V_2O_5/AC催化剂脱硝过程中若干重要问题的研究
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摘要
煤炭是我国最丰富的化石能源，我国以煤炭为主要一次能源的格局在未来相当长时期内不会发生改变。煤炭在我国的主要利用方式是直接燃烧，用量占煤炭总消耗量的80%以上。煤炭的大量燃烧已经导致我国的很多地区呈现严重的煤烟型大气污染，NOx（氮氧化物，简称硝）是主要污染物之一，其对人体健康和生态环境均构成了巨大的威胁。
烟气脱硝的技术很多，但以NH_3为还原剂的选择性催化还原（SCR）法在世界上应用最多、研究最广、技术最成熟且最有成效。针对目前以V_2O_5/TiO_2催化剂为代表的中温脱硝技术（～400℃）所存在的问题，前人研究开发了以活性焦为载体的V_2O_5/AC催化剂，发现其具有较高的低温（～200℃）脱硝活性和抗SO_2毒化性能，应用前景广阔，研究范畴涉及制备条件、反应行为、SO_2和H_2O的影响、反应机理和动力学等。然而到目前为止，人们在活性焦性质对中毒物硫铵盐稳定性的影响、SO_2影响催化剂脱硝的机理、SCR反应选择性、催化剂的热稳定性及挥发性重金属Hg对催化剂脱硝行为的影响等方面还缺乏认识。本论文针对上述问题进行了深入研究，得到以下主要结论：
（1）脱硝过程中产生的中毒物NH_4HSO_4首先沉积在AC表面的强吸附位上，随着其量的增加再逐渐沉积在弱吸附位上。在惰性气氛中，NH_4HSO_4在AC表面的程序升温分解过程为两步反应机理：从170℃起生成NH_3和H_2SO_4，后者在较高的温度下被AC还原为SO_2气体。NO的存在和V_2O_5的担载不影响该两步反应机理。
（2）V_2O_5/AC催化剂的低温抗SO_2毒化能力源于上述AC对H_2SO_4较强的低温还原能力，从而恢复其孔结构。在本文的实验条件范围内，AC的比表面积和孔体积对H_2SO_4的还原行为没有影响；AC中的含N和含O官能团有利于H_2SO_4的还原；AC中的某些矿物质会和H_2SO_4（或NH_4HSO_4）反应生成金属硫酸盐；V_2O_5的存在和气氛中的NO不利于H_2SO_4的还原。
（3）温度低于175℃时，NH_4HSO_4抑制AC的脱硝活性，且抑制作用随NH_4HSO_4量增加而加剧；高于175℃时，NH_4HSO_4促进AC的脱硝活性，且促进作用随NH_4HSO_4量增加而增大。在本文实验条件范围内，AC的比表面积和孔体积对其脱硝活性几乎没有影响，NH_4HSO_4对AC脱硝活性的影响与其比表面积和孔体积大小无关；NH_4HSO_4对化学性质不同的AC的脱硝活性影响略有不同。
（4）SO_2对催化剂脱硝的影响具有多重作用：一方面，SO_2与O_2+H_2O+NH_3原位生成的硫铵盐对脱硝具有促进作用，另一方面，硫酸（或硫铵盐）堵孔、SO_2与NH_3竞争V_2O_5表面活性位，两者对脱硝具有抑制作用。在本文的实验条件下，SO_2与NH_3的竞争吸附所表现的抑制作用显著于硫酸（或硫铵盐）对脱硝的作用，因此总体表现为SO_2抑制脱硝。
（5）在150-250℃之间，V_2O_5/AC脱硝生成的副产物N_2O很少，浓度在10ppm以下。N_2O源于AC和NH_3共同还原NO的反应。V_2O_5的担载量对N_2O的生成没有显著影响，SO_2和H_2O略微促进了N_2O的生成。V_2O_5的担载量对SCR反应的选择性（即对主产物N_2的选择性）有显著促进作用，0.91wt%的V_2O_5就足以使N_2的选择性保持在95%以上。
（6）V_2O_5担载量和反应温度均促进AC的氧化。SO_2也促进AC的氧化，尤其是在SO_2通入反应器初期。该促进作用源于SO_2和O_2及H_2O在催化剂表面生成的硫酸与AC中的含碳氧官能团发生的反应。AC表面的某些含碳氧官能团不能与氧气发生反应，却能被硫酸氧化。
（7）无论V_2O_5/AC表面是否吸附有汞，升高反应温度均促进其脱硝活性。汞对催化剂的脱硝有抑制作用，该作用随汞含量和反应温度升高而加剧。H_2O和SO_2加剧了汞对V_2O_5/AC脱硝的毒化作用。汞吸附对NH_3在催化剂表面的吸附和氧化行为没有影响，其对脱硝的毒化作用可能源于抑制了吸附的NH_3和NO之间的反应。
Coal is the richest fossil energy in China. The dominant role of coal inthe structure of primary energy in China will do not change for a long time inthe future. Combustion is the traditional mode of coal utilization in China,which takes up more than80%of the total consumption. Combustion of suchgreat amount of coal has already led to serious coal-burning air pollution inour country. NOx is one of the main pollutants in flue gases, which hasbrought tremendous threat on human health and ecological environment.
Among various technologies developed, selective catalytic reduction(SCR) of NOXwith NH_3is recognized to be the most widespread and effectivetechnology for NOXabatement from flue gases of stationary sources. Aimingat the problems of V_2O_5/TiO_2based mid-temperature catalysts (usable ataround400oC), activated coke supported V_2O_5(V_2O_5/AC) catalyst wasinvented, which has a high low-temperature (～200oC) SCR catalytic activityand resistance to SO_2poisoning. Thus, this catalyst was studied extensively inthe past decade including preparation techniques, reaction behaviors, effects ofSO_2and H_2O, reaction mechanism and kinetics etc. So far, however, effect ofAC’s properties on stability of ammonium sulfates, mechanism of SO_2 influence on SCR behavior, SCR selectivity to N_2, thermal stability of catalyst,and effect of Hg on SCR activity are not well understood, which are studiedsystematacially in this paper.
The major conclusions obtained are as follows:
(1) NH_4HSO_4tends to anchor at strong adsorption sites of AC initially atlower loadings and then progressively at weak adsorption sites with theincrease of NH_4HSO_4. Decomposition of NH_4HSO_4on AC follows two-stepreaction mechanism: formation of NH_3and H_2SO_4(leading to release of NH_3)starting at about170oC, and reduction of H_2SO_4(or SO_2-4) by AC to form SO_2at higher temperatures. The presence of NO and V_2O_5do not affect thistwo-step reaction mechanism.
(2) The reduction of H_2SO_4to SO_2by AC support is responsible for theV_2O_5/AC catalyst’s low-temperature resistance to SO_2poisoning since it freesthe pores of AC. In the experimental conditions, the BET surface area andpore volume of AC do not affect the reduction behavior of H_2SO_4, regardlessof the presence of NO. The oxygen and nitrogen containing functional groupsin AC benefit the reduction of H_2SO_4, while the minerals in AC areunfavorable to the reduction of H_2SO_4. V_2O_5loaded on AC and NO in the gasboth inhibit reduction of H_2SO_4to SO_2.
(3) NH_4HSO_4inhibits the SCR activity of AC below175oC, and theinhibiting effect aggravates with the increase of NH_4HSO_4; NH_4HSO_4promotes the SCR activity above175oC, and the promoting effect increases with the increase of NH_4HSO_4. In the experimental conditions, the BETsurface area and pore volume of AC do not affect its SCR activity, and alsohave no relationship with the effect of NH_4HSO_4on SCR activity.
(4) The effect of on-line gaseous SO_2on SCR activity of V_2O_5/ACcatalyst is different from that of pre-loaded NH_4HSO_4. SO_2has multi-role onSCR activity of V_2O_5/AC: on one hand, the sulfate species formed by SO_2andO_2+H_2O+NH_3can promote the catalytic activity; on the other hand, blockingthe pores of catalyst by sulfate species and competitive adsorption of SO_2withNH_3on V_2O_5surface both inhibit the catalytic activity. In the experimentalconditions, the inhibiting effect by competitive adsorption of SO_2with NH_3isobviously larger than the effect by sulfate species, thus SO_2inhibits SCRactivity of V_2O_5/AC.
(5) The N_2O formation over V_2O_5/AC catalyst during SCR of NO by NH_3is generally low, less than10ppm in the temperature range of150-250oC.N_2O is formed from reduction of NO by both AC and NH_3. V_2O_5contributeslittle to the N_2O formation while SO_2+H_2O slightly accelerate N_2O formation.SCR selectivity to N_2is obviously promoted by V_2O_5and0.91wt%V_2O_5issufficient to yield a N_2selectivity of higher than95%.
(6) Oxidation of the AC support to CO_2occurs in the SCR process and itsrate increases with an increase in V_2O_5loading and reaction temperature. SO_2in the gas promotes AC oxidation to CO_2due to formation of sulfuric acid onthe surface, which reacts with the carbon-and-oxygen containing functional groups on the AC. Some of the carbon-and-oxygen containing functionalgroups do not react with O_2under the conditions used, but can be oxidized bysulfuric acid.
(7) SCR activity of V_2O_5/AC catalyst increases with the increasingtemperature, regardless of the adsorption of Hg on its surface. Hg adsorptioninhibits the catalytic activity, and the inhibiting effect aggravates with theincreasing Hg adsorption quantity and reaction temperature. The presence ofH_2O+SO_2strengthens the inhibiting effect of Hg on V_2O_5/AC. The adsorptionand oxidation behaviors of NH_3over V_2O_5/AC are not influenced by Hgadsorption.
烟气脱硝的技术很多，但以NH_3为还原剂的选择性催化还原（SCR）法在世界上应用最多、研究最广、技术最成熟且最有成效。针对目前以V_2O_5/TiO_2催化剂为代表的中温脱硝技术（～400℃）所存在的问题，前人研究开发了以活性焦为载体的V_2O_5/AC催化剂，发现其具有较高的低温（～200℃）脱硝活性和抗SO_2毒化性能，应用前景广阔，研究范畴涉及制备条件、反应行为、SO_2和H_2O的影响、反应机理和动力学等。然而到目前为止，人们在活性焦性质对中毒物硫铵盐稳定性的影响、SO_2影响催化剂脱硝的机理、SCR反应选择性、催化剂的热稳定性及挥发性重金属Hg对催化剂脱硝行为的影响等方面还缺乏认识。本论文针对上述问题进行了深入研究，得到以下主要结论：
（1）脱硝过程中产生的中毒物NH_4HSO_4首先沉积在AC表面的强吸附位上，随着其量的增加再逐渐沉积在弱吸附位上。在惰性气氛中，NH_4HSO_4在AC表面的程序升温分解过程为两步反应机理：从170℃起生成NH_3和H_2SO_4，后者在较高的温度下被AC还原为SO_2气体。NO的存在和V_2O_5的担载不影响该两步反应机理。
（2）V_2O_5/AC催化剂的低温抗SO_2毒化能力源于上述AC对H_2SO_4较强的低温还原能力，从而恢复其孔结构。在本文的实验条件范围内，AC的比表面积和孔体积对H_2SO_4的还原行为没有影响；AC中的含N和含O官能团有利于H_2SO_4的还原；AC中的某些矿物质会和H_2SO_4（或NH_4HSO_4）反应生成金属硫酸盐；V_2O_5的存在和气氛中的NO不利于H_2SO_4的还原。
（3）温度低于175℃时，NH_4HSO_4抑制AC的脱硝活性，且抑制作用随NH_4HSO_4量增加而加剧；高于175℃时，NH_4HSO_4促进AC的脱硝活性，且促进作用随NH_4HSO_4量增加而增大。在本文实验条件范围内，AC的比表面积和孔体积对其脱硝活性几乎没有影响，NH_4HSO_4对AC脱硝活性的影响与其比表面积和孔体积大小无关；NH_4HSO_4对化学性质不同的AC的脱硝活性影响略有不同。
（4）SO_2对催化剂脱硝的影响具有多重作用：一方面，SO_2与O_2+H_2O+NH_3原位生成的硫铵盐对脱硝具有促进作用，另一方面，硫酸（或硫铵盐）堵孔、SO_2与NH_3竞争V_2O_5表面活性位，两者对脱硝具有抑制作用。在本文的实验条件下，SO_2与NH_3的竞争吸附所表现的抑制作用显著于硫酸（或硫铵盐）对脱硝的作用，因此总体表现为SO_2抑制脱硝。
（5）在150-250℃之间，V_2O_5/AC脱硝生成的副产物N_2O很少，浓度在10ppm以下。N_2O源于AC和NH_3共同还原NO的反应。V_2O_5的担载量对N_2O的生成没有显著影响，SO_2和H_2O略微促进了N_2O的生成。V_2O_5的担载量对SCR反应的选择性（即对主产物N_2的选择性）有显著促进作用，0.91wt%的V_2O_5就足以使N_2的选择性保持在95%以上。
（6）V_2O_5担载量和反应温度均促进AC的氧化。SO_2也促进AC的氧化，尤其是在SO_2通入反应器初期。该促进作用源于SO_2和O_2及H_2O在催化剂表面生成的硫酸与AC中的含碳氧官能团发生的反应。AC表面的某些含碳氧官能团不能与氧气发生反应，却能被硫酸氧化。
（7）无论V_2O_5/AC表面是否吸附有汞，升高反应温度均促进其脱硝活性。汞对催化剂的脱硝有抑制作用，该作用随汞含量和反应温度升高而加剧。H_2O和SO_2加剧了汞对V_2O_5/AC脱硝的毒化作用。汞吸附对NH_3在催化剂表面的吸附和氧化行为没有影响，其对脱硝的毒化作用可能源于抑制了吸附的NH_3和NO之间的反应。
Coal is the richest fossil energy in China. The dominant role of coal inthe structure of primary energy in China will do not change for a long time inthe future. Combustion is the traditional mode of coal utilization in China,which takes up more than80%of the total consumption. Combustion of suchgreat amount of coal has already led to serious coal-burning air pollution inour country. NOx is one of the main pollutants in flue gases, which hasbrought tremendous threat on human health and ecological environment.
Among various technologies developed, selective catalytic reduction(SCR) of NOXwith NH_3is recognized to be the most widespread and effectivetechnology for NOXabatement from flue gases of stationary sources. Aimingat the problems of V_2O_5/TiO_2based mid-temperature catalysts (usable ataround400oC), activated coke supported V_2O_5(V_2O_5/AC) catalyst wasinvented, which has a high low-temperature (～200oC) SCR catalytic activityand resistance to SO_2poisoning. Thus, this catalyst was studied extensively inthe past decade including preparation techniques, reaction behaviors, effects ofSO_2and H_2O, reaction mechanism and kinetics etc. So far, however, effect ofAC’s properties on stability of ammonium sulfates, mechanism of SO_2 influence on SCR behavior, SCR selectivity to N_2, thermal stability of catalyst,and effect of Hg on SCR activity are not well understood, which are studiedsystematacially in this paper.
The major conclusions obtained are as follows:
(1) NH_4HSO_4tends to anchor at strong adsorption sites of AC initially atlower loadings and then progressively at weak adsorption sites with theincrease of NH_4HSO_4. Decomposition of NH_4HSO_4on AC follows two-stepreaction mechanism: formation of NH_3and H_2SO_4(leading to release of NH_3)starting at about170oC, and reduction of H_2SO_4(or SO_2-4) by AC to form SO_2at higher temperatures. The presence of NO and V_2O_5do not affect thistwo-step reaction mechanism.
(2) The reduction of H_2SO_4to SO_2by AC support is responsible for theV_2O_5/AC catalyst’s low-temperature resistance to SO_2poisoning since it freesthe pores of AC. In the experimental conditions, the BET surface area andpore volume of AC do not affect the reduction behavior of H_2SO_4, regardlessof the presence of NO. The oxygen and nitrogen containing functional groupsin AC benefit the reduction of H_2SO_4, while the minerals in AC areunfavorable to the reduction of H_2SO_4. V_2O_5loaded on AC and NO in the gasboth inhibit reduction of H_2SO_4to SO_2.
(3) NH_4HSO_4inhibits the SCR activity of AC below175oC, and theinhibiting effect aggravates with the increase of NH_4HSO_4; NH_4HSO_4promotes the SCR activity above175oC, and the promoting effect increases with the increase of NH_4HSO_4. In the experimental conditions, the BETsurface area and pore volume of AC do not affect its SCR activity, and alsohave no relationship with the effect of NH_4HSO_4on SCR activity.
(4) The effect of on-line gaseous SO_2on SCR activity of V_2O_5/ACcatalyst is different from that of pre-loaded NH_4HSO_4. SO_2has multi-role onSCR activity of V_2O_5/AC: on one hand, the sulfate species formed by SO_2andO_2+H_2O+NH_3can promote the catalytic activity; on the other hand, blockingthe pores of catalyst by sulfate species and competitive adsorption of SO_2withNH_3on V_2O_5surface both inhibit the catalytic activity. In the experimentalconditions, the inhibiting effect by competitive adsorption of SO_2with NH_3isobviously larger than the effect by sulfate species, thus SO_2inhibits SCRactivity of V_2O_5/AC.
(5) The N_2O formation over V_2O_5/AC catalyst during SCR of NO by NH_3is generally low, less than10ppm in the temperature range of150-250oC.N_2O is formed from reduction of NO by both AC and NH_3. V_2O_5contributeslittle to the N_2O formation while SO_2+H_2O slightly accelerate N_2O formation.SCR selectivity to N_2is obviously promoted by V_2O_5and0.91wt%V_2O_5issufficient to yield a N_2selectivity of higher than95%.
(6) Oxidation of the AC support to CO_2occurs in the SCR process and itsrate increases with an increase in V_2O_5loading and reaction temperature. SO_2in the gas promotes AC oxidation to CO_2due to formation of sulfuric acid onthe surface, which reacts with the carbon-and-oxygen containing functional groups on the AC. Some of the carbon-and-oxygen containing functionalgroups do not react with O_2under the conditions used, but can be oxidized bysulfuric acid.
(7) SCR activity of V_2O_5/AC catalyst increases with the increasingtemperature, regardless of the adsorption of Hg on its surface. Hg adsorptioninhibits the catalytic activity, and the inhibiting effect aggravates with theincreasing Hg adsorption quantity and reaction temperature. The presence ofH_2O+SO_2strengthens the inhibiting effect of Hg on V_2O_5/AC. The adsorptionand oxidation behaviors of NH_3over V_2O_5/AC are not influenced by Hgadsorption.
引文
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