基于磺化聚苯乙烯模板的各向异性和多孔微球的制备
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摘要
聚合物微球作为一种新型的功能材料,因其在纳米技术、生物技术、电子学和清洁能源领域的广泛应用,近年来一直备受科学界和工业界的关注。各种聚合物微球层出不穷,其中一些产品已经商业化。随着研究的深入,传统的各项同性球型微球,已经不能满足实际应用的需求。在理论研究和应用需求的双重推动下,一些具有特殊化学组成与结构形貌的新型聚合物微球不断涌现,其中最引人注目的是Janus(又称各向异性微球)微球和多孔微球。Janus微球因其在化学组成和结构上具有的不对称结构,可用于构筑新型乳化剂、磁性双功能材料、光学材料和催化剂；而多孔微球相对于中空微球,具有更高的比表面积和更低的密度,在表面学科相关的领域中具有广泛的应用前景。虽然Janus和多孔微球的研究已经取得一定的进展,但是目前这两者的研究各行其道,缺乏相互联系与贯通。如何设计全新的制备路线,将Janus形貌与多孔结构相结合,已成为一个亟待解决的科学问题。
本论文不仅着眼于合成新型多孔或Janus微球,而且将多孔微球的制备方法与Janus形貌相结合,构建同时具有多孔结构的复合Janus微球。全文以具有双亲性的磺化聚苯乙烯(SPS)微球为线索,首先完善辐射种子溶胀聚合法在制备多孔微球方面的研究；随后将此方法扩展至制备具有复杂结构的Janus微球；最后,本论文设计出两种新型聚合方法,即辐射乳液冷冻聚合和辐射种子冷冻聚合,并利用低温条件,合成高分子多孔或Janus微球。全文可分为以下四部分：
一、以交联磺化聚苯乙烯(CSPS)微球为种子,通过辐射种子聚合法制备多孔材料。本章利用亚微米级CSPS微球(200nm)可被溶胀为凝胶状结构这一特点,首先以甲基丙烯酸甲酯(MMA)/水的体系溶胀CSPS微球,借助辐射在室温引发聚合,一步法制备出海绵型多孔材料。其中,纳米级的PMMA粒子相互连接,构成海绵型结构的主体,而亚微米级的CSPS-PMMA共聚微球分散于主体材料之中。氮气吸附结果表明,此多孔材料具有高比表面积(29m2/g)和均一的孔径(60-120nm)。机理研究发现,原微球中可溶性的CSPS链段,是构成海绵型结构的必要条件。进一步研究发现,海绵型多孔材料的形貌可以通过CSPS微球、单体和交联剂的加入量来进行调节。然后,我们将银离子吸附于CSPS微球的磺酸根上,利用高能射线辐射引发聚合,并同时将银离子还原,一步法制备了银负载的海绵型多孔材料。
二：通过不对称溶解溶胀法,合成无机／高分子复合Janus微球。在本章中,我们首先利用种子分散聚合和磺化改性,制备出具有偏心结构的SPS/SiO2复合微球。随后以其为种子微球,利用水/乙醇/正庚烷构成的混合溶剂,通过不对称溶胀溶解过程,制备出两种新型SPS/SiO2复合Janus微球,即海葵型和多孔雪人型。当混合溶剂的配比为5：5：0.1时,可以得到海葵型微球,其形貌为“盛开”的SPS基质簇拥着Si02核的花朵；当正庚烷的加入量翻倍后,则可得到多孔雪人型微球。在溶胀溶解过程中,正庚烷能够溶胀溶解SPS/SiO2微球；水可以与微球表面磺酸根基团作用。而乙醇则可以降低水与正庚烷之间的表面张力,促进溶胀溶解过程的进行。研究发现,混合溶剂的配比、原SPS/SiO2微球的尺寸和磺化取代度,均会对最终产物的形貌产生影响。
三：各向异性多孔复合微球的制备与CdS负载。在第二章的研究基础上,以大直径和低磺化取代度的SPS/SiO2微球为种子,利用水/乙醇/正庚烷构成的混合溶剂,在70度下通过溶胀-渗透过程,成功制备出同时具有各向异性性质和多孔结构的有机/无机复合微球(Anisotropic Porous Composite Microspheres, APC)。电子显微镜和氮气吸附的结果表明,APC微球同时具有大孔和介孔结构,比表面积为11.2m2/g,孔径分布在20-110nm之间。通过对溶胀-渗透过程的跟踪,发现溶胀机理主要包含两个过程：首先SPS很快被正庚烷溶胀溶解,形成介孔结构；随后水和乙醇逐步渗透去微球中,形成大孔结构。在此基础上,我们将制备的APC微球作为载体,通过辐射还原法,将荧光性的CdS纳米粒子锚定于APC微球之上,负载率高达57.6%。
四：辐射冷冻聚合法制备多孔和各向异性微球。我们发展了两种全新的聚合方法：辐射乳液冷冻聚合和辐射种子冷冻聚合。其基本思路是通过速冻过程,将传统O/W体系中的水相固化为冰,使单体液滴成为具有“硬壁”的微反应容器。随后利用高能射线辐射法,在零度以下的环境中引发聚合反应。首先利用辐射细乳液冷冻聚合,制备出微米级多孔聚合物微球。研究发现,其聚合机理类似界面聚合。多孔聚合物微球形貌可以通过外加引发剂和改变辐照时间来进行控制。随后我们以SPS微球作为种子,通过辐射种子冷冻聚合,使用MMA和St为单体,分别得到了水滴型和核桃型的聚合物微球。进一步研究发现,如果升高种子微球的浓度,可以制备出“竹节型”的自组装体。
In recent years, as a novel functional material, polymer microspheres have attracted much attention from both fields of science and industry, due to their widely applications in nanotechnology, biotechnology, electronics, and clean energy. Therefore, various kinds of polymer microspheres have been synthesized, and some of the products have been commercialized. Furthermore, as the study extends, the traditional isotropic spherical microspheres can no longer meet the requirements of practical applications. Under the impulse of dual factors of theoretical research and application demand, novel polymer microspheres, which have special chemical composition and morphology, are springing up. Among them, Janus (anisotropic) and porous microspheres are the most attractive ones. Janus microspheres, with asymmetric structure and/or composition, can be used as amphiphilic surfactants, magnetic bifunctional materials, optical materials, and catalyst. Meanwhile, porous microspheres, which have a higher specific surface area and lower density to the original hollow microspheres, have been widely applied to the field of surface science. Certain progress has been made in the research of Janus and porous microspheres, but there is still little relation between the two useful morphologies. How to design a new synthetic route, which can combine Janus morphology with porous structure, has become a pressing issue.
In this thesis, we not only focus on the preparation of novel porous or Janus microspheres, but also combine them together to fabricate Janus microspheres with porous structure. The amphiphilic sulfonated polystyrene (SPS) microspheres are used as the clue. Firstly, radiation seeded polymerization method is employed to fill the scientific gap in the preparation of porous microspheres. Secondly, this method is extended to the synthesis of the Janus microspheres with complex structure. Finally, a novel kind of polymerization method:radiation freezing emulsion polymerization is designed to synthesize porous and Janus polymer microspheres at the temperature of subzero. This thesis can be divided into the following four parts:
(1) The fabrication of sponge-like porous materials based on swollen crosslinked sulfonated polystyrene (CSPS) microspheres through radiation polymerization. In this chapter, we discovered that submicro-sized CSPS microspheres (200nm) can be swollen into a gel-like structure. Based on this feature, CSPS microspheres are first swollen in methyl methacrylate(MMA)/water system, and then the polymerization of MMA is initiated by y-ray. As a result, a novel kind of sponge-like material, with the porous structure fixed by interlinked PMMA nanoparticles and micron-sized CSPS-PMMA microspheres, is one-step fabricated. The nitrogen adsorption isotherm discloses that the material has a high specific surface area of29m2/g and a narrow pore size distribution of60-120nm. The formation mechanism discloses that the soluble CSPS segments, which contain in the original microspheres, are essential to the sponge-like structure. Subsequently, the final morphology of sponge-like materials can be controlled by the weight ratio of CSPS microspheres, monomer, and crosslinking agent. Finally, the rich sulfonic groups in the CSPS microspheres can be used to adsorb Ag ions. So that after the radiation polymerization and reduction, Ag-loaded sponge-like materials can be one-step fabricated.
(2) Synthesis of polymer/inorganic Janus microspheres via asymmetric swelling-dissolving process. In this chapter, at first, decentered sulfonated polystyrene/SiO2(SPS/SiO2) microspheres are synthesized by the seeded dispersion polymerization and the sulfonated modification. Then two kinds of new anisotropic SPS/SiO2composite microspheres, i.e., actinia-like and porous snowman-like particles are easily fabricated by taking advantages of the asymmetric swelling-dissolving property of the original SPS/SiO2microspheres in a ternary mixing solvent (water/ethanol/heptane). Actinia-like microspheres, with a silica core embedded in a "blooming" SPS matrix, are obtained when the composition of the mixed solvent is5:5:0.1. If the amount of heptane in the mixed solvent is doubled, porous snowman-like microspheres are produced. Moreover, during this process, heptane can swell and dissolve these particles; water can react with the sulfonic groups existing on the surfaces of the SPS/SiO2microspheres; ethanol can reduce the surface tension between water and heptane, and promote the swelling-dissolving process. Finally, we discover that the composition of the ternary mixing solvent, the size and sulfonated degree of the original SPS/SiO2microspheres, will strongly impact on the final morphology of the product.
(3) The fabrication of anisotropic porous composite (APC) microspheres and application as scaffolds of CdS nanoparticles. In this chapter, based on the above research, SPS/SiO2microspheres with large diameter and low sulfonated degree are used as the template to fabricate APC microspheres, via a swelling-osmosis process in a ternary mixing solvent (water/ethanol/heptane) at70℃. Electron microscope images and nitrogen adsorption results disclose that the specific surface area and pore size distribution of the APC microspheres are11.2m2/g and20-110nm respectively, which indicates that the microsphere has hierarchically porous structure. In addition, by tracking the swelling-osmosis process, we find that the mechanism consists of two stages:firstly, the SPS part is quickly swollen and dissolved by heptane, and the mesopores structure is formed; secondly, water and ethanol slowly osmosis into these microspheres, and the macropores structure is obtained. Finally, the prepared APC microspheres are utilized as scaffolds to load fluoresce CdS nanoparticles through y-ray reduction, and the loading rate is up to57.6%.
(4) Synthesis of porous and Janus microspheres via radiation freezing polymerization. In this chapter, we design two new polymerization methods:radiation emulsion freezing polymerization and radiation seeded freezing polymerization. The basic idea is to freeze the aqueous phase of traditional O/W system to the ice, so that the monomer droplets change into micro reactor vessel with "hard wall". Then, y-ray is utilized here to initiate the polymerization at subzero temperature. Micron-sized porous polymer microspheres can be obtained through radiation miniemulsion freezing polymerization. The mechanism is similar to the interfacial polymerization, and the morphology can be controlled by varying the total adsorbed dose and the addition of chemical initiator. Meanwhile, waterdrop-like and walnut-like Janus microspheres can be obtained through radiation seeded freezing polymerization, while the monomer is St and MMA respectively. In addition, if we raise the concentration of SPS microspheres,"bamboo-like" self-assembly can be formed.
本论文不仅着眼于合成新型多孔或Janus微球,而且将多孔微球的制备方法与Janus形貌相结合,构建同时具有多孔结构的复合Janus微球。全文以具有双亲性的磺化聚苯乙烯(SPS)微球为线索,首先完善辐射种子溶胀聚合法在制备多孔微球方面的研究；随后将此方法扩展至制备具有复杂结构的Janus微球；最后,本论文设计出两种新型聚合方法,即辐射乳液冷冻聚合和辐射种子冷冻聚合,并利用低温条件,合成高分子多孔或Janus微球。全文可分为以下四部分：
一、以交联磺化聚苯乙烯(CSPS)微球为种子,通过辐射种子聚合法制备多孔材料。本章利用亚微米级CSPS微球(200nm)可被溶胀为凝胶状结构这一特点,首先以甲基丙烯酸甲酯(MMA)/水的体系溶胀CSPS微球,借助辐射在室温引发聚合,一步法制备出海绵型多孔材料。其中,纳米级的PMMA粒子相互连接,构成海绵型结构的主体,而亚微米级的CSPS-PMMA共聚微球分散于主体材料之中。氮气吸附结果表明,此多孔材料具有高比表面积(29m2/g)和均一的孔径(60-120nm)。机理研究发现,原微球中可溶性的CSPS链段,是构成海绵型结构的必要条件。进一步研究发现,海绵型多孔材料的形貌可以通过CSPS微球、单体和交联剂的加入量来进行调节。然后,我们将银离子吸附于CSPS微球的磺酸根上,利用高能射线辐射引发聚合,并同时将银离子还原,一步法制备了银负载的海绵型多孔材料。
二：通过不对称溶解溶胀法,合成无机／高分子复合Janus微球。在本章中,我们首先利用种子分散聚合和磺化改性,制备出具有偏心结构的SPS/SiO2复合微球。随后以其为种子微球,利用水/乙醇/正庚烷构成的混合溶剂,通过不对称溶胀溶解过程,制备出两种新型SPS/SiO2复合Janus微球,即海葵型和多孔雪人型。当混合溶剂的配比为5：5：0.1时,可以得到海葵型微球,其形貌为“盛开”的SPS基质簇拥着Si02核的花朵；当正庚烷的加入量翻倍后,则可得到多孔雪人型微球。在溶胀溶解过程中,正庚烷能够溶胀溶解SPS/SiO2微球；水可以与微球表面磺酸根基团作用。而乙醇则可以降低水与正庚烷之间的表面张力,促进溶胀溶解过程的进行。研究发现,混合溶剂的配比、原SPS/SiO2微球的尺寸和磺化取代度,均会对最终产物的形貌产生影响。
三：各向异性多孔复合微球的制备与CdS负载。在第二章的研究基础上,以大直径和低磺化取代度的SPS/SiO2微球为种子,利用水/乙醇/正庚烷构成的混合溶剂,在70度下通过溶胀-渗透过程,成功制备出同时具有各向异性性质和多孔结构的有机/无机复合微球(Anisotropic Porous Composite Microspheres, APC)。电子显微镜和氮气吸附的结果表明,APC微球同时具有大孔和介孔结构,比表面积为11.2m2/g,孔径分布在20-110nm之间。通过对溶胀-渗透过程的跟踪,发现溶胀机理主要包含两个过程：首先SPS很快被正庚烷溶胀溶解,形成介孔结构；随后水和乙醇逐步渗透去微球中,形成大孔结构。在此基础上,我们将制备的APC微球作为载体,通过辐射还原法,将荧光性的CdS纳米粒子锚定于APC微球之上,负载率高达57.6%。
四：辐射冷冻聚合法制备多孔和各向异性微球。我们发展了两种全新的聚合方法：辐射乳液冷冻聚合和辐射种子冷冻聚合。其基本思路是通过速冻过程,将传统O/W体系中的水相固化为冰,使单体液滴成为具有“硬壁”的微反应容器。随后利用高能射线辐射法,在零度以下的环境中引发聚合反应。首先利用辐射细乳液冷冻聚合,制备出微米级多孔聚合物微球。研究发现,其聚合机理类似界面聚合。多孔聚合物微球形貌可以通过外加引发剂和改变辐照时间来进行控制。随后我们以SPS微球作为种子,通过辐射种子冷冻聚合,使用MMA和St为单体,分别得到了水滴型和核桃型的聚合物微球。进一步研究发现,如果升高种子微球的浓度,可以制备出“竹节型”的自组装体。
In recent years, as a novel functional material, polymer microspheres have attracted much attention from both fields of science and industry, due to their widely applications in nanotechnology, biotechnology, electronics, and clean energy. Therefore, various kinds of polymer microspheres have been synthesized, and some of the products have been commercialized. Furthermore, as the study extends, the traditional isotropic spherical microspheres can no longer meet the requirements of practical applications. Under the impulse of dual factors of theoretical research and application demand, novel polymer microspheres, which have special chemical composition and morphology, are springing up. Among them, Janus (anisotropic) and porous microspheres are the most attractive ones. Janus microspheres, with asymmetric structure and/or composition, can be used as amphiphilic surfactants, magnetic bifunctional materials, optical materials, and catalyst. Meanwhile, porous microspheres, which have a higher specific surface area and lower density to the original hollow microspheres, have been widely applied to the field of surface science. Certain progress has been made in the research of Janus and porous microspheres, but there is still little relation between the two useful morphologies. How to design a new synthetic route, which can combine Janus morphology with porous structure, has become a pressing issue.
In this thesis, we not only focus on the preparation of novel porous or Janus microspheres, but also combine them together to fabricate Janus microspheres with porous structure. The amphiphilic sulfonated polystyrene (SPS) microspheres are used as the clue. Firstly, radiation seeded polymerization method is employed to fill the scientific gap in the preparation of porous microspheres. Secondly, this method is extended to the synthesis of the Janus microspheres with complex structure. Finally, a novel kind of polymerization method:radiation freezing emulsion polymerization is designed to synthesize porous and Janus polymer microspheres at the temperature of subzero. This thesis can be divided into the following four parts:
(1) The fabrication of sponge-like porous materials based on swollen crosslinked sulfonated polystyrene (CSPS) microspheres through radiation polymerization. In this chapter, we discovered that submicro-sized CSPS microspheres (200nm) can be swollen into a gel-like structure. Based on this feature, CSPS microspheres are first swollen in methyl methacrylate(MMA)/water system, and then the polymerization of MMA is initiated by y-ray. As a result, a novel kind of sponge-like material, with the porous structure fixed by interlinked PMMA nanoparticles and micron-sized CSPS-PMMA microspheres, is one-step fabricated. The nitrogen adsorption isotherm discloses that the material has a high specific surface area of29m2/g and a narrow pore size distribution of60-120nm. The formation mechanism discloses that the soluble CSPS segments, which contain in the original microspheres, are essential to the sponge-like structure. Subsequently, the final morphology of sponge-like materials can be controlled by the weight ratio of CSPS microspheres, monomer, and crosslinking agent. Finally, the rich sulfonic groups in the CSPS microspheres can be used to adsorb Ag ions. So that after the radiation polymerization and reduction, Ag-loaded sponge-like materials can be one-step fabricated.
(2) Synthesis of polymer/inorganic Janus microspheres via asymmetric swelling-dissolving process. In this chapter, at first, decentered sulfonated polystyrene/SiO2(SPS/SiO2) microspheres are synthesized by the seeded dispersion polymerization and the sulfonated modification. Then two kinds of new anisotropic SPS/SiO2composite microspheres, i.e., actinia-like and porous snowman-like particles are easily fabricated by taking advantages of the asymmetric swelling-dissolving property of the original SPS/SiO2microspheres in a ternary mixing solvent (water/ethanol/heptane). Actinia-like microspheres, with a silica core embedded in a "blooming" SPS matrix, are obtained when the composition of the mixed solvent is5:5:0.1. If the amount of heptane in the mixed solvent is doubled, porous snowman-like microspheres are produced. Moreover, during this process, heptane can swell and dissolve these particles; water can react with the sulfonic groups existing on the surfaces of the SPS/SiO2microspheres; ethanol can reduce the surface tension between water and heptane, and promote the swelling-dissolving process. Finally, we discover that the composition of the ternary mixing solvent, the size and sulfonated degree of the original SPS/SiO2microspheres, will strongly impact on the final morphology of the product.
(3) The fabrication of anisotropic porous composite (APC) microspheres and application as scaffolds of CdS nanoparticles. In this chapter, based on the above research, SPS/SiO2microspheres with large diameter and low sulfonated degree are used as the template to fabricate APC microspheres, via a swelling-osmosis process in a ternary mixing solvent (water/ethanol/heptane) at70℃. Electron microscope images and nitrogen adsorption results disclose that the specific surface area and pore size distribution of the APC microspheres are11.2m2/g and20-110nm respectively, which indicates that the microsphere has hierarchically porous structure. In addition, by tracking the swelling-osmosis process, we find that the mechanism consists of two stages:firstly, the SPS part is quickly swollen and dissolved by heptane, and the mesopores structure is formed; secondly, water and ethanol slowly osmosis into these microspheres, and the macropores structure is obtained. Finally, the prepared APC microspheres are utilized as scaffolds to load fluoresce CdS nanoparticles through y-ray reduction, and the loading rate is up to57.6%.
(4) Synthesis of porous and Janus microspheres via radiation freezing polymerization. In this chapter, we design two new polymerization methods:radiation emulsion freezing polymerization and radiation seeded freezing polymerization. The basic idea is to freeze the aqueous phase of traditional O/W system to the ice, so that the monomer droplets change into micro reactor vessel with "hard wall". Then, y-ray is utilized here to initiate the polymerization at subzero temperature. Micron-sized porous polymer microspheres can be obtained through radiation miniemulsion freezing polymerization. The mechanism is similar to the interfacial polymerization, and the morphology can be controlled by varying the total adsorbed dose and the addition of chemical initiator. Meanwhile, waterdrop-like and walnut-like Janus microspheres can be obtained through radiation seeded freezing polymerization, while the monomer is St and MMA respectively. In addition, if we raise the concentration of SPS microspheres,"bamboo-like" self-assembly can be formed.
引文
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