PEO-PPO-PEO水溶液胶束化与凝胶化行为研究
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摘要
本论文利用耗散粒子动力学模拟方法并结合流变和同步辐射小角x射线散射等实验手段研究了嵌段共聚物聚氧乙烯-聚氧丙烯-聚氧乙烯（PEO-PPO-PEO）水溶液体系的胶束化和凝胶化行为，探讨了亲水的PEO嵌段长度对PEO-PPO-PEO水溶液胶束化和凝胶化行为的影响，明晰了17R4（PO14-EO24-PO14）的添加对PEO-PPO-PEO水溶液凝胶化行为以及凝胶结构转变的影响规律，预测了PEO-PPO-PEO水溶液体系的胶束化和凝胶化机理，这些结果能够为聚合物凝胶材料的设计和应用提供可靠的理论指导。
具体内容包括：
采用耗散粒子动力学模拟方法并结合实验研究了PEO-PPO-PEO水溶液的胶束化和凝胶化行为。确定了F127（EO100-PO65-EO100）水溶液的临界胶束浓度和临界凝胶浓度；发现在298K，40wt%浓度以下，F127水溶液中形成以PPO为核、PEO为壳的球状胶束。进一步研究了亲水嵌段长度对胶束结构以及凝胶形成浓度的影响。发现亲水嵌段越短，越有利于长椭球状胶束的形成。在疏水嵌段长度相同的情况下，亲水嵌段越短，胶束聚集数越大，胶束外壳中的亲水链也就越密集，胶束也就越“硬”；反之，则亲水嵌段越长，胶束就越“软”。因此，对于较“硬”的胶束，亲水嵌段越长，临界凝胶浓度越低；而当更长的亲水嵌段长度使得形成较软的胶束时，在一定浓度下，尽管已经形成了逾渗网络结构，但此时网络结构的力学强度很弱。只有当浓度增加到一定程度时，才能形成具有一定力学性能的硬凝胶，因而形成硬凝胶的浓度有所上升。
在PEO-PPO-PEO水溶液中引入添加物，将使体系的胶束化行为和凝胶化行为变得更加复杂，为此，我们详细探讨了添加物对嵌段共聚物水溶液体系胶束化和凝胶化行为的影响。我们将具有不同摩尔比的相反嵌段组成的嵌段共聚物17R4添加到Pluronics P123（EO20-PO70-EO20）、F127（EO100-PO65-EO100）和F108（EO133-PO50-EO133）等水溶液中。通过测量不同混合溶液的流变性质来研究添加17R4对凝胶化行为的影响。当17R4添加到溶液中，P123、F127和F108水溶液的溶胶-凝胶转变温度向高温方向偏移。另外，17R4的存在极大地影响了凝胶的稳定性。这些结果有助于更好地理解Pluronics水溶液的凝胶化行为。
结合流变学频率扫描和同步辐射小角x射线散射（SAXS），研究了17R4含量和温度对17R4/F127混合水溶液的凝胶结构的影响。结果表明，溶胶、软凝胶和硬凝胶分别对应着无序结构、无序与立方相共存结构以及立方相结构。对于F127水溶液体系，可以把F127形成的胶束看成硬球，随着温度的升高，胶束的硬球半径和胶束中F127链的聚集数随之减小，这是因为17R4在较低温度下很难形成胶束，当温度升高时，17R4链参与胶束的形成，从而使胶束数目增加，因此每个胶束中的F127链数也就随之减小。当17R4含量较高时，胶束外壳中F127部分的PEO链段数随着温度升高而减少，胶束外壳变得更软，因此，当17R4/F127摩尔比为2:1时，混合溶液在高温下呈现面心立方（FCC）到体心立方（BCC）的结构转变。
Dissipative particle dynamics simulation method and experimental techniques,such as rheology and small angle x-ray scattering (SAXS), were used to study themicellization and gelation behavior of PEO-PPO-PEO (poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide)) aqueous solution, in which those propertieswere studied, such that the mechanism of the micellization and gelation behavior ofPEO-PPO-PEO aqueous solution, the effect of the length of hydrophilic PEO block onthe micellization and gelation behavior of PEO-PPO-PEO aqueous solution, and theeffect of the addition of17R4(PO14-EO24-PO14) to PEO-PPO-PEO aqueous solution onthe gelation behavior and gel structure transition.
The main content are as follows:
We study the micellization and gelation behavior of triblock copolymerpoly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) in solution by bothDissipative particle dynamics (DPD) simulation method and experimental technics. Thecritical micellization concentration and the critical gelation concentration were obtainedfor the system at298K. The shape of the micelles was spherical as the concentrationwas below40wt%, which is in accordance with experimental results. Furthermore, theeffect of the length of PEO block on micelle shape and gelation behavior was studied.For block copolymer with short length of PEO block, the prolate ellipsoid micellesformed more easily. For Pluronics with similar hydrophobic PPO block length, when thePEO block became shorter, the micelle aggregation number became bigger, and thus thePEO chains in the micelle coronal became denser, so that the micelles were “harder”;otherwise, when the PEO block became longer, the micelles became “softer”. Thus,Thus, for the harder micelles, the critical gelation concentration decreased withincreasing length of PEO block. However, when the length of PEO block was quite long,the softer micelles were formed. Although the network structure is formed throughpercolation, the mechanical property of the formed network is almost invisible. Onlywhen the concentration increased to a very high value, the network showed highmechanical property, and thus the critical concentration when hard gel formedincreased.
The reverse block copolymer PPO-PEO-PPO was introduced into PEO-PPO-PEOaqueous solutions, the micellization and gelation behavior of the system was complex.The reverse block copolymer17R4was added to the Pluronics EO20-PO70-EO20(P123),EO100-PO65-EO100(F127), and EO133-PO50-EO133(F108) aqueous solutions withdifferent molar ratios. The rheological properties of the different mixtures weremeasured to study the additive effect on the gelation behavior. The sol-gel transitiontemperature of the P123, F127and F108solutions shifted to a higher temperature whenadding17R4to the solutions. In addition, the existence of17R4greatly affected thestability of the gels. These results may help us better understand the gelation ofPluronics aqueous solutions.
Rheology and small angle x-ray scattering (SAXS) were used to study the effect ofthe content of17R4and temperature on the gel structure of the17R4/F127mixedsolutions. It was indicated that the structures of sol, soft gel and hard gel werecorresponding to disorder phase, disorder/cubic coexisting phase and cubic phase. Withincreasing temperature, hard sphere radius and aggregation number of micelle decreased.For pure17R4, it is difficult to form micelles. However, when the temperature wasincreased,17R4chains took part in the formation of micelles and therefore the numberof micelles increased, which made the number of F127chains in one micelle decrease.Thus, the number of PEO blocks of F127in coronal part decreased and then the coronalpart became softer. As a result, a FCC(face center cubic)-BCC(body center cubic)transition occurred in the system with17R4/F127molar ratio of2:1.
具体内容包括：
采用耗散粒子动力学模拟方法并结合实验研究了PEO-PPO-PEO水溶液的胶束化和凝胶化行为。确定了F127（EO100-PO65-EO100）水溶液的临界胶束浓度和临界凝胶浓度；发现在298K，40wt%浓度以下，F127水溶液中形成以PPO为核、PEO为壳的球状胶束。进一步研究了亲水嵌段长度对胶束结构以及凝胶形成浓度的影响。发现亲水嵌段越短，越有利于长椭球状胶束的形成。在疏水嵌段长度相同的情况下，亲水嵌段越短，胶束聚集数越大，胶束外壳中的亲水链也就越密集，胶束也就越“硬”；反之，则亲水嵌段越长，胶束就越“软”。因此，对于较“硬”的胶束，亲水嵌段越长，临界凝胶浓度越低；而当更长的亲水嵌段长度使得形成较软的胶束时，在一定浓度下，尽管已经形成了逾渗网络结构，但此时网络结构的力学强度很弱。只有当浓度增加到一定程度时，才能形成具有一定力学性能的硬凝胶，因而形成硬凝胶的浓度有所上升。
在PEO-PPO-PEO水溶液中引入添加物，将使体系的胶束化行为和凝胶化行为变得更加复杂，为此，我们详细探讨了添加物对嵌段共聚物水溶液体系胶束化和凝胶化行为的影响。我们将具有不同摩尔比的相反嵌段组成的嵌段共聚物17R4添加到Pluronics P123（EO20-PO70-EO20）、F127（EO100-PO65-EO100）和F108（EO133-PO50-EO133）等水溶液中。通过测量不同混合溶液的流变性质来研究添加17R4对凝胶化行为的影响。当17R4添加到溶液中，P123、F127和F108水溶液的溶胶-凝胶转变温度向高温方向偏移。另外，17R4的存在极大地影响了凝胶的稳定性。这些结果有助于更好地理解Pluronics水溶液的凝胶化行为。
结合流变学频率扫描和同步辐射小角x射线散射（SAXS），研究了17R4含量和温度对17R4/F127混合水溶液的凝胶结构的影响。结果表明，溶胶、软凝胶和硬凝胶分别对应着无序结构、无序与立方相共存结构以及立方相结构。对于F127水溶液体系，可以把F127形成的胶束看成硬球，随着温度的升高，胶束的硬球半径和胶束中F127链的聚集数随之减小，这是因为17R4在较低温度下很难形成胶束，当温度升高时，17R4链参与胶束的形成，从而使胶束数目增加，因此每个胶束中的F127链数也就随之减小。当17R4含量较高时，胶束外壳中F127部分的PEO链段数随着温度升高而减少，胶束外壳变得更软，因此，当17R4/F127摩尔比为2:1时，混合溶液在高温下呈现面心立方（FCC）到体心立方（BCC）的结构转变。
Dissipative particle dynamics simulation method and experimental techniques,such as rheology and small angle x-ray scattering (SAXS), were used to study themicellization and gelation behavior of PEO-PPO-PEO (poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide)) aqueous solution, in which those propertieswere studied, such that the mechanism of the micellization and gelation behavior ofPEO-PPO-PEO aqueous solution, the effect of the length of hydrophilic PEO block onthe micellization and gelation behavior of PEO-PPO-PEO aqueous solution, and theeffect of the addition of17R4(PO14-EO24-PO14) to PEO-PPO-PEO aqueous solution onthe gelation behavior and gel structure transition.
The main content are as follows:
We study the micellization and gelation behavior of triblock copolymerpoly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) in solution by bothDissipative particle dynamics (DPD) simulation method and experimental technics. Thecritical micellization concentration and the critical gelation concentration were obtainedfor the system at298K. The shape of the micelles was spherical as the concentrationwas below40wt%, which is in accordance with experimental results. Furthermore, theeffect of the length of PEO block on micelle shape and gelation behavior was studied.For block copolymer with short length of PEO block, the prolate ellipsoid micellesformed more easily. For Pluronics with similar hydrophobic PPO block length, when thePEO block became shorter, the micelle aggregation number became bigger, and thus thePEO chains in the micelle coronal became denser, so that the micelles were “harder”;otherwise, when the PEO block became longer, the micelles became “softer”. Thus,Thus, for the harder micelles, the critical gelation concentration decreased withincreasing length of PEO block. However, when the length of PEO block was quite long,the softer micelles were formed. Although the network structure is formed throughpercolation, the mechanical property of the formed network is almost invisible. Onlywhen the concentration increased to a very high value, the network showed highmechanical property, and thus the critical concentration when hard gel formedincreased.
The reverse block copolymer PPO-PEO-PPO was introduced into PEO-PPO-PEOaqueous solutions, the micellization and gelation behavior of the system was complex.The reverse block copolymer17R4was added to the Pluronics EO20-PO70-EO20(P123),EO100-PO65-EO100(F127), and EO133-PO50-EO133(F108) aqueous solutions withdifferent molar ratios. The rheological properties of the different mixtures weremeasured to study the additive effect on the gelation behavior. The sol-gel transitiontemperature of the P123, F127and F108solutions shifted to a higher temperature whenadding17R4to the solutions. In addition, the existence of17R4greatly affected thestability of the gels. These results may help us better understand the gelation ofPluronics aqueous solutions.
Rheology and small angle x-ray scattering (SAXS) were used to study the effect ofthe content of17R4and temperature on the gel structure of the17R4/F127mixedsolutions. It was indicated that the structures of sol, soft gel and hard gel werecorresponding to disorder phase, disorder/cubic coexisting phase and cubic phase. Withincreasing temperature, hard sphere radius and aggregation number of micelle decreased.For pure17R4, it is difficult to form micelles. However, when the temperature wasincreased,17R4chains took part in the formation of micelles and therefore the numberof micelles increased, which made the number of F127chains in one micelle decrease.Thus, the number of PEO blocks of F127in coronal part decreased and then the coronalpart became softer. As a result, a FCC(face center cubic)-BCC(body center cubic)transition occurred in the system with17R4/F127molar ratio of2:1.
引文
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