有机相纳滤传递机理的研究
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摘要
纳滤(NF)是介于反渗透(RO)与超滤(UF)之间的一种膜技术,已在水处理、食品、制药、化学工业等诸多领域得到广泛的工业应用。纳滤膜分离技术应用于有机相中时,被称为耐溶剂纳滤(SRNF),它具有传统分离技术(如蒸馏和结晶)不可比拟的优点：无需任何添加剂,分离过程无相变,在较温和的温度条件下操作物质不易失活和降解,在较低压力下就可回收有机溶剂,减轻了环境污染,并且可以显著降低能耗。尽管SRNF技术的优点很多,但是大规模的SRNF过程很少。与传统的水相NF过程相比,SRNF过程由于溶质—溶剂—膜间复杂的相互作用使其传递过程更难以预测,而且,溶剂和溶质通过有机相SRNF膜的传递是受粘性流机理还是扩散机理控制至今尚无定论。现有的传递模型的缺陷,以及缺乏普适性的传递膜型等问题都严重阻碍了SRNF技术的工业应用,因此,探讨有机相中的NF传递机理已经成为当前国内外学者的研究热点。
首先,本文选用SRNF疏水膜(STARMEMTM122膜),在SterlitechHP4750死端流膜分离装置中测定了8种有机溶剂的通量。鉴于溶剂通过SRNF膜的传递与溶剂的性质(如分子量、粘度、摩尔体积和介电常数等)和膜-溶剂间的相互作用(如膜-溶剂溶解度参数差、膜-溶剂表面张力差等)有关,本文采用相关分析方法,对文献中常用的各种溶剂参数和溶剂—膜间相互作用参数与23种溶剂通量数据的相关性进行了研究,发现溶剂的粘度、介电常数、膜—溶剂溶解度参数差和膜—溶剂表面张力差与通量具有较高的相关系数。因此,对于所研究的SRNF膜体系,可以确定这四个参数是影响膜通量的主要因素。
然后,在不完全溶解-扩散模型基础上,考虑这些参数对溶剂通量的影响,建立了一个新的半经验溶剂传递模型。为了验证新模型描述溶剂传递行为的普遍适用性,在多种纯溶剂体系和二元混合溶剂体系中,利用本文测定的通量数据以及文献数据,将新建模型和5种文献模型对溶剂渗透系数的预测性进行对比,发现对于不同膜体系中的全体溶剂,本模型都表现出很高的相关性,并且溶剂渗透系数的实验值与模型计算值的标准误差较小,说明本模型能很好地预测纯溶剂和二元混合溶剂通过疏水SRNF膜的传递过程。这些结果证明,新模型适用于不同疏水膜体系,而且粘性流-扩散机理可以很好地描述溶剂在疏水性耐溶剂纳滤膜中的传递过程。
在NF膜分离过程中,溶质分子的尺寸和形状显著影响着溶质的传递和截留特性。当利用纳滤截留模型去预测膜对溶质分子的截留率时,无论是通过致密膜的溶解—扩散模型还是通过多孔膜的孔流模型,都需要确定一些与溶质的分子尺寸相关的模型参数。现有的分子尺寸参数对于表征溶质在某个NF膜体系中的截留行为是有用的,但并不适于描述大范围膜体系中的溶质传递过程。本文考虑溶剂对溶质分子性质的影响,根据溶质分子的全优化构型计算得到了一个新的分子几何尺寸参数(“计算平均尺寸”),同时利用实验截留数据和文献数据,在不同的有机相和水相NF膜体系中,对新参数描述溶质截留行为的适用性进行了评价。
最后,本文选择了一系列分子量在116～228Da的中性乙酸酯类化合物(包括直链的、带支链的、带环己烷的和芳香乙酸酯)作为溶质,测定了它们在甲醇中通过三种SRNF膜(STARMEMTM122膜、STARMEMTM240膜和MPF-44膜)的截留数据；发现对于具有相近分子量而分子结构不同的溶质分子,直链的传递优于环状的,而带支链的具有最慢的传递速度。为了关联截留率与溶质的分子尺寸和形状之间的关系,将“计算平均尺寸”与8个常用的分子尺寸参数(包括分子量、Stokes直径、当量摩尔直径、经验有效直径、回转半径、“计算分子直径”、“分子长度”以及“分子宽度”)进行了对比分析,发现仅有“计算平均尺寸”与溶质在全部有机相和水相膜体系中的截留率显著相关。并且,通过对有机相和水相中的不同膜体系进行的相关和回归分析,证明了本文提出的“计算平均尺寸”是一个恰当的分子尺寸描述符,可以作为一个普遍适用的模型参数用在溶解—扩散模型中,并且能够很好地描述溶质在有机相和水相体系中的截留行为。
Nanofiltration (NF) is a relatively new membrane technique located between ultrafiltration (UF) and reverse osmosis (RO), and its application has been gaining popularity in water treatment, food, pharmaceutical and chemical industries. Solvent resistant nanofiltration (SRNF) may be considered as an extension to the NF process applied in organic solvent system. The advantages of SRNF are numerous, for example, the process is free of phase transition and the use of additives. Thermal degradation and deactivation can be minimized during the separation process due to the mild operation temperature. Organic solvents can be recycled at low pressure so as to decrease their emission to the environment, and reduce the energy consumption as compared with alternative unit operations like distillation and crystallization. Despite these advantages, the running large-scale SRNF processes are quite limited. Compared to the traditional NF process, the SRNF is less predictable due to the complicated solvent-solute-membrane interactions and the limited knowledge on the membrane transport mechanism, that is, whether transport (both solvent and solute) through SRNF membrane in organic solvent is dominated by viscous flow or diffusion. Present transport models have various limitations and a generalized model is not available, which hindered the practical applications of organic solvent nanofiltration. Therefore, investigation into the transport mechanisms of nanofiltration in organic solvent system is a frontier research area in the world.
Firstly, the permeation of eight organic solvents through hydrophobic SRNF membrane (STARMEMTM122 membrane) has been measured in a Sterlitech HP4750 dead-end filtration cell. Considering the dependence of solvent flux on both solvent properties (such as molecular weight, viscosity, mole volume, and dielectric constant) and membrane-solvent interaction (such as membrane-solvent solubility parameter difference and membrane-solvent surface tension difference), correlation analysis is performed between the flux of 23 solvents and various solvent property parameters and membrane-solvent interaction parameters. Higher correlation coefficient is found between solvent flux and four parameters (solvent viscosity, dielectric constant, membrane-solvent solubility parameter difference and membrane-solvent surface tension difference). For the SRNF membrane systems studied, therefore, the four parameters may be confirmed as the main factors influencing the membrane flux.
Then, taking the effect of the four parameters on solvent flux into account, a new semi-empirical solvent transport model based on the solution-diffusion with imperfection model has been developed, and its universal applicability is demonstrated by describing solvent transport behaviour in a wide range of pure solvent and binary solvent mixtures. The predictive ability of the new model was compared to five existing models by using the experimental results of solvent flux combined with some reference data. For the whole solvents studied, the new model shows a high correlation and minor standard errors between experimental and predicted solvent permeation, implying that the model may well describe the transport behaviour of pure solvent and binary solvent mixtures through hydrophobic SRNF membranes. The results demonstrate the suitability of the new model for the different hydrophobic membrane systems, and show that the viscous-diffusive transport mechanism may well describe the solvent permeation through hydrophobic solvent resistant nanofiltration membrane.
In the NF membrane filtration process, the size and shape of a solute molecule significantly affects its transport and retention characteristics. When estimating the retention of a solute with a predictive model (either solution-diffusion model or pore flow model), some parameters associated with the effective solute size must be known. Present size descriptors could be used to describe solute retention for some membranes, however, they would often not apply equally to a wide range of membranes. In this study, according to the molecular geometry optimization, the influence of solvent on the molecular geometry was considered explicitly for the determination of a new molecular geometric size parameter ("calculated mean size"). The suitability of "calculated mean size" for describing solute retention behaviour is evaluated based on large amount of reference data and statistically compared with those previously reported geometric size descriptors.
Finally, retention data for a series of small and neutral solutes in methanol are measured through three different SRNF membranes. The neutral solutes include linear alkyl-acetates, branched alkyl-acetates, cyclohexyl-acetates and aromatic acetates with molecular weight ranging from 116 to 228 g mol-1. For those solutes with approximately the same MW but different molecular shape, all three membranes show preferential transport of straight-chained solutes over cyclic solutes, while the branched solutes revealed the lowest permeability. In order to correlate the retention with the molecule size and shape of the solutes, eight traditional molecular size descriptors (MW, the Stokes diameter, the equivalent molar diameter, the empirical effective diameter, radius of gyration, "calculated molecular diameter", "molecular width", and "molecular length"), were compared to "calculated mean size". A strong correlation between molecular size and solute retention across a range of membranes in aqueous and non-aqueous systems was only found with "calculated mean size". In addition, correlation and regression analyses for various NF membranes in aqueous and non-aqueous systems were performed. The results justified "calculated mean size" as the most characteristic size parameter that can suitably discriminate the solutes molecules, and as a universal model parameter of the solution-diffusion model for well describing solute retention behaviour in aqueous and non-aqueous systems.
首先,本文选用SRNF疏水膜(STARMEMTM122膜),在SterlitechHP4750死端流膜分离装置中测定了8种有机溶剂的通量。鉴于溶剂通过SRNF膜的传递与溶剂的性质(如分子量、粘度、摩尔体积和介电常数等)和膜-溶剂间的相互作用(如膜-溶剂溶解度参数差、膜-溶剂表面张力差等)有关,本文采用相关分析方法,对文献中常用的各种溶剂参数和溶剂—膜间相互作用参数与23种溶剂通量数据的相关性进行了研究,发现溶剂的粘度、介电常数、膜—溶剂溶解度参数差和膜—溶剂表面张力差与通量具有较高的相关系数。因此,对于所研究的SRNF膜体系,可以确定这四个参数是影响膜通量的主要因素。
然后,在不完全溶解-扩散模型基础上,考虑这些参数对溶剂通量的影响,建立了一个新的半经验溶剂传递模型。为了验证新模型描述溶剂传递行为的普遍适用性,在多种纯溶剂体系和二元混合溶剂体系中,利用本文测定的通量数据以及文献数据,将新建模型和5种文献模型对溶剂渗透系数的预测性进行对比,发现对于不同膜体系中的全体溶剂,本模型都表现出很高的相关性,并且溶剂渗透系数的实验值与模型计算值的标准误差较小,说明本模型能很好地预测纯溶剂和二元混合溶剂通过疏水SRNF膜的传递过程。这些结果证明,新模型适用于不同疏水膜体系,而且粘性流-扩散机理可以很好地描述溶剂在疏水性耐溶剂纳滤膜中的传递过程。
在NF膜分离过程中,溶质分子的尺寸和形状显著影响着溶质的传递和截留特性。当利用纳滤截留模型去预测膜对溶质分子的截留率时,无论是通过致密膜的溶解—扩散模型还是通过多孔膜的孔流模型,都需要确定一些与溶质的分子尺寸相关的模型参数。现有的分子尺寸参数对于表征溶质在某个NF膜体系中的截留行为是有用的,但并不适于描述大范围膜体系中的溶质传递过程。本文考虑溶剂对溶质分子性质的影响,根据溶质分子的全优化构型计算得到了一个新的分子几何尺寸参数(“计算平均尺寸”),同时利用实验截留数据和文献数据,在不同的有机相和水相NF膜体系中,对新参数描述溶质截留行为的适用性进行了评价。
最后,本文选择了一系列分子量在116～228Da的中性乙酸酯类化合物(包括直链的、带支链的、带环己烷的和芳香乙酸酯)作为溶质,测定了它们在甲醇中通过三种SRNF膜(STARMEMTM122膜、STARMEMTM240膜和MPF-44膜)的截留数据；发现对于具有相近分子量而分子结构不同的溶质分子,直链的传递优于环状的,而带支链的具有最慢的传递速度。为了关联截留率与溶质的分子尺寸和形状之间的关系,将“计算平均尺寸”与8个常用的分子尺寸参数(包括分子量、Stokes直径、当量摩尔直径、经验有效直径、回转半径、“计算分子直径”、“分子长度”以及“分子宽度”)进行了对比分析,发现仅有“计算平均尺寸”与溶质在全部有机相和水相膜体系中的截留率显著相关。并且,通过对有机相和水相中的不同膜体系进行的相关和回归分析,证明了本文提出的“计算平均尺寸”是一个恰当的分子尺寸描述符,可以作为一个普遍适用的模型参数用在溶解—扩散模型中,并且能够很好地描述溶质在有机相和水相体系中的截留行为。
Nanofiltration (NF) is a relatively new membrane technique located between ultrafiltration (UF) and reverse osmosis (RO), and its application has been gaining popularity in water treatment, food, pharmaceutical and chemical industries. Solvent resistant nanofiltration (SRNF) may be considered as an extension to the NF process applied in organic solvent system. The advantages of SRNF are numerous, for example, the process is free of phase transition and the use of additives. Thermal degradation and deactivation can be minimized during the separation process due to the mild operation temperature. Organic solvents can be recycled at low pressure so as to decrease their emission to the environment, and reduce the energy consumption as compared with alternative unit operations like distillation and crystallization. Despite these advantages, the running large-scale SRNF processes are quite limited. Compared to the traditional NF process, the SRNF is less predictable due to the complicated solvent-solute-membrane interactions and the limited knowledge on the membrane transport mechanism, that is, whether transport (both solvent and solute) through SRNF membrane in organic solvent is dominated by viscous flow or diffusion. Present transport models have various limitations and a generalized model is not available, which hindered the practical applications of organic solvent nanofiltration. Therefore, investigation into the transport mechanisms of nanofiltration in organic solvent system is a frontier research area in the world.
Firstly, the permeation of eight organic solvents through hydrophobic SRNF membrane (STARMEMTM122 membrane) has been measured in a Sterlitech HP4750 dead-end filtration cell. Considering the dependence of solvent flux on both solvent properties (such as molecular weight, viscosity, mole volume, and dielectric constant) and membrane-solvent interaction (such as membrane-solvent solubility parameter difference and membrane-solvent surface tension difference), correlation analysis is performed between the flux of 23 solvents and various solvent property parameters and membrane-solvent interaction parameters. Higher correlation coefficient is found between solvent flux and four parameters (solvent viscosity, dielectric constant, membrane-solvent solubility parameter difference and membrane-solvent surface tension difference). For the SRNF membrane systems studied, therefore, the four parameters may be confirmed as the main factors influencing the membrane flux.
Then, taking the effect of the four parameters on solvent flux into account, a new semi-empirical solvent transport model based on the solution-diffusion with imperfection model has been developed, and its universal applicability is demonstrated by describing solvent transport behaviour in a wide range of pure solvent and binary solvent mixtures. The predictive ability of the new model was compared to five existing models by using the experimental results of solvent flux combined with some reference data. For the whole solvents studied, the new model shows a high correlation and minor standard errors between experimental and predicted solvent permeation, implying that the model may well describe the transport behaviour of pure solvent and binary solvent mixtures through hydrophobic SRNF membranes. The results demonstrate the suitability of the new model for the different hydrophobic membrane systems, and show that the viscous-diffusive transport mechanism may well describe the solvent permeation through hydrophobic solvent resistant nanofiltration membrane.
In the NF membrane filtration process, the size and shape of a solute molecule significantly affects its transport and retention characteristics. When estimating the retention of a solute with a predictive model (either solution-diffusion model or pore flow model), some parameters associated with the effective solute size must be known. Present size descriptors could be used to describe solute retention for some membranes, however, they would often not apply equally to a wide range of membranes. In this study, according to the molecular geometry optimization, the influence of solvent on the molecular geometry was considered explicitly for the determination of a new molecular geometric size parameter ("calculated mean size"). The suitability of "calculated mean size" for describing solute retention behaviour is evaluated based on large amount of reference data and statistically compared with those previously reported geometric size descriptors.
Finally, retention data for a series of small and neutral solutes in methanol are measured through three different SRNF membranes. The neutral solutes include linear alkyl-acetates, branched alkyl-acetates, cyclohexyl-acetates and aromatic acetates with molecular weight ranging from 116 to 228 g mol-1. For those solutes with approximately the same MW but different molecular shape, all three membranes show preferential transport of straight-chained solutes over cyclic solutes, while the branched solutes revealed the lowest permeability. In order to correlate the retention with the molecule size and shape of the solutes, eight traditional molecular size descriptors (MW, the Stokes diameter, the equivalent molar diameter, the empirical effective diameter, radius of gyration, "calculated molecular diameter", "molecular width", and "molecular length"), were compared to "calculated mean size". A strong correlation between molecular size and solute retention across a range of membranes in aqueous and non-aqueous systems was only found with "calculated mean size". In addition, correlation and regression analyses for various NF membranes in aqueous and non-aqueous systems were performed. The results justified "calculated mean size" as the most characteristic size parameter that can suitably discriminate the solutes molecules, and as a universal model parameter of the solution-diffusion model for well describing solute retention behaviour in aqueous and non-aqueous systems.
引文
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