含不同离子的液晶离聚物及其PBT/PP共混物的制备和性能研究
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摘要
近年来,由于液晶聚合物(Liquid crystalline polymer, LCP)具有高模量、高强度、良好的化学稳定性和尺寸稳定性、较低的热膨胀系数等优良性能,因而在复合材料方面得到广泛应用。但大部分LCP与热塑性聚合物属于不相容体系,这种不相容导致了两相之间的界面粘结力较差,共混物的力学性能不如预期的理想,因此,通常可以通过共聚引入极性基团、化学改性引入极性基团、接枝、嵌段共聚-共混、加入增容剂、形成IPN结构、形成氢键等途径来改善共混体系的相容性。
本文采用了加入含有离子基团的液晶离聚物来改善共混体系相容性的方法。液晶离聚物是指含有离子基团的液晶聚合物,它可以通过离子的相互作用使液晶聚合物与其他热塑性聚合物的相互作用增强,相容性得以改善,同时由于液晶中刚性基元的存在,在共混体系中起到了微纤增强作用,大大改善加工性能、降低了加工温度和粘度。它综合离聚物和液晶聚合物两方面的内容,是一种新型的功能高分子,是目前液晶聚合物研究领域的前沿课题之一,不仅具有重要的理论意义,而且在与其他热塑性聚合物共混制备性能优良的复合材料方面具有广阔的应用前景。
本论文设计并合成了互变向列相液晶单体对苯二甲酸二-(4-羧基苯)酯(M1),将其与1,10-癸二醇、1,12-十二烷二醇和亮黄(BY)按不同比例进行溶液缩聚反应,制备了一系列含有磺酸离子的主链液晶离聚物(MLCl-Sn)。结果表明：随着BY含量的增加,MLCI-Sn的Tg逐渐增加：MLCI-Sn的Tm出现了先增加后降低的趋势；MLCI-Sn的液晶区间先增加后变窄；MLCI-Sn的热分解温度在300℃以上,具有良好的热稳定性；MLCI-Sn的织构为向列相。
将合成的液晶单体对苯二甲酸二-(4-羧基苯)酯(M1)与1,10-癸二醇、1,12-十二烷二醇和2,5-二羟基苯甲酸按比例进行溶液缩聚反应,制备了一种含有羧酸离子的主链液晶离聚物(MLCI-C5)。MLCl-C5液晶离聚物的液晶类型为向列相,其液晶区间为172℃,热稳定性良好。
合成了一种互变向列相液晶单体4-乙氧基苯甲酸-4'-烯丙氧基联苯单酯(M2),离子单体4-烯丙氧基苯甲酸(M3),将液晶单体和离子单体接枝共聚到含氢聚硅氧烷主链上,合成了含有羧酸离子的侧链液晶离聚物(SLCI-C5)。液晶离聚物SLCI-C5的液晶类型为向列相,其液晶区间为149℃,具有良好的热稳定性。
合成的液晶单体4-乙氧基苯甲酸-4'-烯丙氧基联苯单酯(M2),离子单体N-烯丙基溴化吡啶(M4),将液晶单体和离子单体接枝共聚到含氢聚硅氧烷主链上,合成了含有铵离子的侧链液晶离聚物(SLCI-N5).液晶离聚物SLCI-N5的液晶类型为向列相,其液晶区间为251℃。
将合成的液晶离聚物MLCI-S5和MLCI-C5分别与PBT.PP进行了熔融共混制备了PBT/PP/MLCI-S5和PBT/PP/MLCI-C5共混物。在升温过程中,MLCI-S5的加入,降低了PBT的Tg,改善了PBT和PP之间的相容性；随着MLCI-S5含量的增加,PP的Tc没有发生变化,PBT的Tc向低温移动。MLCI-C5的加入,使PBT和PP的熔融温度均略有升高；而对PBT和PP(降温)结晶行为的影响则不尽相同,MLCI-C5的存在使PP的结晶温度略有升高,但升高幅度基本不受液晶离聚物含量的影响；与之相反,PBT的结晶温度则因液晶离聚物的存在而降低,DSC曲线中观察到的PP和PBT的结晶峰相互靠近,证实了MLCI-C5的加入起到了增容的作用。SEM和红外图像系统结果证实了当MLCI-S5的加入5wt%时,共混体系的分散得到了改善,PP分散相的相区尺寸变小,MLCI-S5介于PBT和PP两相界面之间,增加了PBT和PP之间的界面粘结力,改善了二者之间的相容性；过量MLCI-S5的加入,由于液晶离聚物的聚集,使分散效果变差。当MLCI-C5加入9wt%时,共混体系的分散效果最好,PP分散相的相区尺寸变小；过量的MLCI-C5加入,分散变差。力学性能结果表明：当加入适量的MLCI-S5(5wt％),共混物的拉伸强度和断裂伸长率达到最大值；当MLCI-C5含量为9wt%时,共混物的拉伸强度达到最大值；当MLCI-C5含量为15wt%时,共混物的断裂伸长率达到最大值。
将合成的液晶离聚物SLCI-C5和SLCI-N5分别与PBT.PP进行了熔融共混制备了PBT/PP/SLCI-C5和PBT/PP/SLCI-N5共混物。SLCI-C5和SLCI-N5对共混体系热力学性能的影响与MLCI-C5对共混体系的影响结果相似,证实了SLCI-C5和SLCI-N5的加入起到了增容的作用。SEM和红外图像系统结果表明：当SLCI-C5加入7wt%时,共混体系的分散得到了改善,增加了二者之间的相容性；过量SLCI-C5的加入,分散效果变差。当SLCI-N5的含量也加入到7wt%时,由于液晶离聚物与PBT的离子-偶极作用使共混体系的分散得到了改善；加入过量的SLCI-N5,由于液晶离聚物中离子的聚集作用,使分散效果变差。力学性能结果表明：随之SLCI-C5含量的增加,共混物的拉伸强度和断裂伸长率也随之增加,当含量为7wt%时,共混物的力学性能达到最大值；当SLCI-N5含量为7wt%时,共混物的力学性能达到最大值。而加入过量的液晶离聚物,共混物的拉伸强度和断裂伸长率有不同程度的降低。
Recently, Liquid crystalline polymers (LCPs) with high strength and stiffness, high chemical resistance, good dimensional stability and low linear thermal expansion coefficient are attractive high performance engineering materials. Most LCPs and thermoplastic are immiscible at the molecular level. The incompatibility between the matrix polymers and dispersed LCP phase leads to poor interfacial adhesion. Accordingly, the mechanical strength of the LCP/thermoplastic blends is considerably lower than that expected from theoretical calculation. Therefore, compatibilization with appropriate agents is required to improve the adhesion between the LCP fibril and thermoplastic blends interface, for example copolymer induced polar groups, chemistrical modify induced polar group, graft, block copolymer-blend, adding compotibilizer, forming IPN network, and hydrogen bond.
In this paper, the compatibilizing method is adding liquid crystalline ionomer containing ion group in blend. Liquid crystalline ionomers (LCIs) are liquid crystalline polymers containing ionic groups and the properties of LCIs are superior to the LCPs because of the compatibilization in composites by the function of ionic groups between the molecule chains. Moreover, the mesogenic phase has high degree of long-range order that enabling them to orient along the flow direction during processing. This leads to the formation of fine fibrils at an appropriate range of LCP concentration under certain processing conditions. The fine fibrils reinforce the matrix of thermoplastics effectively, giving rise to the development of polymer composites that commonly known as in situ composites. Therefore, LCIs are one new kind of function polymer materials and have been one of important research project in the field of LCPs. It is necessary and interesting to study LCIs, which provides theoretical basis and novel thought to synthesize and prepare the composites with other polymers, especially in the fields of the blends with advantageous properties.
In this paper, a series of main-chain liquid crystalline ionomers containing sulfonic ion (MLCI-Sns) are prepared by an interfacial condensation reaction of enantiotropic nematic mesogenic monomer (1,4-phenylene-dicarbonic acid bis (4-carboxyl phenyl) ester,1,10-sebacoyl dihydroxy,1,12-dodecanedioyl dihydroxy and brittle yellow (BY content between 0 and 8%). For MLCI-Sns, the glass transition temperature increases slightly with increasing the sulfonate group content. However, the melt temperature becomes increase first and then decrease with increasing the sulfonate group content. The liquid crystalline mesogenic regions of the MLCI-Sns become broad first and then narrow with increasing sulfonate group content. The decomposed temperature is up to 300℃, so the MLCI-Sns exhibited good thermal stability. They are main-chain liquid crystalline ionomers with nematic schlieren textures.
A main-chain liquid crystalline ionomer containing carboxylic ion (MLCI-C5) by use of an interfacial condensation reaction from 4-phenylene-dicarbonic acid bis (4-carboxyl phenyl) ester,1,10-sebacoyl dihydroxy,1,12-dodecanedioyl dihydroxy and 2,5-dihydroxybenzoic acid is synthesized. It is main-chain liquid crystalline ionomers with nematic schlieren textures. The liquid crystalline mesogenic region of the MLCI-C5 is 172℃. The MLCI-C5 exhibits good thermal stability.
The MLCI-S5 and MLCI-C5 has been blended with PBT and PP, respectivley. DSC result shows the Tg of PBT decreased with the increase of MLCI-S5 content. It can be explained to improve interphase adhesion between a PBT-rich phase and PP-rich phase by adding the MLCI-S5. DSC result shows that some specific interaction is occurred between PBT (and PP) and MLCI-C5, which increase the Tm of PBT (and PP) component in the polymer blends. The crystallization rate of PBT is retarded due to hydrogen-bonding interactions between the MLCI-C5 and PBT in the blend. SEM and FTIR analysis identifies the intermolecular interaction between MLCI-S5 and PBT/PP phase, and the interaction results in a stronger interfacial adhesion between PBT and PP phase, and a much finer dispersion of the PP in PBT matrix, while excess of MLCI-S5 leads to coagulation of MLCI-S5 and PP phase. The addition of MLCI-C5 (9wt%) lead to finer and better dispersed of PP polymer in the blends relative to the blends with no MLCI-C5 added. A small amount of added MLCI-S5 will improve tensile strength and elongation at break, but MLCI-S5-rich domains form with excess MLCI-S5 addition will impair the mechanical performances. The mechanical properties are improved when the proper amount of MLCI-C5 is added, which enable improve adhesion at the interface.
The SLCI-C5 containing 4-(4-ethoxybenzyloxy)-4'-allyloxybiphenyl as enantiotropic nematic mesogenic monomer M2 and 4-allyoxybenzoic acids as ionic monomer M3 is synthesized by graft copolymerization upon polymethylhydrosiloxane. It is side-chain liquid crystalline ionomers with nematic schlieren textures. The liquid crystalline mesogenic regions of the SLCI-C5 are 149℃. The SLCI-C5 exhibits good thermal stability.
The SLCI-N5 containing 4-(4-ethoxybenzyloxy)-4'-allyloxybiphenyl as mesogenic monomer M2 and allytriethlammonium bromide as ionic monomer M4 is synthesized by graft copolymerization upon polymethylhydrosiloxane. The liquid crystalline mesogenic regions of the SLCI-N5 are 251℃. The SLCI-N5 exhibits good thermal stability. It is side-chain liquid crystalline ionomers with nematic schlieren textures.
The side-chain liquid crystalline ionomer containing carboxylic ion (SLCI-C5) and the side-chain liquid crystalline ionomer containing ammonium ion (SLCI-N5) are used in the blends of PBT and PP by melt-mixing, respectivly. DSC results of PBT/PP/SLCI-C5 and PBT/PP/SLCI-C5 blends are the same to the results of PBT/PP/MLCI-C5 blends.SEM and FTIR observation shows that the addition of SLCI-C5 and SLCI-N5significantly reduces the size of the dispersed phase and improves PP dispersion within the PBT matrix. The utilization of SLCI-C5 results in a stronger interfacial adhesion between PP and PBT phases and improves the mechanical performances of PBT/PP/SLCI-C5 blends. The mechanical properties of PBT/PP/SLCI-N5 blendsalso increase with the addition of SLCI-N5. When the SLCI-N5 content is 7wt%, the mechanic properties are best. The utilization of SLCI-N5 results in a stronger interfacial adhesion between PP and PBT phases and improves the mechanical performances of PBT/PP/SLCI-N5 blends. However, when the content of SLCI being added to the blends is surplus, the mechanical performances of blends are decreasing.
本文采用了加入含有离子基团的液晶离聚物来改善共混体系相容性的方法。液晶离聚物是指含有离子基团的液晶聚合物,它可以通过离子的相互作用使液晶聚合物与其他热塑性聚合物的相互作用增强,相容性得以改善,同时由于液晶中刚性基元的存在,在共混体系中起到了微纤增强作用,大大改善加工性能、降低了加工温度和粘度。它综合离聚物和液晶聚合物两方面的内容,是一种新型的功能高分子,是目前液晶聚合物研究领域的前沿课题之一,不仅具有重要的理论意义,而且在与其他热塑性聚合物共混制备性能优良的复合材料方面具有广阔的应用前景。
本论文设计并合成了互变向列相液晶单体对苯二甲酸二-(4-羧基苯)酯(M1),将其与1,10-癸二醇、1,12-十二烷二醇和亮黄(BY)按不同比例进行溶液缩聚反应,制备了一系列含有磺酸离子的主链液晶离聚物(MLCl-Sn)。结果表明：随着BY含量的增加,MLCI-Sn的Tg逐渐增加：MLCI-Sn的Tm出现了先增加后降低的趋势；MLCI-Sn的液晶区间先增加后变窄；MLCI-Sn的热分解温度在300℃以上,具有良好的热稳定性；MLCI-Sn的织构为向列相。
将合成的液晶单体对苯二甲酸二-(4-羧基苯)酯(M1)与1,10-癸二醇、1,12-十二烷二醇和2,5-二羟基苯甲酸按比例进行溶液缩聚反应,制备了一种含有羧酸离子的主链液晶离聚物(MLCI-C5)。MLCl-C5液晶离聚物的液晶类型为向列相,其液晶区间为172℃,热稳定性良好。
合成了一种互变向列相液晶单体4-乙氧基苯甲酸-4'-烯丙氧基联苯单酯(M2),离子单体4-烯丙氧基苯甲酸(M3),将液晶单体和离子单体接枝共聚到含氢聚硅氧烷主链上,合成了含有羧酸离子的侧链液晶离聚物(SLCI-C5)。液晶离聚物SLCI-C5的液晶类型为向列相,其液晶区间为149℃,具有良好的热稳定性。
合成的液晶单体4-乙氧基苯甲酸-4'-烯丙氧基联苯单酯(M2),离子单体N-烯丙基溴化吡啶(M4),将液晶单体和离子单体接枝共聚到含氢聚硅氧烷主链上,合成了含有铵离子的侧链液晶离聚物(SLCI-N5).液晶离聚物SLCI-N5的液晶类型为向列相,其液晶区间为251℃。
将合成的液晶离聚物MLCI-S5和MLCI-C5分别与PBT.PP进行了熔融共混制备了PBT/PP/MLCI-S5和PBT/PP/MLCI-C5共混物。在升温过程中,MLCI-S5的加入,降低了PBT的Tg,改善了PBT和PP之间的相容性；随着MLCI-S5含量的增加,PP的Tc没有发生变化,PBT的Tc向低温移动。MLCI-C5的加入,使PBT和PP的熔融温度均略有升高；而对PBT和PP(降温)结晶行为的影响则不尽相同,MLCI-C5的存在使PP的结晶温度略有升高,但升高幅度基本不受液晶离聚物含量的影响；与之相反,PBT的结晶温度则因液晶离聚物的存在而降低,DSC曲线中观察到的PP和PBT的结晶峰相互靠近,证实了MLCI-C5的加入起到了增容的作用。SEM和红外图像系统结果证实了当MLCI-S5的加入5wt%时,共混体系的分散得到了改善,PP分散相的相区尺寸变小,MLCI-S5介于PBT和PP两相界面之间,增加了PBT和PP之间的界面粘结力,改善了二者之间的相容性；过量MLCI-S5的加入,由于液晶离聚物的聚集,使分散效果变差。当MLCI-C5加入9wt%时,共混体系的分散效果最好,PP分散相的相区尺寸变小；过量的MLCI-C5加入,分散变差。力学性能结果表明：当加入适量的MLCI-S5(5wt％),共混物的拉伸强度和断裂伸长率达到最大值；当MLCI-C5含量为9wt%时,共混物的拉伸强度达到最大值；当MLCI-C5含量为15wt%时,共混物的断裂伸长率达到最大值。
将合成的液晶离聚物SLCI-C5和SLCI-N5分别与PBT.PP进行了熔融共混制备了PBT/PP/SLCI-C5和PBT/PP/SLCI-N5共混物。SLCI-C5和SLCI-N5对共混体系热力学性能的影响与MLCI-C5对共混体系的影响结果相似,证实了SLCI-C5和SLCI-N5的加入起到了增容的作用。SEM和红外图像系统结果表明：当SLCI-C5加入7wt%时,共混体系的分散得到了改善,增加了二者之间的相容性；过量SLCI-C5的加入,分散效果变差。当SLCI-N5的含量也加入到7wt%时,由于液晶离聚物与PBT的离子-偶极作用使共混体系的分散得到了改善；加入过量的SLCI-N5,由于液晶离聚物中离子的聚集作用,使分散效果变差。力学性能结果表明：随之SLCI-C5含量的增加,共混物的拉伸强度和断裂伸长率也随之增加,当含量为7wt%时,共混物的力学性能达到最大值；当SLCI-N5含量为7wt%时,共混物的力学性能达到最大值。而加入过量的液晶离聚物,共混物的拉伸强度和断裂伸长率有不同程度的降低。
Recently, Liquid crystalline polymers (LCPs) with high strength and stiffness, high chemical resistance, good dimensional stability and low linear thermal expansion coefficient are attractive high performance engineering materials. Most LCPs and thermoplastic are immiscible at the molecular level. The incompatibility between the matrix polymers and dispersed LCP phase leads to poor interfacial adhesion. Accordingly, the mechanical strength of the LCP/thermoplastic blends is considerably lower than that expected from theoretical calculation. Therefore, compatibilization with appropriate agents is required to improve the adhesion between the LCP fibril and thermoplastic blends interface, for example copolymer induced polar groups, chemistrical modify induced polar group, graft, block copolymer-blend, adding compotibilizer, forming IPN network, and hydrogen bond.
In this paper, the compatibilizing method is adding liquid crystalline ionomer containing ion group in blend. Liquid crystalline ionomers (LCIs) are liquid crystalline polymers containing ionic groups and the properties of LCIs are superior to the LCPs because of the compatibilization in composites by the function of ionic groups between the molecule chains. Moreover, the mesogenic phase has high degree of long-range order that enabling them to orient along the flow direction during processing. This leads to the formation of fine fibrils at an appropriate range of LCP concentration under certain processing conditions. The fine fibrils reinforce the matrix of thermoplastics effectively, giving rise to the development of polymer composites that commonly known as in situ composites. Therefore, LCIs are one new kind of function polymer materials and have been one of important research project in the field of LCPs. It is necessary and interesting to study LCIs, which provides theoretical basis and novel thought to synthesize and prepare the composites with other polymers, especially in the fields of the blends with advantageous properties.
In this paper, a series of main-chain liquid crystalline ionomers containing sulfonic ion (MLCI-Sns) are prepared by an interfacial condensation reaction of enantiotropic nematic mesogenic monomer (1,4-phenylene-dicarbonic acid bis (4-carboxyl phenyl) ester,1,10-sebacoyl dihydroxy,1,12-dodecanedioyl dihydroxy and brittle yellow (BY content between 0 and 8%). For MLCI-Sns, the glass transition temperature increases slightly with increasing the sulfonate group content. However, the melt temperature becomes increase first and then decrease with increasing the sulfonate group content. The liquid crystalline mesogenic regions of the MLCI-Sns become broad first and then narrow with increasing sulfonate group content. The decomposed temperature is up to 300℃, so the MLCI-Sns exhibited good thermal stability. They are main-chain liquid crystalline ionomers with nematic schlieren textures.
A main-chain liquid crystalline ionomer containing carboxylic ion (MLCI-C5) by use of an interfacial condensation reaction from 4-phenylene-dicarbonic acid bis (4-carboxyl phenyl) ester,1,10-sebacoyl dihydroxy,1,12-dodecanedioyl dihydroxy and 2,5-dihydroxybenzoic acid is synthesized. It is main-chain liquid crystalline ionomers with nematic schlieren textures. The liquid crystalline mesogenic region of the MLCI-C5 is 172℃. The MLCI-C5 exhibits good thermal stability.
The MLCI-S5 and MLCI-C5 has been blended with PBT and PP, respectivley. DSC result shows the Tg of PBT decreased with the increase of MLCI-S5 content. It can be explained to improve interphase adhesion between a PBT-rich phase and PP-rich phase by adding the MLCI-S5. DSC result shows that some specific interaction is occurred between PBT (and PP) and MLCI-C5, which increase the Tm of PBT (and PP) component in the polymer blends. The crystallization rate of PBT is retarded due to hydrogen-bonding interactions between the MLCI-C5 and PBT in the blend. SEM and FTIR analysis identifies the intermolecular interaction between MLCI-S5 and PBT/PP phase, and the interaction results in a stronger interfacial adhesion between PBT and PP phase, and a much finer dispersion of the PP in PBT matrix, while excess of MLCI-S5 leads to coagulation of MLCI-S5 and PP phase. The addition of MLCI-C5 (9wt%) lead to finer and better dispersed of PP polymer in the blends relative to the blends with no MLCI-C5 added. A small amount of added MLCI-S5 will improve tensile strength and elongation at break, but MLCI-S5-rich domains form with excess MLCI-S5 addition will impair the mechanical performances. The mechanical properties are improved when the proper amount of MLCI-C5 is added, which enable improve adhesion at the interface.
The SLCI-C5 containing 4-(4-ethoxybenzyloxy)-4'-allyloxybiphenyl as enantiotropic nematic mesogenic monomer M2 and 4-allyoxybenzoic acids as ionic monomer M3 is synthesized by graft copolymerization upon polymethylhydrosiloxane. It is side-chain liquid crystalline ionomers with nematic schlieren textures. The liquid crystalline mesogenic regions of the SLCI-C5 are 149℃. The SLCI-C5 exhibits good thermal stability.
The SLCI-N5 containing 4-(4-ethoxybenzyloxy)-4'-allyloxybiphenyl as mesogenic monomer M2 and allytriethlammonium bromide as ionic monomer M4 is synthesized by graft copolymerization upon polymethylhydrosiloxane. The liquid crystalline mesogenic regions of the SLCI-N5 are 251℃. The SLCI-N5 exhibits good thermal stability. It is side-chain liquid crystalline ionomers with nematic schlieren textures.
The side-chain liquid crystalline ionomer containing carboxylic ion (SLCI-C5) and the side-chain liquid crystalline ionomer containing ammonium ion (SLCI-N5) are used in the blends of PBT and PP by melt-mixing, respectivly. DSC results of PBT/PP/SLCI-C5 and PBT/PP/SLCI-C5 blends are the same to the results of PBT/PP/MLCI-C5 blends.SEM and FTIR observation shows that the addition of SLCI-C5 and SLCI-N5significantly reduces the size of the dispersed phase and improves PP dispersion within the PBT matrix. The utilization of SLCI-C5 results in a stronger interfacial adhesion between PP and PBT phases and improves the mechanical performances of PBT/PP/SLCI-C5 blends. The mechanical properties of PBT/PP/SLCI-N5 blendsalso increase with the addition of SLCI-N5. When the SLCI-N5 content is 7wt%, the mechanic properties are best. The utilization of SLCI-N5 results in a stronger interfacial adhesion between PP and PBT phases and improves the mechanical performances of PBT/PP/SLCI-N5 blends. However, when the content of SLCI being added to the blends is surplus, the mechanical performances of blends are decreasing.
引文
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