等离子体催化氨分解制氢的协同效应研究
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摘要
氨分解是极具吸引力的燃料电池原位供氢方法。然而,已有报道主要采用热催化法分解氨气制氢,其中贵金属Ru活性最好但价格昂贵,而其它金属尤其非贵金属活性很低。本论文利用介质阻挡放电等离子体提高了非贵金属催化剂的低温催化活性,从而建立了基于非贵金属的等离子体催化氨分解制氢新方法,并取得以下结果和结论：
1.将介质阻挡放电等离子体和非贵金属催化剂耦合用于氨分解制氢反应中,获得了显著的协同效应。例如,在10g体相Fe基催化剂存在下,NH3进料量为40ml/min、410℃的条件下,氨气转化率由热催化法的7.8%提高至99.9%(32.4W),氨气完全转化的温度比热催化法降低了140℃；制氢能量效率由单纯等离子体法的0.43mol/kW-h提高至4.96mol/kW-h。
2.催化剂在协同效应中占据主导地位。首先,催化剂能够回收利用等离子体放电电热而使反应物得到活化,提高制氢能量效率；其次,催化剂表面放电改善了等离子体放电效果,由不均匀的丝状放电转变为较均匀的微放电、增加放电区面积和放电电流,电子密度得到大幅度增加,使得反应物分子与电子发生非弹性碰撞而被活化的概率增加；此外,催化剂表面放电使得催化剂能够直接利用等离子体区的活性物种。
3.等离子体在协同效应中起到重要的辅助作用。首先,用自行建立的等离子体脱附技术以及OES、FTIR和15NH3同位素示踪研究发现：等离子体区的活性物种(NH3*、NH2·、NH等)与催化剂表面吸附态的含N物种的相互作用(Eley-Rideal过程)能够促进产物N物种的脱附,解决了催化剂被强吸附N原子毒化(金属氮化物)的问题；其次,反应物NH3分子被放电活化成活性物种(以NH3*为主),且NH3*物种的浓度与氨分解活性有直接对应关系,由此判断NH3*物种易于在催化剂表面吸附活化。
4.负载型催化剂的金属和载体种类对协同效应具有显著影响。首先,在Fe、Co、Ni和Cu四种金属催化剂中,Co为最佳活性组分,其金属-氮键(M-N)强度适中,即：易形成又易断裂,有利于催化循环,且催化剂表面中间态物种浓度及表面放电面积较大,有利于表面化学反应的发生；其次,在等离子体环境下,载体的相对介电常数显著影响其等离子体催化氨分解协同能力,是选择等离子体催化体系中催化剂载体的重要依据。
5.改进催化剂制备工艺可使等离子体催化氨分解的转化率和制氢能效分别提高40%和2倍多；等离子体催化体系更适合选用高进料速度(～200ml/min);催化剂用量存在最佳值(体相Fe基催化剂10g)；在等离子体环境下,助剂KCl、KNO3、La(NO3)3、 Ce(NO3)3改性催化剂反而使其氨分解反应活性降低,有别于热催化研究。
Ammonia decomposition reaction has received an increasing attention due to the potential of using ammonia as a hydrogen storage medium in hydrogen economy. So far, only noble metal Ru exhibits good catalytic activity for ammonia decomposition in thermal catalysis mode, but metal Ru is too expensive for wide use. The problem of cheap metal catalysts such as supported Fe, Co, Ni lies in the very slow recombinative desorption of the surface adsorbed N atoms. In this study, the activity of the cheap metal catalysts was greatly enhanced by placing the catalyst bed into the plasma zone. Systematic studies were carried out to get insight into the activity enhancement. The following results and conclusions were obtained:
1. A strong synergy was observed in ammonia decomposition when placing the cheap catalyst into the dielectric barrier discharge (DBD) plasma. For example, in the conditions of NH3flow rate being40ml/min, reaction temperature being410"C, input power being32.4W, when a bulk. Fe-based catalyst was used (10g), the ammonia conversion increased from7.8%to99.9%and the reaction temperature decreased by140℃compared to the thermal catalysis. The energy efficiency of H2production increased from0.43mol/kW-h to4.96mol/kW-h compared with the plasma only.
2. The catalyst played a chief role in the synergy of plasma catalysis for ammonia decomposition. First, the catalyst increases the energy efficiency of the plasma by making use of the concomitant heat of the discharge. Second, the discharge was modified by the discharge of catalyst surface, changing from filamentary discharge to microdischarge which increased the uniformity and currents of discharge. Such a modification led to the increase of electron density and inelastic collision of NH3molecules with the electrons. Third, the catalyst can exploit the active species such as excited ammonia molecule (NH3*) to accelerate ammonia conversion.
3. The vital role of plasma for the catalyst was to eliminate the rate-limiting step of the recombinative desorption of surface-adsorbed N atoms. This was confirmed by the self-established plasma desorption technique and other means such as OES, FTIR and15NH3isotope tracing. The acceleration of the recombinative desorption rate of surface-adsorbed N atoms was mainly implemented by heavy active species such as NH3*, NH2·and NH·instead of electrons.
4. Metals and supports both had strong effects on the synergy of plasma and catalyst. Among Fe, Co, Ni and Cu, the supported Co catalyst exhibited the strongest synergy because the moderate strength of Co-N bond favored the formation and cleavage of M-N. More importantly, it was found that the dielectric constant of support had a close relationship with the ammonia conversion, which means that the dielectric constant is an important criterion to choose the support of catalyst in the plasma-catalysis mode.
5. After improvement of catalyst preparation, the ammonia conversion and energy efficiency of Hi production increased by40%and more than two times, respectively. There are optimal values for catalyst dosage (10g for the bulk Fe-based catalyst) and feed flow of reactant (～200ml/min). In the presence of plasma, the activity of catalyst modified by promoter (KCl, KNO3, La(NO3)3or Ce(NO3)3) decreased for ammonia decomposition, which is dfferent from the condition of thermal catalysis.
1.将介质阻挡放电等离子体和非贵金属催化剂耦合用于氨分解制氢反应中,获得了显著的协同效应。例如,在10g体相Fe基催化剂存在下,NH3进料量为40ml/min、410℃的条件下,氨气转化率由热催化法的7.8%提高至99.9%(32.4W),氨气完全转化的温度比热催化法降低了140℃；制氢能量效率由单纯等离子体法的0.43mol/kW-h提高至4.96mol/kW-h。
2.催化剂在协同效应中占据主导地位。首先,催化剂能够回收利用等离子体放电电热而使反应物得到活化,提高制氢能量效率；其次,催化剂表面放电改善了等离子体放电效果,由不均匀的丝状放电转变为较均匀的微放电、增加放电区面积和放电电流,电子密度得到大幅度增加,使得反应物分子与电子发生非弹性碰撞而被活化的概率增加；此外,催化剂表面放电使得催化剂能够直接利用等离子体区的活性物种。
3.等离子体在协同效应中起到重要的辅助作用。首先,用自行建立的等离子体脱附技术以及OES、FTIR和15NH3同位素示踪研究发现：等离子体区的活性物种(NH3*、NH2·、NH等)与催化剂表面吸附态的含N物种的相互作用(Eley-Rideal过程)能够促进产物N物种的脱附,解决了催化剂被强吸附N原子毒化(金属氮化物)的问题；其次,反应物NH3分子被放电活化成活性物种(以NH3*为主),且NH3*物种的浓度与氨分解活性有直接对应关系,由此判断NH3*物种易于在催化剂表面吸附活化。
4.负载型催化剂的金属和载体种类对协同效应具有显著影响。首先,在Fe、Co、Ni和Cu四种金属催化剂中,Co为最佳活性组分,其金属-氮键(M-N)强度适中,即：易形成又易断裂,有利于催化循环,且催化剂表面中间态物种浓度及表面放电面积较大,有利于表面化学反应的发生；其次,在等离子体环境下,载体的相对介电常数显著影响其等离子体催化氨分解协同能力,是选择等离子体催化体系中催化剂载体的重要依据。
5.改进催化剂制备工艺可使等离子体催化氨分解的转化率和制氢能效分别提高40%和2倍多；等离子体催化体系更适合选用高进料速度(～200ml/min);催化剂用量存在最佳值(体相Fe基催化剂10g)；在等离子体环境下,助剂KCl、KNO3、La(NO3)3、 Ce(NO3)3改性催化剂反而使其氨分解反应活性降低,有别于热催化研究。
Ammonia decomposition reaction has received an increasing attention due to the potential of using ammonia as a hydrogen storage medium in hydrogen economy. So far, only noble metal Ru exhibits good catalytic activity for ammonia decomposition in thermal catalysis mode, but metal Ru is too expensive for wide use. The problem of cheap metal catalysts such as supported Fe, Co, Ni lies in the very slow recombinative desorption of the surface adsorbed N atoms. In this study, the activity of the cheap metal catalysts was greatly enhanced by placing the catalyst bed into the plasma zone. Systematic studies were carried out to get insight into the activity enhancement. The following results and conclusions were obtained:
1. A strong synergy was observed in ammonia decomposition when placing the cheap catalyst into the dielectric barrier discharge (DBD) plasma. For example, in the conditions of NH3flow rate being40ml/min, reaction temperature being410"C, input power being32.4W, when a bulk. Fe-based catalyst was used (10g), the ammonia conversion increased from7.8%to99.9%and the reaction temperature decreased by140℃compared to the thermal catalysis. The energy efficiency of H2production increased from0.43mol/kW-h to4.96mol/kW-h compared with the plasma only.
2. The catalyst played a chief role in the synergy of plasma catalysis for ammonia decomposition. First, the catalyst increases the energy efficiency of the plasma by making use of the concomitant heat of the discharge. Second, the discharge was modified by the discharge of catalyst surface, changing from filamentary discharge to microdischarge which increased the uniformity and currents of discharge. Such a modification led to the increase of electron density and inelastic collision of NH3molecules with the electrons. Third, the catalyst can exploit the active species such as excited ammonia molecule (NH3*) to accelerate ammonia conversion.
3. The vital role of plasma for the catalyst was to eliminate the rate-limiting step of the recombinative desorption of surface-adsorbed N atoms. This was confirmed by the self-established plasma desorption technique and other means such as OES, FTIR and15NH3isotope tracing. The acceleration of the recombinative desorption rate of surface-adsorbed N atoms was mainly implemented by heavy active species such as NH3*, NH2·and NH·instead of electrons.
4. Metals and supports both had strong effects on the synergy of plasma and catalyst. Among Fe, Co, Ni and Cu, the supported Co catalyst exhibited the strongest synergy because the moderate strength of Co-N bond favored the formation and cleavage of M-N. More importantly, it was found that the dielectric constant of support had a close relationship with the ammonia conversion, which means that the dielectric constant is an important criterion to choose the support of catalyst in the plasma-catalysis mode.
5. After improvement of catalyst preparation, the ammonia conversion and energy efficiency of Hi production increased by40%and more than two times, respectively. There are optimal values for catalyst dosage (10g for the bulk Fe-based catalyst) and feed flow of reactant (～200ml/min). In the presence of plasma, the activity of catalyst modified by promoter (KCl, KNO3, La(NO3)3or Ce(NO3)3) decreased for ammonia decomposition, which is dfferent from the condition of thermal catalysis.
引文
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