新颖形态功能高分子材料的设计、合成与性能研究
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摘要
本文旨在新颖形态(空核／孔壳结构、光控交联胶束以及有序微凝胶晶态结构)功能高分子材料的设计、合成及其在环境、医药等领域的应用研究。
随着功能高分子材料在抗癌药物载体和环境友好等应用方面的不断发展,越来越多的新颖形态功能高分子材料走进人们的视野。论文系统总结、评述了特殊形态的功能高分子材料的设计、制备及其相关应用进展；开发了空核/孔壳结构聚砜微球,并应用于油水分离方面的研究；设计合成了两种光控释药的交联胶束载体(葡聚糖-血红素,聚乙烯醇-血红素)以实现化疗、光动力学疗法相结合的多重抗癌作用；合成了有序结构的晶态聚丙烯酸微凝胶；利用现代仪器技术,分析和表征不同聚合物材料的合成及其在乳液体系下的各种新颖形态的形成情况。
本论文的主要内容如下：
1.利用溶剂蒸发法制备出粒径均一的孔状聚砜微球。通过对乳化剂类型、反应温度、乳液类型等实验参数的调控,掌握多孔聚砜微球的形态控制因素。实验结果表明所选用的乳化剂类型对孔状聚砜微球的形成起着至关重要的作用,利用油酸作为乳化剂可以得到空核／孔壳结构聚砜微球。接触角测试结果表明,不同形貌的聚砜微球的疏水亲油性能并没有明显的改变。然而在油水分离上却存在一定差距,其中空核／孔壳结构聚砜微球具有最佳吸油能力,究其原因在于这种特殊的空核／孔壳结构不仅有利于漂浮性能,更可以作为油的储仓,吸附大量漂浮在水面的油,其吸油能力达到了33.6g/g,是原始聚砜粉末的44.8倍。该聚砜微球制备简单,并且由于其特殊的孔隙结构有望在油水分离、环境净化方面得到广泛应用。
2.设计开发了基于血红素中双键交联的葡聚糖(聚乙烯醇)胶束,用于化疗药物5-氟尿嘧啶的装载和光控释放,以及与光动力学疗法的协同抗肿瘤作用。交联后的胶束稳定性增强,对高度稀释能保持稳定,有望在体内安全输运。体外实验表明交联的载5-氟尿嘧啶的胶束对5-氟尿嘧啶的释放具有光响应性：对于葡聚糖-血红素交联胶束,在非光照情况下383分钟内只有约15%的5-氟尿嘧啶释放出来,在光照下,383分钟后释放出92%的5-氟尿嘧啶；而对于聚乙烯醇-血红素交联胶束,其稳定性提高,在光照下360分钟后释放出36%的5-氟尿嘧啶。采用1,3-二苯基异苯并呋喃作为探针分子,通过紫外光谱检测表明所制备的载药交联胶束在光照下也能产生单线态氧,源于交联胶束中血红素的光敏性。MTT和荧光显微镜观察结果表明,激光照射下载药交联胶束具有多重抗肿瘤效果。该葡聚糖(聚乙烯醇)衍生物交联胶束制备简单,具有良好的降解性、生物相容性和潜在的多重抗癌作用,在抗癌领域具有良好的应用前景。
3.利用表面活性剂既可以作为聚合物结晶的成核剂,又可以在聚合反应过程中充当乳化剂的特性,设计实验方案使乳液聚合过程中的表面活性剂(十二烷基硫酸钠)充当成核剂,在聚合反应过程中实现结晶过程。实验结果表明简单乳液聚合方法可以得到晶态聚丙烯酸微凝胶晶体。在聚合反应过程中通过乳化剂与聚合物之间的作用,使其在聚合过程中自组装形成晶态结构。在此基础上,探讨反应条件(如反应温度、破乳剂NaCl加入量等)对聚丙烯酸微凝胶结晶性的影响。研究了结晶性聚丙烯酸微凝胶的力学性能,其杨氏模量为非晶态的7.8倍。这表明晶态结构的形成有利于材料力学性能的改善。
The studies on design, synthesis of functional polymer with novel morphology (hollow core/pore shell structure, cross-linked micelles as photo-responsive and microcrystalline gels) and their applications in environment, medicine and other fields are the main aims of this disfucation.
With the constant development of functional polymer on biocompatibility and environmental friendliness, more and more functional polymer with novel morphology come into people's field of vision. The research progress of design, synthesis and applications of them are reviewed in this paper; Polysulfone (PSF) microspheres with hollow core/pore shell structure are developed and applied in oil-water sparation; Two kinds of cross-linking micelles (dextran-hemin, polyvinyl alcohol-hemin) as photo-responsive release drugs carriers, combining chemotherapy and photodynamic therapy for multimodal cancer therapy, are designed and synthesized; The microcrystalline polyacrylic acid gels are synthesized by emulsion polymerization. The modern instrument technology is used for characterizing the synthesis and varies of structure of polymers in the emulsion system.
The main contents and results of the work are as follows:
1. The porous polysulfone (PSF) microspheres are prepared by using emulsion solvent evaporation technique. The morphology can be controlled by varying the type of surfactant, the preparation temperature and the emulsion type from W/O to either O/W or multiple W/O/W. The results demonstrate that the type of surfactant is the important point in to the morphology. The PSF microspheres with hollow core/pore shell structure can be obtained using oleic acid as surfactant. Contact angles test show that there is no obvious difference among all kinds of microspheres, but a considerable gap in the oil-water separation. The PSF microspheres with hollow core/pore shell structure have higher absorption capacity, causing by floatation performance and high porosity and appropriate void size of sorbent provided large amounts of storage volume for oil, acting as an oil reservoir, which was the key for the high adsorption capacity. The separation efficiency of the porous PSF microspheres is33.6g/g, which is44.8times higher than that of the pristine PSF powder. The PSF microspheres possess simple and excellent pore structure, which is expected to be widely used in oil-water separation.
2. Double bond in hemin-crosslinked dextran (polyvinyl alcohol) micelles were designed for photo-triggered release of5-fluorouracil (5FU), an antitumor drug. The crosslinked micelles were stable even high dilution, In vitro release studies showed light-responsive release of5FU. For the cross-linking micelles of dextran-hemin, only15%5FU was released from dextran-hemin, after383min in10mM PB.92%5FU was released in383min in laser irradiation under the same conditions. However, for the cross-linking micelles of polyvinyl alcohol-hemin, the stability become higher,36%5FU was released in360min in laser irradiation. Using1,3-Diphenylisobenzofuran (DPBF) as a chemical trapping agent, the as-prepared crosslinked micelles can generate singlet oxygen effectively through ultravioler spectroscopy detecting device, this is due to photosensitive of heme. The photo-responsive5-FU loaded cross-linked micelles combining chemotherapy and photodynamic therapy observed by MTT and fluorescence microscopy. These novel nano-vehicles have the advantages of convenient preparation, favorable biocompatibility, degradability, and effective antitumor activity with promising applications.
3. Surfactant has dual roles of polymer crystallization nucleating agent and emulsifiers in the polymerization process. Experiment design will be in the process of emulsion polymerization. In this system, emulsion (sodium dodecyl sulfate) acts as a nucleating agent. Experimental results show that microcrystalline polyacrylic acid gels can be obtained through a simple emulsion polymerization method. In the process of polymerization, proper emulsifier holds the adjacent molecules together, making PAA microgels growth along crystallographically possible reactive directions. The experimental conditions influence the crystallinity and morphology of PAA microgels. It should be noted that the Young's modulus of microcrystalline polyacrylic acid gels is7.8times of amorphous gel. This indicates that the synthesis of microcrystalline PAA gles is conducive to improve mechanical properties.
随着功能高分子材料在抗癌药物载体和环境友好等应用方面的不断发展,越来越多的新颖形态功能高分子材料走进人们的视野。论文系统总结、评述了特殊形态的功能高分子材料的设计、制备及其相关应用进展；开发了空核/孔壳结构聚砜微球,并应用于油水分离方面的研究；设计合成了两种光控释药的交联胶束载体(葡聚糖-血红素,聚乙烯醇-血红素)以实现化疗、光动力学疗法相结合的多重抗癌作用；合成了有序结构的晶态聚丙烯酸微凝胶；利用现代仪器技术,分析和表征不同聚合物材料的合成及其在乳液体系下的各种新颖形态的形成情况。
本论文的主要内容如下：
1.利用溶剂蒸发法制备出粒径均一的孔状聚砜微球。通过对乳化剂类型、反应温度、乳液类型等实验参数的调控,掌握多孔聚砜微球的形态控制因素。实验结果表明所选用的乳化剂类型对孔状聚砜微球的形成起着至关重要的作用,利用油酸作为乳化剂可以得到空核／孔壳结构聚砜微球。接触角测试结果表明,不同形貌的聚砜微球的疏水亲油性能并没有明显的改变。然而在油水分离上却存在一定差距,其中空核／孔壳结构聚砜微球具有最佳吸油能力,究其原因在于这种特殊的空核／孔壳结构不仅有利于漂浮性能,更可以作为油的储仓,吸附大量漂浮在水面的油,其吸油能力达到了33.6g/g,是原始聚砜粉末的44.8倍。该聚砜微球制备简单,并且由于其特殊的孔隙结构有望在油水分离、环境净化方面得到广泛应用。
2.设计开发了基于血红素中双键交联的葡聚糖(聚乙烯醇)胶束,用于化疗药物5-氟尿嘧啶的装载和光控释放,以及与光动力学疗法的协同抗肿瘤作用。交联后的胶束稳定性增强,对高度稀释能保持稳定,有望在体内安全输运。体外实验表明交联的载5-氟尿嘧啶的胶束对5-氟尿嘧啶的释放具有光响应性：对于葡聚糖-血红素交联胶束,在非光照情况下383分钟内只有约15%的5-氟尿嘧啶释放出来,在光照下,383分钟后释放出92%的5-氟尿嘧啶；而对于聚乙烯醇-血红素交联胶束,其稳定性提高,在光照下360分钟后释放出36%的5-氟尿嘧啶。采用1,3-二苯基异苯并呋喃作为探针分子,通过紫外光谱检测表明所制备的载药交联胶束在光照下也能产生单线态氧,源于交联胶束中血红素的光敏性。MTT和荧光显微镜观察结果表明,激光照射下载药交联胶束具有多重抗肿瘤效果。该葡聚糖(聚乙烯醇)衍生物交联胶束制备简单,具有良好的降解性、生物相容性和潜在的多重抗癌作用,在抗癌领域具有良好的应用前景。
3.利用表面活性剂既可以作为聚合物结晶的成核剂,又可以在聚合反应过程中充当乳化剂的特性,设计实验方案使乳液聚合过程中的表面活性剂(十二烷基硫酸钠)充当成核剂,在聚合反应过程中实现结晶过程。实验结果表明简单乳液聚合方法可以得到晶态聚丙烯酸微凝胶晶体。在聚合反应过程中通过乳化剂与聚合物之间的作用,使其在聚合过程中自组装形成晶态结构。在此基础上,探讨反应条件(如反应温度、破乳剂NaCl加入量等)对聚丙烯酸微凝胶结晶性的影响。研究了结晶性聚丙烯酸微凝胶的力学性能,其杨氏模量为非晶态的7.8倍。这表明晶态结构的形成有利于材料力学性能的改善。
The studies on design, synthesis of functional polymer with novel morphology (hollow core/pore shell structure, cross-linked micelles as photo-responsive and microcrystalline gels) and their applications in environment, medicine and other fields are the main aims of this disfucation.
With the constant development of functional polymer on biocompatibility and environmental friendliness, more and more functional polymer with novel morphology come into people's field of vision. The research progress of design, synthesis and applications of them are reviewed in this paper; Polysulfone (PSF) microspheres with hollow core/pore shell structure are developed and applied in oil-water sparation; Two kinds of cross-linking micelles (dextran-hemin, polyvinyl alcohol-hemin) as photo-responsive release drugs carriers, combining chemotherapy and photodynamic therapy for multimodal cancer therapy, are designed and synthesized; The microcrystalline polyacrylic acid gels are synthesized by emulsion polymerization. The modern instrument technology is used for characterizing the synthesis and varies of structure of polymers in the emulsion system.
The main contents and results of the work are as follows:
1. The porous polysulfone (PSF) microspheres are prepared by using emulsion solvent evaporation technique. The morphology can be controlled by varying the type of surfactant, the preparation temperature and the emulsion type from W/O to either O/W or multiple W/O/W. The results demonstrate that the type of surfactant is the important point in to the morphology. The PSF microspheres with hollow core/pore shell structure can be obtained using oleic acid as surfactant. Contact angles test show that there is no obvious difference among all kinds of microspheres, but a considerable gap in the oil-water separation. The PSF microspheres with hollow core/pore shell structure have higher absorption capacity, causing by floatation performance and high porosity and appropriate void size of sorbent provided large amounts of storage volume for oil, acting as an oil reservoir, which was the key for the high adsorption capacity. The separation efficiency of the porous PSF microspheres is33.6g/g, which is44.8times higher than that of the pristine PSF powder. The PSF microspheres possess simple and excellent pore structure, which is expected to be widely used in oil-water separation.
2. Double bond in hemin-crosslinked dextran (polyvinyl alcohol) micelles were designed for photo-triggered release of5-fluorouracil (5FU), an antitumor drug. The crosslinked micelles were stable even high dilution, In vitro release studies showed light-responsive release of5FU. For the cross-linking micelles of dextran-hemin, only15%5FU was released from dextran-hemin, after383min in10mM PB.92%5FU was released in383min in laser irradiation under the same conditions. However, for the cross-linking micelles of polyvinyl alcohol-hemin, the stability become higher,36%5FU was released in360min in laser irradiation. Using1,3-Diphenylisobenzofuran (DPBF) as a chemical trapping agent, the as-prepared crosslinked micelles can generate singlet oxygen effectively through ultravioler spectroscopy detecting device, this is due to photosensitive of heme. The photo-responsive5-FU loaded cross-linked micelles combining chemotherapy and photodynamic therapy observed by MTT and fluorescence microscopy. These novel nano-vehicles have the advantages of convenient preparation, favorable biocompatibility, degradability, and effective antitumor activity with promising applications.
3. Surfactant has dual roles of polymer crystallization nucleating agent and emulsifiers in the polymerization process. Experiment design will be in the process of emulsion polymerization. In this system, emulsion (sodium dodecyl sulfate) acts as a nucleating agent. Experimental results show that microcrystalline polyacrylic acid gels can be obtained through a simple emulsion polymerization method. In the process of polymerization, proper emulsifier holds the adjacent molecules together, making PAA microgels growth along crystallographically possible reactive directions. The experimental conditions influence the crystallinity and morphology of PAA microgels. It should be noted that the Young's modulus of microcrystalline polyacrylic acid gels is7.8times of amorphous gel. This indicates that the synthesis of microcrystalline PAA gles is conducive to improve mechanical properties.
引文
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