天然高分子材料在渗透汽化膜分离己内酰胺—水体系中的应用
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摘要
渗透汽化膜分离作为一种新型分离技术,具有其他传统分离技术所不具备的优势：选择性高、操作简便、能耗低、环境友好清洁、过程不受汽液平衡的限制等。本课题选用的分离体系为已内酰胺-水,已内酰胺(CPL)为中国石化股份有限公司巴陵石化分公司引进的由荷兰DSM公司研发的HPO工艺。
已内酰胺作为尼龙-6的单体,是一种重要的有机化工原料。由于少许痕量的水和其他杂质都会影响生产化纤和树脂的质量。因此,对已内酰胺脱水提出了很高的要求。传统的已内酰胺脱水技术是指在工业上采用三效蒸发减压蒸馏装置从水-已内酰胺溶液中结晶制备已内酰胺。这种方法存在中压蒸汽消耗大、热传质效率低、污染物转入第二相、操作费用高等缺点,近年来研究人员开始寻找新的技术来改进或替代CPL水溶液的脱水工艺。
众所周知,渗透汽化膜分离过程最重要也是最核心的环节就是能找到一种合适的膜材料,经过最简单易行的处理,达到最佳的渗透汽化分离效果。加之现在日益恶化的环境问题,也促使人们越来越倾向于寻找一种无毒、可自然环境降解、兼容性好的纯天然高分子膜材料。本文就是基于以上几点,进行了多种膜材料的探讨性试验。
本试验以魔芋葡甘聚糖(KGM)、壳聚糖(CS)为主要的高分子膜材料,结合聚乙烯醇(PVA)和聚丙烯酸(PAA)这两种同样对环境无毒害的传统高分子材料,以戊二醛为交联剂,聚丙烯腈(PAN)超滤膜为底膜,制备了KGM交联膜、KGM-PVA交联共混膜、KGM-CS交联共混膜、CS-PVA交联共混膜以及CS-PAA共混膜。通过红外光谱(FT-IR)、X-射线衍射(XRD)、热分析(TGA, DTG, DSC)和扫描电镜(SEM)等表征手段对聚合物膜的结构形态和物理化学性质进行了表征,分析了聚合物膜材料自身特性与其在CPL/水体系中的溶胀行为和分离性能之间的关系。
KGM交联膜的渗透汽化试验中,探讨了膜中交联剂的含量、进料液温度、进料液组成对渗透汽化膜分离性能的影响。结果表明,交联剂的加入降低了膜在体系中的溶胀度,增加了膜的热稳定性,并且随着交联剂含量的增加,渗透通量减小,分离因子增加；料液温度的升高,增加了膜的通量,减小了分离因子；料液组分的增大,也会使膜的通量减小,分离因子增大。组分渗透通量的自然对数值与操作绝对温度的倒数遵循Arrhenius定律,通过这一经典式子算出的活化能也验证了膜的亲水性质。
对于KGM-PVA交联共混膜,一定范围内膜材料中KGM含量的增加,会造成膜溶胀度与通量的增加,分离因子的降低；KGM-CS交联共混膜在体系内的渗透汽化性质跟KGM-PVA交联共混膜不同：膜内CS含量在一定范围的增加,导致通量的先减小后增大,分离因子则先增大后基本保持不变；CS-PVA交联共混膜膜组分的变化情况也较复杂：随着膜内PVA含量的增大,通量的变化情况是先增大后减小,分离因子正好相反。CS-PAA共混膜在渗透汽化试验中显示的特性为：随着膜内PAA含量的增加,膜耐热性质逐步变差,膜通量在减少,分离因子增加。料液温度的升高和料液组分中CPL含量的减小,都会造成这三组膜的渗透通量的增大和分离因子的减小。
在传质模型的建立上选择了经典的溶解-扩散模型,对已内酰胺-水体系中各种渗透汽化膜的性能进行了综合评价：a)在对总传质系数的模拟中发现,随着温度升高和水含量的增加,水的总传质系数都在不断增大；对于过程总活化能的模拟结果却显示改变组分或交联度的比例时,活化能变化的趋势往往并不是单一的,任一单一组分含量过高往往都会造成渗透活化能上升。印证了通过共混改性的膜比纯聚合物膜更有利于组分的进一步渗透。b)在水组分及已内酰胺组分渗透系数的模拟中发现,随着温度升高和料液中已内酰胺比例的升高,已内酰胺组分渗透系数明显上升,而这些条件变化时水组分的渗透系数变化不大,由此造成膜的选择性会随着温度及料液组成发生明显变化。对实验结果的数据模拟证明了本文中制备的几种渗透汽化膜基本符合溶解-扩散模型,从理论上分析了影响渗透汽化分离过程的因素,为渗透汽化用于已内酰胺-水体系的分离提供了理论依据。
Pervaporation (PV) as a novel separation technology, compared with other traditional methods, has far more effective characters due to high selectivity, simplicity, low energy consumption, environmental-friendly cleaning and breaking through the limits of vapor-liquid equilibrium. The study is based on seperation of solution mixied withε-Caprolactam(CPL) and water, CPL from the HPO technology introduced by Baling Petrochemical Co. Ltd. (SINOPEC, China) from DSM Corporation (Dutch).
s-Caprolactam (CPL), as the monomer of nylon-6, is an important organic chemical material. Since CPL is a very heat sensitive substance and has lower volatility than water. A small trace of water and other impurities will affect the production of fiber and resin.Thus, dehydration of CPL is a demanding profession. Traditional separation techniques, crystallization under a reduced pressure distillation through triple-effect evaporation sets, is often widely adopted by chemical industry in manufacture of CPL. But disadvantages, such as large consumption of steam pressure, low heat transfer coefficient and the pollutants into the second phase, make researchers look for a new or alternative technology to improve the dehydration process in CPL aqueous solution.
As it is well known that a suitable membrane material is the most important technologic process in PV. And then, with as simply treated as possible, people can achieve the best effect of pervaporation. In addition, worsening environmental problems led to an increasing tendency to find the nontoxic, environmental-friendly macromolecule materails. In this dissertation, several materials were discussed.
KGM and chitosan(CS) as the main membrane materials, combined with Poly (vinyl alcohol) (PVA) and Poly(acrylic acid)(PAA), which were also nontoxic, environmental-friendly, cross-linked by Glutaraldehyde, were layed on the (PAN) ultrafiltration membrane chosen as supported substrate layer. Following the methods above, KGM crosslinked membranes, KGM-PVA/PAN, KGM-CS/PAN, CS-PVA/PAN and CS-PAA/PAN were prepared to the separation of CPL/water mixtures. The membranes were characterized by FT-IR, XRD, TGA, DTG, DSC and SEM to analyze the relationships between the structures and characteristics of polymer membranes and swelling behavior and separation performances.
On KGM crosslinked membranes, effects of crosslinking agents loading, feed temperature, feed composition in PV performances, were investigated. The experimental results indicated that with the crosslinking agents loading in the membranes rising, the degree of swelling (D.S) decreased, but the thermal stability of polymer membranes increased. Through evaluating the pervaporation performance, we came to a conclusion that with the increase of crosslinker content, permeation flux decreased and separation factor increased. Temperature of mixtures increasd, flux of membranes increased and the separation factor reduces; CPL concentration in the mixtures increase would also reduced the flux and increased separation factor. The experimental results also showed that the temperature dependence of the pervaporation flux agreed well with the Arrhenius relationship and activation energy ((?)E) is also calculated to verify the nature of the hydrophilic membrane.
The law of KGM-PVA cross-linked blend membranes in the CPL/water system by pervaporation is as follows:to some extent, the more KGM content in the membrane, the more swelling and flux, but the lower separation factor; The law was different in KGM-CS crosslinked blend membranes to that of KGM-PVA blend membranes: content of CS in membrane increasing maked the flux reduce first and then increase, separation factor was increase first and them remained basically unchanged; The law of CS-PVA cross-linked blend membranes are more complex:as CS content increased in membranes, the changes of flux first increased and then decreased, the separation factor is just the opposite; CS-PAA blend membranes in pervaporation experiments show the characteristics as follows:with the increase of the content of PAA in membranes, membrane flux was higher and separation factor was lower. When liquid temperature and water content in liquid components increased, permeation flux of three groups of membranes concerned above increased and the separation factor of them decreased.
The classical solution- diffusion model was chosen as transport model to evaluation the pervaporation performance of the membranes, which were used in our study, for separation of caprolactam - water system:a) through simulating transport coefficients in the model, with the temperature and water content increased, the water transport coefficients were increasing. The results of total activation energy simulated in the model had shown that with the change of ratio in composition or the ratio of crosslinking agents, the change in the trend of activation energy is often not single, and the more single component content, the more activation energy. It is confirmed that multi-component membrane is more conducive to the further penetration than one-component membrane. b)It was shown that with the increase of temperature and CPL content, CPL transport coefficients were increasing but the water transport coefficients didn't change much, resulting that selectivity of membrane changed as the liquid temperature and composition change significantly. The simulation of different membranes in this study proved that the data used in this article of several pervaporation membranes were in line with the classical solution - diffusion model and the results would have a certain guiding significance for description of the membrane structure and choices of pervaporation conditions in industrial applications of pervaporation separation of caprolactam-water system.
已内酰胺作为尼龙-6的单体,是一种重要的有机化工原料。由于少许痕量的水和其他杂质都会影响生产化纤和树脂的质量。因此,对已内酰胺脱水提出了很高的要求。传统的已内酰胺脱水技术是指在工业上采用三效蒸发减压蒸馏装置从水-已内酰胺溶液中结晶制备已内酰胺。这种方法存在中压蒸汽消耗大、热传质效率低、污染物转入第二相、操作费用高等缺点,近年来研究人员开始寻找新的技术来改进或替代CPL水溶液的脱水工艺。
众所周知,渗透汽化膜分离过程最重要也是最核心的环节就是能找到一种合适的膜材料,经过最简单易行的处理,达到最佳的渗透汽化分离效果。加之现在日益恶化的环境问题,也促使人们越来越倾向于寻找一种无毒、可自然环境降解、兼容性好的纯天然高分子膜材料。本文就是基于以上几点,进行了多种膜材料的探讨性试验。
本试验以魔芋葡甘聚糖(KGM)、壳聚糖(CS)为主要的高分子膜材料,结合聚乙烯醇(PVA)和聚丙烯酸(PAA)这两种同样对环境无毒害的传统高分子材料,以戊二醛为交联剂,聚丙烯腈(PAN)超滤膜为底膜,制备了KGM交联膜、KGM-PVA交联共混膜、KGM-CS交联共混膜、CS-PVA交联共混膜以及CS-PAA共混膜。通过红外光谱(FT-IR)、X-射线衍射(XRD)、热分析(TGA, DTG, DSC)和扫描电镜(SEM)等表征手段对聚合物膜的结构形态和物理化学性质进行了表征,分析了聚合物膜材料自身特性与其在CPL/水体系中的溶胀行为和分离性能之间的关系。
KGM交联膜的渗透汽化试验中,探讨了膜中交联剂的含量、进料液温度、进料液组成对渗透汽化膜分离性能的影响。结果表明,交联剂的加入降低了膜在体系中的溶胀度,增加了膜的热稳定性,并且随着交联剂含量的增加,渗透通量减小,分离因子增加；料液温度的升高,增加了膜的通量,减小了分离因子；料液组分的增大,也会使膜的通量减小,分离因子增大。组分渗透通量的自然对数值与操作绝对温度的倒数遵循Arrhenius定律,通过这一经典式子算出的活化能也验证了膜的亲水性质。
对于KGM-PVA交联共混膜,一定范围内膜材料中KGM含量的增加,会造成膜溶胀度与通量的增加,分离因子的降低；KGM-CS交联共混膜在体系内的渗透汽化性质跟KGM-PVA交联共混膜不同：膜内CS含量在一定范围的增加,导致通量的先减小后增大,分离因子则先增大后基本保持不变；CS-PVA交联共混膜膜组分的变化情况也较复杂：随着膜内PVA含量的增大,通量的变化情况是先增大后减小,分离因子正好相反。CS-PAA共混膜在渗透汽化试验中显示的特性为：随着膜内PAA含量的增加,膜耐热性质逐步变差,膜通量在减少,分离因子增加。料液温度的升高和料液组分中CPL含量的减小,都会造成这三组膜的渗透通量的增大和分离因子的减小。
在传质模型的建立上选择了经典的溶解-扩散模型,对已内酰胺-水体系中各种渗透汽化膜的性能进行了综合评价：a)在对总传质系数的模拟中发现,随着温度升高和水含量的增加,水的总传质系数都在不断增大；对于过程总活化能的模拟结果却显示改变组分或交联度的比例时,活化能变化的趋势往往并不是单一的,任一单一组分含量过高往往都会造成渗透活化能上升。印证了通过共混改性的膜比纯聚合物膜更有利于组分的进一步渗透。b)在水组分及已内酰胺组分渗透系数的模拟中发现,随着温度升高和料液中已内酰胺比例的升高,已内酰胺组分渗透系数明显上升,而这些条件变化时水组分的渗透系数变化不大,由此造成膜的选择性会随着温度及料液组成发生明显变化。对实验结果的数据模拟证明了本文中制备的几种渗透汽化膜基本符合溶解-扩散模型,从理论上分析了影响渗透汽化分离过程的因素,为渗透汽化用于已内酰胺-水体系的分离提供了理论依据。
Pervaporation (PV) as a novel separation technology, compared with other traditional methods, has far more effective characters due to high selectivity, simplicity, low energy consumption, environmental-friendly cleaning and breaking through the limits of vapor-liquid equilibrium. The study is based on seperation of solution mixied withε-Caprolactam(CPL) and water, CPL from the HPO technology introduced by Baling Petrochemical Co. Ltd. (SINOPEC, China) from DSM Corporation (Dutch).
s-Caprolactam (CPL), as the monomer of nylon-6, is an important organic chemical material. Since CPL is a very heat sensitive substance and has lower volatility than water. A small trace of water and other impurities will affect the production of fiber and resin.Thus, dehydration of CPL is a demanding profession. Traditional separation techniques, crystallization under a reduced pressure distillation through triple-effect evaporation sets, is often widely adopted by chemical industry in manufacture of CPL. But disadvantages, such as large consumption of steam pressure, low heat transfer coefficient and the pollutants into the second phase, make researchers look for a new or alternative technology to improve the dehydration process in CPL aqueous solution.
As it is well known that a suitable membrane material is the most important technologic process in PV. And then, with as simply treated as possible, people can achieve the best effect of pervaporation. In addition, worsening environmental problems led to an increasing tendency to find the nontoxic, environmental-friendly macromolecule materails. In this dissertation, several materials were discussed.
KGM and chitosan(CS) as the main membrane materials, combined with Poly (vinyl alcohol) (PVA) and Poly(acrylic acid)(PAA), which were also nontoxic, environmental-friendly, cross-linked by Glutaraldehyde, were layed on the (PAN) ultrafiltration membrane chosen as supported substrate layer. Following the methods above, KGM crosslinked membranes, KGM-PVA/PAN, KGM-CS/PAN, CS-PVA/PAN and CS-PAA/PAN were prepared to the separation of CPL/water mixtures. The membranes were characterized by FT-IR, XRD, TGA, DTG, DSC and SEM to analyze the relationships between the structures and characteristics of polymer membranes and swelling behavior and separation performances.
On KGM crosslinked membranes, effects of crosslinking agents loading, feed temperature, feed composition in PV performances, were investigated. The experimental results indicated that with the crosslinking agents loading in the membranes rising, the degree of swelling (D.S) decreased, but the thermal stability of polymer membranes increased. Through evaluating the pervaporation performance, we came to a conclusion that with the increase of crosslinker content, permeation flux decreased and separation factor increased. Temperature of mixtures increasd, flux of membranes increased and the separation factor reduces; CPL concentration in the mixtures increase would also reduced the flux and increased separation factor. The experimental results also showed that the temperature dependence of the pervaporation flux agreed well with the Arrhenius relationship and activation energy ((?)E) is also calculated to verify the nature of the hydrophilic membrane.
The law of KGM-PVA cross-linked blend membranes in the CPL/water system by pervaporation is as follows:to some extent, the more KGM content in the membrane, the more swelling and flux, but the lower separation factor; The law was different in KGM-CS crosslinked blend membranes to that of KGM-PVA blend membranes: content of CS in membrane increasing maked the flux reduce first and then increase, separation factor was increase first and them remained basically unchanged; The law of CS-PVA cross-linked blend membranes are more complex:as CS content increased in membranes, the changes of flux first increased and then decreased, the separation factor is just the opposite; CS-PAA blend membranes in pervaporation experiments show the characteristics as follows:with the increase of the content of PAA in membranes, membrane flux was higher and separation factor was lower. When liquid temperature and water content in liquid components increased, permeation flux of three groups of membranes concerned above increased and the separation factor of them decreased.
The classical solution- diffusion model was chosen as transport model to evaluation the pervaporation performance of the membranes, which were used in our study, for separation of caprolactam - water system:a) through simulating transport coefficients in the model, with the temperature and water content increased, the water transport coefficients were increasing. The results of total activation energy simulated in the model had shown that with the change of ratio in composition or the ratio of crosslinking agents, the change in the trend of activation energy is often not single, and the more single component content, the more activation energy. It is confirmed that multi-component membrane is more conducive to the further penetration than one-component membrane. b)It was shown that with the increase of temperature and CPL content, CPL transport coefficients were increasing but the water transport coefficients didn't change much, resulting that selectivity of membrane changed as the liquid temperature and composition change significantly. The simulation of different membranes in this study proved that the data used in this article of several pervaporation membranes were in line with the classical solution - diffusion model and the results would have a certain guiding significance for description of the membrane structure and choices of pervaporation conditions in industrial applications of pervaporation separation of caprolactam-water system.
引文
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