高稳定性YSZ-LSCF双相中空纤维氧分离膜和反应器性能研究
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摘要
陶瓷氧分离膜是一种正在研究的低成本的制氧新技术,其制氧成本比空分法要下降30%以上,特别是与下游涉氧工艺耦合构建膜反应器,更是具有许多潜在的应用。膜反应器应用需要材料同时具有高的氧渗透性能和在氧化性气氛及强还原性气氛下良好的稳定性,现有的透氧膜材料很难同时达到要求。本论文发明了一种具有良好稳定性的膜材料并将其制备成中空纤维膜,利用纤维膜壁薄,单位面积氧渗透速率高,单位体积膜面积大的优点,在透氧膜应用于膜反应器方面取得了突破性进展。
第一章主要介绍了陶瓷透氧膜的背景,基本原理以及典型应用,同时介绍了中空纤维膜的研究进展。
第二章率先提出了一种双相复合的陶瓷透氧膜材料体系：Zl0.84Y0.16O1.92-La0.8Sr0.2Cr0.5Fe0.5O3(YSZ-LSCF),并采用相转换/烧结法制备了该双相材料的中空纤维膜。空气中1430℃烧结10h后的YSZ-LSCF中空纤维膜外径为1.82mm,壁厚为0.34mm,膜管具有典型的非对称结构且达到气密。当一根4.46cm长的中空纤维膜管外侧处于空气中,内侧用30ml/min的纯的CO吹扫时,950℃下的透氧速率高达3.8ml cm-2min-1,且在近500的连续测量中保持稳定。当将膜管降至室温并重新升到950℃时,透氧速率保持一致。测量后的膜管无任何相组成以及微结构的变化,表明膜管具有优异的稳定性和抗热震性。在900℃-1000℃温度范围内,膜管内CO氧化的转化率仅与透过O：量／注入CO量比例有关,即仅与反应化学计量比有关,这表明CO在膜管内的氧化反应属于快反应,能达到化学平衡状态。在此基础上采用等温柱塞流模型结合Wagner方程模拟了中空纤维膜的氧渗透行为,该模拟方法可以得到中空纤维膜轴向上任一处的气体组成和氧渗透速率,对评估中空纤维膜的性能具有重要参考意义。
第三章研究了在YSZ-LSCF中空纤维膜内部不负载催化剂或负载上LSCF粉体作为催化剂,以及不同质量分数的Ru/LSCF作为催化剂时得到的膜反应器用作CH4催化部分氧化的性能。负载Ru (33%wt)/LSCF的YSZ-LSCF中空纤维膜反应器表现出了优异的CH4部分氧化催化性能。制备得到的催化剂厚度约为5μm,估算出的Ru的使用量约为7.6mg/cm2,封接后的YSZ-LSCF中空纤维膜反应器有效长度约为5.77cm。在950℃时,当CH4注入量为超过16ml/min后,该反应器总的透氧速率能高达17.1ml/min,面积归一化之后为7.9ml/min/cm2。继续增加CH4注入量时,透氧速率基本稳定,当CH4注入量升高到31.6ml/min时,注入的CH4/透过的O2接近部分氧化化学计量比2：1时,CH4转化率高达90%以上,CO和H2的选择性分别为100%和93%,合成气的生产速率达到83.8ml/min,且在在600h的连续测量中保持稳定。生成的合成气中H2/CO比例稳定在1.85左右,接近POM的化学计量比2,适合用于F-T反应变为液体燃料。同时生成的合成气中O/C比例大于1,处于Ni基阳极的非积碳区,当用作片状固体氧化物燃料电池(SOFC)的燃料时,即使在很低的电流密度200mA/cm2下,在30h的连续测量中,电池输出电压也能保持稳定。在800h的POM反应后,YSZ-LSCF透氧膜没有任何还原迹象,表现出良好的稳定性,但Ru (33%wt)/LSCF催化剂层存在少量物理性的流失。需要进一步提高催化剂与基体的附着能力。
第四章研究了在YSZ-LSCF中空纤维膜内部负载Ni/LSCF催化剂得到的膜反应器用作CH4催化部分氧化的性能。当在催化剂浆料中加入Na2SiO4·9H2O并采用水作为分散剂时,Ni/LSCF催化剂层与YSZ-LSCF中空纤维膜的附着强度能得到明显改善,这是因为Na2SiO4·9H2O溶于水后产生的小颗粒的Si溶胶可以起到粘合剂的作用。直接涂敷Ni/LSCF催化剂的YSZ-LSCF中空纤维膜反应器在950℃,CH4注入量：透过02量控制在部分氧化的化学计量比2：1附近时的CH4转化率的衰减速率为4.29%/100h,而改进的添加Na2SiO4·9H2O后涂敷Ni/LSCF催化剂的YSZ-LSCF中空纤维膜反应器在相似的条件下近800h连续测量中的CH4转化率衰减速率仅为9.18%/1000h。后一种膜反应器(长度为8.30cm)在长达800h的测量中膜反应器表现出来非常高而且稳定的CO和H2选择性；CO选择性在95%以上H2选择性在85%以上,尾气中H2/CO的比例在1.75左右,接近CH4部分氧化的产物的化学计量比,有少量的H2被氧化生成了H20。膜反应器的CO,H2的生成速率分别高达32.7ml/min和57.2ml/min。也就是,每分钟能产生89.9ml的合成气,面积归一化后为29.2ml/min/cm2。膜反应器的透氧速率维持在21.7ml/min左右,面积归一化后为7.1ml/min/cm2。证明当使用普通金属Ni作为催化剂也能得到具有良好部分氧化催化性能的膜反应器。
第五章研究了在YSZ-LSCF中空纤维膜内部负载PdO/LSCF催化剂得到的膜反应器用作CH4催化燃烧的性能。在950℃甲烷流量5.65ml/min条件下,在近200h的连续测量中,甲烷的转化率保持在99.5%以上,CO2选择性在90%以上,氧渗透速率约为4.57ml/min/cm2,且均基本保持稳定。测试后膜管相结构和微观结构无任何变化。说明催化剂负载的YSZ-LSCF双相中空纤维膜管可以用来进行甲烷催化燃烧反应供热和进行随后的CO2捕获。
第六章研究了一种中空纤维透氧膜的集成方式,将多根中空纤维膜管胚体并排一步烧结成中空纤维膜板。当采用YSZ-La0.8Sr0.2Mn03(LSM)作为试验模型体系时,烧结的中空纤维膜板脖颈处相互连接并共烧到一起的长度超过200μm。强度分析测试表明中空纤维膜板具有比单根中空纤维膜更好的机械性能,而且结合紧密。透氧性能测试表明这种集成方式对膜本身的透氧性能并无影响,得到的中空纤维膜板具有与单根中空纤维膜相近的透氧速率。在此基础上还进一步提出将二维的中空纤维膜板集成成三维的中空纤维膜块的方法并进行了初步尝试。
第七章总结了本论文的研究工作,并对陶瓷中空纤维氧分离膜反应器的应用前景和主要挑战进行了展望。
The ceramic oxygen-permeable membrane is a new technology being studied, which can reduce the oxygen production cost by more than30%over the present cryogenic distillation process. It has many potential applications, especially when used as membrane reactor coupled with downstream oxygen-consuming reactions. When involving membrane reactor applications, the membrane material need to possess not only high oxygen permeability but also good stability under the oxidizing atmosphere and strong reducing atmosphere. The existing material cannot simultaneously meet these requirements. In this thesis, we have explored a dual-phase composite which shows outstanding stability. When fabricated it into hollow fiber geometry, the oxygen permeation performance can largely enhanced. This is because that the hollow fiber has a thinner wall thickness and thus imposes less resistance to the permeation of oxygen. Besides, the hollow fiber has a small outer diameter, thus a large quantity of membranes can be packed in a module. Based on these advantages, the ceramic oxygen-permeable hollow fiber is promising in membrane reactor applications.
Chapter1introduces the background and typical applications of ceramic oxygen-permeable membranes. The concepts and theories of oxygen permeation for dense ceramic membranes are reviewed, and the research progress of the hollow fiber membrane is introduced as well.
In Chapter2, dual phase composite of Zr0.84Y0.16O1.92(YSZ) and La0.8Sr0.2Cr0.5Fe0.5O3(LSCF) are explored for oxygen separation application. The hollow fiber precursor is prepared by phase inversion/sintering technology. After sintering in air at1430℃for10hours, the hollow fiber membrane turns to be gas-tight and shows an asymmetric structure with out diameter of1.82mm, wall thickness of0.34mm. The oxygen permeability of the YSZ-LSCF hollow fiber is measured with its shell side to the ambient air and feed the core side with pure CO. The oxygen permeation flux can reach as high as3.8ml cm-2min-1with a4.46cm-long hollow fiber when CO feed rate was30ml/min at950℃, and remain almost unchanged in more than500h continuous measurements. Almost same value of oxygen pemieation rate was obtained after cooling down to room temperature and then reheating up to950℃, indicating good heat-shock-resistance of the fiber. SEM observation reveals that the500h oxygen permeation test under the stringent conditions did not cause significant change to the microstructure of the membrane. CO oxidation reaction in the membrane mode had a fast kinetics and can be simulated using the plug flow model. The calculated outlet CO and CO2concentration for various CO feed rate are in good agreement with the measured ones, verifying the validity of the simulation method. The simulation makes it possible to determine the axial profiles of CO and CO2concentration and oxygen partial pressure (at the lumen side) and corresponding oxygen permeation rate which are hardly possible to measure experimentally.
In Chapter3, a partial oxidation of methane (POM) membrane reactor is built using the YSZ-LSCF hollow fiber membrane coated with Ru/LSCF as catalyst. The influence of the weight percentage of Ru in the catalyst to the catalytic activity is studied. When the weight percentage of Ru in the catalyst increased to33%, the membrane reactor shows outstanding POM performances. With a5.77cm-long hollow fiber coated with5μm Ru(33%wt)/LSCF catalyst (-7.6mg Ru/cm2inner surface area), an oxygen permeation flux as high as17.1ml/min (7.9ml/min/cm2) is observed when CH4feed rate reach over16ml/min at950℃. At a higher CH4feed rate of31.6ml/min, the CH4feed rate/oxygen permeation flux ratio becomes near the stoichiometric ratio of the POM reaction. CH4conversion over90%, CO selectivity near100%and H2selectivity over93%can be observed. The formation rate of the syngas (CO+H2) is over83.8ml/min and the H2/CO ratio in the syngas is near1.85, which is suitable for the Fischer-Tropsch synthesis. The membrane reactor gives a stable performance in more than600h continuous measurements. The O/C ratio in the syngas is high than1, which located in the theoretical no carbon deposition area of the Ni-based anode of solid oxide fuel cell (SOFC). So the effluent syngas is a suitable fuel for SOFC. A disk SOFC can stably run on the fuel produced from methane by the membrane reactor even at low current density of200mA/cm2. The output voltage remains almost unchanged in30h measurement. After800h experiment under POM condition, the YSZ-LSCF hollow fiber remains intact but loss of Ru/LSCF catalyst is observed. The adherence of the catalyst to the membrane need to be improved.
In Chapter4, Ni/LSCF is used as POM catalyst instead of Ru/LSCF since Ru is a noble metal. The influence of the composition of the catalyst slurry to the adherence of the catalyst layer is studied. When Na2SiO4·9H2O is added into the catalyst slurry and H2O is used as solvent, the adherence of the Ni/LSCF catalyst to the YSZ-LSCF hollow fiber membrane can be improved, which is due to the Si sol formed after Na2SiO4·9H2O dissolved in water. The Si sol acts as a binder. The adherence of the Ni/LSCF catalyst layer can significantly affect the POM performance of the YSZ-LSCF catalytic hollow fiber membrane. In long-term stability experiments, the CH4conversion decrease rate is4.29%/100h for catalyst with bad adherence (without Na2SiO4·9H2O) and9.18%/1000h for catalyst with good adherence (with Na2SiO·9H2O), respectively. When catalyst with good adherence is used, a8.30cm-long hollow fiber membrane reactor shows good POM performance, CO selectivity over95%, H2selectivity over92%, H2/CO ratio near1.75. The CO and H2formation rate are32.7ml/min and57.2ml/min respectively and oxygen permeation rate is7.1ml/min/cm2, showing Ni/LSCF is also a promising POM catalyst.
Chapter5presents a study on CH4combustion membrane reactor which composed of YSZ-LSCF hollow fiber and PdO/LSCF catalyst. At CH4feed rate of5.65ml/min and temperature of950℃, CH4can combust into CO2and H2O in the membrane reactor with CH4conversion over99.5%and CO2selectivity over90%. The oxygen permeation flux is4.57ml/min/cm2. All these data is stable in near200h measurement. The phase composition and microstructure of the used membrane remains almost unchanged. This membrane reactor holds applications in CH4catalytic combustion at low temperature for heat and CO2capture.
In Chapter6, a new type of hollow fiber membrane integration module is put forward and its perfonnance in oxygen separation is investigated. The dual phase hollow fiber, consisting of Zr0.84Y0.16O1.92(YSZ) and La0.8Sr0.2MnO3-δ(LSM), is fonned by the phase inversion method. Then five neck-by-neck fibers are co-sintered together to form a plate module at1350℃. The perfomiances of the module for oxygen separation have been studied at different temperatures, feed gases and flow rates. An oxygen permeation flux of1.52ml/min is obtained under air/He(100ml/min) gradient at950℃(Plate length:280mm Hollow fiber O.D.:1.76mm Wall thickness:0.24mm). When sweep gas switched from He to CO2, the oxygen permeation flux almost remain unchanged. The hollow fiber membrane plate shows better mechanical performance than one single fiber. Based on this kind of integration way, further experiments have been done on co-sintering several plates to a block.
Chapter7summarizes the research conducted in this thesis, and presents recommendations for further research.
第一章主要介绍了陶瓷透氧膜的背景,基本原理以及典型应用,同时介绍了中空纤维膜的研究进展。
第二章率先提出了一种双相复合的陶瓷透氧膜材料体系：Zl0.84Y0.16O1.92-La0.8Sr0.2Cr0.5Fe0.5O3(YSZ-LSCF),并采用相转换/烧结法制备了该双相材料的中空纤维膜。空气中1430℃烧结10h后的YSZ-LSCF中空纤维膜外径为1.82mm,壁厚为0.34mm,膜管具有典型的非对称结构且达到气密。当一根4.46cm长的中空纤维膜管外侧处于空气中,内侧用30ml/min的纯的CO吹扫时,950℃下的透氧速率高达3.8ml cm-2min-1,且在近500的连续测量中保持稳定。当将膜管降至室温并重新升到950℃时,透氧速率保持一致。测量后的膜管无任何相组成以及微结构的变化,表明膜管具有优异的稳定性和抗热震性。在900℃-1000℃温度范围内,膜管内CO氧化的转化率仅与透过O：量／注入CO量比例有关,即仅与反应化学计量比有关,这表明CO在膜管内的氧化反应属于快反应,能达到化学平衡状态。在此基础上采用等温柱塞流模型结合Wagner方程模拟了中空纤维膜的氧渗透行为,该模拟方法可以得到中空纤维膜轴向上任一处的气体组成和氧渗透速率,对评估中空纤维膜的性能具有重要参考意义。
第三章研究了在YSZ-LSCF中空纤维膜内部不负载催化剂或负载上LSCF粉体作为催化剂,以及不同质量分数的Ru/LSCF作为催化剂时得到的膜反应器用作CH4催化部分氧化的性能。负载Ru (33%wt)/LSCF的YSZ-LSCF中空纤维膜反应器表现出了优异的CH4部分氧化催化性能。制备得到的催化剂厚度约为5μm,估算出的Ru的使用量约为7.6mg/cm2,封接后的YSZ-LSCF中空纤维膜反应器有效长度约为5.77cm。在950℃时,当CH4注入量为超过16ml/min后,该反应器总的透氧速率能高达17.1ml/min,面积归一化之后为7.9ml/min/cm2。继续增加CH4注入量时,透氧速率基本稳定,当CH4注入量升高到31.6ml/min时,注入的CH4/透过的O2接近部分氧化化学计量比2：1时,CH4转化率高达90%以上,CO和H2的选择性分别为100%和93%,合成气的生产速率达到83.8ml/min,且在在600h的连续测量中保持稳定。生成的合成气中H2/CO比例稳定在1.85左右,接近POM的化学计量比2,适合用于F-T反应变为液体燃料。同时生成的合成气中O/C比例大于1,处于Ni基阳极的非积碳区,当用作片状固体氧化物燃料电池(SOFC)的燃料时,即使在很低的电流密度200mA/cm2下,在30h的连续测量中,电池输出电压也能保持稳定。在800h的POM反应后,YSZ-LSCF透氧膜没有任何还原迹象,表现出良好的稳定性,但Ru (33%wt)/LSCF催化剂层存在少量物理性的流失。需要进一步提高催化剂与基体的附着能力。
第四章研究了在YSZ-LSCF中空纤维膜内部负载Ni/LSCF催化剂得到的膜反应器用作CH4催化部分氧化的性能。当在催化剂浆料中加入Na2SiO4·9H2O并采用水作为分散剂时,Ni/LSCF催化剂层与YSZ-LSCF中空纤维膜的附着强度能得到明显改善,这是因为Na2SiO4·9H2O溶于水后产生的小颗粒的Si溶胶可以起到粘合剂的作用。直接涂敷Ni/LSCF催化剂的YSZ-LSCF中空纤维膜反应器在950℃,CH4注入量：透过02量控制在部分氧化的化学计量比2：1附近时的CH4转化率的衰减速率为4.29%/100h,而改进的添加Na2SiO4·9H2O后涂敷Ni/LSCF催化剂的YSZ-LSCF中空纤维膜反应器在相似的条件下近800h连续测量中的CH4转化率衰减速率仅为9.18%/1000h。后一种膜反应器(长度为8.30cm)在长达800h的测量中膜反应器表现出来非常高而且稳定的CO和H2选择性；CO选择性在95%以上H2选择性在85%以上,尾气中H2/CO的比例在1.75左右,接近CH4部分氧化的产物的化学计量比,有少量的H2被氧化生成了H20。膜反应器的CO,H2的生成速率分别高达32.7ml/min和57.2ml/min。也就是,每分钟能产生89.9ml的合成气,面积归一化后为29.2ml/min/cm2。膜反应器的透氧速率维持在21.7ml/min左右,面积归一化后为7.1ml/min/cm2。证明当使用普通金属Ni作为催化剂也能得到具有良好部分氧化催化性能的膜反应器。
第五章研究了在YSZ-LSCF中空纤维膜内部负载PdO/LSCF催化剂得到的膜反应器用作CH4催化燃烧的性能。在950℃甲烷流量5.65ml/min条件下,在近200h的连续测量中,甲烷的转化率保持在99.5%以上,CO2选择性在90%以上,氧渗透速率约为4.57ml/min/cm2,且均基本保持稳定。测试后膜管相结构和微观结构无任何变化。说明催化剂负载的YSZ-LSCF双相中空纤维膜管可以用来进行甲烷催化燃烧反应供热和进行随后的CO2捕获。
第六章研究了一种中空纤维透氧膜的集成方式,将多根中空纤维膜管胚体并排一步烧结成中空纤维膜板。当采用YSZ-La0.8Sr0.2Mn03(LSM)作为试验模型体系时,烧结的中空纤维膜板脖颈处相互连接并共烧到一起的长度超过200μm。强度分析测试表明中空纤维膜板具有比单根中空纤维膜更好的机械性能,而且结合紧密。透氧性能测试表明这种集成方式对膜本身的透氧性能并无影响,得到的中空纤维膜板具有与单根中空纤维膜相近的透氧速率。在此基础上还进一步提出将二维的中空纤维膜板集成成三维的中空纤维膜块的方法并进行了初步尝试。
第七章总结了本论文的研究工作,并对陶瓷中空纤维氧分离膜反应器的应用前景和主要挑战进行了展望。
The ceramic oxygen-permeable membrane is a new technology being studied, which can reduce the oxygen production cost by more than30%over the present cryogenic distillation process. It has many potential applications, especially when used as membrane reactor coupled with downstream oxygen-consuming reactions. When involving membrane reactor applications, the membrane material need to possess not only high oxygen permeability but also good stability under the oxidizing atmosphere and strong reducing atmosphere. The existing material cannot simultaneously meet these requirements. In this thesis, we have explored a dual-phase composite which shows outstanding stability. When fabricated it into hollow fiber geometry, the oxygen permeation performance can largely enhanced. This is because that the hollow fiber has a thinner wall thickness and thus imposes less resistance to the permeation of oxygen. Besides, the hollow fiber has a small outer diameter, thus a large quantity of membranes can be packed in a module. Based on these advantages, the ceramic oxygen-permeable hollow fiber is promising in membrane reactor applications.
Chapter1introduces the background and typical applications of ceramic oxygen-permeable membranes. The concepts and theories of oxygen permeation for dense ceramic membranes are reviewed, and the research progress of the hollow fiber membrane is introduced as well.
In Chapter2, dual phase composite of Zr0.84Y0.16O1.92(YSZ) and La0.8Sr0.2Cr0.5Fe0.5O3(LSCF) are explored for oxygen separation application. The hollow fiber precursor is prepared by phase inversion/sintering technology. After sintering in air at1430℃for10hours, the hollow fiber membrane turns to be gas-tight and shows an asymmetric structure with out diameter of1.82mm, wall thickness of0.34mm. The oxygen permeability of the YSZ-LSCF hollow fiber is measured with its shell side to the ambient air and feed the core side with pure CO. The oxygen permeation flux can reach as high as3.8ml cm-2min-1with a4.46cm-long hollow fiber when CO feed rate was30ml/min at950℃, and remain almost unchanged in more than500h continuous measurements. Almost same value of oxygen pemieation rate was obtained after cooling down to room temperature and then reheating up to950℃, indicating good heat-shock-resistance of the fiber. SEM observation reveals that the500h oxygen permeation test under the stringent conditions did not cause significant change to the microstructure of the membrane. CO oxidation reaction in the membrane mode had a fast kinetics and can be simulated using the plug flow model. The calculated outlet CO and CO2concentration for various CO feed rate are in good agreement with the measured ones, verifying the validity of the simulation method. The simulation makes it possible to determine the axial profiles of CO and CO2concentration and oxygen partial pressure (at the lumen side) and corresponding oxygen permeation rate which are hardly possible to measure experimentally.
In Chapter3, a partial oxidation of methane (POM) membrane reactor is built using the YSZ-LSCF hollow fiber membrane coated with Ru/LSCF as catalyst. The influence of the weight percentage of Ru in the catalyst to the catalytic activity is studied. When the weight percentage of Ru in the catalyst increased to33%, the membrane reactor shows outstanding POM performances. With a5.77cm-long hollow fiber coated with5μm Ru(33%wt)/LSCF catalyst (-7.6mg Ru/cm2inner surface area), an oxygen permeation flux as high as17.1ml/min (7.9ml/min/cm2) is observed when CH4feed rate reach over16ml/min at950℃. At a higher CH4feed rate of31.6ml/min, the CH4feed rate/oxygen permeation flux ratio becomes near the stoichiometric ratio of the POM reaction. CH4conversion over90%, CO selectivity near100%and H2selectivity over93%can be observed. The formation rate of the syngas (CO+H2) is over83.8ml/min and the H2/CO ratio in the syngas is near1.85, which is suitable for the Fischer-Tropsch synthesis. The membrane reactor gives a stable performance in more than600h continuous measurements. The O/C ratio in the syngas is high than1, which located in the theoretical no carbon deposition area of the Ni-based anode of solid oxide fuel cell (SOFC). So the effluent syngas is a suitable fuel for SOFC. A disk SOFC can stably run on the fuel produced from methane by the membrane reactor even at low current density of200mA/cm2. The output voltage remains almost unchanged in30h measurement. After800h experiment under POM condition, the YSZ-LSCF hollow fiber remains intact but loss of Ru/LSCF catalyst is observed. The adherence of the catalyst to the membrane need to be improved.
In Chapter4, Ni/LSCF is used as POM catalyst instead of Ru/LSCF since Ru is a noble metal. The influence of the composition of the catalyst slurry to the adherence of the catalyst layer is studied. When Na2SiO4·9H2O is added into the catalyst slurry and H2O is used as solvent, the adherence of the Ni/LSCF catalyst to the YSZ-LSCF hollow fiber membrane can be improved, which is due to the Si sol formed after Na2SiO4·9H2O dissolved in water. The Si sol acts as a binder. The adherence of the Ni/LSCF catalyst layer can significantly affect the POM performance of the YSZ-LSCF catalytic hollow fiber membrane. In long-term stability experiments, the CH4conversion decrease rate is4.29%/100h for catalyst with bad adherence (without Na2SiO4·9H2O) and9.18%/1000h for catalyst with good adherence (with Na2SiO·9H2O), respectively. When catalyst with good adherence is used, a8.30cm-long hollow fiber membrane reactor shows good POM performance, CO selectivity over95%, H2selectivity over92%, H2/CO ratio near1.75. The CO and H2formation rate are32.7ml/min and57.2ml/min respectively and oxygen permeation rate is7.1ml/min/cm2, showing Ni/LSCF is also a promising POM catalyst.
Chapter5presents a study on CH4combustion membrane reactor which composed of YSZ-LSCF hollow fiber and PdO/LSCF catalyst. At CH4feed rate of5.65ml/min and temperature of950℃, CH4can combust into CO2and H2O in the membrane reactor with CH4conversion over99.5%and CO2selectivity over90%. The oxygen permeation flux is4.57ml/min/cm2. All these data is stable in near200h measurement. The phase composition and microstructure of the used membrane remains almost unchanged. This membrane reactor holds applications in CH4catalytic combustion at low temperature for heat and CO2capture.
In Chapter6, a new type of hollow fiber membrane integration module is put forward and its perfonnance in oxygen separation is investigated. The dual phase hollow fiber, consisting of Zr0.84Y0.16O1.92(YSZ) and La0.8Sr0.2MnO3-δ(LSM), is fonned by the phase inversion method. Then five neck-by-neck fibers are co-sintered together to form a plate module at1350℃. The perfomiances of the module for oxygen separation have been studied at different temperatures, feed gases and flow rates. An oxygen permeation flux of1.52ml/min is obtained under air/He(100ml/min) gradient at950℃(Plate length:280mm Hollow fiber O.D.:1.76mm Wall thickness:0.24mm). When sweep gas switched from He to CO2, the oxygen permeation flux almost remain unchanged. The hollow fiber membrane plate shows better mechanical performance than one single fiber. Based on this kind of integration way, further experiments have been done on co-sintering several plates to a block.
Chapter7summarizes the research conducted in this thesis, and presents recommendations for further research.
引文
[1]国家能源科技“十二五”规划2011
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