各向异性（Janus）和多孔聚合物微球的制备及其形态控制研究
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摘要
高分子微球材料的发展对人类的经济与生活带来了巨大的影响,例如,高分子微球在涂料、化妆品、感光材料、生物医药等领域都占有重要的地位。影响高分子微球应用的最关键因素便是高分子微球的形态和尺寸特征。因此,对高分子微球的形态控制研究一直是科学家比较关注的课题。随着研究的深入,人们制备出不同形态和结构的微球,其中最引人关注的便是各向异性(Janus)微球和多孔聚合物微球。Janus微球具有形态或化学组成的不对称性质。然而,与合成普通聚合物微球几乎是随心所欲的情形相比,Janus微球的制备难度较大,因为对于一个微球,由于热力学稳定性的要求,其表面自由能趋向于最低,导致最终微球极易成为具有均匀表面和能量最低的规则球形。所以,采用传统合成聚合物微球的方法是很难得到Janus微球的。Janus微球的制备与形态控制是目前材料科学领域中颇具挑战性的工作,其制备过程要从热力学和动力学两个方面来调控。另外,多孔聚合物微球由于其具有低密度和高比表面积等特点备受材料学家的关注。由于Janus微球的制备在热力学和动力学上与多孔聚合物微球的形成之间存在着密切的关系,因此,对Janus微球和多孔聚合物微球的形态控制研究,无论在基础理论研究还是应用研究方面都将具有重要意义。
本论文以乳液聚合制备形态可控Janus微球和多孔聚合物微球为目标,以界面物理化学的理论为基础,不同乳液体系(种子乳液、细乳液、Pickering乳液)为研究对象,研究不同聚合物相分离过程中的热力学和动力学规律。主要内容如下：
1.溶剂挥发相分离法制备PS/PMMA Janus微球。设计合成不同分子量PS和PMMA聚合物,研究其在甲苯溶剂挥发过程中,在不同浓度乳化剂溶液中的相分离行为。含有低分子量L-PS和L-PMMA (Mw≈6.0×104 g/mol)的PS/PMMA微球的形态随着OP-10浓度的增加分别为酒窝形、橡子形和半球形；而含有高分子量H-PS和H-PMMA (Mw≈3.3×105 g/mol)的微球形态随着OP-10浓度的增加分别为酒窝形,半球形和雪人形。我们首次研究了分子量大小与乳化剂浓度对界面张力的影响,并通过对铺展系数的分析,研究相分离过程中影响聚合物微球形态的因素。实验结果表明,非离子乳化剂的浓度和聚合物的分子量均对最终Janus微球的形态有较大影响：
2.辐射种子乳液聚合制备雪人形高分子微球。首先利用无皂乳液聚合制备出单分散表面羧基化的PS交联微球,然后通过单体的溶胀过程,再经60Coγ射线辐射引发聚合,由于在聚合时高分子交联种子微球会产生弹性收缩力,将新生成的聚合物挤出,从而形成雪人形聚合物微球。我们详细研究了单体和种子微球的质量溶胀比、溶液pH值、辐射剂量率等因素对雪人形Janus微球形成的影响,发现γ射线辐射种子乳液聚合是常温制备纳米级雪人形微球的有效方法。
3.辐射细乳液聚合制备有机／无机杂化Janus微球。(1)合成部分改性的Si02微球并以此微球为种子,利用辐射细乳液聚合液滴成核机理制备有机／无机杂化Janus微球。改变单体与二氧化硅微球的质量比,可以得到蘑菇形、空鸡蛋形和碗形聚合物Janus微球;(2)合成表面完全改性的Si02微球并以此为种子,进行辐射细乳液聚合,聚合时发生相分离,首次制备出单孔碗形聚合物微球(纳米碗形聚合物壳层底部均有一个小孔)。此结构可以通过单体与种子微球的质量比简单调控,在药物可控释放和催化体系中有潜在的应用前景；(3)利用硅烷偶联剂和有机单体同时在细乳液液滴中发生聚合并产生相分离,制备出有机／无机杂化微球,并研究其形态影响因素。
4.利用磺化交联聚苯乙烯微球为种子进行辐射乳液聚合,制备核桃状多孔聚合物微球。首先制备单分散磺化交联聚苯乙烯微球,由于表面磺酸根基团有良好的亲水性,将其分散于水中后,加入单体并搅拌形成Pickering乳液。在搅拌过程中,磺化聚苯乙烯微球会被单体和水所溶胀,辐射聚合后形成核桃状多孔聚合物微球。磺化程度、单体和磺化微球的质量溶胀比是影响聚合物多孔微球形态的主要因素。另外,银纳米颗粒或其他金属颗粒很容易负载到微球的表面,在催化剂、传感器、太阳能电池和光子晶体领域有广阔的应用前景。
5.利用非聚合的方法制备笼空状多孔聚合物微球。磺化聚苯乙烯微球分散于水和乙醇的混合溶剂中后,加入一定量的正庚烷,加热搅拌一定的时间使磺化聚苯乙烯微球被混合溶剂和正庚烷所溶胀,体系降温后便得到了笼空状多孔聚苯乙烯微球。加热温度和醇水比例是影响多孔聚合物微球形态的主要因素。
The development of polymer particles has great influence on our economy and life. For example, polymer particles have increasingly become an important subject with desirable physical properties applied as coatings, light-sensing materials, bio-medicine, and so on. Since the morphology and size of particles is the key factors to determine potential applications of polymer particles, great interest has been focused on the morphology control of polymer particles. Various of morphological particles have been prepared. Amongst, Janus particles and multihollow polymer particles have received considerable attention over the last decade. Because of its anisotropic surface chemical composition compared with a homogeneous shape, Janus particles have some unique properties. However, due to the asymmetric feature in the particles, the preparation of Janus particles remains challenging for a long time. The final morphology is determined by the competition between thermodynamic and kinetic factors. Multihollow polymer particles have a unique advantage in a low density and high specific surface area. Because the formation mechanism of Janus and multihollow particles involves the interactions between thermodynamic and kinetic factors, the preparation and morphology control of Janus and multihollow polymer particles have great significance not only in enriching the theory in interface and colloid surface science, but also in expanding their practice application fields. This paper aims at the preparation of Janus and multihollow polymer particles with controllable morphologies from different emulsion system (seed emulsion, miniemulsion, Pickering emulsion) based on the interface physical chemistry theory. The main content is as following:
1. The effects of the concentration of polyoxyethylene octylphenyl ether (OP-10) as a nonionic surfactant and the molecular weight of polymers (polystyrene (PS) and poly (methyl methacrylate) (PMMA)) on the morphology of anisotropic PS/PMMA composite particles were investigated. In the case of polymers with lower molecular weight (Mws≈6.0×104 g/mol), the PS/PMMA composite particles have dimple, via acorn, to hemispherical shapes along with the increase of the OP-10 concentration. On the other hand, when the polymers have higher molecular weight (Mw≈3.3×105 g/mol), the morphology of PS/PMMA composite particles changed from dimple, via hemispherical, to snowman-like structure while the concentration of OP-10 was increased. This work first studied on the influence of molecular weight of PS and PMMA on the final morphology of anisotropic PS/PMMA composite particles. Furthermore, thermodynamic analysis was first discussed from the viewpoint of spreading coefficients:The results indicated that both the concentration of OP-10 in aqueous solution and the molecular weight of polymers were very important to the final morphology of anisotropic composite particles.
2. Snowman-like polymer particles were prepared by radiation seed emulsion polymerization. The monodisperse crosslinked PS seed particles with surface modified by carboxyl groups were first prepared by emulsifier free emulsion polymerization. These seed particles were first swollen by monomer, and then the polymerization was induced by 60Co y-ray. During the polymerization, a new phase was pushed out by elastic stress, and the snownman-like polymer particles were formed. The effects of the weight ratio of seed/monomer, pH, and the dose rate were examined in detail. Finally, we found radiation seed emulsion polymerization was an efficient way to produce snownman-like polymer particles at room temperature.
3. Hybrid Janus particles were prepared by radiation miniemulsion polymerization. (1) Novel PS/silica hybrid particles with various morphologies were first prepared byγ-radiation miniemulsion polymerization in the presence of partially modified silica particles. The final morphology depends on the weight ratio of monomer/silica. The PS/silica hybrid Janus particles present mushroom-like, hollow-egg-like and bowl-like structures respectively, with the increase of the weight ratio of monomer/silica. The formation mechanism of the anisotropic PS/silica hybrid particles related with the droplet nucleation of miniemulsion polymerization; (2) In addition, we presented a facile route to prepare a new type of polystyrene nanobowls (there was a small hole at the bottom of each nanobowl) by phase separation during radiation miniemulsion polymerization. The nanostructures could be easily controlled by the weight ratio of monomer/silica. Furthermore, this nanostructure was first discovered, which could have wide potential applications, such as, controlled drug release system and catalytic applications; (3) Furthermore, the hybrid materials were prepared by simultaneous polymerization of silane coupling agent and organic monomers. During the polymerization, phase separation happened and novel morphologies were obtained.
4. Novel walnut-like multihollow polymer particles were first prepared byγ-ray radiation emulsion polymerization using the crosslinked and sulfonated polystyrene spheres (CSP) as the template. The formation process was studied in detail and the morphology of walnut-like multihollow polystyrene particles could be controlled by the content of crosslinking agent, sulfonation time of CSP particles and the weight ratio of monomer/CSP. In addition, bonding Ag nanoparticles onto the surface of walnut multihollow polymer particles was achieved, which could be extended to other noble metal nanoparticles and have wide range of potential applications, such as catalysts, sensors, solar cells and photonic crystals.
5. Cage-like multihollow polymer particles were prepared by non-polymerization method. Sulfonated PS particles were first dispersed into the mixture of water and ethanol, and then a certain amount of heptane was added. The sulfonated PS particles were swollen by the mixture solvent and heptane. Cage-like polymer particles were obtained after cooling down to room temperature. Both the heating temperature and the ratio of water/ethanol were important to the final morphology of multihollow polymer particles.
本论文以乳液聚合制备形态可控Janus微球和多孔聚合物微球为目标,以界面物理化学的理论为基础,不同乳液体系(种子乳液、细乳液、Pickering乳液)为研究对象,研究不同聚合物相分离过程中的热力学和动力学规律。主要内容如下：
1.溶剂挥发相分离法制备PS/PMMA Janus微球。设计合成不同分子量PS和PMMA聚合物,研究其在甲苯溶剂挥发过程中,在不同浓度乳化剂溶液中的相分离行为。含有低分子量L-PS和L-PMMA (Mw≈6.0×104 g/mol)的PS/PMMA微球的形态随着OP-10浓度的增加分别为酒窝形、橡子形和半球形；而含有高分子量H-PS和H-PMMA (Mw≈3.3×105 g/mol)的微球形态随着OP-10浓度的增加分别为酒窝形,半球形和雪人形。我们首次研究了分子量大小与乳化剂浓度对界面张力的影响,并通过对铺展系数的分析,研究相分离过程中影响聚合物微球形态的因素。实验结果表明,非离子乳化剂的浓度和聚合物的分子量均对最终Janus微球的形态有较大影响：
2.辐射种子乳液聚合制备雪人形高分子微球。首先利用无皂乳液聚合制备出单分散表面羧基化的PS交联微球,然后通过单体的溶胀过程,再经60Coγ射线辐射引发聚合,由于在聚合时高分子交联种子微球会产生弹性收缩力,将新生成的聚合物挤出,从而形成雪人形聚合物微球。我们详细研究了单体和种子微球的质量溶胀比、溶液pH值、辐射剂量率等因素对雪人形Janus微球形成的影响,发现γ射线辐射种子乳液聚合是常温制备纳米级雪人形微球的有效方法。
3.辐射细乳液聚合制备有机／无机杂化Janus微球。(1)合成部分改性的Si02微球并以此微球为种子,利用辐射细乳液聚合液滴成核机理制备有机／无机杂化Janus微球。改变单体与二氧化硅微球的质量比,可以得到蘑菇形、空鸡蛋形和碗形聚合物Janus微球;(2)合成表面完全改性的Si02微球并以此为种子,进行辐射细乳液聚合,聚合时发生相分离,首次制备出单孔碗形聚合物微球(纳米碗形聚合物壳层底部均有一个小孔)。此结构可以通过单体与种子微球的质量比简单调控,在药物可控释放和催化体系中有潜在的应用前景；(3)利用硅烷偶联剂和有机单体同时在细乳液液滴中发生聚合并产生相分离,制备出有机／无机杂化微球,并研究其形态影响因素。
4.利用磺化交联聚苯乙烯微球为种子进行辐射乳液聚合,制备核桃状多孔聚合物微球。首先制备单分散磺化交联聚苯乙烯微球,由于表面磺酸根基团有良好的亲水性,将其分散于水中后,加入单体并搅拌形成Pickering乳液。在搅拌过程中,磺化聚苯乙烯微球会被单体和水所溶胀,辐射聚合后形成核桃状多孔聚合物微球。磺化程度、单体和磺化微球的质量溶胀比是影响聚合物多孔微球形态的主要因素。另外,银纳米颗粒或其他金属颗粒很容易负载到微球的表面,在催化剂、传感器、太阳能电池和光子晶体领域有广阔的应用前景。
5.利用非聚合的方法制备笼空状多孔聚合物微球。磺化聚苯乙烯微球分散于水和乙醇的混合溶剂中后,加入一定量的正庚烷,加热搅拌一定的时间使磺化聚苯乙烯微球被混合溶剂和正庚烷所溶胀,体系降温后便得到了笼空状多孔聚苯乙烯微球。加热温度和醇水比例是影响多孔聚合物微球形态的主要因素。
The development of polymer particles has great influence on our economy and life. For example, polymer particles have increasingly become an important subject with desirable physical properties applied as coatings, light-sensing materials, bio-medicine, and so on. Since the morphology and size of particles is the key factors to determine potential applications of polymer particles, great interest has been focused on the morphology control of polymer particles. Various of morphological particles have been prepared. Amongst, Janus particles and multihollow polymer particles have received considerable attention over the last decade. Because of its anisotropic surface chemical composition compared with a homogeneous shape, Janus particles have some unique properties. However, due to the asymmetric feature in the particles, the preparation of Janus particles remains challenging for a long time. The final morphology is determined by the competition between thermodynamic and kinetic factors. Multihollow polymer particles have a unique advantage in a low density and high specific surface area. Because the formation mechanism of Janus and multihollow particles involves the interactions between thermodynamic and kinetic factors, the preparation and morphology control of Janus and multihollow polymer particles have great significance not only in enriching the theory in interface and colloid surface science, but also in expanding their practice application fields. This paper aims at the preparation of Janus and multihollow polymer particles with controllable morphologies from different emulsion system (seed emulsion, miniemulsion, Pickering emulsion) based on the interface physical chemistry theory. The main content is as following:
1. The effects of the concentration of polyoxyethylene octylphenyl ether (OP-10) as a nonionic surfactant and the molecular weight of polymers (polystyrene (PS) and poly (methyl methacrylate) (PMMA)) on the morphology of anisotropic PS/PMMA composite particles were investigated. In the case of polymers with lower molecular weight (Mws≈6.0×104 g/mol), the PS/PMMA composite particles have dimple, via acorn, to hemispherical shapes along with the increase of the OP-10 concentration. On the other hand, when the polymers have higher molecular weight (Mw≈3.3×105 g/mol), the morphology of PS/PMMA composite particles changed from dimple, via hemispherical, to snowman-like structure while the concentration of OP-10 was increased. This work first studied on the influence of molecular weight of PS and PMMA on the final morphology of anisotropic PS/PMMA composite particles. Furthermore, thermodynamic analysis was first discussed from the viewpoint of spreading coefficients:The results indicated that both the concentration of OP-10 in aqueous solution and the molecular weight of polymers were very important to the final morphology of anisotropic composite particles.
2. Snowman-like polymer particles were prepared by radiation seed emulsion polymerization. The monodisperse crosslinked PS seed particles with surface modified by carboxyl groups were first prepared by emulsifier free emulsion polymerization. These seed particles were first swollen by monomer, and then the polymerization was induced by 60Co y-ray. During the polymerization, a new phase was pushed out by elastic stress, and the snownman-like polymer particles were formed. The effects of the weight ratio of seed/monomer, pH, and the dose rate were examined in detail. Finally, we found radiation seed emulsion polymerization was an efficient way to produce snownman-like polymer particles at room temperature.
3. Hybrid Janus particles were prepared by radiation miniemulsion polymerization. (1) Novel PS/silica hybrid particles with various morphologies were first prepared byγ-radiation miniemulsion polymerization in the presence of partially modified silica particles. The final morphology depends on the weight ratio of monomer/silica. The PS/silica hybrid Janus particles present mushroom-like, hollow-egg-like and bowl-like structures respectively, with the increase of the weight ratio of monomer/silica. The formation mechanism of the anisotropic PS/silica hybrid particles related with the droplet nucleation of miniemulsion polymerization; (2) In addition, we presented a facile route to prepare a new type of polystyrene nanobowls (there was a small hole at the bottom of each nanobowl) by phase separation during radiation miniemulsion polymerization. The nanostructures could be easily controlled by the weight ratio of monomer/silica. Furthermore, this nanostructure was first discovered, which could have wide potential applications, such as, controlled drug release system and catalytic applications; (3) Furthermore, the hybrid materials were prepared by simultaneous polymerization of silane coupling agent and organic monomers. During the polymerization, phase separation happened and novel morphologies were obtained.
4. Novel walnut-like multihollow polymer particles were first prepared byγ-ray radiation emulsion polymerization using the crosslinked and sulfonated polystyrene spheres (CSP) as the template. The formation process was studied in detail and the morphology of walnut-like multihollow polystyrene particles could be controlled by the content of crosslinking agent, sulfonation time of CSP particles and the weight ratio of monomer/CSP. In addition, bonding Ag nanoparticles onto the surface of walnut multihollow polymer particles was achieved, which could be extended to other noble metal nanoparticles and have wide range of potential applications, such as catalysts, sensors, solar cells and photonic crystals.
5. Cage-like multihollow polymer particles were prepared by non-polymerization method. Sulfonated PS particles were first dispersed into the mixture of water and ethanol, and then a certain amount of heptane was added. The sulfonated PS particles were swollen by the mixture solvent and heptane. Cage-like polymer particles were obtained after cooling down to room temperature. Both the heating temperature and the ratio of water/ethanol were important to the final morphology of multihollow polymer particles.
引文
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