基于甲壳型液晶高分子相重入现象的研究
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摘要
本论文从甲壳型液晶高分子的化学结构出发，紧紧围绕其特殊的相重入行为，设计并合成具有不同化学结构的甲壳型液晶高分子，深入研究此类聚合物化学结构与相重入行为的关系。同时，通过无规共聚和共混手段，实现对甲壳型液晶高分子相重入行为的调控，达到对甲壳型液晶高分子相重入现象本质的认识和利用，同时加深对甲壳型液晶高分子的液晶相形成机制的理解。因此，论文的主要内容包括以下几个方面：
1.通过分子结构的设计，合成了不同长度，不同连接方式，不同拓扑结构的烷烃尾链及不同刚性核长度的甲壳型液晶高分子，聚2，5-二[(4-烷氧基)苯氧羰基]苯乙烯(P-OCm)，聚2，5-二[(4-烷氧基羰基)苯氧羰基]苯乙烯(P-OOCm)，聚2，5-二[(4-Y-烷氧基羰基)苯氧羰基]苯乙烯(P-OOYm)，聚2，5-二[(4′-烷氧基)联苯氧羰基]苯乙烯(P-Cm)。研究结果表明，微小的结构改变对甲壳型液晶高分子相重入行为有很大影响。在P-OCm体系中，随着烷烃尾链长度的增加，甲壳型液晶高分子表现出三种相行为。第一种，当m=1和2时，聚合物形成稳定的六方柱状相；第二种，当m=4，6和10时，聚合物在低温形成重入各向同性相，高温形成柱状相。并且将此类聚合物命名为第一类相重入行为的甲壳型液晶高分子；第三种，当m=10，12，14，16和18时，随着温度的增加，聚合物相结构的变化过程为：侧基烷烃的结晶—近晶A相—重入各向同性相—柱状向列相—各向同性相(假设的)。并且将此类聚合物命名为第二类相重入行为的甲壳型液晶高分子。在P-OOCm体系中，大多数聚合物难于形成柱状相，而且即使聚合物形成柱状相，其出现的温度较高。在P-OOYm体系中，所有聚合物都表现出第一类甲壳型液晶高分子的相重入行为。在P-Cm体系中，由于刚性核长度增加，侧基之间的相互作用增加，聚合物只能形成稳定的近晶A相。
2.通过ATRP的方法合成了一系列不同分子量的聚2，5-二[(4-十八烷氧基)苯氧羰基]苯乙烯(P-OC18s)，详细考察了分子量对甲壳型液晶高分子相重入行为的影响。研究表明，当分子量≤4.4×104时，聚合物只能形成近晶A相和各向同性相。而当分子量≥5.2×104时，聚合物随着温度的增加，其相转变过程为侧基烷烃的结晶相—近晶A相—重入各向同性相—柱状相—各向同性相(假定的)。降温时，其相转变过程是可逆的。同时，随着分子量的增加，玻璃化温度(Tg)和近晶A相到各向同性相的转变温度轻微增加，而重入各向同性相到柱状相的转变温度急剧增加。
3.通过自由基聚合的方法合成了一系列含有不同比例的不同烷烃尾链长度的甲壳型液晶高分子单体的共聚物，poly{M-OC1(x)-co-M-OC4(y)}s, poly{M-OC1(x)-co-M-OC18(y)}s和poly{M-OC4(x)-co-M-OC18(y)s。研究结果表明，在共聚物poly{M-OC1(x)-co-M-OC4(y)}s体系中，所有聚合物都能形成液晶相。而在共聚物poly{M-OC1(x)-co-M-OC18(y)}s和poly{M-OC4(x)-co-M-OC18(y)s体系中，共聚物的相行为强烈依赖于两者单体的投料比。当两单体的投料比在一定比例区间时，尽管均聚物都能形成液晶相，但共聚物不能形成液晶相。
4.通过自由基聚合的方法合成了一系列含有不同比例的不同刚性核长度的甲壳型液晶高分子单体的共聚物，poly (M-OC18-co-M-C18)。研究了共聚物中不同长度的刚性核含量对甲壳型液晶高分子共聚物相重入行为的影响。研究结果表明，随着长的刚性核含量的增加，共聚物形成的近晶相变得更加稳定，同时Tg增加。相反，共聚物的重入各向同性相的出现变得更加困难。
5.选取十八烷醇作为溶剂分子，通过溶液混和，制备出不同质量浓度的P-OC18s溶液。实验结果表明，十八烷醇的含量对聚合物的相重入行为有很大的影响。第一，当十八烷醇含量小于5%时，聚合物溶液相行为与均聚物P-OC18s的相同，表现出第二类甲壳型液晶高分子相重入行为。第二，当十八烷醇的含量处于5%到30%之间，聚合物溶液的相行为表现出第一类甲壳型液晶高分子相重入行为。并且随着十八烷醇含量的增加，一方面聚合物出现柱状相的温度逐渐降低，另一方面聚合物形成柱子的直径逐渐增加。第三，当十八烷醇的含量高于30%时，聚合物溶液不能形成液晶相。
This dissertation is focused on the investigation of the phase behavior and phasestructures of mesogen-jacketed liquid crystalline polymers (MJLCPs) with thedifferent chemical structures in order to study the structure–phase reentrantrelationship in liquid crystalline polymers. Meantime, phase reentrant behavior ofMJLCPs can be tailored through copolymerization and blends. Through the studying,we can obtain knowledge about the phase reentrant behavior and can get theinformation of the structure variation of MJLCPs and pocking mode molecular chain.The main topics of this paper are as follows:
(1) Four series of polymers, poly{2,5-bis[(4-alkoxyphenyl)oxycarbonyl]styrenes}(P-OCm, m=1,2,4,6,8,10,12,14,16and18), poly{2,5-bis[(4-alkoxy carbonylphenyl)oxycarbonyl]styrenes}(P-OOCm, m=1,2,3,4,6,8,10,12,14,16and18),poly{2,5-bis [(4-Y-alkoxy carbonylphenyl)oxycarbonyl]-styrenes}(P-OOYm, m=1,2and3) and poly{2,5-bis [(4-alkoxybiphenyl)oxycarbonyl]-styrenes}(P-Cm, m=8,10,12,14and18) were designed and successfully synthesized via free radicalpolymerization. The phase structures and transitions of the polymers wereinvestigated by the combination of techniques including differential scanningcalorimetry, wide-angle X-ray diffraction, polarized optical microscopy, andrheological measurement. The experimental results revealed that the phase reentrantbehavior of MJLCPs was strongly depended on the length of rigid core and tail. ForP-OCm, when m was1and2, the polymers showed only a stable liquid crystallinephase above Tg. Second, with the increasing length of alkoxy tails, the P-OCm (m=4,6,8) presented a re-entrant isotropic phase above Tg and a liquid crystalline phase athigher temperature. They are considered to be the first kind of MJLCPs with are-entrant phase.Third, the P-OCm (m=10,12,14,16,18) exhibited an unusualre-entrant isotropic phase which was separating smectic A (SA) phase (in lowtemperature) and columnar phases (in high temperature). They are considered to bethe second kind of MJLCPs with a re-entrant phase. For P-OOCm, the most ofpolymers hard formed the columnar phases in high temperature. For P-OOYm, allpolymers formed a re-entrant isotropic phase above Tg. For P-Cm, the polymersdeveloped into a well-defined SAphase, which indicated that the lateral substitution oflong rigid mesogens strongly reduced the ability of forming columnar polymers.
(2) A series of comb-like polymers, poly{2,5-bis[(4-octadecyloxyphenyl)oxycarbonyl]-styrenes}(P-OC18s) with different molecular weights (Mn) and lowmolecular weight distributions have been successfully synthesized via atom transferradical polymerization. One hand, phase behaviors of the alkyl tails were stronglyinfluenced by the mesogens of polymers, leading to the poor packing of the alkyl tailsand the low melting. The other hand, the liquid crystalline (LC) phase structures ofpolymers were found to be strongly Mndependent. The samples with Mn≤4.6×104formed a SAphase in low temperature and an isotropic phase in high temperature. Thesamples with Mn≥5.2×104displayed a re-entrant isotropic phase which was separatingthe SAphase and columnar nematic phase. Meantime, the experiment results showedthat Tg and the transition temperature from SAphase to isotropic phase both slightlyincreased with the increase of the Mns, however, the transition temperature fromisotropic phase to columnar phase sharply decreased with the molecular weightsimproved.
(3) Based on2,5-bis[(4-alkoxyphenyl)oxycarbonyl]styrenes (M-OCm, m is thenumber of the carbons of alkyl tails,, m=1,4and18), three series of binarycopolymers with high Mn,{poly(M-OC1-co-M-OC4), poly(M-OC1-co-M-OC18)and poly(M-OC4-co-M-OC18)} have been prepared via free radical polymerization.The results showed that LC phase structures of copolymers, containing SAphase,re-entrant isotropic phase, columnar phase and isotropic phase, were stronglydepended on the composition and the alkyl length due to the competing among thesteric effect, the microphase separation and the driving force of the entropy. Whenone of them occupied a dominant position, the LC phase structure can be presentedfor the copolymers. Otherwise, the LC phase structure is lost despite the pair ofcorresponding homopolymers forming mesogenic structure.
(4) A series of binary copolymers, poly{2,5-bis[(4-octadecyloxyphenyl)oxycarbonyl]-styrene-co-2,5-bis[(4-octadecyloxybiphenyl)oxycarbonyl]-styrene}{poly(M-OC18-co-M-C18)}, were synthesized via free radical polymerization. Theexperimental results revealed that Tg of the copolymers and the phase transitiontemperature from SAphase to isotropic phase both increased with the molar fractionof2,5-bis[(4-octadecyloxybiphenyl)oxycarbonyl]-styrene (M-C18) in feed. Inaddition, when the feed was below0.3, a column nematic phase was formed in hightemperature.
(5) The octadecanol solution of P-OC18s with different the mass concentration of P-OC18s were prepared by solution method. The experiment results showed thatwhen the mass concentration of octadecanol was below5%, the SA—re-entrantisotropic phase—columnar phase transition takes place upon increasing thetemperature in the octadecanol solution of P-OC18s. Secondly, when the massconcentration of octadecanol was between5%and30%, a re-entrant isotropic phaseand columnar phase (at high temperature) were presented. Moreover, with theincrease of octadecanol, one hand, the transition temperature from isotropic phase tocolumnar phase decreased to119from240oC. On the other hand, the diameter ofcolumnar phase increased. Thirdly, when the mass concentration of octadecanol wasabove30%, the isotropic phase was only formed.
1.通过分子结构的设计，合成了不同长度，不同连接方式，不同拓扑结构的烷烃尾链及不同刚性核长度的甲壳型液晶高分子，聚2，5-二[(4-烷氧基)苯氧羰基]苯乙烯(P-OCm)，聚2，5-二[(4-烷氧基羰基)苯氧羰基]苯乙烯(P-OOCm)，聚2，5-二[(4-Y-烷氧基羰基)苯氧羰基]苯乙烯(P-OOYm)，聚2，5-二[(4′-烷氧基)联苯氧羰基]苯乙烯(P-Cm)。研究结果表明，微小的结构改变对甲壳型液晶高分子相重入行为有很大影响。在P-OCm体系中，随着烷烃尾链长度的增加，甲壳型液晶高分子表现出三种相行为。第一种，当m=1和2时，聚合物形成稳定的六方柱状相；第二种，当m=4，6和10时，聚合物在低温形成重入各向同性相，高温形成柱状相。并且将此类聚合物命名为第一类相重入行为的甲壳型液晶高分子；第三种，当m=10，12，14，16和18时，随着温度的增加，聚合物相结构的变化过程为：侧基烷烃的结晶—近晶A相—重入各向同性相—柱状向列相—各向同性相(假设的)。并且将此类聚合物命名为第二类相重入行为的甲壳型液晶高分子。在P-OOCm体系中，大多数聚合物难于形成柱状相，而且即使聚合物形成柱状相，其出现的温度较高。在P-OOYm体系中，所有聚合物都表现出第一类甲壳型液晶高分子的相重入行为。在P-Cm体系中，由于刚性核长度增加，侧基之间的相互作用增加，聚合物只能形成稳定的近晶A相。
2.通过ATRP的方法合成了一系列不同分子量的聚2，5-二[(4-十八烷氧基)苯氧羰基]苯乙烯(P-OC18s)，详细考察了分子量对甲壳型液晶高分子相重入行为的影响。研究表明，当分子量≤4.4×104时，聚合物只能形成近晶A相和各向同性相。而当分子量≥5.2×104时，聚合物随着温度的增加，其相转变过程为侧基烷烃的结晶相—近晶A相—重入各向同性相—柱状相—各向同性相(假定的)。降温时，其相转变过程是可逆的。同时，随着分子量的增加，玻璃化温度(Tg)和近晶A相到各向同性相的转变温度轻微增加，而重入各向同性相到柱状相的转变温度急剧增加。
3.通过自由基聚合的方法合成了一系列含有不同比例的不同烷烃尾链长度的甲壳型液晶高分子单体的共聚物，poly{M-OC1(x)-co-M-OC4(y)}s, poly{M-OC1(x)-co-M-OC18(y)}s和poly{M-OC4(x)-co-M-OC18(y)s。研究结果表明，在共聚物poly{M-OC1(x)-co-M-OC4(y)}s体系中，所有聚合物都能形成液晶相。而在共聚物poly{M-OC1(x)-co-M-OC18(y)}s和poly{M-OC4(x)-co-M-OC18(y)s体系中，共聚物的相行为强烈依赖于两者单体的投料比。当两单体的投料比在一定比例区间时，尽管均聚物都能形成液晶相，但共聚物不能形成液晶相。
4.通过自由基聚合的方法合成了一系列含有不同比例的不同刚性核长度的甲壳型液晶高分子单体的共聚物，poly (M-OC18-co-M-C18)。研究了共聚物中不同长度的刚性核含量对甲壳型液晶高分子共聚物相重入行为的影响。研究结果表明，随着长的刚性核含量的增加，共聚物形成的近晶相变得更加稳定，同时Tg增加。相反，共聚物的重入各向同性相的出现变得更加困难。
5.选取十八烷醇作为溶剂分子，通过溶液混和，制备出不同质量浓度的P-OC18s溶液。实验结果表明，十八烷醇的含量对聚合物的相重入行为有很大的影响。第一，当十八烷醇含量小于5%时，聚合物溶液相行为与均聚物P-OC18s的相同，表现出第二类甲壳型液晶高分子相重入行为。第二，当十八烷醇的含量处于5%到30%之间，聚合物溶液的相行为表现出第一类甲壳型液晶高分子相重入行为。并且随着十八烷醇含量的增加，一方面聚合物出现柱状相的温度逐渐降低，另一方面聚合物形成柱子的直径逐渐增加。第三，当十八烷醇的含量高于30%时，聚合物溶液不能形成液晶相。
This dissertation is focused on the investigation of the phase behavior and phasestructures of mesogen-jacketed liquid crystalline polymers (MJLCPs) with thedifferent chemical structures in order to study the structure–phase reentrantrelationship in liquid crystalline polymers. Meantime, phase reentrant behavior ofMJLCPs can be tailored through copolymerization and blends. Through the studying,we can obtain knowledge about the phase reentrant behavior and can get theinformation of the structure variation of MJLCPs and pocking mode molecular chain.The main topics of this paper are as follows:
(1) Four series of polymers, poly{2,5-bis[(4-alkoxyphenyl)oxycarbonyl]styrenes}(P-OCm, m=1,2,4,6,8,10,12,14,16and18), poly{2,5-bis[(4-alkoxy carbonylphenyl)oxycarbonyl]styrenes}(P-OOCm, m=1,2,3,4,6,8,10,12,14,16and18),poly{2,5-bis [(4-Y-alkoxy carbonylphenyl)oxycarbonyl]-styrenes}(P-OOYm, m=1,2and3) and poly{2,5-bis [(4-alkoxybiphenyl)oxycarbonyl]-styrenes}(P-Cm, m=8,10,12,14and18) were designed and successfully synthesized via free radicalpolymerization. The phase structures and transitions of the polymers wereinvestigated by the combination of techniques including differential scanningcalorimetry, wide-angle X-ray diffraction, polarized optical microscopy, andrheological measurement. The experimental results revealed that the phase reentrantbehavior of MJLCPs was strongly depended on the length of rigid core and tail. ForP-OCm, when m was1and2, the polymers showed only a stable liquid crystallinephase above Tg. Second, with the increasing length of alkoxy tails, the P-OCm (m=4,6,8) presented a re-entrant isotropic phase above Tg and a liquid crystalline phase athigher temperature. They are considered to be the first kind of MJLCPs with are-entrant phase.Third, the P-OCm (m=10,12,14,16,18) exhibited an unusualre-entrant isotropic phase which was separating smectic A (SA) phase (in lowtemperature) and columnar phases (in high temperature). They are considered to bethe second kind of MJLCPs with a re-entrant phase. For P-OOCm, the most ofpolymers hard formed the columnar phases in high temperature. For P-OOYm, allpolymers formed a re-entrant isotropic phase above Tg. For P-Cm, the polymersdeveloped into a well-defined SAphase, which indicated that the lateral substitution oflong rigid mesogens strongly reduced the ability of forming columnar polymers.
(2) A series of comb-like polymers, poly{2,5-bis[(4-octadecyloxyphenyl)oxycarbonyl]-styrenes}(P-OC18s) with different molecular weights (Mn) and lowmolecular weight distributions have been successfully synthesized via atom transferradical polymerization. One hand, phase behaviors of the alkyl tails were stronglyinfluenced by the mesogens of polymers, leading to the poor packing of the alkyl tailsand the low melting. The other hand, the liquid crystalline (LC) phase structures ofpolymers were found to be strongly Mndependent. The samples with Mn≤4.6×104formed a SAphase in low temperature and an isotropic phase in high temperature. Thesamples with Mn≥5.2×104displayed a re-entrant isotropic phase which was separatingthe SAphase and columnar nematic phase. Meantime, the experiment results showedthat Tg and the transition temperature from SAphase to isotropic phase both slightlyincreased with the increase of the Mns, however, the transition temperature fromisotropic phase to columnar phase sharply decreased with the molecular weightsimproved.
(3) Based on2,5-bis[(4-alkoxyphenyl)oxycarbonyl]styrenes (M-OCm, m is thenumber of the carbons of alkyl tails,, m=1,4and18), three series of binarycopolymers with high Mn,{poly(M-OC1-co-M-OC4), poly(M-OC1-co-M-OC18)and poly(M-OC4-co-M-OC18)} have been prepared via free radical polymerization.The results showed that LC phase structures of copolymers, containing SAphase,re-entrant isotropic phase, columnar phase and isotropic phase, were stronglydepended on the composition and the alkyl length due to the competing among thesteric effect, the microphase separation and the driving force of the entropy. Whenone of them occupied a dominant position, the LC phase structure can be presentedfor the copolymers. Otherwise, the LC phase structure is lost despite the pair ofcorresponding homopolymers forming mesogenic structure.
(4) A series of binary copolymers, poly{2,5-bis[(4-octadecyloxyphenyl)oxycarbonyl]-styrene-co-2,5-bis[(4-octadecyloxybiphenyl)oxycarbonyl]-styrene}{poly(M-OC18-co-M-C18)}, were synthesized via free radical polymerization. Theexperimental results revealed that Tg of the copolymers and the phase transitiontemperature from SAphase to isotropic phase both increased with the molar fractionof2,5-bis[(4-octadecyloxybiphenyl)oxycarbonyl]-styrene (M-C18) in feed. Inaddition, when the feed was below0.3, a column nematic phase was formed in hightemperature.
(5) The octadecanol solution of P-OC18s with different the mass concentration of P-OC18s were prepared by solution method. The experiment results showed thatwhen the mass concentration of octadecanol was below5%, the SA—re-entrantisotropic phase—columnar phase transition takes place upon increasing thetemperature in the octadecanol solution of P-OC18s. Secondly, when the massconcentration of octadecanol was between5%and30%, a re-entrant isotropic phaseand columnar phase (at high temperature) were presented. Moreover, with theincrease of octadecanol, one hand, the transition temperature from isotropic phase tocolumnar phase decreased to119from240oC. On the other hand, the diameter ofcolumnar phase increased. Thirdly, when the mass concentration of octadecanol wasabove30%, the isotropic phase was only formed.
引文
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