聚合物微凝胶的微流控制备及形貌与功能调控研究
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摘要
近年来,通过微流控技术并结合物理或化学交联可制备形貌可调的聚合物微／纳米水凝胶颗粒。由于该技术可以实现微粒的尺寸和形貌的精确调控,因而被广泛应用于药物载体材料,光子晶体材料,以及纳米复合结构材料的制备等方面。
本文利用微流控技术制备了尺寸均一的海藻酸钠单乳液及复合乳液液滴,通过外场离子交联并调控外场收集液黏度的方法成功地实现了形貌可调微凝胶颗粒的制备。初步探讨了不同形貌微凝胶颗粒的形成机理。其次,利用沉淀聚合法得到的单分散聚-N-异丙基丙烯酰胺纳米凝胶颗粒来构建光子晶体悬浮液。通过双乳液微流控技术与紫外光固化技术制备了以光固化树脂为壳,以纳米凝胶基光子晶体悬浮液为核的光子晶体微球,并对所得到的光子晶体微球的光学性能进行了调控。将所得的光子晶体微球通过离心法制备了Janus结构的光子晶体微球,并探讨了Janus结构与离心条件间的对应关系。本论文包括以下主要内容：
1、利用微流控技术制备了尺寸均一的海藻酸钠单乳液液滴,以含有甘油和离子交联剂乙酸钡(或氯化钙)的水溶液作为收集液,使得到的海藻酸钠乳液液滴通过离子交联得到海藻酸钡(钙)微凝胶颗粒。通过调节收集液中甘油的含量实现对收集液黏度的调节,从而可以得到不同形貌的微凝胶颗粒。通过调节流速及收集液高度等实验参数实现了微凝胶颗粒形貌的调节。不同形貌的微凝胶颗粒来进行药物释放实验结果表明,微凝胶的形貌对于模型药物的释放速率有重要影响。
2、利用微流控技术制备了以硝基甲烷溶液为核,以海藻酸钠水溶液为壳的双乳液液滴,以含不同浓度甘油的交联剂溶液来收集该复合液滴得到了不同形貌的微凝胶颗粒。通过调节复合物液滴的结构,海藻酸钠的浓度以及复合物液滴的内核成分等,系统地研究了最终得到的微凝胶颗粒的形貌变化规律。探讨了不同形貌微凝胶颗粒的形成机理。通过加入量子点及荧光小分子成功地实现了对微凝胶的功能化。
3、利用沉淀聚合法合成了单分散聚-N-异丙基丙烯酰胺基纳米凝胶颗粒的乳液。通过可控挥发自组装得到了浓缩的不同颜色的纳米凝胶悬浮液。以可光聚合的乙氧基化的三羟甲基丙烷三丙烯酸酯作为外部相,以多色的纳米凝胶悬浮液为内部相,通过微流控技术制备了核壳型的不同颜色的光子晶体微球。研究了得到的光子晶体微球的光学性质随着温度改变的变化趋势。通过小分子荧光物质和量子点掺杂的方法实现了对所得到微球的功能化。以上述核壳型光子晶体微球为研究对象,通过离心力诱导微球内部纳米凝胶的聚集而形成Janus超结构微球球。系统地研究了离心温度、离心速度、以及离心时间对于微球内部形貌的影响。同时,研究了在随结构变化过程中,微球的光学性能的变化趋势。通过将树脂层中加入单分散的二氧化硅纳米颗粒,成功实现了双禁带光子晶体微球的制备。以水热还原法合成了尺寸均一的金纳米粒子。通过乳液聚合制备单分散的聚-N-异丙基丙烯酰胺基纳米凝胶颗粒,在聚合反应过程中加入金纳米颗粒的水分散液,得到了以金纳米颗粒为核,以聚-N-异丙基丙烯酰胺为壳的杂化纳米凝胶颗粒。通过调节金纳米颗粒的加入量实现了对杂化纳米凝胶中金颗粒的数目的调节。以该杂化纳米凝胶为构筑单元,通过加热退火法制备了杂化纳米凝胶光子晶体。研究了杂化纳米凝胶的浓度对于微球的光学性质的影响。
Recently, preparation of polymer microparticles with tunable morphology based on polymer micro/nanogels could be achieved by microfluidic technique, combinning physical or chemical cross linking methods. Owning to the finely tunable diameters and morphology of the particles by microfluidic technique, it have been widely applied to the fabrication of drug delivery materials, photonic structured materials and complex structured materials, among others.
Uniform alginate sodium based single emulsion and double emulsion droplets were created through microfluidic technique. By combinning external ionic cross linking and adjustment of external collecting solutions viscosity, we could achieve the regulation of the resultingmicrogels' morphology. Also, the formation mechnism of the different morphology microgels was discussed. By utilization of the precipitation polymerization method, we produce monodisperse poly-N-isopropylacrylamide nanogels which can be used to form colorful photonic crystal dispersions. Core/shell photonic crystal microspheres using photo polymerizable resin as shell, nanogels based photonic crystal dispersions as the core can be prepared by double emulsion microfluidic technique, combinning UV light solidification method. Then, the Janus photonic crystal microspheres based on the core/shell microsphere were formed by a simple centrifugation method. Relatonship between the Janus structure and centrifugation conditions was also investigated. This dissertaion are consisted of several sections as the following:
1. Uniform alginate sodium emulsion droplets were created by microfluidic technique. The emulsion droplets were cross-linked by using aqueous solution of barium acetate(or calcium chloride) and glycerol as the collecting solution. Morphology of the microgels were tuned by tailoring the viscosity of the collecting solution by simply varying the concentrations of glycerol. The morphology variation was measured by optical microscopy and scanning electron microscopy(SEM). The drug release experiment was conducted by using the microgels as the drug delivery carrier, and the result indicate the morphology of the microgels have significant impact on the drug release behavior.
2. Monodisperse double emulsion droplets with alginate sodium solution as the shell and nitromethane solution as the core were created by microfluidic technique. The emulsion droplets were collected by different viscosities of collecting solution and different morphology of microgels were obtained. The resultanting microgels morphology variation trend was systematically investigated. The effects of the double emulsion droplets'sturcture, concentration of alginate sodium solutions and the component of the droplets'core part on the microgels morphology was systematically investigated. The formation mechanism of different morphology microgels was studied.
3. The monodispersed poly-N-isopropylacrylamide nanogel particles were synthesized by precipitation polymerization method. Different colors of nanogel dispersions were obtained by controlling evaperation self assembly method. Different colors of core/shell photonic crystal microsphereswere obtained by empolying the photopolymerizable ethoxylated trimethylolpropane triacrylate (ETPTA) resin as the shell part and the colorful nanogel dispersions as the inner core. The microsphere's optical property variation trend with the temperature change was investigasted. The microspheres were functionlized by addition of small fluorescent molecules and quantum dots (QDs). The Janus supraparticles based on the above mentioned core/shell microspheres were formed through a centrifuge force induced method. The effect of the centrifugation temperature, centrifugation speed and centrifugation time on the microsphere's inner morphologywere systematically investigated. Optical properties variation trend with the microsphere's inner structure change was studied. Double stop band photonic crystal microspherses were successfully prepared by addition of the monodisperse SiO2nanoparticles into the shell part. The monodisperse Au nanoparticles were synthesized by the sodium citrate hydrothermal reduction. Core/shell hybrid nanogel particles with the gold nanoparticles as the core and the poly-N-isopropylacrylamide as the shell were fabricated by the traditional emulsion polymerization method. The amount of the gold nanoparticles inside the hybrid nanogels could be controlled by the addition the gold nanoparticles dispersion's volume.The hybrid nanogels photonic crystal structured microspheres were formed by using the hybrid nanogel dispersions as the building blocks assisted by the annealing method. The effect of hybrid nanogels'concentration on the microspheres'optical property was also investigated.
本文利用微流控技术制备了尺寸均一的海藻酸钠单乳液及复合乳液液滴,通过外场离子交联并调控外场收集液黏度的方法成功地实现了形貌可调微凝胶颗粒的制备。初步探讨了不同形貌微凝胶颗粒的形成机理。其次,利用沉淀聚合法得到的单分散聚-N-异丙基丙烯酰胺纳米凝胶颗粒来构建光子晶体悬浮液。通过双乳液微流控技术与紫外光固化技术制备了以光固化树脂为壳,以纳米凝胶基光子晶体悬浮液为核的光子晶体微球,并对所得到的光子晶体微球的光学性能进行了调控。将所得的光子晶体微球通过离心法制备了Janus结构的光子晶体微球,并探讨了Janus结构与离心条件间的对应关系。本论文包括以下主要内容：
1、利用微流控技术制备了尺寸均一的海藻酸钠单乳液液滴,以含有甘油和离子交联剂乙酸钡(或氯化钙)的水溶液作为收集液,使得到的海藻酸钠乳液液滴通过离子交联得到海藻酸钡(钙)微凝胶颗粒。通过调节收集液中甘油的含量实现对收集液黏度的调节,从而可以得到不同形貌的微凝胶颗粒。通过调节流速及收集液高度等实验参数实现了微凝胶颗粒形貌的调节。不同形貌的微凝胶颗粒来进行药物释放实验结果表明,微凝胶的形貌对于模型药物的释放速率有重要影响。
2、利用微流控技术制备了以硝基甲烷溶液为核,以海藻酸钠水溶液为壳的双乳液液滴,以含不同浓度甘油的交联剂溶液来收集该复合液滴得到了不同形貌的微凝胶颗粒。通过调节复合物液滴的结构,海藻酸钠的浓度以及复合物液滴的内核成分等,系统地研究了最终得到的微凝胶颗粒的形貌变化规律。探讨了不同形貌微凝胶颗粒的形成机理。通过加入量子点及荧光小分子成功地实现了对微凝胶的功能化。
3、利用沉淀聚合法合成了单分散聚-N-异丙基丙烯酰胺基纳米凝胶颗粒的乳液。通过可控挥发自组装得到了浓缩的不同颜色的纳米凝胶悬浮液。以可光聚合的乙氧基化的三羟甲基丙烷三丙烯酸酯作为外部相,以多色的纳米凝胶悬浮液为内部相,通过微流控技术制备了核壳型的不同颜色的光子晶体微球。研究了得到的光子晶体微球的光学性质随着温度改变的变化趋势。通过小分子荧光物质和量子点掺杂的方法实现了对所得到微球的功能化。以上述核壳型光子晶体微球为研究对象,通过离心力诱导微球内部纳米凝胶的聚集而形成Janus超结构微球球。系统地研究了离心温度、离心速度、以及离心时间对于微球内部形貌的影响。同时,研究了在随结构变化过程中,微球的光学性能的变化趋势。通过将树脂层中加入单分散的二氧化硅纳米颗粒,成功实现了双禁带光子晶体微球的制备。以水热还原法合成了尺寸均一的金纳米粒子。通过乳液聚合制备单分散的聚-N-异丙基丙烯酰胺基纳米凝胶颗粒,在聚合反应过程中加入金纳米颗粒的水分散液,得到了以金纳米颗粒为核,以聚-N-异丙基丙烯酰胺为壳的杂化纳米凝胶颗粒。通过调节金纳米颗粒的加入量实现了对杂化纳米凝胶中金颗粒的数目的调节。以该杂化纳米凝胶为构筑单元,通过加热退火法制备了杂化纳米凝胶光子晶体。研究了杂化纳米凝胶的浓度对于微球的光学性质的影响。
Recently, preparation of polymer microparticles with tunable morphology based on polymer micro/nanogels could be achieved by microfluidic technique, combinning physical or chemical cross linking methods. Owning to the finely tunable diameters and morphology of the particles by microfluidic technique, it have been widely applied to the fabrication of drug delivery materials, photonic structured materials and complex structured materials, among others.
Uniform alginate sodium based single emulsion and double emulsion droplets were created through microfluidic technique. By combinning external ionic cross linking and adjustment of external collecting solutions viscosity, we could achieve the regulation of the resultingmicrogels' morphology. Also, the formation mechnism of the different morphology microgels was discussed. By utilization of the precipitation polymerization method, we produce monodisperse poly-N-isopropylacrylamide nanogels which can be used to form colorful photonic crystal dispersions. Core/shell photonic crystal microspheres using photo polymerizable resin as shell, nanogels based photonic crystal dispersions as the core can be prepared by double emulsion microfluidic technique, combinning UV light solidification method. Then, the Janus photonic crystal microspheres based on the core/shell microsphere were formed by a simple centrifugation method. Relatonship between the Janus structure and centrifugation conditions was also investigated. This dissertaion are consisted of several sections as the following:
1. Uniform alginate sodium emulsion droplets were created by microfluidic technique. The emulsion droplets were cross-linked by using aqueous solution of barium acetate(or calcium chloride) and glycerol as the collecting solution. Morphology of the microgels were tuned by tailoring the viscosity of the collecting solution by simply varying the concentrations of glycerol. The morphology variation was measured by optical microscopy and scanning electron microscopy(SEM). The drug release experiment was conducted by using the microgels as the drug delivery carrier, and the result indicate the morphology of the microgels have significant impact on the drug release behavior.
2. Monodisperse double emulsion droplets with alginate sodium solution as the shell and nitromethane solution as the core were created by microfluidic technique. The emulsion droplets were collected by different viscosities of collecting solution and different morphology of microgels were obtained. The resultanting microgels morphology variation trend was systematically investigated. The effects of the double emulsion droplets'sturcture, concentration of alginate sodium solutions and the component of the droplets'core part on the microgels morphology was systematically investigated. The formation mechanism of different morphology microgels was studied.
3. The monodispersed poly-N-isopropylacrylamide nanogel particles were synthesized by precipitation polymerization method. Different colors of nanogel dispersions were obtained by controlling evaperation self assembly method. Different colors of core/shell photonic crystal microsphereswere obtained by empolying the photopolymerizable ethoxylated trimethylolpropane triacrylate (ETPTA) resin as the shell part and the colorful nanogel dispersions as the inner core. The microsphere's optical property variation trend with the temperature change was investigasted. The microspheres were functionlized by addition of small fluorescent molecules and quantum dots (QDs). The Janus supraparticles based on the above mentioned core/shell microspheres were formed through a centrifuge force induced method. The effect of the centrifugation temperature, centrifugation speed and centrifugation time on the microsphere's inner morphologywere systematically investigated. Optical properties variation trend with the microsphere's inner structure change was studied. Double stop band photonic crystal microspherses were successfully prepared by addition of the monodisperse SiO2nanoparticles into the shell part. The monodisperse Au nanoparticles were synthesized by the sodium citrate hydrothermal reduction. Core/shell hybrid nanogel particles with the gold nanoparticles as the core and the poly-N-isopropylacrylamide as the shell were fabricated by the traditional emulsion polymerization method. The amount of the gold nanoparticles inside the hybrid nanogels could be controlled by the addition the gold nanoparticles dispersion's volume.The hybrid nanogels photonic crystal structured microspheres were formed by using the hybrid nanogel dispersions as the building blocks assisted by the annealing method. The effect of hybrid nanogels'concentration on the microspheres'optical property was also investigated.
引文
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