铈改性钛基纳米管的脱硝活性及抗碱/碱土金属中毒性能研究
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摘要
氮氧化物是烟气中的主要污染物之一,选择性催化还原法是国内外首选的脱硝技术。目前广泛使用的钒基催化剂具有有毒、易发生碱／碱土金属中毒的缺陷。基于此,本文系统研究了具有优异脱硝活性、选择性和抗碱／碱土金属中毒性能的新型铈改性钛基纳米管脱硝催化剂,为改进脱硝催化剂和解决催化剂中毒问题作出积极有益的探索。
首先,本文研究了铈添加量、焙烧温度和钛基纳米管的pH值对催化剂结构和脱硝活性的影响,获得了具有优异脱硝活性和选择性的钛基纳米管催化剂制备工艺。通过优化工艺制得的催化剂在270-500℃的反应温度区间内脱硝效率维持在96%以上,300-450℃时脱硝效率更是接近100%。
在优化制备工艺的基础上,本文对铈钛催化剂的构效关系进行了深入探讨,发现氧化铈负载在不同形貌的钛载体材料上之后,其物理化学特性和催化特性有所不同,三价铈和氧空位的生成对其催化活性具有决定性影响。氧化铈负载在钛基纳米管上具有特别突出的脱硝活性,这不仅与钛基纳米管较大的比表面积相关,还与其特殊的纳米管道结构有关。钛基纳米管的管道约束了氧化铈的生长,对氧化铈的氧化还原特性具有一定的调变作用,且钛基纳米管对氨气有独特的吸附能力,有利于SCR脱硝反应的进行。
随后,本文考察了铈钛纳米颗粒催化剂因碱/碱土金属导致的严重失活现象,发现其失活的主因不是酸性位的破坏,而是活性氧化铈形态的变化。加入Na+或Ca2+后,在熔盐熔化作用下,无定形的氧化铈转化为结晶态的氧化铈,Ce3+和氧空位急剧减少,氧化铈还原速率减慢,氧化铈的氧化还原循环受阻,因此失活。
与铈钛纳米颗粒催化剂不同的是,本文开发的铈改性钛基纳米管表现出优异的抗钠中毒性能,干混法添加Na/Ce摩尔比为1的Na之后,催化剂在350℃时仍能维持90%的脱硝活性,浸渍法负载Na+之后,在350℃左右仍能维持超过80%的脱硝活性。其抗中毒性能源于钛基纳米管对活性氧化铈的保护作用：钛基纳米管的管壁将固体金属毒物隔绝在管壁外,从而保护了管道内的活性氧化铈,使得管道内的氧化铈免遭毒害；同时,质子化的钛基纳米管具有较强的离子交换能力,可以将碱／碱土金属离子通过离子交换固定在管壁层间,阻止他们毒害活性氧化铈。
最后,本文针对“壳保护”抗中毒机理进行了拓展研究,发现管状结构的完好程度和钛基纳米管的离子交换能力是有效保护氧化铈的关键影响因素。一旦管状结构被破坏,钛基纳米管对氧化铈的双重保护作用将消失,氧化铈将迅速失活；乙醇浸泡处理可以增加钛基纳米管层间的OH基团数量,使得可供离子交换的质子增多,捕获碱／碱土金属离子的能力也相应增强,最终有效提高催化剂对碱／碱土金属的抗性。分别添加了与Ce的摩尔比为1的Na+、K+、Ca2+后,反应温度350℃时的脱硝效率仍可分别维持在97%、88%和95%。
NOx is one of the key air pollutants from flue gas, and selective catalytic reduction with NH3was the most reliable method to reduce the emission of NOx from stationary sources. Although vanadia-based catalysts have been extensively employed in commercial SCR processes, the drawbacks associated with the toxicity of vanadium pentoxide to environment and the alkali&alkaline earth metal poisoning still remain. Aiming to develop non-vanadia deNOx catalysts with high activity and remarkable resistance to alkali&alkaline earth metal poisoning, the structure, SCR performance and resistance to poisons of ceria doped titanate nanotubes (Ce/TNTs) were systematically investigated in this paper.
Firstly, the preparation process of highly active and selective Ce/TNTs was optimized. It was found that the Ce loading, the calcination temperature and the pH value of TNTs all significantly influenced the SCR performance of Ce/TNTs. The NO conversion over the optimal catalyst exceeded96%at270-500℃and was even close to100%at300-450℃.
Secondly, the relationship between the structure of the titanium supports and the performance of ceria was studied. It was observed that the nature of titanium supports had significantly influenced the chemical state of Ce because of their special surface properties and unique structures and morphologies, leading to the presence of different catalytic performances for each catalyst. In comparison with the catalysts supported by TiO2nanoparticles, the Ce/TNTs showed a superiority in SCR of NO due to the improved redox potential and special adsorption of NH3.
Thirdly, the deactivation mechanism of Ce/TiO2SCR catalysts by the deposition of Na+and Ca2+ions was proposed. Ce/TiO2catalyst using TiO2particle as the support was deactivated seriously by the deposition of Na+or Ca2+ions. It was found that amorphous ceria was dominant in the fresh Ce/TiO2catalyst, but the amorphous ceria would grow to ceria crystal during the calcination process with the deposition of Na-or Ca2+ions. Then, the dispersion of ceria on the surface of T1O2became worse and the surface Ce3+transformed to Ce4+.This transformation directly led to the disappearance of oxygen vacancy in ceria particles and slowed down the reduction rate of ceria. Thus, the rate of oxidation/reduction recycle was declined. Though the acidity of Ce/TiO2changed little, the enlargement of ceria nanoparticles and the restrained Ce4+/Ce3+redox recycle rate resulted in the decline of SCR activity of Ce/TiO2catalys.
Finally, the resistance of Ce/TNTs to alkali poisoning was investigated. Ce/TNTs showed a remarkable resistance to alkali metal poisoning in deNOx application, where the NO conversion at350℃maintained at90%after wet-impregnation of Na (Na/Ce molar ratio at1) and kept at80%after solid Na mixing. The catalyst effectively shielded the main active phase, CeO2, from the poisons with the tubular channel of H2Ti12O25. Furthermore, the poisons (e.g., Na+) could also be stabilized in the interlayer of H2Ti12O25through ion exchange. This catalyst developed herein gives a new sight for the design of "shell protection" catalysts to improve their tolerance to poisons. In addition, the maintenance of the tubular morphology and the capacity of ion-exchange were the two key factors that determined the alkaline resistance. Treating the TNTs with ethanol could increase the amount of ion-exhangenable OH group and consequently improved the resistance. In such a case, the NO conversion at350℃still maintained at97%,88%and95%after Na+, K+and Ca2+adding.
首先,本文研究了铈添加量、焙烧温度和钛基纳米管的pH值对催化剂结构和脱硝活性的影响,获得了具有优异脱硝活性和选择性的钛基纳米管催化剂制备工艺。通过优化工艺制得的催化剂在270-500℃的反应温度区间内脱硝效率维持在96%以上,300-450℃时脱硝效率更是接近100%。
在优化制备工艺的基础上,本文对铈钛催化剂的构效关系进行了深入探讨,发现氧化铈负载在不同形貌的钛载体材料上之后,其物理化学特性和催化特性有所不同,三价铈和氧空位的生成对其催化活性具有决定性影响。氧化铈负载在钛基纳米管上具有特别突出的脱硝活性,这不仅与钛基纳米管较大的比表面积相关,还与其特殊的纳米管道结构有关。钛基纳米管的管道约束了氧化铈的生长,对氧化铈的氧化还原特性具有一定的调变作用,且钛基纳米管对氨气有独特的吸附能力,有利于SCR脱硝反应的进行。
随后,本文考察了铈钛纳米颗粒催化剂因碱/碱土金属导致的严重失活现象,发现其失活的主因不是酸性位的破坏,而是活性氧化铈形态的变化。加入Na+或Ca2+后,在熔盐熔化作用下,无定形的氧化铈转化为结晶态的氧化铈,Ce3+和氧空位急剧减少,氧化铈还原速率减慢,氧化铈的氧化还原循环受阻,因此失活。
与铈钛纳米颗粒催化剂不同的是,本文开发的铈改性钛基纳米管表现出优异的抗钠中毒性能,干混法添加Na/Ce摩尔比为1的Na之后,催化剂在350℃时仍能维持90%的脱硝活性,浸渍法负载Na+之后,在350℃左右仍能维持超过80%的脱硝活性。其抗中毒性能源于钛基纳米管对活性氧化铈的保护作用：钛基纳米管的管壁将固体金属毒物隔绝在管壁外,从而保护了管道内的活性氧化铈,使得管道内的氧化铈免遭毒害；同时,质子化的钛基纳米管具有较强的离子交换能力,可以将碱／碱土金属离子通过离子交换固定在管壁层间,阻止他们毒害活性氧化铈。
最后,本文针对“壳保护”抗中毒机理进行了拓展研究,发现管状结构的完好程度和钛基纳米管的离子交换能力是有效保护氧化铈的关键影响因素。一旦管状结构被破坏,钛基纳米管对氧化铈的双重保护作用将消失,氧化铈将迅速失活；乙醇浸泡处理可以增加钛基纳米管层间的OH基团数量,使得可供离子交换的质子增多,捕获碱／碱土金属离子的能力也相应增强,最终有效提高催化剂对碱／碱土金属的抗性。分别添加了与Ce的摩尔比为1的Na+、K+、Ca2+后,反应温度350℃时的脱硝效率仍可分别维持在97%、88%和95%。
NOx is one of the key air pollutants from flue gas, and selective catalytic reduction with NH3was the most reliable method to reduce the emission of NOx from stationary sources. Although vanadia-based catalysts have been extensively employed in commercial SCR processes, the drawbacks associated with the toxicity of vanadium pentoxide to environment and the alkali&alkaline earth metal poisoning still remain. Aiming to develop non-vanadia deNOx catalysts with high activity and remarkable resistance to alkali&alkaline earth metal poisoning, the structure, SCR performance and resistance to poisons of ceria doped titanate nanotubes (Ce/TNTs) were systematically investigated in this paper.
Firstly, the preparation process of highly active and selective Ce/TNTs was optimized. It was found that the Ce loading, the calcination temperature and the pH value of TNTs all significantly influenced the SCR performance of Ce/TNTs. The NO conversion over the optimal catalyst exceeded96%at270-500℃and was even close to100%at300-450℃.
Secondly, the relationship between the structure of the titanium supports and the performance of ceria was studied. It was observed that the nature of titanium supports had significantly influenced the chemical state of Ce because of their special surface properties and unique structures and morphologies, leading to the presence of different catalytic performances for each catalyst. In comparison with the catalysts supported by TiO2nanoparticles, the Ce/TNTs showed a superiority in SCR of NO due to the improved redox potential and special adsorption of NH3.
Thirdly, the deactivation mechanism of Ce/TiO2SCR catalysts by the deposition of Na+and Ca2+ions was proposed. Ce/TiO2catalyst using TiO2particle as the support was deactivated seriously by the deposition of Na+or Ca2+ions. It was found that amorphous ceria was dominant in the fresh Ce/TiO2catalyst, but the amorphous ceria would grow to ceria crystal during the calcination process with the deposition of Na-or Ca2+ions. Then, the dispersion of ceria on the surface of T1O2became worse and the surface Ce3+transformed to Ce4+.This transformation directly led to the disappearance of oxygen vacancy in ceria particles and slowed down the reduction rate of ceria. Thus, the rate of oxidation/reduction recycle was declined. Though the acidity of Ce/TiO2changed little, the enlargement of ceria nanoparticles and the restrained Ce4+/Ce3+redox recycle rate resulted in the decline of SCR activity of Ce/TiO2catalys.
Finally, the resistance of Ce/TNTs to alkali poisoning was investigated. Ce/TNTs showed a remarkable resistance to alkali metal poisoning in deNOx application, where the NO conversion at350℃maintained at90%after wet-impregnation of Na (Na/Ce molar ratio at1) and kept at80%after solid Na mixing. The catalyst effectively shielded the main active phase, CeO2, from the poisons with the tubular channel of H2Ti12O25. Furthermore, the poisons (e.g., Na+) could also be stabilized in the interlayer of H2Ti12O25through ion exchange. This catalyst developed herein gives a new sight for the design of "shell protection" catalysts to improve their tolerance to poisons. In addition, the maintenance of the tubular morphology and the capacity of ion-exchange were the two key factors that determined the alkaline resistance. Treating the TNTs with ethanol could increase the amount of ion-exhangenable OH group and consequently improved the resistance. In such a case, the NO conversion at350℃still maintained at97%,88%and95%after Na+, K+and Ca2+adding.
引文
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