透氧膜反应器焦炉煤气重整制氢催化剂研究
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摘要
焦炉煤气是炼焦过程的副产物,含有大量的H_2、CH_4和CO组份,是一种优良的制氢原料。我国焦炉煤气虽然资源丰富,但实际利用的数量和水平很低,造成了严重的资源浪费和环境污染。氢作为一种清洁能源,受到世界各国的普遍重视。如将焦炉煤气进行回收并用于制氢,不仅能够产生巨大的经济效益,同时也为环境保护做出重要的贡献。
焦炉煤气中甲烷的部分氧化重整是获得H_2的有效途径,但常规甲烷部分氧化重整(POM)需要用纯氧作为反应原料气,这导致过程成本的增加。混合导体透氧膜构建的膜反应器应用于POM过程,使得制氧过程与催化氧化过程耦合在一个反应器内完成,不仅简化了操作,也降低了生产成本。本论文对焦炉煤气甲烷部分氧化重整热力学平衡进行了计算,实验考察了透氧膜反应器内不同催化剂催化性能,提出了透氧膜反应器中焦炉煤气部分氧化催化重整的反应机理,研究开发了焦炉煤气水蒸气重整反应的催化剂。
论文对焦炉煤气甲烷部分氧化重整进行了热力学分析。考察焦炉煤气原始氢含量、CH_4/O_2摩尔比和反应温度及水蒸气加入量对焦炉煤气甲烷部分氧化重整效果的影响。计算表明,最佳的CH_4/O_2比应该在2左右。低于此值后,氢和一氧化碳的选择性会急剧变小;而高于此值时甲烷转化率略微减少,但固态碳生成或一氧化碳的选择性降低。反应温度的升高有利于甲烷转化率、氢和一氧化碳选择性的提高,也有利于减少固体碳的生产量。适量水蒸气的添加可以调节反应的热平衡,也可以少许增加反应气的氢含量。
采用浸渍法制备碱金属氧化物(Li_2O)和稀土金属氧化物(La_2O_3或CeO_2)助剂改性的Ni/Li_2O/REOx/γ-Al_2O_3 (REOx为La_2O_3或CeO_2)催化剂,测定其在BaCo_(0.7)Fe_(0.2)Nb_(0.1)O_(3-δ) (BCFNO)透氧膜反应器中焦炉煤气甲烷部分氧化重整时的透氧性能。CeO_2助剂修饰Ni/Li_2O/γ-Al_2O_3催化剂,产生的透氧量随CeO_2增大而增大。而La_2O_3助剂修饰Ni/Li_2O/γ-Al_2O_3催化剂,适量La_2O_3有利于提高透氧量,La_2O_3过高反而会降低透氧量。Li_2O助剂修饰的Ni/La_2O_3/γ-Al_2O_3催化剂与La_2O_3修饰的催化剂效果相近。
在BCFNO透氧膜反应器上对NiO/MgO固溶体催化剂进行了100小时的考察,结果表明该催化剂重整反应性能较好。在875°C下分别获得17.2 mL/cm2/min透氧量、94.1%甲烷转化率、75%氢和108%一氧化碳选择性。长时间实验过程中膜反应器和催化剂未出现异常,表明此NiO/MgO固溶体催化剂具有较好的催化活性和稳定性。论文还对比分析了钴镁固溶体催化剂和镍镁固溶体催化剂在BCFNO透氧膜反应器内焦炉煤气甲烷部分氧化重整性能。
根据实验结果推断了膜反应器中焦炉煤气重整反应的机理:首先是焦炉煤气中的H_2在催化剂活性组分Ni颗粒上解离,解离后的氢向高活性位迁移(“三相界面”)并与膜表面侧晶格氧(或O~(2-))反应生成H_2O。同时CH_4也可能在催化剂表面活性位上裂解,裂解后的碳沉积在催化剂表面。甲烷裂解后形成的氢迁移到三相界面和膜表面侧晶格氧(或O~(2-))反应生成H_2O。三相界面处形成的H_2O与催化剂表面沉积的碳反应,生成H_2和CO。未反应完的H_2O和剩余CH_4在催化层重整段发生水蒸气重整反应,生成H_2和CO,致使H_2和CO选择性增大。
透氧膜反应器中的催化剂功能分别在二个区域内实现:接近膜表面的催化区域使得氢解离而与膜透过的氧反应生成H_2O,氢可能是反应气体本身所带有的,或者是甲烷在催化剂上裂解所产生的。远离膜表面的催化区域实现了氧化反应产生的水与剩余甲烷的重整。
采用镍镁固溶体催化剂研究了焦炉煤气中甲烷的水蒸气重整催化性能。考察Ni负载量、反应温度、水碳比等因素对催化活性的影响。结果表明:NiO/MgO固溶体催化剂具有良好的活性,重整过程中水碳比和反应温度对CH_4和CO_2转化率影响较大。在875oC,低水碳比(H_2O/CH_4=1)条件下进行了100 h稳定性实验,CH_4转化率保持在97%左右,产生的氢为原始氢2.5倍。镍镁固溶体催化剂具有良好的催化活性和稳定性,适合于焦炉煤气在远离膜表面的催化区域内的水蒸气重整。
Coke oven gas (COG), a byproduct in the coke-making process, which mainly containing H_2, CH_4, CO, and small amounts of other matters, is a good raw material of H_2 production. The production of COG is huge in China, however only part of produced COG is simply utilized as fuel. A large amount of COG is directly burnt at the end of an opened chimney and then directly discharged into atmospheres, thus resulting in a serious air pollution. Hydrogen as a clean energy has been received a widespread attention around the world. Production of hydrogen by converting COG not only resolves the environment pollution problem but also brings down the cost of the hydrogen production.
Partial oxidation of methane (POM) in COG is a promising technology and the most economic way to obtain hydrogen. However, the main difficulty with POM lied in the consumption of large quantities of expensive pure oxygen that was produced through cryogenic air separation process. Coupling POM with a mixed ionic and electronic conductor oxygen permeation membrane could allow for the separation of oxygen and the catalytic oxidation in one unit, therefore not only simplifing the operation unit, but also reducing the production cost. The thermodynamic analysis of the POM in COG is discussed in this paper. Then the performance of several catalysts packed on the BaCo0.7Fe0.2Nb0.1O3-δ(BCFNO) membrane reactor is investigated for catalytic partial oxidation reforming of COG. As well as the reaction pathways of the reforming of COG in BCFNO membrane reactor are proposed according to the investigations in different membrane reactor configurations and different kinds of gas. Finally a Ni-based catalyst for steam reforming of COG was reported.
Firstly, the profound thermodynamic analysis of hydrogen production of COG by POM was presented in this paper. The effect of the original hydrogen, steam addition, reaction temperature, energy consumption of steam addition and the ratio of CH_4/O_2 on the conversion of CH_4 and the selectivity of H_2 or CO for COG reforming are carefully examined. The results show the optimization of CH_4/O_2 molar ratio should be 2. The H_2 and CO selectivity would decrease sharply, when the CH_4/O_2 molar ratio <2. However, when CH_4/O_2 molar ratio>2, CH_4 conversion would decrease slowly, while solid carbon would be generated, and CO selectivity would be decreased. With increase of reaction temperature, the CH_4 conversion, H_2 and CO selectivity would increase and the formation of solid carbon could be suppressed. The optimal steam addition could change the enthalpy of reaction, also could enhance the H_2 yields.
Ni/Li_2O/REOx/γ-Al_2O_3 catalysts with different Li_2O contents and different REOx (La_2O_3 or CeO_2) contents were prepared by impregnation method and investigated the catalytic performance for POM in COG on BCFNO membrane reactor here. Results showed that the Ni/Li_2O/γ-Al_2O_3 catalysts modified by different CeO_2 contents were benefited to enhance oxygen permeation, and oxygen permeation increased with increasing the CeO_2 contents. For the Ni/Li_2O/γ-Al_2O_3 catalysts modified by different La_2O_3 contents, oxygen permeation increased firstly then decreased with increasing the La_2O_3 contents. And the effect of Li_2O on oxygen permeation was same to the Ni/Li_2O/γ-Al_2O_3 catalysts modified by La_2O_3.
The catalytic performance for POM of COG of NiO/MgO solid solution catalyst packed on BCFNO membrane reactor is also investigated here. The reforming process is performed successfully: 94.1% of CH_4 conversion, 75% of H_2 selectivity, 108% of CO selectivity and 17.2 mL/cm2/min of oxygen permeation flux are achieved at 875 oC. The reaction has been steadily carried out for more than 100 h. The results showed that the NiO/MgO solid solution catalyst had a good catalytic activity and stability. Comparison over CoO/MgO solid solution and NiO/MgO solid solution catalyst for the performance of POM in BCFNO membrane reactor are also analyzed.
According to the results of the reforming of COG in BCFNO membrane reactor, the reaction scheme was proposed that H_2 could be dissociated on the active Ni surface to H. Then H migrated to the“triphase boundary”reacted with lattice oxygen or oxygen ionic to form H_2O. The cracking of CH_4 also might be existed formed surface Ni ??? Cspecies and H. The H repeated former again. The oxidized product, H_2O can further react with the Ni ??? Cspecies, forming the metal Ni0, H_2 and CO. And also the H_2O formed could react with the residual CH_4 on the catalyst-bed to form H_2 and CO.
The catalyst function was achieved in two regions in an oxygen permeation membrane reactor: H_2 dissociated and reacted with lattice oxygen or oxygen ionic to form H_2O near the membrane surface, The Hydrogen might come from the reaction gas or the cracking of CH_4 on catalyst. The H_2O formed could react with the residual CH_4 away from the membrane surface area.
At last the steam reforming of COG for hydrogen production was investigated over the NiO/MgO solid solution catalysts reduced at high temperature. It was found that the NiO/MgO catalyst possessed good catalytic activity, and the conversions of CH_4 and CO_2 were greatly affected by the reaction temperature and water to methane (S/C) mole ratio. During the tested period of 100 h under a low S/C ratio of 1.0 at 875 oC, the conversions of CH_4 kept constant values around 97% and the hydrogen volume content was enhanced from 58.2% in the original COG to 77.7% by 1.5 times. These results show that the NiO/MgO catalyst was efficient and stable for the steam reforming of COG to amplify hydrogen in COG.
焦炉煤气中甲烷的部分氧化重整是获得H_2的有效途径,但常规甲烷部分氧化重整(POM)需要用纯氧作为反应原料气,这导致过程成本的增加。混合导体透氧膜构建的膜反应器应用于POM过程,使得制氧过程与催化氧化过程耦合在一个反应器内完成,不仅简化了操作,也降低了生产成本。本论文对焦炉煤气甲烷部分氧化重整热力学平衡进行了计算,实验考察了透氧膜反应器内不同催化剂催化性能,提出了透氧膜反应器中焦炉煤气部分氧化催化重整的反应机理,研究开发了焦炉煤气水蒸气重整反应的催化剂。
论文对焦炉煤气甲烷部分氧化重整进行了热力学分析。考察焦炉煤气原始氢含量、CH_4/O_2摩尔比和反应温度及水蒸气加入量对焦炉煤气甲烷部分氧化重整效果的影响。计算表明,最佳的CH_4/O_2比应该在2左右。低于此值后,氢和一氧化碳的选择性会急剧变小;而高于此值时甲烷转化率略微减少,但固态碳生成或一氧化碳的选择性降低。反应温度的升高有利于甲烷转化率、氢和一氧化碳选择性的提高,也有利于减少固体碳的生产量。适量水蒸气的添加可以调节反应的热平衡,也可以少许增加反应气的氢含量。
采用浸渍法制备碱金属氧化物(Li_2O)和稀土金属氧化物(La_2O_3或CeO_2)助剂改性的Ni/Li_2O/REOx/γ-Al_2O_3 (REOx为La_2O_3或CeO_2)催化剂,测定其在BaCo_(0.7)Fe_(0.2)Nb_(0.1)O_(3-δ) (BCFNO)透氧膜反应器中焦炉煤气甲烷部分氧化重整时的透氧性能。CeO_2助剂修饰Ni/Li_2O/γ-Al_2O_3催化剂,产生的透氧量随CeO_2增大而增大。而La_2O_3助剂修饰Ni/Li_2O/γ-Al_2O_3催化剂,适量La_2O_3有利于提高透氧量,La_2O_3过高反而会降低透氧量。Li_2O助剂修饰的Ni/La_2O_3/γ-Al_2O_3催化剂与La_2O_3修饰的催化剂效果相近。
在BCFNO透氧膜反应器上对NiO/MgO固溶体催化剂进行了100小时的考察,结果表明该催化剂重整反应性能较好。在875°C下分别获得17.2 mL/cm2/min透氧量、94.1%甲烷转化率、75%氢和108%一氧化碳选择性。长时间实验过程中膜反应器和催化剂未出现异常,表明此NiO/MgO固溶体催化剂具有较好的催化活性和稳定性。论文还对比分析了钴镁固溶体催化剂和镍镁固溶体催化剂在BCFNO透氧膜反应器内焦炉煤气甲烷部分氧化重整性能。
根据实验结果推断了膜反应器中焦炉煤气重整反应的机理:首先是焦炉煤气中的H_2在催化剂活性组分Ni颗粒上解离,解离后的氢向高活性位迁移(“三相界面”)并与膜表面侧晶格氧(或O~(2-))反应生成H_2O。同时CH_4也可能在催化剂表面活性位上裂解,裂解后的碳沉积在催化剂表面。甲烷裂解后形成的氢迁移到三相界面和膜表面侧晶格氧(或O~(2-))反应生成H_2O。三相界面处形成的H_2O与催化剂表面沉积的碳反应,生成H_2和CO。未反应完的H_2O和剩余CH_4在催化层重整段发生水蒸气重整反应,生成H_2和CO,致使H_2和CO选择性增大。
透氧膜反应器中的催化剂功能分别在二个区域内实现:接近膜表面的催化区域使得氢解离而与膜透过的氧反应生成H_2O,氢可能是反应气体本身所带有的,或者是甲烷在催化剂上裂解所产生的。远离膜表面的催化区域实现了氧化反应产生的水与剩余甲烷的重整。
采用镍镁固溶体催化剂研究了焦炉煤气中甲烷的水蒸气重整催化性能。考察Ni负载量、反应温度、水碳比等因素对催化活性的影响。结果表明:NiO/MgO固溶体催化剂具有良好的活性,重整过程中水碳比和反应温度对CH_4和CO_2转化率影响较大。在875oC,低水碳比(H_2O/CH_4=1)条件下进行了100 h稳定性实验,CH_4转化率保持在97%左右,产生的氢为原始氢2.5倍。镍镁固溶体催化剂具有良好的催化活性和稳定性,适合于焦炉煤气在远离膜表面的催化区域内的水蒸气重整。
Coke oven gas (COG), a byproduct in the coke-making process, which mainly containing H_2, CH_4, CO, and small amounts of other matters, is a good raw material of H_2 production. The production of COG is huge in China, however only part of produced COG is simply utilized as fuel. A large amount of COG is directly burnt at the end of an opened chimney and then directly discharged into atmospheres, thus resulting in a serious air pollution. Hydrogen as a clean energy has been received a widespread attention around the world. Production of hydrogen by converting COG not only resolves the environment pollution problem but also brings down the cost of the hydrogen production.
Partial oxidation of methane (POM) in COG is a promising technology and the most economic way to obtain hydrogen. However, the main difficulty with POM lied in the consumption of large quantities of expensive pure oxygen that was produced through cryogenic air separation process. Coupling POM with a mixed ionic and electronic conductor oxygen permeation membrane could allow for the separation of oxygen and the catalytic oxidation in one unit, therefore not only simplifing the operation unit, but also reducing the production cost. The thermodynamic analysis of the POM in COG is discussed in this paper. Then the performance of several catalysts packed on the BaCo0.7Fe0.2Nb0.1O3-δ(BCFNO) membrane reactor is investigated for catalytic partial oxidation reforming of COG. As well as the reaction pathways of the reforming of COG in BCFNO membrane reactor are proposed according to the investigations in different membrane reactor configurations and different kinds of gas. Finally a Ni-based catalyst for steam reforming of COG was reported.
Firstly, the profound thermodynamic analysis of hydrogen production of COG by POM was presented in this paper. The effect of the original hydrogen, steam addition, reaction temperature, energy consumption of steam addition and the ratio of CH_4/O_2 on the conversion of CH_4 and the selectivity of H_2 or CO for COG reforming are carefully examined. The results show the optimization of CH_4/O_2 molar ratio should be 2. The H_2 and CO selectivity would decrease sharply, when the CH_4/O_2 molar ratio <2. However, when CH_4/O_2 molar ratio>2, CH_4 conversion would decrease slowly, while solid carbon would be generated, and CO selectivity would be decreased. With increase of reaction temperature, the CH_4 conversion, H_2 and CO selectivity would increase and the formation of solid carbon could be suppressed. The optimal steam addition could change the enthalpy of reaction, also could enhance the H_2 yields.
Ni/Li_2O/REOx/γ-Al_2O_3 catalysts with different Li_2O contents and different REOx (La_2O_3 or CeO_2) contents were prepared by impregnation method and investigated the catalytic performance for POM in COG on BCFNO membrane reactor here. Results showed that the Ni/Li_2O/γ-Al_2O_3 catalysts modified by different CeO_2 contents were benefited to enhance oxygen permeation, and oxygen permeation increased with increasing the CeO_2 contents. For the Ni/Li_2O/γ-Al_2O_3 catalysts modified by different La_2O_3 contents, oxygen permeation increased firstly then decreased with increasing the La_2O_3 contents. And the effect of Li_2O on oxygen permeation was same to the Ni/Li_2O/γ-Al_2O_3 catalysts modified by La_2O_3.
The catalytic performance for POM of COG of NiO/MgO solid solution catalyst packed on BCFNO membrane reactor is also investigated here. The reforming process is performed successfully: 94.1% of CH_4 conversion, 75% of H_2 selectivity, 108% of CO selectivity and 17.2 mL/cm2/min of oxygen permeation flux are achieved at 875 oC. The reaction has been steadily carried out for more than 100 h. The results showed that the NiO/MgO solid solution catalyst had a good catalytic activity and stability. Comparison over CoO/MgO solid solution and NiO/MgO solid solution catalyst for the performance of POM in BCFNO membrane reactor are also analyzed.
According to the results of the reforming of COG in BCFNO membrane reactor, the reaction scheme was proposed that H_2 could be dissociated on the active Ni surface to H. Then H migrated to the“triphase boundary”reacted with lattice oxygen or oxygen ionic to form H_2O. The cracking of CH_4 also might be existed formed surface Ni ??? Cspecies and H. The H repeated former again. The oxidized product, H_2O can further react with the Ni ??? Cspecies, forming the metal Ni0, H_2 and CO. And also the H_2O formed could react with the residual CH_4 on the catalyst-bed to form H_2 and CO.
The catalyst function was achieved in two regions in an oxygen permeation membrane reactor: H_2 dissociated and reacted with lattice oxygen or oxygen ionic to form H_2O near the membrane surface, The Hydrogen might come from the reaction gas or the cracking of CH_4 on catalyst. The H_2O formed could react with the residual CH_4 away from the membrane surface area.
At last the steam reforming of COG for hydrogen production was investigated over the NiO/MgO solid solution catalysts reduced at high temperature. It was found that the NiO/MgO catalyst possessed good catalytic activity, and the conversions of CH_4 and CO_2 were greatly affected by the reaction temperature and water to methane (S/C) mole ratio. During the tested period of 100 h under a low S/C ratio of 1.0 at 875 oC, the conversions of CH_4 kept constant values around 97% and the hydrogen volume content was enhanced from 58.2% in the original COG to 77.7% by 1.5 times. These results show that the NiO/MgO catalyst was efficient and stable for the steam reforming of COG to amplify hydrogen in COG.
引文
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