMimMS与SBR分子之间均可发生巯烯反应。不同之处在于,前者主要以高活性的端双键为主,而后者,在两个咪唑阳离子的催化下,BMimMS可以与SBR分子端双键和内双键均发生有效反应。MimMP和BMimMS的加入可有效促进硫化,改善HNTs在橡胶基体中的分散,可有效增强SBR-HNTs的界面相互作用,显著提高复合材料的力学性能。由于BMimMS可以与HNTs外表面的SiOSi发生氢键相互作用,故而其对HNTs分散、SBR-HNTs界面相互作用力以及材料的最终性能的改善均优于MimMP。
Room temperature ionic liquid (RTIL) was utilized as interfacial modifier for rubber/filler composites with novel interfacial structure and good performance. The affinities of RTIL towards various fillers and their reaction with SBR chains were studied. The influence of RTILs on the microstructure and performance was systemically investigated。
RTIL, comprised of an organic cation and an organic or inorganic anion, is molten salt with a molten temperature lower than 100℃. For their specific characteristics such as near vapor pressure, high polarity, good thermalstability, wide potential, excellent solubility, high electric and ionic conductivity, RTILs have been widely explored as green solvent, high efficient media, electrolyte and catalysis. RTIL can be interacted with various fillers via the widely reported interactions. So, they can be potentially utilized as interfacial modifiers for polymer/filler composites and greatly improve the performance of the composites.
One kind of common RTIL, 1-butyl-3-methylimidazolium hexafluorophosphate rate (BmimPF6) could be interacted with carbon black (CB) via cation-πinteraction. Together with microwave irradiation, CB was modified and the structure of CB was found to be substantially changed. BmimPF6 was decomposed on the CB surface. The modified carbon black was found to be with larger surface area, increased graphitization, obviously decreased microcrystalline size and higher content of mesopores. The reinforcement of m-CB towards styrene butadiene rubber (SBR), butadiene rubber (BR) and nitrile butadiene rubber (NBR) was studied. The preparing parameters were optimized. At a low loading of filler, m-CB could more effectively reinforce rubber matrix. While at a high loading of filler, there is no practical difference between m-CB and CB according to the performance of the vulcanizates. The increased interfacial interaction and the higher orientation of the segments in the sticky layer were both responsible.
Two kinds of RTILs with polymerizable groups,1-methylimidazolium sorbate (MimS) and 1-methylimidazolium methacrylate (MimMa) were designed and prepared. The performance of the modified SBR/silica composites was characterized and the related mechanism was studied. The incorporation of MimS and MimMa could effectively restrain the filler networking in the rubber matrix, accelerate the vulcanization, obviously improve the dispersion of silica, strengthen the SBR-silica interfacial interaction and largely improve the mechanical performance of SBR/silica vulcanizates.
RTIL containing thiol group,1-methylimidazolium propionate (MimMP), was prepared and investigated as interfacial modifier for SBR/silica composites. MimMP could be reacted with SBR chains via the thiol-ene reaction between the thiol group in MimMP and the double bond in SBR chains. The reactive sites in SBR were mainly the side double bonds. MimS and MimMa could be interacted with silica by hydrogen bonding, which could weaken the filler-filler interaction, restrain the filler networking of silica and improve the dispersion of silica in rubber matrix. Thiol and imidazolium cation in MimMP could accelerate the vulcanization. Both the thiol-ene reaction and the hydrogen bonding are responsible for the increased SBR-silica interfacial interaction and the improved mechanical performance of SBR/silica vulcanizates.
A kind of RTIL with thiol group and Gemini structure, bis(1-methylimidazolium) mercaptosuccinate (BMimMS), was synthesized. Both MimMP and BMimMS were utilized as interfacial modifiers for SBR/halloysite nanotubes (HNTs) composites. MimMP and BMimMS could be hydrogen bonded with HNTs but with a subtle difference on the mechanism. MimMP could be interacted with the aluminol (A1OH), silanol (SiOH) and aluminum oxide (A1OA1) of HNTs. BMimMS could be interacted with the A1OH, SiOH and silicon oxide (SiOSi). Both MimMP and BMimMS could be grafted onto SBR chains with thiol-ene reaction. MimMP could be mainly reacted with the side double bonds in SBR. While in that of BMimMS, the active sites were almost equally originated from the side double bonds and the inside double bonds possibly due to its Gemini structure. The incorporation of MimMP and BMimMS could effectively accelerate vulcanization, improve the HNTs dispersion, strengthen the SBR-HNTs interfacial bonding and enhance the mechanical performance of the vulcanizates. Because BMimMS could be interacted with the outward surface of HNTs, BMimMS could be more effective in improving the HNTs dispersion, the interfacial bonding and the final performance of the vulcanizates in comparison with that of MimMP.
引文
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