碳纳米管负载过渡金属氮化物的合成及其在氨分解制氢中的催化性能研究
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摘要
质子交换膜燃料电池（PEMFC）以氢气作为燃料，无污染、质量轻、效率高，在电动汽车及各种可移动设备的动力电源方面具有潜在的应用前景。氨催化分解产物为H_2和N_2，不含易使燃料电池电极中毒的CO_x，被认为是最有希望用于车载质子交换膜燃料电池的制氢技术。然而，现有催化剂的制氢效率还不能满足车载燃料电池。因此，设计和合成高效稳定的氨分解催化剂具有重要的意义。过渡金属氮化物在许多涉氢反应中表现出与贵金属相类似的催化性能，有望成为新一代氨分解催化剂。鉴于此，本文以碳纳米管为载体，采用程序升温氮化法制备出性能优异的负载型钴钼双金属氮化物催化剂，对其制备条件、反应工艺以及反应机理等进行了研究，应用多种先进的表征手段对催化剂形貌、结构进行了细致而深入的研究，并与其催化性能相关联。主要包括以下几部分内容：
1.论文首先对催化剂的活性组分进行了筛选。以碳纳米管为载体，采用程序升温氮化法制备了四种单组分金属氮化物（CoN_x/CNTs、F eN_x/CNTs、M oN_x/CNTs和NiN_x/CNTs）催化剂，并研究了它们的催化性能。进而选用Co和Mo制备出双组分金属氮化物催化剂。结果表明，当Co含量为2wt%、Mo含量为15wt%时，CoMoN_x/CNTs催化剂具有较好的氨分解活性。通过XRD、H_2-TPR以及XPS等表征发现，CoMoN_x/CNTs催化剂中存在γ-Mo2N、Co3Mo3N和Co4N等多种形式的氮化物，可能还有少量的MoO_3或CoMoO_4。CoMoN_x/CNTs催化剂表面Mo离子主要以Mo6+的高价态形式存在，其次还有少量的Mo~(4+)和Mo~(δ+)(0<δ <4)存在。
2.研究了K、Ba、La、Ce和Zr等助剂对CoMoN_x/CNTs催化剂活性和稳定性的影响。结果发现，L a修饰的CoMoN_x/CNTs催化剂性能最好。X RD、B ET、T G-DSC、H_2-TPD、 H_2-TPR和XPS等测试结果表明，L a的引入，增加了催化剂表面低价态钼物种Mo~(δ+)(0<δ <4)的含量；降低了催化剂表面钝化层中氧化物的还原温度以及催化剂对H_2和N_2的吸附作用；提高了催化剂表面活性组分的分散度以及催化剂的热稳定性。
3.金属氮化物的生成是“局部规整反应”，制备过程中氮化空速、升温速率、氮化温度、氮化气体组成和前驱体等对其结构和性能都有重要的影响。XRD和元素分析结果显示,提高空速有助于晶粒度小的氮化物生成。升温速率过快与过慢都不利于晶相完整、晶粒细小的氮化物形成。H2/N2-TPD结果表明,700℃下氮化得到的催化剂对氮气和氢气的吸附作用较弱,有利于氨分解反应的进行。XPS结果显示,当低温段V(H2):V(N2)=5：1,高温段V(N2):V(H2)=1:1时,催化剂表面低价态钼物种Moδ+(0<δ<4)所占的比例最高。
4.考察了反应温度、反应气体空速以及氨气初始浓度对La-CoMoNx/CNTs催化剂氨分解活性的影响。结果表明,反应温度越高,催化剂上氨转化率越高。在同一温度下,空速越高,氨转化率越低。氨转化率与氨气初始浓度无关。最佳反应工艺条件为：反应气空速确定为10000h-1,反应温度以650℃左右为宜。
5.比较了La-CoMoNx/CNTs催化剂与文献中报道的Ru/CNTs催化剂以及工业合成氨用熔铁催化剂的氨分解活性,并对其稳定性进行了研究。结果表明,本实验制备的La-CoMoNx/CNTs催化剂具有很好的催化活性,650℃时,氨转化率可达99%以上,且具有良好的稳定性。
6.确定了La-CoMoNx/CNTs催化剂上氨分解反应的本征动力学方程为：
同时验证了La-CoMoNx/CNTs催化剂上氨分解反应遵循Temkin-Pyzhev机理,表面氮原子的结合脱附为反应的速度控制步骤。
本论文的创新之处：
1.研制出适用于为燃料电池提供氢源的氨分解反应的La-CoMoNx/CNTs催化剂,该催化剂具有优异的催化活性以及良好的稳定性,优于目前工业合成氨中使用的熔铁催化剂以及文献中报道的Ru/CNTs等催化剂,在氨分解制氢反应中具有很好的应用前景。
2.确定了La-CoMoNx/CNTs催化剂上氨分解反应的本征动力学方程为：
同时验证了La-CoMoNx/CNTs催化剂上氨分解反应遵循Temkin-Pyzhev机理,表面氮原子的结合脱附为反应的速度控制步骤。
Proton exchange membrane fuel cell(PEMFC) is the most promising power source for electric cars as well as portable equipments due to its favorable advantages, such as high efficiency,low weight and less environmental impact. In recent years, ammonia decomposition has been attracted considerable attentions due to its use as a COx-free source of hydrogen for proton exchange membrane fuel cells. However, the activities of the present catalysts for ammonia decomposition are still low and could not meet the demand of on-board fuel cells. Therefore, the design and synthesis of highly efficient and stable catalysts for ammonia decomposition are of great significance.Transition metal nitrides are metallic interstitial compounds with unique physical and chemical properties because the element N fills into the metallic crystalline structure. They exhibit the catalytic characteristics similar to the precious metals and have shown excellent properties in a number of hydrogen-involved reactions such as ammonia synthesis and decomposition, HDN, HDS and F-T synthesis. A series of Co-Mo nitride catalysts supported on carbon nanotubes were synthesized through temperature programmed reaction. The physicochemical properties of the catalysts were characterized by XRD, BET, XRD, BET, SEM, TG/DSC, H_2-TPR/TPD, XPS techniques. In the meantime, the kinetic behavior of the ammonia decomposition reaction over high stable La-CoMoN_x/CNTs catalyst was investigated. A mechanism of the ammonia decomposition was proposed.
Some details are as follows:
1. A series of carbon nanotubes supported transition metal nitrides such as CoN_x/CNTs, FeN_x/CNTs, MoN_x/CNTs and NiN_x/CNTs were prepared by temperature programmed method in N_2-H_2mixture gases. Their surface composition and catalytic performance for ammonia decomposition were compared. Furthermore, the CoMoN_x/CNTscatalyst with Co content of2wt%and Mo content of15wt%was found to be the most suitable catalyst for ammonia decomposition. The XRD results indicated that the activity centers are not a single phase, but the various kinds of γ-Mo2N, Co3Mo3N and Co4N, even a certain quantity of MoO_3and CoMoO_4. The XPS results suggested that there were Mo~(6+), Mo~(4+) and Mo~(δ+)(0<δ <4) ions on the surface of the Co-Mo nitride catalysts.
2. The effects of cationic promoters (K, Ba, La, Ce and Zr) on the catalytic performance and surface properties of the catalysts were investigated. It was found that doping appropriate amount of K, Ba, La, Ce and Zr into CoMoNx/CNTs catalysts improved the catalytic activity to some extent, and the La-CoMoNx/CNTs catalyst showed the highest ammonia conversion of99%at650℃. The results of XRD, BET, TG/DSC, H2-TPR/TPD and XPS indicated that that the addition of promoters changed the state of active sites and the content of low valence molybdenum species Moδ+(0<δ<4), and the distribution of active species increased and the catalytic stability improved.
3. The influence of the synthesis factors, such as including preparation methods, calcination temperature and type of oxide precursors, space velocity of nitriding gases, N2-H2ratio and nitriding temperature on catalytic activity of CoMoNx/CNTs was investigated in detail. The results showed the optimal nitriding conditions were as follows:the calcination temperature was500℃, calcination time was4h, the nitriding temperature was700℃, GHSV was10000h-1, the heating rate was1℃/min(300-500℃) and2.5℃/min(500-700℃), while the composition of nitriding gases was V(H2):V(N2)=5:1(300～500℃) and V(N2):V(H2)=1:1(500～700℃).
4. The influence of reaction conditions including temperature, time, space velocity and pressure were studied. The results showed that temperature and space velocity have remarked influence on the catalytic activity of La-CoMoNx/CNTs for ammonia decomposition. The ammonia conversion increased with the increasing of reaction temperatures, reaching more than99%at650℃. It was also found that the ammonia conversion increased with the decreasing of GHSV of ammonia at the same temperature, and the content of ammonia in the raw materials had no effect on its activity. The optimal reaction conditions were as follows: the reaction temperature was about650℃and GHSV was10000h-1
5. Thermal stability experiment shown that La-CoMoNx/CNTs catalyst had a better thermal stability, and the ammonia conversion maintained above95%for30h at600℃and NH3space velocity of5000h-1
6. The reaction kinetics equation of ammonia decomposition on La-CoMoNx/CNTs was determined:
The reaction mechanism was proposed. The reaction rate of ammonia decomposition over La-CoMoNx/CNTs was controlled by the combination desorption of nitrogen on the surface of the catalyst.
The inovation of this dissertation are as follows:
1. The La-CoMoNx/CNTs catalyst with good activity and stability for ammonia decomposition to produce hydrogen for fuel cells has been developed.
2. The reaction kinetics equation of ammonia decomposition on La-CoMoNx/CNTs was determined:
The reaction mechanism was proposed. The reaction rate of ammonia decomposition over La-CoMoNx/CNTs was controlled by the combination desorption of nitrogen on the surface of the catalyst.
1.论文首先对催化剂的活性组分进行了筛选。以碳纳米管为载体，采用程序升温氮化法制备了四种单组分金属氮化物（CoN_x/CNTs、F eN_x/CNTs、M oN_x/CNTs和NiN_x/CNTs）催化剂，并研究了它们的催化性能。进而选用Co和Mo制备出双组分金属氮化物催化剂。结果表明，当Co含量为2wt%、Mo含量为15wt%时，CoMoN_x/CNTs催化剂具有较好的氨分解活性。通过XRD、H_2-TPR以及XPS等表征发现，CoMoN_x/CNTs催化剂中存在γ-Mo2N、Co3Mo3N和Co4N等多种形式的氮化物，可能还有少量的MoO_3或CoMoO_4。CoMoN_x/CNTs催化剂表面Mo离子主要以Mo6+的高价态形式存在，其次还有少量的Mo~(4+)和Mo~(δ+)(0<δ <4)存在。
2.研究了K、Ba、La、Ce和Zr等助剂对CoMoN_x/CNTs催化剂活性和稳定性的影响。结果发现，L a修饰的CoMoN_x/CNTs催化剂性能最好。X RD、B ET、T G-DSC、H_2-TPD、 H_2-TPR和XPS等测试结果表明，L a的引入，增加了催化剂表面低价态钼物种Mo~(δ+)(0<δ <4)的含量；降低了催化剂表面钝化层中氧化物的还原温度以及催化剂对H_2和N_2的吸附作用；提高了催化剂表面活性组分的分散度以及催化剂的热稳定性。
3.金属氮化物的生成是“局部规整反应”，制备过程中氮化空速、升温速率、氮化温度、氮化气体组成和前驱体等对其结构和性能都有重要的影响。XRD和元素分析结果显示,提高空速有助于晶粒度小的氮化物生成。升温速率过快与过慢都不利于晶相完整、晶粒细小的氮化物形成。H2/N2-TPD结果表明,700℃下氮化得到的催化剂对氮气和氢气的吸附作用较弱,有利于氨分解反应的进行。XPS结果显示,当低温段V(H2):V(N2)=5：1,高温段V(N2):V(H2)=1:1时,催化剂表面低价态钼物种Moδ+(0<δ<4)所占的比例最高。
4.考察了反应温度、反应气体空速以及氨气初始浓度对La-CoMoNx/CNTs催化剂氨分解活性的影响。结果表明,反应温度越高,催化剂上氨转化率越高。在同一温度下,空速越高,氨转化率越低。氨转化率与氨气初始浓度无关。最佳反应工艺条件为：反应气空速确定为10000h-1,反应温度以650℃左右为宜。
5.比较了La-CoMoNx/CNTs催化剂与文献中报道的Ru/CNTs催化剂以及工业合成氨用熔铁催化剂的氨分解活性,并对其稳定性进行了研究。结果表明,本实验制备的La-CoMoNx/CNTs催化剂具有很好的催化活性,650℃时,氨转化率可达99%以上,且具有良好的稳定性。
6.确定了La-CoMoNx/CNTs催化剂上氨分解反应的本征动力学方程为：
同时验证了La-CoMoNx/CNTs催化剂上氨分解反应遵循Temkin-Pyzhev机理,表面氮原子的结合脱附为反应的速度控制步骤。
本论文的创新之处：
1.研制出适用于为燃料电池提供氢源的氨分解反应的La-CoMoNx/CNTs催化剂,该催化剂具有优异的催化活性以及良好的稳定性,优于目前工业合成氨中使用的熔铁催化剂以及文献中报道的Ru/CNTs等催化剂,在氨分解制氢反应中具有很好的应用前景。
2.确定了La-CoMoNx/CNTs催化剂上氨分解反应的本征动力学方程为：
同时验证了La-CoMoNx/CNTs催化剂上氨分解反应遵循Temkin-Pyzhev机理,表面氮原子的结合脱附为反应的速度控制步骤。
Proton exchange membrane fuel cell(PEMFC) is the most promising power source for electric cars as well as portable equipments due to its favorable advantages, such as high efficiency,low weight and less environmental impact. In recent years, ammonia decomposition has been attracted considerable attentions due to its use as a COx-free source of hydrogen for proton exchange membrane fuel cells. However, the activities of the present catalysts for ammonia decomposition are still low and could not meet the demand of on-board fuel cells. Therefore, the design and synthesis of highly efficient and stable catalysts for ammonia decomposition are of great significance.Transition metal nitrides are metallic interstitial compounds with unique physical and chemical properties because the element N fills into the metallic crystalline structure. They exhibit the catalytic characteristics similar to the precious metals and have shown excellent properties in a number of hydrogen-involved reactions such as ammonia synthesis and decomposition, HDN, HDS and F-T synthesis. A series of Co-Mo nitride catalysts supported on carbon nanotubes were synthesized through temperature programmed reaction. The physicochemical properties of the catalysts were characterized by XRD, BET, XRD, BET, SEM, TG/DSC, H_2-TPR/TPD, XPS techniques. In the meantime, the kinetic behavior of the ammonia decomposition reaction over high stable La-CoMoN_x/CNTs catalyst was investigated. A mechanism of the ammonia decomposition was proposed.
Some details are as follows:
1. A series of carbon nanotubes supported transition metal nitrides such as CoN_x/CNTs, FeN_x/CNTs, MoN_x/CNTs and NiN_x/CNTs were prepared by temperature programmed method in N_2-H_2mixture gases. Their surface composition and catalytic performance for ammonia decomposition were compared. Furthermore, the CoMoN_x/CNTscatalyst with Co content of2wt%and Mo content of15wt%was found to be the most suitable catalyst for ammonia decomposition. The XRD results indicated that the activity centers are not a single phase, but the various kinds of γ-Mo2N, Co3Mo3N and Co4N, even a certain quantity of MoO_3and CoMoO_4. The XPS results suggested that there were Mo~(6+), Mo~(4+) and Mo~(δ+)(0<δ <4) ions on the surface of the Co-Mo nitride catalysts.
2. The effects of cationic promoters (K, Ba, La, Ce and Zr) on the catalytic performance and surface properties of the catalysts were investigated. It was found that doping appropriate amount of K, Ba, La, Ce and Zr into CoMoNx/CNTs catalysts improved the catalytic activity to some extent, and the La-CoMoNx/CNTs catalyst showed the highest ammonia conversion of99%at650℃. The results of XRD, BET, TG/DSC, H2-TPR/TPD and XPS indicated that that the addition of promoters changed the state of active sites and the content of low valence molybdenum species Moδ+(0<δ<4), and the distribution of active species increased and the catalytic stability improved.
3. The influence of the synthesis factors, such as including preparation methods, calcination temperature and type of oxide precursors, space velocity of nitriding gases, N2-H2ratio and nitriding temperature on catalytic activity of CoMoNx/CNTs was investigated in detail. The results showed the optimal nitriding conditions were as follows:the calcination temperature was500℃, calcination time was4h, the nitriding temperature was700℃, GHSV was10000h-1, the heating rate was1℃/min(300-500℃) and2.5℃/min(500-700℃), while the composition of nitriding gases was V(H2):V(N2)=5:1(300～500℃) and V(N2):V(H2)=1:1(500～700℃).
4. The influence of reaction conditions including temperature, time, space velocity and pressure were studied. The results showed that temperature and space velocity have remarked influence on the catalytic activity of La-CoMoNx/CNTs for ammonia decomposition. The ammonia conversion increased with the increasing of reaction temperatures, reaching more than99%at650℃. It was also found that the ammonia conversion increased with the decreasing of GHSV of ammonia at the same temperature, and the content of ammonia in the raw materials had no effect on its activity. The optimal reaction conditions were as follows: the reaction temperature was about650℃and GHSV was10000h-1
5. Thermal stability experiment shown that La-CoMoNx/CNTs catalyst had a better thermal stability, and the ammonia conversion maintained above95%for30h at600℃and NH3space velocity of5000h-1
6. The reaction kinetics equation of ammonia decomposition on La-CoMoNx/CNTs was determined:
The reaction mechanism was proposed. The reaction rate of ammonia decomposition over La-CoMoNx/CNTs was controlled by the combination desorption of nitrogen on the surface of the catalyst.
The inovation of this dissertation are as follows:
1. The La-CoMoNx/CNTs catalyst with good activity and stability for ammonia decomposition to produce hydrogen for fuel cells has been developed.
2. The reaction kinetics equation of ammonia decomposition on La-CoMoNx/CNTs was determined:
The reaction mechanism was proposed. The reaction rate of ammonia decomposition over La-CoMoNx/CNTs was controlled by the combination desorption of nitrogen on the surface of the catalyst.
引文
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