碳载体纳米催化剂的制备及其催化去除氮氧化物的应用
摘要
从燃煤电厂、垃圾焚烧锅炉、柴油机和汽车中排放出的氮氧化物会导致酸雨、光化学烟雾以及臭氧层的破坏,从而对人类的健康和生存构成极大危害。NOx的排放已经引起了世界各国的广泛关注和高度重视。面对日益增加的NOx排放,人们采取多种办法对其进行控制。选择性还原技术(SCR)被证明是最有效的减少NOx的方法。而开发新型高效的催化剂又是SCR技术的关键。
本论文采用湿化学方法制备了一系列的碳基催化剂并检测了它们的催化脱硝性能。首先,将碳纳米管引入传统催化剂V205-TiO2体系中,取得了很好的催化性能。为了进一步提高催化剂的性能,Mn, Ce, Mo, Cr, Ni, Co掺入已经优化好的催化剂V2O5-TiO2-CNTs中,发现CeOχ可有效地提高SCR活性。我们还通过浸渍法制备了三种不同碳材料负载CuOχ的催化剂并发现了一种简单的可恢复失活催化剂性能的方法。
在传统催化剂V2O5/TiO2中加入碳纳米管可极大促进催化剂的脱硝性能。加入10%碳管的催化剂效果最好,在300℃可达到89%的脱除效率。引入的碳纳米管可增加催化剂的比表面积、孔体积、酸度和氧化还原性能。高的氧化性能可以促进NO氧化成NO2进而提高NOx去除率。另外,V2O5/TiO2-CNTs催化剂对二氧化硫和水有很好的抵抗作用。
把MnOx加入到V2O5/TiO2-CNT可以实现综合高温活性钒和低温活性锰的目标。在2750C时,V205-MnOx/Ti02-CNTs催化剂可达到99%的脱除效率。从TOF的计算可以看出,用机械法制备的钒锰复合催化剂上钒和锰有相互促进作用。由于碳管的引入使得钒锰结合不紧密从而避免了抑制作用。同时,由掺杂引起的酸强度的增加和氧化性能的提高也有助于SCR的催化性能。
通过溶胶凝胶法把Co. Ce. Cr> Mo和Ni掺入到催化剂V2O5/TiO2-CNTs中。其中,Ce可有效促进NH3-SCR反应。大量Ce3+的存在可以增加化学吸附氧,进而利于催化反应的进行。CeOx可以抑制催化剂的团聚而增加其比表面积和分散性。掺入CeOx后,催化剂的酸度和氧化还原性能都有所提高。由8O2引起的催化剂中毒与反应温度和空速有极大关系,低温和高的空速容易使催化剂中毒。为了保持催化剂的活性,至少2%的O2浓度是需要的。
在碳纳米管、活性炭和石墨负载CuOx催化剂中,碳管是最好的载体。CuOx-CNTs在250℃可达到67%的转化效率。碳纳米管负载CuOx优异的催化性能可能来自于Cu良好的分散性、大量Cu+的存在和强酸性位的存在。
Nitrogen oxides (NOx) discharged from power plants, waste incinerators, industrial boilers, engines, and automobiles can result in acid rain, photochemical smog, and ozone depletion. These adverse effects have aroused worldwide attention. Due to the increasing threat of NOx to the environment, many approaches have been investigated to control NOx emission. Selective catalytic reduction (SCR) technique has been proven to be one of the most effective methods for reducing NOx emissions. The keypoint for SCR technique is to develop novel and effective catalysts at low temperatures.
In my thesis, we prepared a series of carbon supported catalysts through wet chemical methods and examined their catalytic performance for NOx removal. Great promotion effect was achieved upon introduction of carbon nanotubes to traditional catalyst V2Os-TiO2. To further improve catalytic reactivity of optimized catalyst, we dope a series of additional element such as Mn, Ce, Mo, Cr, Ni, Co to catalyst V2O5-TiO2-CNTs. Experimental results showed that CeOx can enhance SCR activity of catalysts greatly. We also synthesized three kind of catalysts in which carbon materials support CuOx and found a simple way to regenerate the deactivated catalysts.
The introduction of carbon nanotubes to catalyst V2O5-TiO2 can promote its SCR performance greatly. The best reactivity of catalyst was achieved by doped 10% carbon nanotubes, the removal efficiency for NOx can reach up to 89%at 300℃.The specific surface, pore volume, acidity and reducibility of catalyst increased with introduction of carbon nanotubes. The high reducibility can enhance the oxidation efficiency of NO to NO2. The catalyst V2O5-TiO2-CNTs has a good resistence to SO2 and H2O.
The combination of low-temperature active MnOx and high-temperature active V2O5 was accomplished by adding MnOx into V2O5/TiO2-CNT composites. A NOX removal efficiency of 99%was observed over V2O5-MnOx/TiO2-CNTs at 275℃under a GHSV of 36000 h"1. TOF results suggest a possible constructive interaction between V2O5 and MnOx for catalysts prepared by mechanical mixing. The possible separation of Mn and V with the assistance of CNTs and the increase of reducibility and acidic strength all contribute to the improvement of catalytic activity.
Co, Ce. Cr, Mo, Ni were introduced to catalyst V2O5/T1O2-CNTS with sol-gel method and Ce was proved to be most effective to promote NH3-SCR activity. A large number of Ce3+contributes to the increase of chemisorbed oxygen, which favors the SCR activity. The aggregation of catalyst might be inhibited by CeOx thus result to the increase of specific surface. Moreover, the increase of surface acidity and reducibility both contribute to the extra NOx conversion upon addition of CeOx-The deactivation of catalyst VCeqTiC caused by SO2 depends on reaction temperatures and gas velocity strongly. And at least 2%of oxygen in exhaust gas is essential to keep high SCR activity.
Cu-CNTs was prepared by wet impregnation method and a NOx removal efficiency of 67%was achieved at 250℃. which could be attributed to the good dispersion of CuOx, the existence of Cu+and strong acid sites on the catalysts" surface. Moreover, the regeneration of deactivated catalyst CuOx-CNTs caused by SO2 could be achieved by heating the catalyst in N2 at 300℃.
本论文采用湿化学方法制备了一系列的碳基催化剂并检测了它们的催化脱硝性能。首先,将碳纳米管引入传统催化剂V205-TiO2体系中,取得了很好的催化性能。为了进一步提高催化剂的性能,Mn, Ce, Mo, Cr, Ni, Co掺入已经优化好的催化剂V2O5-TiO2-CNTs中,发现CeOχ可有效地提高SCR活性。我们还通过浸渍法制备了三种不同碳材料负载CuOχ的催化剂并发现了一种简单的可恢复失活催化剂性能的方法。
在传统催化剂V2O5/TiO2中加入碳纳米管可极大促进催化剂的脱硝性能。加入10%碳管的催化剂效果最好,在300℃可达到89%的脱除效率。引入的碳纳米管可增加催化剂的比表面积、孔体积、酸度和氧化还原性能。高的氧化性能可以促进NO氧化成NO2进而提高NOx去除率。另外,V2O5/TiO2-CNTs催化剂对二氧化硫和水有很好的抵抗作用。
把MnOx加入到V2O5/TiO2-CNT可以实现综合高温活性钒和低温活性锰的目标。在2750C时,V205-MnOx/Ti02-CNTs催化剂可达到99%的脱除效率。从TOF的计算可以看出,用机械法制备的钒锰复合催化剂上钒和锰有相互促进作用。由于碳管的引入使得钒锰结合不紧密从而避免了抑制作用。同时,由掺杂引起的酸强度的增加和氧化性能的提高也有助于SCR的催化性能。
通过溶胶凝胶法把Co. Ce. Cr> Mo和Ni掺入到催化剂V2O5/TiO2-CNTs中。其中,Ce可有效促进NH3-SCR反应。大量Ce3+的存在可以增加化学吸附氧,进而利于催化反应的进行。CeOx可以抑制催化剂的团聚而增加其比表面积和分散性。掺入CeOx后,催化剂的酸度和氧化还原性能都有所提高。由8O2引起的催化剂中毒与反应温度和空速有极大关系,低温和高的空速容易使催化剂中毒。为了保持催化剂的活性,至少2%的O2浓度是需要的。
在碳纳米管、活性炭和石墨负载CuOx催化剂中,碳管是最好的载体。CuOx-CNTs在250℃可达到67%的转化效率。碳纳米管负载CuOx优异的催化性能可能来自于Cu良好的分散性、大量Cu+的存在和强酸性位的存在。
Nitrogen oxides (NOx) discharged from power plants, waste incinerators, industrial boilers, engines, and automobiles can result in acid rain, photochemical smog, and ozone depletion. These adverse effects have aroused worldwide attention. Due to the increasing threat of NOx to the environment, many approaches have been investigated to control NOx emission. Selective catalytic reduction (SCR) technique has been proven to be one of the most effective methods for reducing NOx emissions. The keypoint for SCR technique is to develop novel and effective catalysts at low temperatures.
In my thesis, we prepared a series of carbon supported catalysts through wet chemical methods and examined their catalytic performance for NOx removal. Great promotion effect was achieved upon introduction of carbon nanotubes to traditional catalyst V2Os-TiO2. To further improve catalytic reactivity of optimized catalyst, we dope a series of additional element such as Mn, Ce, Mo, Cr, Ni, Co to catalyst V2O5-TiO2-CNTs. Experimental results showed that CeOx can enhance SCR activity of catalysts greatly. We also synthesized three kind of catalysts in which carbon materials support CuOx and found a simple way to regenerate the deactivated catalysts.
The introduction of carbon nanotubes to catalyst V2O5-TiO2 can promote its SCR performance greatly. The best reactivity of catalyst was achieved by doped 10% carbon nanotubes, the removal efficiency for NOx can reach up to 89%at 300℃.The specific surface, pore volume, acidity and reducibility of catalyst increased with introduction of carbon nanotubes. The high reducibility can enhance the oxidation efficiency of NO to NO2. The catalyst V2O5-TiO2-CNTs has a good resistence to SO2 and H2O.
The combination of low-temperature active MnOx and high-temperature active V2O5 was accomplished by adding MnOx into V2O5/TiO2-CNT composites. A NOX removal efficiency of 99%was observed over V2O5-MnOx/TiO2-CNTs at 275℃under a GHSV of 36000 h"1. TOF results suggest a possible constructive interaction between V2O5 and MnOx for catalysts prepared by mechanical mixing. The possible separation of Mn and V with the assistance of CNTs and the increase of reducibility and acidic strength all contribute to the improvement of catalytic activity.
Co, Ce. Cr, Mo, Ni were introduced to catalyst V2O5/T1O2-CNTS with sol-gel method and Ce was proved to be most effective to promote NH3-SCR activity. A large number of Ce3+contributes to the increase of chemisorbed oxygen, which favors the SCR activity. The aggregation of catalyst might be inhibited by CeOx thus result to the increase of specific surface. Moreover, the increase of surface acidity and reducibility both contribute to the extra NOx conversion upon addition of CeOx-The deactivation of catalyst VCeqTiC caused by SO2 depends on reaction temperatures and gas velocity strongly. And at least 2%of oxygen in exhaust gas is essential to keep high SCR activity.
Cu-CNTs was prepared by wet impregnation method and a NOx removal efficiency of 67%was achieved at 250℃. which could be attributed to the good dispersion of CuOx, the existence of Cu+and strong acid sites on the catalysts" surface. Moreover, the regeneration of deactivated catalyst CuOx-CNTs caused by SO2 could be achieved by heating the catalyst in N2 at 300℃.
引文
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