Mn改性的Pd/Ba/Al催化剂上NO_x存储—还原反应性能研究
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摘要
NOx存储-还原(NSR)技术是一种可以脱除贫燃尾气中NOx的有效方法,最早由日本丰田汽车公司提出,近年来受到人们的广泛关注和重视。现阶段,NSR催化剂的研究主要集中在Pt-Ba-Al体系,该类催化剂在高温(>350℃)具有较好的脱除效率,但当温度降低时,贫燃阶段NO、不能有效的在催化剂上存储,从而降低了催化剂的NOx脱除效率。
本论文采用等体积浸渍法制备了Pd/Mn/Ba/Al系列催化剂,考察了催化剂在不同温度点的存储活性及存储-还原循环中NO、的脱除效率,并用DRIFTS、TPD、TPSR等方法对表面吸附物种的形成及吸附物种的反应情况进行了研究,主要研究内容和实验结果如下：
1.研究了NSR催化剂在不同温度点的NOx存储性能,结果表明：当Mn单独作为NOx存储组分时,其低温(30～300℃)具有较好的NOx存储能力,但400℃以上的NOx存储能力急剧下降。当Ba作为NOx存储组分时,NOx存储量随温度上升呈现：先上升再下降的趋势,并在400℃,达到最大NOx存储量。当Mn和Ba共同作为存储组分时,Mn的加入显著提高了传统Pd/Ba/Al催化剂低温段的NOx存储量,并在300℃至400℃的宽温度区间获得了850μmol·g-1的NOx存储量。
2.研究了NOx在Pd/Ba/Al、Pd/Mn/Al和Pd/Mn/Ba/Al催化剂上的形成物种,结果表明：亚硝酸盐和硝酸盐是NOx在催化剂上存储的主要形式。随着吸附温度的升高(>300℃),硝酸盐为催化剂表面的主要NOx存储物种。在吸附温度为300℃时,Mn上的硝酸盐已经分解,故不能直接提供NOx存储位,但与Ba的协同作用,却促进了Pd/Mn/Ba/Al催化剂表面在低温(<400℃)硝酸盐的生成。
3.以NOx吸附后在惰性气氛中的程序升温研究为手段,考察了Pd/Ba/Al、Pd/Mn/Al和Pd/Mn/Ba/Al催化剂上吸附的NOx物种的热稳定性,结果表明：亚硝酸盐的热稳定性较差,而以硝酸盐形式存储的NOx的热稳定性较高。由于存储在Mn上的NOx主要以亚硝酸盐形式存在,故热稳定性较差,存储在Ba上的硝酸盐的分解温度较高(>500℃)；由于Mn和Ba的协同作用,使得存储在Pd/Mn/Ba/Al催化剂上的硝酸盐的分解温度略有降低。
4.通过对比Mn/Ba/Al、Pd/Ba/Al、Pd/Mn/Al和Pd/Mn/Ba/Al催化剂吸附NOx后在5% H2/Ar气氛中的TPSR结果表明：Mn对催化NOx还原的能力较差,但Pd的加入能显著降低NOx的还原温度。这对于催化剂在NOx存储-还原循环中的还原再生过程具有重要意义。
5.考察了Pd/Ba/Al、Pd/Mn/Al和Pd/Mn/Ba/Al催化剂上NOx存储-还原循环脱除活性,结果表明：Pd/Ba/Al催化剂活性温度窗口很窄,NOx脱除效率仅在400℃较高,达到62%；Pd/Mn/Al催化剂的NOx脱除效率整体较低,但在300℃～400℃温度范围可获得30%的NOx脱除率；由于Mn的加入,Pd/Mn/Ba/Al催化剂的低温活性较Pd/Ba/Al催化剂有显著提高,300℃时,NOx脱除率提高了3倍多,由16%提高至53%。
NOx storage-reduction (NSR) technology can effectively remove NOx in the lean burn conditions, which was first proposed by the Toyota Corporation, and caused wide public attention. At present, the research on the catalysts mainly focus on the Pt-Ba-Al System. This kind of catalyst had excellent activity above 350℃, but when the temperature decreased, NO can not be effectively stored on the catalyst in the lean phase, thereby reduced the NOx removal efficiency of the catalysts.
The performance of NOx storage capacity (NSC) and the activity of storage-reduction over a series of Pd/Mn/Ba/Al catalysts were investigated at different temperatures. The Pd catalysts were prepared by incipient impregnation and characterized by DRIFTS、TPD and TPSR. Some meaningful results were got as follows:
1). The NOx storage capacity was studied over a series of catalysts at different temperature, it is found that the storage capacity of the catalyst is high at 30-300℃and decrease sharply at 400℃when Mn used as the storage component only; the NOx storage capacity first increased and then decreased with increasing temperature, and reached the maximum value at 400℃, when the Ba uesd as the storage component; The addition of Mn can significantly improved the storage activity of the traditional catalyst Pd/Ba/Al at low temperature, and the NOx storage capacity reached 850μmol·g-1 at 300-400℃, when the Mn and Ba used as the storage components together.
2). Study of the formed species of NOx on the Pd/Ba/Al、Pd/Mn/Al and Pd/Mn/Ba/Al catalysts, it is found that the nitrite and nitrate were the main species on the catalysts.As the adsorption temperature up 300℃, the nitrate is the main NOx storage species, but the nitrate on the Mn was unstable and Mn couldn't provide the storage spaces at this temperature. However, the synergistic effect of Mn and Ba could promote the nitrate formed on the Pd/Mn/Ba/Al catalyst at the low temperature (<400℃).
3). Study of the thermal stability of NOx species on the Pd/Ba/Al、Pd/Mn/Al and Pd/Mn/Ba/Al catalysts through the NOx-TPD, it is found that the thermal stability of nitrite is poor and nitrate is better. The nitrite is the main species on Mn and has poor thermal stability, the decomposition temperature of nitrate on the Ba was higher (> 500℃). The synergistic effect of Mn and Ba could promote the decompostion and decreased the decomposition temperature of nitrate on the Pd/Mn/Ba/Al catalyst.
4). Compared the NOX reduction activity of Mn/Ba/Al、Pd/Ba/Al、Pd/Mn/Al and Pd/Mn/Ba/Al catalysts, addition of Mn reduce the capacity of NOx reduction by H2-TPSR. But the reduction temperautre significantly decreased through adding Pd. This is important for reduction and regeneration of catalysts in the NOX storage-reduction (cycling).
5). The temperature window of activity on the Pa/Ba/Al catalyst was narrow, the NOX conversion reached 62% at 400℃. The total NOX conversion was lower over the Pd/Mn/Al catalyst, reached 30% at 300-400℃. Compared to Pd/Ba/Al, the NOX conversion of the PMBA catalyst is three times at 300℃, from 16% to 53%.
本论文采用等体积浸渍法制备了Pd/Mn/Ba/Al系列催化剂,考察了催化剂在不同温度点的存储活性及存储-还原循环中NO、的脱除效率,并用DRIFTS、TPD、TPSR等方法对表面吸附物种的形成及吸附物种的反应情况进行了研究,主要研究内容和实验结果如下：
1.研究了NSR催化剂在不同温度点的NOx存储性能,结果表明：当Mn单独作为NOx存储组分时,其低温(30～300℃)具有较好的NOx存储能力,但400℃以上的NOx存储能力急剧下降。当Ba作为NOx存储组分时,NOx存储量随温度上升呈现：先上升再下降的趋势,并在400℃,达到最大NOx存储量。当Mn和Ba共同作为存储组分时,Mn的加入显著提高了传统Pd/Ba/Al催化剂低温段的NOx存储量,并在300℃至400℃的宽温度区间获得了850μmol·g-1的NOx存储量。
2.研究了NOx在Pd/Ba/Al、Pd/Mn/Al和Pd/Mn/Ba/Al催化剂上的形成物种,结果表明：亚硝酸盐和硝酸盐是NOx在催化剂上存储的主要形式。随着吸附温度的升高(>300℃),硝酸盐为催化剂表面的主要NOx存储物种。在吸附温度为300℃时,Mn上的硝酸盐已经分解,故不能直接提供NOx存储位,但与Ba的协同作用,却促进了Pd/Mn/Ba/Al催化剂表面在低温(<400℃)硝酸盐的生成。
3.以NOx吸附后在惰性气氛中的程序升温研究为手段,考察了Pd/Ba/Al、Pd/Mn/Al和Pd/Mn/Ba/Al催化剂上吸附的NOx物种的热稳定性,结果表明：亚硝酸盐的热稳定性较差,而以硝酸盐形式存储的NOx的热稳定性较高。由于存储在Mn上的NOx主要以亚硝酸盐形式存在,故热稳定性较差,存储在Ba上的硝酸盐的分解温度较高(>500℃)；由于Mn和Ba的协同作用,使得存储在Pd/Mn/Ba/Al催化剂上的硝酸盐的分解温度略有降低。
4.通过对比Mn/Ba/Al、Pd/Ba/Al、Pd/Mn/Al和Pd/Mn/Ba/Al催化剂吸附NOx后在5% H2/Ar气氛中的TPSR结果表明：Mn对催化NOx还原的能力较差,但Pd的加入能显著降低NOx的还原温度。这对于催化剂在NOx存储-还原循环中的还原再生过程具有重要意义。
5.考察了Pd/Ba/Al、Pd/Mn/Al和Pd/Mn/Ba/Al催化剂上NOx存储-还原循环脱除活性,结果表明：Pd/Ba/Al催化剂活性温度窗口很窄,NOx脱除效率仅在400℃较高,达到62%；Pd/Mn/Al催化剂的NOx脱除效率整体较低,但在300℃～400℃温度范围可获得30%的NOx脱除率；由于Mn的加入,Pd/Mn/Ba/Al催化剂的低温活性较Pd/Ba/Al催化剂有显著提高,300℃时,NOx脱除率提高了3倍多,由16%提高至53%。
NOx storage-reduction (NSR) technology can effectively remove NOx in the lean burn conditions, which was first proposed by the Toyota Corporation, and caused wide public attention. At present, the research on the catalysts mainly focus on the Pt-Ba-Al System. This kind of catalyst had excellent activity above 350℃, but when the temperature decreased, NO can not be effectively stored on the catalyst in the lean phase, thereby reduced the NOx removal efficiency of the catalysts.
The performance of NOx storage capacity (NSC) and the activity of storage-reduction over a series of Pd/Mn/Ba/Al catalysts were investigated at different temperatures. The Pd catalysts were prepared by incipient impregnation and characterized by DRIFTS、TPD and TPSR. Some meaningful results were got as follows:
1). The NOx storage capacity was studied over a series of catalysts at different temperature, it is found that the storage capacity of the catalyst is high at 30-300℃and decrease sharply at 400℃when Mn used as the storage component only; the NOx storage capacity first increased and then decreased with increasing temperature, and reached the maximum value at 400℃, when the Ba uesd as the storage component; The addition of Mn can significantly improved the storage activity of the traditional catalyst Pd/Ba/Al at low temperature, and the NOx storage capacity reached 850μmol·g-1 at 300-400℃, when the Mn and Ba used as the storage components together.
2). Study of the formed species of NOx on the Pd/Ba/Al、Pd/Mn/Al and Pd/Mn/Ba/Al catalysts, it is found that the nitrite and nitrate were the main species on the catalysts.As the adsorption temperature up 300℃, the nitrate is the main NOx storage species, but the nitrate on the Mn was unstable and Mn couldn't provide the storage spaces at this temperature. However, the synergistic effect of Mn and Ba could promote the nitrate formed on the Pd/Mn/Ba/Al catalyst at the low temperature (<400℃).
3). Study of the thermal stability of NOx species on the Pd/Ba/Al、Pd/Mn/Al and Pd/Mn/Ba/Al catalysts through the NOx-TPD, it is found that the thermal stability of nitrite is poor and nitrate is better. The nitrite is the main species on Mn and has poor thermal stability, the decomposition temperature of nitrate on the Ba was higher (> 500℃). The synergistic effect of Mn and Ba could promote the decompostion and decreased the decomposition temperature of nitrate on the Pd/Mn/Ba/Al catalyst.
4). Compared the NOX reduction activity of Mn/Ba/Al、Pd/Ba/Al、Pd/Mn/Al and Pd/Mn/Ba/Al catalysts, addition of Mn reduce the capacity of NOx reduction by H2-TPSR. But the reduction temperautre significantly decreased through adding Pd. This is important for reduction and regeneration of catalysts in the NOX storage-reduction (cycling).
5). The temperature window of activity on the Pa/Ba/Al catalyst was narrow, the NOX conversion reached 62% at 400℃. The total NOX conversion was lower over the Pd/Mn/Al catalyst, reached 30% at 300-400℃. Compared to Pd/Ba/Al, the NOX conversion of the PMBA catalyst is three times at 300℃, from 16% to 53%.
引文
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