基于PTFE微粉和PDMS材料渗透汽化膜制备及其性能表征
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摘要
目前,生产废水及生活废水中常含有挥发性有机物(VOC)。由于其毒性大、可生化性差,因此治理难度较大,危害环境安全。与此同时,VOC是重要的化工原料,其回收有重要的经济价值。因此,VOC的治理一直是近几年研究的热点。渗透汽化(PV)膜分离法由于具有相变质量小、效率高、能耗低、设备简单及工艺放大效应小等优点,逐渐在环境保护中得到应用。本文利用聚四氟乙烯(PTFE)微粉和硅橡胶(PDMS)膜材料,制备了几种PTFE-PDMS共混渗透汽化膜,研究了PTFE-PDMS膜结构、溶解-扩散性能、渗透汽化低浓度氯仿或乙醇水溶液性能及渗透汽化过程的传质阻力等。研究结果如下：
首先,制各了不同组成的PTFE-PDMS渗透汽化平板膜,采用SEM-EDAX、FT-IR、 XRD、DSC、TG和水接触角等方法,研究了PTFE-PDMS渗透汽化膜结构及性能,考察了PTFE-PDMS渗透汽化膜的溶胀和渗透汽化性能。结果表明：PTFE-PDMS渗透汽化膜为致密膜,PTFE与PDMS间相容性较好,没有相分离现象；PTFE与PDMS间为物理混合；随着PTFE填加量的增加,PTFE-PDMS膜结晶度、水接触角和热稳定性增加,膜在氯仿或乙醇水溶液中溶胀度降低,而力学性能呈现先增加后减小的趋势；PTFE的加入提高了PDMS膜的渗透汽化性能,对氯仿水体系,PTFE在膜内含量30%时分离指数最大,进料温度50℃、渗透侧真空度2.2mmHg、料液氯仿浓度620mg/L、流速400mL/min条件下,总通量31.9g/(m2·h),分离因子3215；而对乙醇水体系,PTFE在膜内含量10%时分离指数最大,进料温度60℃、料液流速1600mL/min和渗透侧压力120mmHg下,料液乙醇质量分数为10%条件下,总通量52.2g/(m2·h),分离因子10。
其次,根据溶解-扩散理论,研究了单组分溶剂氯仿、乙醇及水在PTFE-PDMS膜中的溶解及扩散性能。同温度下,随着PTFE在膜内填加量的增加,氯仿和水在PTFE-PDMS膜中溶解度w∞,c和w∞,w呈减小趋势,乙醇w∞,E值呈现先增加后减小的趋势；随溶解温度的升高,相同组成PTFE-PDMS膜内的w∞,c值基本不变,w∞,E和w∞w值呈增加趋势。而且溶解度大小顺序为w∞,c>w∞,E>w∞,w,说明PTFE-PDMS膜是亲有机疏水膜。氯仿、乙醇和水在PTFE-PDMS膜内扩散系数D呈现较为复杂的变化,其大小顺序遵循DC>DE>DW。PTFE的填加提高了PDMS膜的氯仿渗透系数PC、乙醇渗透系数PE、水渗透系数PW,而且氯仿对水及乙醇对水的理想分离系数αs,C和αs,E均得到提高。
随后,制备了两种分别以无纺布PET和超滤膜PVDF为底膜的PTFE-PDMS/PET及PTFE-PDMS/PVDF渗透汽化复合膜,讨论了其渗透汽化低浓度氯仿水溶液及PTFE-PDMS/PET膜渗透汽化乙醇水溶液的分离性能,考察了料液浓度、料液温度、渗透侧压力等条件对膜渗透汽化性能的影响。结果表明,PTFE-PDMS/PET及PTFE-PDMS/PVDF膜渗透汽化氯仿水溶液性能变化趋势基本相同,不同之处在于PTFE-PDMS/PET膜通量小于PTFE-PDMS/PVDF膜的通量,而PTFE-PDMS/PET膜分离因子大于PTFE-PDMS/PVDF膜的分离因子。对于PTFE-PDMS/PET渗透汽化乙醇水溶液性能,料液浓度增加,总通量、乙醇通量和分离因子增加；总通量、乙醇通量和分离因子均随温度的升高而增加；随着料液流量的增加,总通量、乙醇和分离因子呈缓慢增加趋势,变化较小,说明乙醇水体系的渗透汽化不会出现较明显的传质边界层。
然后,基于溶解-扩散理论和串联阻力模型分析了氯仿水溶液渗透汽化过程中氯仿传质机理。随料液中氯仿浓度的增加,氯仿渗透系数Kc.t线性增加,而水Kw.t略有线性减小趋势：随料液流速的增加,边界层厚度逐渐减薄,氯仿边界层传质系数Kb逐渐增加,传质阻力Rb逐渐减小。当Re为133时,Rb是Rm的29倍,氯仿传质过程由Rb控制。当Re达到5330时,Rt逐渐接近Rm,此时Rb极小,氯仿传质过程由Rm控制。
最后,制备了PTFE-PDMS/PVDF中空纤维膜和外压式膜组件。以实际工业排放水配制氯仿水溶液,讨论了活性层厚度、料液浓度、料液温度、渗透侧压力、料液流速和运行时间对膜渗透汽化性能的影响。结果表明,随着活性层厚度的增加,总通量减少而分离因子增加；料液浓度增加,总通量呈线性增加而分离因子呈下降趋势；渗透侧压力降低,渗透通量和分离因子都增加；料液流速增加,渗透通量和分离因子都增加：料液温度升高,总通量及分离因子皆呈增加趋势。渗透汽化连续运行11天,通量略有增加而分离因子有下降趋势。适宜的操作条件为：膜活性层厚度13.8μm、料液氯仿浓度小于350ppm、渗透侧压力2.2mmHg、Re1932、料液温度60℃。
There are much volatile organic compounds (VOC) in industrial and domestic wastewater at present. It is difficult to treat VOC which can endanger environmental safe because of toxity and low biochemical degradation. At the same time, VOC is an important chemical raw material, and its recovery has important economic value. Therefore, the treatment of VOC is a research hotpot recently. The membrane separation technology of pervaporation, which have the advantages of low mass in phase transition, efficiency, low power consumption with simple equipment and low technological scale up effect, are preferred ways of environmental protection. In this paper, several kinds of PTFE-PDMS composite pervaporation membranes were prepared using PTFE micro-powder and PDMS membrane materials. PTFE-PDMS pervaporation membrane structures, solution-diffusion properties, permeation performance for dilute chloroform or ethanol organic aqueous solution and the mass transfer resistance in permeation were investigated. The conclusions were as follows:
Firstly, PTFE-PDMS pervaporation flat-sheet membranes prepared with different ratioes of PTFE into PDMS. The structures and characterizations of PTFE-PDMS pervaporation membranes were studied by SEM-EDAX, FT-IR, XRD, DSC, TG and water contact angle method. The properties of membrane swelling behavior and permeation were discussed. The experimental results showed that PTFE-PDMS membranes were dense and no phase separations due to the good compatibility between organophilic PTFE particles and organophilic PDMS. The PTFE particles are only physically blended with the PDMS polymer matrix. With an increase of PTFE, the crystallinity, the water contact angle and thermal stability of the PTFE-PDMS membranes were enhanced, but the swelling degree in chloroform or ethanol aqueous solutions were reduced. And the mechanical strength was increased greatly at first and then decreased with an increase of PTFE. The examinations showed that the PTFE filled PDMS membranes exhibited striking advantages in flux and separation factor as compared with unfilled PDMS membranes. For chloroform aqueous solutions, separation index was best when the content of the PTFE micro-powder additive in PDMS composite membrane was30wt.%. For the30%PTFE-PDMS membrane, the total fluxes and the separation factor can reach31.9g/(m2·h) and3215respectively at the condition of feed temperature50℃, permeate pressure2.2mmHg, feed concentration620mg/L, feed flow400mL/min. But for ethanol aqueous solutions, the PTFE additive in PDMS composite membrane was10wt.%. For the10%PTFE-PDMS membrane, the total fluxes and the separation factor can reach52.2g/(m2·h) and10respectively at the condition of feed temperature60℃, permeate pressure120mmHg, feed concentration10wt.%, feed flow1600mL/min.
Then, on the basis of solution-diffusion theory, the sorption and diffusion behaviors of pure solvents such as chloroform, ethanol and water in the composite membranes were investigated. The results showed that at the same temperature, the solubility w∝,c and w∞,W of chloroform and water in PTFE-PDMS membranes decreased respectively with increasing PTFE content, but the w∞,E of ethanol first increased then decreased. With an increase of solubility temperature, w∞,c for PTFE-PDMS membranes with same proportion unchanged, but w∞,E and w∞,W increased. The order of solubility is w∞,c> w∞,E> w∞,W, which proved that PTFE-PDMS membrane was water repellent. The diffusion coefficients of chloroform, ethanol and water in the composite membranes have a complex change, and the order is DC> DE>DW. Adding PTFE in PDMS increased permeation coefficient Pc, PE and PW of chloroform, ethanol and water respectively, and the ideal separation selectivities for both chloroform to water and ethanol to water, αs,C and αs,E, increased.
Next, two kinds of PTFE-PDMS pervaoparation membranes, PTFE-PDMS/PET and PTFE-PDMS/PVDF pervaoparation composite membranes were fabricated, in which PET non-woven fabrics and PVDF UF membrane were as the support layers. The pervaporation performances of PTFE-PDMS membranes, PTFE-PDMS/PET composite membrane for dilute chloroform aqueous solutions and PTFE-PDMS/PVDF composite membrane for ethanol aqueous solutions were investigated. The effects of feed concentration, feed temperature and permeate-side vacuum on the PV performance of the composite membrane were studied. The examinations showed that the two kind of composite membranes exhibited a similar trend. The difference was that the permeation fluxes of PTFE-PDMS/PET membrane for chloroform aqueous solutions were lower than that of PTFE-PDMS/PVDF, and the separation factor of PTFE-PDMS/PET membrane for chloroform aqueous solutions were higher than that of PTFE-PDMS/PVDF. For the permeation of PTFE-PDMS/PET for ethanol aqueous solution, total and ethanol flux and separation factor all increased with feed concentration increasing. With an increase of temperature, total and ethanol flux and separation factor all increased. Total, water and ethanol flux and separation factor all increased lightly with feed flow increased. That proved there is no obvious mass transfer boundary layer when the PTFE-PDMS/PET membrane was used to permeate ethanol aqueous solution.
After that, mass transfer process of permeation for chloroform aqueous solution on the basis of solution-diffusion theory and resistance in series model was analyzed. With an increase of chloroform content in feed, chloroform permeation coefficient, KC,t, increased linearly, but water permeation coefficient, Kw,t, decreased linearly. With an increase of feed flow, boundary layer thickness was reduced gradually, so chloroform permeation coefficient in boundary layer, Kb, increased gradually and mass transfer Resistance, Rb, decreased gradually. When Re for feed flow is133, Rb was29times over Rm, which proved that chloroform mass transfer process was controlled by Rb, When Re for feed flow is5330, Rt was closed to Rm and Rb can be ignored, which proved that chloroform mass transfer process was controlled by Rm.
Finally, PTFE-PDMS/PVDF hollow fiber pervaporation membrane and external pressure membrane module were prepared. The effects of active layer thickness, feed concentration, feed temperature, permeate-side vacuum, feed flow and operating time on the PV performance of the composite membrane were studied. The results showed that with an increase of active layer thickness, total flux decreased but separation factor increased. When feed concentration increased, total flux increased linearly but separation factor decreased. Both total flux and separation factor increased with permeation pressure decreased. With feed flow or feed temperature increased, both total flux and separation factor increased. Total flux decreased but separation factor increased lightly after11operating days. The suitable pervaporation condition is:active layer thickness13.8μm, low feed concentration (less than350ppm), permeate pressure2.2mmHg, Re1932and feed temperature60℃.
首先,制各了不同组成的PTFE-PDMS渗透汽化平板膜,采用SEM-EDAX、FT-IR、 XRD、DSC、TG和水接触角等方法,研究了PTFE-PDMS渗透汽化膜结构及性能,考察了PTFE-PDMS渗透汽化膜的溶胀和渗透汽化性能。结果表明：PTFE-PDMS渗透汽化膜为致密膜,PTFE与PDMS间相容性较好,没有相分离现象；PTFE与PDMS间为物理混合；随着PTFE填加量的增加,PTFE-PDMS膜结晶度、水接触角和热稳定性增加,膜在氯仿或乙醇水溶液中溶胀度降低,而力学性能呈现先增加后减小的趋势；PTFE的加入提高了PDMS膜的渗透汽化性能,对氯仿水体系,PTFE在膜内含量30%时分离指数最大,进料温度50℃、渗透侧真空度2.2mmHg、料液氯仿浓度620mg/L、流速400mL/min条件下,总通量31.9g/(m2·h),分离因子3215；而对乙醇水体系,PTFE在膜内含量10%时分离指数最大,进料温度60℃、料液流速1600mL/min和渗透侧压力120mmHg下,料液乙醇质量分数为10%条件下,总通量52.2g/(m2·h),分离因子10。
其次,根据溶解-扩散理论,研究了单组分溶剂氯仿、乙醇及水在PTFE-PDMS膜中的溶解及扩散性能。同温度下,随着PTFE在膜内填加量的增加,氯仿和水在PTFE-PDMS膜中溶解度w∞,c和w∞,w呈减小趋势,乙醇w∞,E值呈现先增加后减小的趋势；随溶解温度的升高,相同组成PTFE-PDMS膜内的w∞,c值基本不变,w∞,E和w∞w值呈增加趋势。而且溶解度大小顺序为w∞,c>w∞,E>w∞,w,说明PTFE-PDMS膜是亲有机疏水膜。氯仿、乙醇和水在PTFE-PDMS膜内扩散系数D呈现较为复杂的变化,其大小顺序遵循DC>DE>DW。PTFE的填加提高了PDMS膜的氯仿渗透系数PC、乙醇渗透系数PE、水渗透系数PW,而且氯仿对水及乙醇对水的理想分离系数αs,C和αs,E均得到提高。
随后,制备了两种分别以无纺布PET和超滤膜PVDF为底膜的PTFE-PDMS/PET及PTFE-PDMS/PVDF渗透汽化复合膜,讨论了其渗透汽化低浓度氯仿水溶液及PTFE-PDMS/PET膜渗透汽化乙醇水溶液的分离性能,考察了料液浓度、料液温度、渗透侧压力等条件对膜渗透汽化性能的影响。结果表明,PTFE-PDMS/PET及PTFE-PDMS/PVDF膜渗透汽化氯仿水溶液性能变化趋势基本相同,不同之处在于PTFE-PDMS/PET膜通量小于PTFE-PDMS/PVDF膜的通量,而PTFE-PDMS/PET膜分离因子大于PTFE-PDMS/PVDF膜的分离因子。对于PTFE-PDMS/PET渗透汽化乙醇水溶液性能,料液浓度增加,总通量、乙醇通量和分离因子增加；总通量、乙醇通量和分离因子均随温度的升高而增加；随着料液流量的增加,总通量、乙醇和分离因子呈缓慢增加趋势,变化较小,说明乙醇水体系的渗透汽化不会出现较明显的传质边界层。
然后,基于溶解-扩散理论和串联阻力模型分析了氯仿水溶液渗透汽化过程中氯仿传质机理。随料液中氯仿浓度的增加,氯仿渗透系数Kc.t线性增加,而水Kw.t略有线性减小趋势：随料液流速的增加,边界层厚度逐渐减薄,氯仿边界层传质系数Kb逐渐增加,传质阻力Rb逐渐减小。当Re为133时,Rb是Rm的29倍,氯仿传质过程由Rb控制。当Re达到5330时,Rt逐渐接近Rm,此时Rb极小,氯仿传质过程由Rm控制。
最后,制备了PTFE-PDMS/PVDF中空纤维膜和外压式膜组件。以实际工业排放水配制氯仿水溶液,讨论了活性层厚度、料液浓度、料液温度、渗透侧压力、料液流速和运行时间对膜渗透汽化性能的影响。结果表明,随着活性层厚度的增加,总通量减少而分离因子增加；料液浓度增加,总通量呈线性增加而分离因子呈下降趋势；渗透侧压力降低,渗透通量和分离因子都增加；料液流速增加,渗透通量和分离因子都增加：料液温度升高,总通量及分离因子皆呈增加趋势。渗透汽化连续运行11天,通量略有增加而分离因子有下降趋势。适宜的操作条件为：膜活性层厚度13.8μm、料液氯仿浓度小于350ppm、渗透侧压力2.2mmHg、Re1932、料液温度60℃。
There are much volatile organic compounds (VOC) in industrial and domestic wastewater at present. It is difficult to treat VOC which can endanger environmental safe because of toxity and low biochemical degradation. At the same time, VOC is an important chemical raw material, and its recovery has important economic value. Therefore, the treatment of VOC is a research hotpot recently. The membrane separation technology of pervaporation, which have the advantages of low mass in phase transition, efficiency, low power consumption with simple equipment and low technological scale up effect, are preferred ways of environmental protection. In this paper, several kinds of PTFE-PDMS composite pervaporation membranes were prepared using PTFE micro-powder and PDMS membrane materials. PTFE-PDMS pervaporation membrane structures, solution-diffusion properties, permeation performance for dilute chloroform or ethanol organic aqueous solution and the mass transfer resistance in permeation were investigated. The conclusions were as follows:
Firstly, PTFE-PDMS pervaporation flat-sheet membranes prepared with different ratioes of PTFE into PDMS. The structures and characterizations of PTFE-PDMS pervaporation membranes were studied by SEM-EDAX, FT-IR, XRD, DSC, TG and water contact angle method. The properties of membrane swelling behavior and permeation were discussed. The experimental results showed that PTFE-PDMS membranes were dense and no phase separations due to the good compatibility between organophilic PTFE particles and organophilic PDMS. The PTFE particles are only physically blended with the PDMS polymer matrix. With an increase of PTFE, the crystallinity, the water contact angle and thermal stability of the PTFE-PDMS membranes were enhanced, but the swelling degree in chloroform or ethanol aqueous solutions were reduced. And the mechanical strength was increased greatly at first and then decreased with an increase of PTFE. The examinations showed that the PTFE filled PDMS membranes exhibited striking advantages in flux and separation factor as compared with unfilled PDMS membranes. For chloroform aqueous solutions, separation index was best when the content of the PTFE micro-powder additive in PDMS composite membrane was30wt.%. For the30%PTFE-PDMS membrane, the total fluxes and the separation factor can reach31.9g/(m2·h) and3215respectively at the condition of feed temperature50℃, permeate pressure2.2mmHg, feed concentration620mg/L, feed flow400mL/min. But for ethanol aqueous solutions, the PTFE additive in PDMS composite membrane was10wt.%. For the10%PTFE-PDMS membrane, the total fluxes and the separation factor can reach52.2g/(m2·h) and10respectively at the condition of feed temperature60℃, permeate pressure120mmHg, feed concentration10wt.%, feed flow1600mL/min.
Then, on the basis of solution-diffusion theory, the sorption and diffusion behaviors of pure solvents such as chloroform, ethanol and water in the composite membranes were investigated. The results showed that at the same temperature, the solubility w∝,c and w∞,W of chloroform and water in PTFE-PDMS membranes decreased respectively with increasing PTFE content, but the w∞,E of ethanol first increased then decreased. With an increase of solubility temperature, w∞,c for PTFE-PDMS membranes with same proportion unchanged, but w∞,E and w∞,W increased. The order of solubility is w∞,c> w∞,E> w∞,W, which proved that PTFE-PDMS membrane was water repellent. The diffusion coefficients of chloroform, ethanol and water in the composite membranes have a complex change, and the order is DC> DE>DW. Adding PTFE in PDMS increased permeation coefficient Pc, PE and PW of chloroform, ethanol and water respectively, and the ideal separation selectivities for both chloroform to water and ethanol to water, αs,C and αs,E, increased.
Next, two kinds of PTFE-PDMS pervaoparation membranes, PTFE-PDMS/PET and PTFE-PDMS/PVDF pervaoparation composite membranes were fabricated, in which PET non-woven fabrics and PVDF UF membrane were as the support layers. The pervaporation performances of PTFE-PDMS membranes, PTFE-PDMS/PET composite membrane for dilute chloroform aqueous solutions and PTFE-PDMS/PVDF composite membrane for ethanol aqueous solutions were investigated. The effects of feed concentration, feed temperature and permeate-side vacuum on the PV performance of the composite membrane were studied. The examinations showed that the two kind of composite membranes exhibited a similar trend. The difference was that the permeation fluxes of PTFE-PDMS/PET membrane for chloroform aqueous solutions were lower than that of PTFE-PDMS/PVDF, and the separation factor of PTFE-PDMS/PET membrane for chloroform aqueous solutions were higher than that of PTFE-PDMS/PVDF. For the permeation of PTFE-PDMS/PET for ethanol aqueous solution, total and ethanol flux and separation factor all increased with feed concentration increasing. With an increase of temperature, total and ethanol flux and separation factor all increased. Total, water and ethanol flux and separation factor all increased lightly with feed flow increased. That proved there is no obvious mass transfer boundary layer when the PTFE-PDMS/PET membrane was used to permeate ethanol aqueous solution.
After that, mass transfer process of permeation for chloroform aqueous solution on the basis of solution-diffusion theory and resistance in series model was analyzed. With an increase of chloroform content in feed, chloroform permeation coefficient, KC,t, increased linearly, but water permeation coefficient, Kw,t, decreased linearly. With an increase of feed flow, boundary layer thickness was reduced gradually, so chloroform permeation coefficient in boundary layer, Kb, increased gradually and mass transfer Resistance, Rb, decreased gradually. When Re for feed flow is133, Rb was29times over Rm, which proved that chloroform mass transfer process was controlled by Rb, When Re for feed flow is5330, Rt was closed to Rm and Rb can be ignored, which proved that chloroform mass transfer process was controlled by Rm.
Finally, PTFE-PDMS/PVDF hollow fiber pervaporation membrane and external pressure membrane module were prepared. The effects of active layer thickness, feed concentration, feed temperature, permeate-side vacuum, feed flow and operating time on the PV performance of the composite membrane were studied. The results showed that with an increase of active layer thickness, total flux decreased but separation factor increased. When feed concentration increased, total flux increased linearly but separation factor decreased. Both total flux and separation factor increased with permeation pressure decreased. With feed flow or feed temperature increased, both total flux and separation factor increased. Total flux decreased but separation factor increased lightly after11operating days. The suitable pervaporation condition is:active layer thickness13.8μm, low feed concentration (less than350ppm), permeate pressure2.2mmHg, Re1932and feed temperature60℃.
引文
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