梳形聚合物的结构和性能
摘要
梳形聚合物是一种具有独特结构和新颖性能的聚合物。本文的研究目的在于深入研究梳形聚合物在本体和溶液中的结构,并探讨结构与性能之间的联系。在总结前人工作的基础上,本文设计合成了两类梳形聚合物,并详细研究了其结构和性能。第一类是可结晶性的梳形聚L-乳酸,它以聚甲基丙烯酸羟乙酯(PHEMA)为主链,以聚L-乳酸(PLLA)为侧链。我们将主要讨论其晶态结构,热性能以及与聚环氧乙烷(PEO)共混的现象。第二类是不对称双亲性梳形聚合物PGMA-g-Py/PNIPAM,该聚合物侧链为亲水的且具有温敏性的聚N-异丙基甲酰胺(PNIPAM),主链为聚甲基丙烯酸环氧丙酯(PGMA),主链的每个重复单元上悬挂有荧光基团芘。我们将主要讨论其在不同溶剂中的结构,自组装行为和光物理性能。
通过原子转移自由基聚合(ATRP)和开环聚合(ROP),合成了PHEMA为主链,以PLLA为侧链的梳形PLLA。通过广角X射线衍射(WAXD),小角X射线散射(SAXS)和差示量热扫描(DSC)研究了梳形PLLA的晶态结构和热性能。WAXD结果显示,梳形PLLA侧链的结晶为103螺旋结构α晶型。通过一维相关函数方法对SAXS数据进行了分析,结果显示,梳形PLLA的结晶片层厚度受结晶温度和梳形分子结构的控制。通过DSC研究了其结晶动力学和熔融行为。结晶动力学的研究表明,梳形PLLA的Avrami指数不随结晶温度变化；且高度支化的结构降低了Avrami指数。熔融行为研究表明,梳形PLLA的熔融峰为双峰,这是由于熔融过程的二次结晶造成的。另外,我们将梳形PLLA与聚乙二醇进行共混,研究了梳形结构对共混物的相容性和晶态结构的影响。
通过点击化学和可逆加成-裂解链转移聚合(RAFT),我们合成了不对称双亲性梳形聚合物PGMA-g-Py/PNIPAM。该聚合物侧链为亲水的且具有温敏性的PNIPAM,主链上悬挂有荧光基团芘。通过凝胶渗透色谱(GPC),核磁共振(NMR),红外吸收(FT-IR)等分析手段表征了该聚合物的分子结构。我们使用荧光光谱的手段对该聚合物在良溶剂四氢呋哺(THF)和选择性溶剂水中的光物理性质进行了研究,并通过超灵敏差示量热扫描(MDSC),透射电子显微镜(TEM),和动态光散射(DLS)研究了该聚合物在水中的自组装行为和最低临界溶解温度(LCST)相转变行为。在良溶剂中,其光物理行为在主链的线团接触浓度之上和之下有明显区别：浓度较低时,芘基团主要产生分子内基激缔合物；浓度较高时,芘基团主要产生分子间基激缔合物。在水溶液中,该聚合物组装成了以带有芘基团的主链为壁,以PNIPAM为冠的囊泡结构。我们通过荧光光谱确定了其临界聚集浓度。由于溶液温度高于LCST时,PNIPAM塌缩并覆盖在囊泡的壁表面,形成较小的囊泡。通过荧光淬灭实验发现,塌缩的PNIPAM可以阻碍部分芘基团和外加淬灭剂的接触,从而实现该囊泡对外界刺激的响应性。
Comb shaped polymers are a kind of polymer with unique structure and novel properties. This thesis would investigate the structure of comb shaped polymer in solution and in bulk, and study the relationship between its structure and its properties. On the basis of reviewing of the progress of other scientists working on this topic, we synthesized two kinds of comb polymer, and studied their structure and properties detailly. In the first part of this study, we synthesized a comb shaped polymer with Poly(L-lactide) (PLLA) with a novel comb conformation was synthesized and its crystallization and thermal properties was studied. PLLA on poly(2-hydroxyethyl methacrylate) (PHEMA) backbone was prepared by a combination of atom transfer radical polymerization (ATRP) and ring-opening polymerization (ROP). The structure of the comb PLLA was analyzed by wide angle x-ray diffraction (WAXD), small angle x-ray scattering (SAXS) and differential scanning calorimetry (DSC). WAXD result indicates that the comb polymer has a crystalline modification with a 103 helical conformation. Lamellar parameters of the crystalline structure were obtained by one-dimension correlation function (1DCF) calculated from SAXS results. The calculations show that the thickness of crystalline layer is controlled by annealing temperature and comb structure. DSC was applied to study kinetics of the crystallization and melting behavior. Avrami exponents at different crystallization temperature were obtained and did not show dependence on annealing temperature, but tend to be decreased by branching conformation. The melting curves show two melting peaks, which was attributed to melt recrystalliztion and the influence of the comb structure on it was discussed. In addition, we blended the comb PLLA with poly(ethyleneoxide), the influences of comb structure on the compatibility and crystalline structure of the blends were discussed.
An amphiphilic comb polymer with pendant pyrene groups and poly(N-isopropylacrylamide) (PNIPAM) side chains was synthesized based on click chemistry and reversible addition-fragmentation chain transfer polymerization. Gel permeation chromatography, FTIR and 1H NMR results all indicated successful synthesis of well-defined comb polymer. The photophysical properties and self-assembly of the polymer in solution were studied by UV-Vis spectroscopy, fluorescence technique and transmission electron microscopy. The intensity ratio of the excimer peak (IE) to the monomer peak (IM) of the comb polymer in THF, was used to monitor the formation of inter-or intramolecular excimer. At low polymer concentration, the value of IE/IM kept unchanged indicating the formation of intramolecular excimer; at high polymer concentration the value increased rapidly with concentration because of the formation of intermolecular excimer. The change of the intensity ratio of the first to the third vibronic band (I1/I3) on the monomer emission of the comb polymer also proved the association of the pendant pyrene groups in THF at high polymer concentration. In aqueous solution, the comb polymer chains self-assembled into vesicles with pyrene groups in the walls and PNIPAM side chains in the coronae. The value of the critical aggregation concentration of the polymer was determined by fluorescence technique. Temperature exerted significant effect on the size and morphology of the vesicles. At a temperature above lower critical solution temperature (LCST) of PNIPAM, PNIPAM brushes in the coronae of vesicles collapsed on the surface of the structures forming nano-sized domains, and vesicles with smaller size were obtained. Fluorescence quenching experiments indicated that the collapsed PNIPAM chains protected a part of pyrene groups from being quenched by nitromethane at a temperature above LCST of PNIPAM.
通过原子转移自由基聚合(ATRP)和开环聚合(ROP),合成了PHEMA为主链,以PLLA为侧链的梳形PLLA。通过广角X射线衍射(WAXD),小角X射线散射(SAXS)和差示量热扫描(DSC)研究了梳形PLLA的晶态结构和热性能。WAXD结果显示,梳形PLLA侧链的结晶为103螺旋结构α晶型。通过一维相关函数方法对SAXS数据进行了分析,结果显示,梳形PLLA的结晶片层厚度受结晶温度和梳形分子结构的控制。通过DSC研究了其结晶动力学和熔融行为。结晶动力学的研究表明,梳形PLLA的Avrami指数不随结晶温度变化；且高度支化的结构降低了Avrami指数。熔融行为研究表明,梳形PLLA的熔融峰为双峰,这是由于熔融过程的二次结晶造成的。另外,我们将梳形PLLA与聚乙二醇进行共混,研究了梳形结构对共混物的相容性和晶态结构的影响。
通过点击化学和可逆加成-裂解链转移聚合(RAFT),我们合成了不对称双亲性梳形聚合物PGMA-g-Py/PNIPAM。该聚合物侧链为亲水的且具有温敏性的PNIPAM,主链上悬挂有荧光基团芘。通过凝胶渗透色谱(GPC),核磁共振(NMR),红外吸收(FT-IR)等分析手段表征了该聚合物的分子结构。我们使用荧光光谱的手段对该聚合物在良溶剂四氢呋哺(THF)和选择性溶剂水中的光物理性质进行了研究,并通过超灵敏差示量热扫描(MDSC),透射电子显微镜(TEM),和动态光散射(DLS)研究了该聚合物在水中的自组装行为和最低临界溶解温度(LCST)相转变行为。在良溶剂中,其光物理行为在主链的线团接触浓度之上和之下有明显区别：浓度较低时,芘基团主要产生分子内基激缔合物；浓度较高时,芘基团主要产生分子间基激缔合物。在水溶液中,该聚合物组装成了以带有芘基团的主链为壁,以PNIPAM为冠的囊泡结构。我们通过荧光光谱确定了其临界聚集浓度。由于溶液温度高于LCST时,PNIPAM塌缩并覆盖在囊泡的壁表面,形成较小的囊泡。通过荧光淬灭实验发现,塌缩的PNIPAM可以阻碍部分芘基团和外加淬灭剂的接触,从而实现该囊泡对外界刺激的响应性。
Comb shaped polymers are a kind of polymer with unique structure and novel properties. This thesis would investigate the structure of comb shaped polymer in solution and in bulk, and study the relationship between its structure and its properties. On the basis of reviewing of the progress of other scientists working on this topic, we synthesized two kinds of comb polymer, and studied their structure and properties detailly. In the first part of this study, we synthesized a comb shaped polymer with Poly(L-lactide) (PLLA) with a novel comb conformation was synthesized and its crystallization and thermal properties was studied. PLLA on poly(2-hydroxyethyl methacrylate) (PHEMA) backbone was prepared by a combination of atom transfer radical polymerization (ATRP) and ring-opening polymerization (ROP). The structure of the comb PLLA was analyzed by wide angle x-ray diffraction (WAXD), small angle x-ray scattering (SAXS) and differential scanning calorimetry (DSC). WAXD result indicates that the comb polymer has a crystalline modification with a 103 helical conformation. Lamellar parameters of the crystalline structure were obtained by one-dimension correlation function (1DCF) calculated from SAXS results. The calculations show that the thickness of crystalline layer is controlled by annealing temperature and comb structure. DSC was applied to study kinetics of the crystallization and melting behavior. Avrami exponents at different crystallization temperature were obtained and did not show dependence on annealing temperature, but tend to be decreased by branching conformation. The melting curves show two melting peaks, which was attributed to melt recrystalliztion and the influence of the comb structure on it was discussed. In addition, we blended the comb PLLA with poly(ethyleneoxide), the influences of comb structure on the compatibility and crystalline structure of the blends were discussed.
An amphiphilic comb polymer with pendant pyrene groups and poly(N-isopropylacrylamide) (PNIPAM) side chains was synthesized based on click chemistry and reversible addition-fragmentation chain transfer polymerization. Gel permeation chromatography, FTIR and 1H NMR results all indicated successful synthesis of well-defined comb polymer. The photophysical properties and self-assembly of the polymer in solution were studied by UV-Vis spectroscopy, fluorescence technique and transmission electron microscopy. The intensity ratio of the excimer peak (IE) to the monomer peak (IM) of the comb polymer in THF, was used to monitor the formation of inter-or intramolecular excimer. At low polymer concentration, the value of IE/IM kept unchanged indicating the formation of intramolecular excimer; at high polymer concentration the value increased rapidly with concentration because of the formation of intermolecular excimer. The change of the intensity ratio of the first to the third vibronic band (I1/I3) on the monomer emission of the comb polymer also proved the association of the pendant pyrene groups in THF at high polymer concentration. In aqueous solution, the comb polymer chains self-assembled into vesicles with pyrene groups in the walls and PNIPAM side chains in the coronae. The value of the critical aggregation concentration of the polymer was determined by fluorescence technique. Temperature exerted significant effect on the size and morphology of the vesicles. At a temperature above lower critical solution temperature (LCST) of PNIPAM, PNIPAM brushes in the coronae of vesicles collapsed on the surface of the structures forming nano-sized domains, and vesicles with smaller size were obtained. Fluorescence quenching experiments indicated that the collapsed PNIPAM chains protected a part of pyrene groups from being quenched by nitromethane at a temperature above LCST of PNIPAM.
引文
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