聚丙烯腈多孔材料的热致相分离法制备及其应用基础研究
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摘要
聚丙烯腈多孔材料具有耐惰性溶剂、耐细菌侵蚀、优良的热和化学稳定性等优点,已被广泛应用于水处理、渗透汽化、酶固定化、生物医药、炭材料等领域。然而,目前其制备手段仍局限于浸没沉淀相转化法,极大地限制了此类材料的进一步发展。作为另一种制备多孔材料的常用方法,热致相分离法以其机理明确和易于控制的优点受到研究者的青睐。本文筛选了一种适合于聚丙烯腈的结晶性稀释剂体系,在此基础上研究了其与聚丙烯腈的热致相分离机理,并用于聚丙烯腈多孔材料的制备、调控及其炭化应用,以期拓展聚丙烯腈的应用范围、丰富热致相分离法的适用领域。具体研究工作内容如下：
基于密度泛函理论计算了聚丙烯腈模型分子与溶剂分子(二甲基砜、二甲基亚砜、碳酸乙烯酯、碳酸丙烯酯、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺)的相互作用。组合浓度、温度相关FTIR和二维红外光谱分析法研究了聚丙烯腈分子链在溶剂中的变化和溶解过程。计算和实验结果表明,二甲基砜与聚丙烯腈的偶极-偶极相互作用最强,二者存在高温溶解、低温分相的热致相分离特点,可选为聚丙烯腈的结晶性稀释剂。
采用DSC、POM、WAXD、SAXS等测试手段研究了聚丙烯腈/二甲基砜体系的结晶行为,绘制了二元相图。该体系发生固-固热致相分离,改变其聚合物浓度制备了具有蜂窝状和柱状孔结构的聚丙烯腈多孔泡沫,其孔结构复刻了二甲基砜在混合体系中的晶体形态。此外,详细探讨了该体系中大尺寸球晶的形态、结构、形成机理。证实了二甲基砜的结晶性及其与聚丙烯腈的偶极-偶极相互作用是形成大球晶的必要条件。
借助热台光学显微镜和DSC等方法研究了聚丙烯腈/二甲基砜/添加剂(丙三醇或聚乙二醇)三元体系的液-液热致相分离过程和液滴生长动力学,绘制了相图。采用预混合加料和一步成型路线,制备了结构多样、孔均匀、孔隙率高、机械性能优良的聚丙烯腈多孔膜。研究结果表明,液-液相分离温度、液滴生长速率、膜孔结构、水通量、机械性能受到聚合物浓度、添加剂含量、聚乙二醇分子量、冷却速率等因素的影响。
采用FTIR、SEM、称重法等方法考察了以聚丙烯腈多孔膜为前体在氧化稳定和炭化过程中聚合物结构、孔形貌、质量损失率等变化。在最佳的升温速率、最高温度、恒温时间等热处理条件下制备了以胞腔孔为主的结构均匀、比表面积大的多孔炭膜。与刚果红、罗丹明B相比,多孔炭膜对甲基橙表现出良好的选择性吸附性和重复使用性能。
Porous polyacrylonitrile (PAN) materials possess excellent resistance to inert solvents and bacterial corrosion, heat and physicochemical stability, so they have been widely used in water treatment, pervaporation, enzyme-immobilization, biological medicine, and carbon materials. However, they are almost made by immersion precipitation phase inversion method, which has limited the further development of PAN. Thermally induced phase separation (TIPS), as another popular way for porous materials, has attracted much attention due to its definite mechanism and ease to control. In this thesis, we selected crystallizable diluent systems for PAN, investigated the specific phase separation mechanism for each PAN/diluent system, and prepared several kinds of porous PAN materials, which were pyrolyzed for porous carbon. This work is expected to expand new applications not only for PAN, but also for TIPS method. Our specific studies are concentrated as follows:
The interactions between PAN and six solvents (dimethyl sulfone (DMSO2), dimethly sulfoxide, ethylene carbonate, propylene carbonate, N,N-dimethyl formamide, N,N-dimethyl acetamide) were discussed by computational calculation based on density functional theories. Moreover, the molecular change and dissolving process of PAN in the solvents were analyzed by concentration-or temperature-dependent FTIR and two-dimensional infrared correlation analysis. The results show that PAN-DMSO2has the strongest dipole-dipole interaction. Moreover, PAN/DMSO2system becomes homogeneous solution at elevated temperature, and undergoes phase separation upon cooling. It means that DMSO2could be an appropriate crystallizable diluent for PAN.
We characterized the crystallization behavior and determined the phase diagram of PAN/DMS02system by using DSC, POM, WAXD, and SXAS methods. The binary system undergoes solid-solid thermally induced phase separation, and PAN foams with honecomb-or channel-like pores can be modulated by varying the polymer composition. It is confirmed that these pores are shaped by DMSO2crystals in the mixtures. On the other hand, giant spherulites came out in PAN/DMS02mixtures, whose morphology, structure and formation mechanism were detailedly discussed. Results indicate that the giant spherulites can be contributed to both the DMSO2crystallization and the dipole-dipole interaction between PAN and DMS02.
Combining optical microscope equipped by hot stage and DSC method, we traced the liquid-liquid phase separation process, studied the droplet growth kinetics, and determined the phase diagrams of PAN/DMS02/additive (glycerol or polyethylene glycol (PEG)) ternary systems. A powder premixing process and one-step molding route were introduced to prepare PAN membranes. The PAN membranes show various structure, uniform pores, high porosity, and excellent mechanical properties. Besides, it exhibits that polymer concentration, additive content, PEG molecular weight, and cooling rate exert influences on the phase separation temperature, the droplet growth rate, pore structure, permeability, and mechanical properties.
To obtain the optimum condition for pyrolysis, PAN membranes were oxidized and carbonized at different conditions, and then their chemical structure, pore morphology, and weight loss were studied by FTIR, SEM, and weighing, respectively. The resultant carbon membranes possess concentrated cellular pores and large specific surface area. Furthermore, they present selective adsorption to methyl orange and good reusability.
基于密度泛函理论计算了聚丙烯腈模型分子与溶剂分子(二甲基砜、二甲基亚砜、碳酸乙烯酯、碳酸丙烯酯、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺)的相互作用。组合浓度、温度相关FTIR和二维红外光谱分析法研究了聚丙烯腈分子链在溶剂中的变化和溶解过程。计算和实验结果表明,二甲基砜与聚丙烯腈的偶极-偶极相互作用最强,二者存在高温溶解、低温分相的热致相分离特点,可选为聚丙烯腈的结晶性稀释剂。
采用DSC、POM、WAXD、SAXS等测试手段研究了聚丙烯腈/二甲基砜体系的结晶行为,绘制了二元相图。该体系发生固-固热致相分离,改变其聚合物浓度制备了具有蜂窝状和柱状孔结构的聚丙烯腈多孔泡沫,其孔结构复刻了二甲基砜在混合体系中的晶体形态。此外,详细探讨了该体系中大尺寸球晶的形态、结构、形成机理。证实了二甲基砜的结晶性及其与聚丙烯腈的偶极-偶极相互作用是形成大球晶的必要条件。
借助热台光学显微镜和DSC等方法研究了聚丙烯腈/二甲基砜/添加剂(丙三醇或聚乙二醇)三元体系的液-液热致相分离过程和液滴生长动力学,绘制了相图。采用预混合加料和一步成型路线,制备了结构多样、孔均匀、孔隙率高、机械性能优良的聚丙烯腈多孔膜。研究结果表明,液-液相分离温度、液滴生长速率、膜孔结构、水通量、机械性能受到聚合物浓度、添加剂含量、聚乙二醇分子量、冷却速率等因素的影响。
采用FTIR、SEM、称重法等方法考察了以聚丙烯腈多孔膜为前体在氧化稳定和炭化过程中聚合物结构、孔形貌、质量损失率等变化。在最佳的升温速率、最高温度、恒温时间等热处理条件下制备了以胞腔孔为主的结构均匀、比表面积大的多孔炭膜。与刚果红、罗丹明B相比,多孔炭膜对甲基橙表现出良好的选择性吸附性和重复使用性能。
Porous polyacrylonitrile (PAN) materials possess excellent resistance to inert solvents and bacterial corrosion, heat and physicochemical stability, so they have been widely used in water treatment, pervaporation, enzyme-immobilization, biological medicine, and carbon materials. However, they are almost made by immersion precipitation phase inversion method, which has limited the further development of PAN. Thermally induced phase separation (TIPS), as another popular way for porous materials, has attracted much attention due to its definite mechanism and ease to control. In this thesis, we selected crystallizable diluent systems for PAN, investigated the specific phase separation mechanism for each PAN/diluent system, and prepared several kinds of porous PAN materials, which were pyrolyzed for porous carbon. This work is expected to expand new applications not only for PAN, but also for TIPS method. Our specific studies are concentrated as follows:
The interactions between PAN and six solvents (dimethyl sulfone (DMSO2), dimethly sulfoxide, ethylene carbonate, propylene carbonate, N,N-dimethyl formamide, N,N-dimethyl acetamide) were discussed by computational calculation based on density functional theories. Moreover, the molecular change and dissolving process of PAN in the solvents were analyzed by concentration-or temperature-dependent FTIR and two-dimensional infrared correlation analysis. The results show that PAN-DMSO2has the strongest dipole-dipole interaction. Moreover, PAN/DMSO2system becomes homogeneous solution at elevated temperature, and undergoes phase separation upon cooling. It means that DMSO2could be an appropriate crystallizable diluent for PAN.
We characterized the crystallization behavior and determined the phase diagram of PAN/DMS02system by using DSC, POM, WAXD, and SXAS methods. The binary system undergoes solid-solid thermally induced phase separation, and PAN foams with honecomb-or channel-like pores can be modulated by varying the polymer composition. It is confirmed that these pores are shaped by DMSO2crystals in the mixtures. On the other hand, giant spherulites came out in PAN/DMS02mixtures, whose morphology, structure and formation mechanism were detailedly discussed. Results indicate that the giant spherulites can be contributed to both the DMSO2crystallization and the dipole-dipole interaction between PAN and DMS02.
Combining optical microscope equipped by hot stage and DSC method, we traced the liquid-liquid phase separation process, studied the droplet growth kinetics, and determined the phase diagrams of PAN/DMS02/additive (glycerol or polyethylene glycol (PEG)) ternary systems. A powder premixing process and one-step molding route were introduced to prepare PAN membranes. The PAN membranes show various structure, uniform pores, high porosity, and excellent mechanical properties. Besides, it exhibits that polymer concentration, additive content, PEG molecular weight, and cooling rate exert influences on the phase separation temperature, the droplet growth rate, pore structure, permeability, and mechanical properties.
To obtain the optimum condition for pyrolysis, PAN membranes were oxidized and carbonized at different conditions, and then their chemical structure, pore morphology, and weight loss were studied by FTIR, SEM, and weighing, respectively. The resultant carbon membranes possess concentrated cellular pores and large specific surface area. Furthermore, they present selective adsorption to methyl orange and good reusability.
引文
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