铁铈蜂窝金属丝网催化剂用于选择催化还原NO_x的研究
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摘要
氨法选择催化还原(NH3-SCR)技术由于其低成本和高效率的特点已成为国内外首选的脱硝技术。目前已广泛应用的商业脱硝催化剂是V2O5-WO3(MoO3)/TiO2,并且在实际工况中为了获得较低的压降,该类催化剂通常以蜂窝整体式催化剂的形式存在。然而,在实际应用中该钒基催化剂仍存在活性组分有毒、活性窗口窄、较高的SO2氧化率和易尘堵等缺陷。针对以上问题,本研究分别从催化剂的载体和活性组分两方面入手进行研究,为新型脱硝催化剂的开发做出积极有益的探索。
首先,本研究采用两步浸渍法制备了以蜂窝金属丝网为载体的钒基脱硝催化剂。通过与具有相同活性组分的蜂窝陶瓷催化剂对比研究发现,蜂窝状金属丝网催化剂表现出了优良的低温活性、抗硫抗水以及抗尘性能。在60h耐硫耐水实验(600ppmSO2+10%H2O)和40h抗尘实验中,蜂窝状金属丝网催化剂的脱硝活性始终保持在92%和90%左右。
而通过对催化剂在耐硫耐水实验前后的各种测试表征和分析后发现,硫酸铵盐的沉积是催化剂在含硫含水气氛中失活的主要原因,且蜂窝状金属丝网催化剂表面的硫酸铵盐含量明显低于蜂窝陶瓷催化剂。这是由于蜂窝状金属丝网催化剂独特的三维通透结构不利于粉末状颗粒物在其表面大量沉积,使其在耐硫耐水及抗尘实验中表现出了优良的脱硝活性。
其次,本研究采用浸渍法制备了掺铁铈钛催化剂,通过活性实验发现铁的加入可以大大提高催化剂的低温SCR舌性与抗硫中毒能力。当Fe/Ti摩尔比为0.2,煅烧温度为500℃时,Fe-Ce/TiO2催化剂在160℃即能到80%左右NO、去除率,且在250℃,11h耐硫实验(500ppm SO2)后仍能保持95%左右的NOx去除率。各种测试表征结果表明：将Fe掺杂入Ce/TiO2催化剂中能够提高催化剂表面NH4+和吸附态NO2的数量,从而促进了催化剂的低温SCR舌性。
在此研究基础上,本研究对上述Fe-Ce/TiO2催化剂进行了SCR机理的研究：当反应温度低于200℃时是典型的Langmuir-Hinshelwood机理,即反应是在吸附态NO2和Lewis酸性位上配位态NH3与Bronsted酸性位上NH4+之间发生；当反应温度高于200℃时是典型的Eley-Rideal机理,即反应是在吸附态NH3和气相/弱吸附态NO之间发生。
最后,本研究以蜂窝状金属丝网为载体,Fe-Ce/TiO2为活性组分制备了整体式催化剂,并比较了不同SO2浓度下Fe-Ce/TiO2/蜂窝金属丝网催化剂的抗硫中毒能力。当反应温度为250℃时经过100h耐硫实验(1000ppm SO2), Fe-Ce/WMH的脱硝活性仍能保持在85%以上。各种测试表征和分析结果表明：在含硫气氛中进行SCR反应时,Fe-Ce/WMH催化剂表面的Ce02易与烟气中的SO2发生反应,并且有少量硫酸铵盐形成。这里,烟气中的SO2会促进催化剂表面Ce4+→Ce3+,从而导致催化剂表面化学吸附氧含量的增多,这可能也是Fe-Ce/WMH在100h耐硫实验中具有优良抗硫中毒能力的重要原因。在整个耐硫过程中Fe-Ce/WMH催化剂表面的反应主要遵循E-R反应机理。
Selective catalytic reduction with NH3(NH3-SCR) is the most reliable method to remove the NOX from stationary sources due to the low cost and high efficiency. Currently, the commercial catalysts for this process are V2O5-WO3(MoO3)/TiO2catalysts and they are preferentially applied in form of monolithic honeycombs due to their low pressure drop. However, these catalysts commonly suffer from the toxicity of active component to environment, the narrow operation temperature window, the high activity for the oxidation of SO2to SO3and easy to dust blocking. Aiming to develop new DeNOx catalyst, catalyst support and active component were investigated in this paper.
Firstly, V2O5-WO3/TiO2/Al2O3/wire-mesh honeycomb catalyst was prepared by a two-step impregnation method. In comparison with ceramic honeycomb catalyst with the same composition, the wire-mesh honeycomb catalyst exhibited good low-temperature activity and resistance to H2O, SO2and dust. During the60h H2O and SO2durability test (600ppm SO2+10%H2O) and40h dust exposure experiment, the wire-mesh honeycomb catalyst could provide nearly92%and90%NOX conversion, respectively. Characteration analyses of fresh and spent catalysts demonstrated that the deposition of sulfate-ammonium salts on catalyst surface was the dominant reason for the catalyst deactivation in the H2O and SO2durability test, and there was less sulfate-ammonium salts deposited on the surface of the wire-mesh honeycomb catalyst than that on the ceramic honeycomb catalyst. For the wire-mesh honeycomb catalyst, the unique three-dimensional structure was unfavorable for the high particle material deposition, which was the reason for the excellent resistance to H2O, SO2and dust.
Secondly, Fe doped Ce/TiO2catalyst was prepared by impregnation method. From the activity test results, it was found that the addition of Fe could enhance the low-temperature activity and sulfur-poisoning resistance of Ce/TiO2. The Fe-Ce/TiO2catalyst with Fe/Ti molar ratio of0.2could attain80%NOx conversion at160℃, provide above85%NOx conversion after11h SO2durability test (500ppm SO2) at250℃. The characteration results indicated that the Fe doping to Ce/TiO2could increase the amount of NH4+and adsorbed NO2on catalyst surface, and thus promte the low-temperature SCR activity.
Furthermore, the SCR reaction mechanism of the Fe-Ce/TiO2catalyst was studied. In the relatively low temperature range (<200℃), coordinated NH3and ionic NH4+sprcies as well as adsorbed NO2were involved in the SCR reaction following a Langmuir-Hinshelwood mechanism. In the relatively high temperature range (>200℃), coordinated NH3and gas-phase/weakly adsorbed NO predominated on the catalyst surface following Eley-Rideal mechanism.
Finally, Fe-Ce/TiO2/Al2O3/wire-mesh honeycomb catalyst was prepared, and its resistance to sulfur-poisoning for different SO2concentrations (100-1000ppm) was investigated. At250℃, the Fe-Ce/TiO2/Al2O3/wire-mesh honeycomb catalyst could provide approximately90%NOX conversion during100h SO2durability test (1000ppm SO2). The characteration results indicated that the sulfation of CeO2occurred preferentially during the SCR reaction in the presence of SO2, and a little sulfate-ammonium salts was formed. The sulfation of CeO2could promote conversion of Ce4+to Ce3+, resulting in the increase of chemisorbed oxygen species which might be the reason for the excellent resistance to sulfur-poisoning of the Fe-Ce/TiO2/Al2O3/wire-mesh honeycomb catalyst. The SCR reaction followed the Eley-Rideal mechanism during the SO2durability test.
首先,本研究采用两步浸渍法制备了以蜂窝金属丝网为载体的钒基脱硝催化剂。通过与具有相同活性组分的蜂窝陶瓷催化剂对比研究发现,蜂窝状金属丝网催化剂表现出了优良的低温活性、抗硫抗水以及抗尘性能。在60h耐硫耐水实验(600ppmSO2+10%H2O)和40h抗尘实验中,蜂窝状金属丝网催化剂的脱硝活性始终保持在92%和90%左右。
而通过对催化剂在耐硫耐水实验前后的各种测试表征和分析后发现,硫酸铵盐的沉积是催化剂在含硫含水气氛中失活的主要原因,且蜂窝状金属丝网催化剂表面的硫酸铵盐含量明显低于蜂窝陶瓷催化剂。这是由于蜂窝状金属丝网催化剂独特的三维通透结构不利于粉末状颗粒物在其表面大量沉积,使其在耐硫耐水及抗尘实验中表现出了优良的脱硝活性。
其次,本研究采用浸渍法制备了掺铁铈钛催化剂,通过活性实验发现铁的加入可以大大提高催化剂的低温SCR舌性与抗硫中毒能力。当Fe/Ti摩尔比为0.2,煅烧温度为500℃时,Fe-Ce/TiO2催化剂在160℃即能到80%左右NO、去除率,且在250℃,11h耐硫实验(500ppm SO2)后仍能保持95%左右的NOx去除率。各种测试表征结果表明：将Fe掺杂入Ce/TiO2催化剂中能够提高催化剂表面NH4+和吸附态NO2的数量,从而促进了催化剂的低温SCR舌性。
在此研究基础上,本研究对上述Fe-Ce/TiO2催化剂进行了SCR机理的研究：当反应温度低于200℃时是典型的Langmuir-Hinshelwood机理,即反应是在吸附态NO2和Lewis酸性位上配位态NH3与Bronsted酸性位上NH4+之间发生；当反应温度高于200℃时是典型的Eley-Rideal机理,即反应是在吸附态NH3和气相/弱吸附态NO之间发生。
最后,本研究以蜂窝状金属丝网为载体,Fe-Ce/TiO2为活性组分制备了整体式催化剂,并比较了不同SO2浓度下Fe-Ce/TiO2/蜂窝金属丝网催化剂的抗硫中毒能力。当反应温度为250℃时经过100h耐硫实验(1000ppm SO2), Fe-Ce/WMH的脱硝活性仍能保持在85%以上。各种测试表征和分析结果表明：在含硫气氛中进行SCR反应时,Fe-Ce/WMH催化剂表面的Ce02易与烟气中的SO2发生反应,并且有少量硫酸铵盐形成。这里,烟气中的SO2会促进催化剂表面Ce4+→Ce3+,从而导致催化剂表面化学吸附氧含量的增多,这可能也是Fe-Ce/WMH在100h耐硫实验中具有优良抗硫中毒能力的重要原因。在整个耐硫过程中Fe-Ce/WMH催化剂表面的反应主要遵循E-R反应机理。
Selective catalytic reduction with NH3(NH3-SCR) is the most reliable method to remove the NOX from stationary sources due to the low cost and high efficiency. Currently, the commercial catalysts for this process are V2O5-WO3(MoO3)/TiO2catalysts and they are preferentially applied in form of monolithic honeycombs due to their low pressure drop. However, these catalysts commonly suffer from the toxicity of active component to environment, the narrow operation temperature window, the high activity for the oxidation of SO2to SO3and easy to dust blocking. Aiming to develop new DeNOx catalyst, catalyst support and active component were investigated in this paper.
Firstly, V2O5-WO3/TiO2/Al2O3/wire-mesh honeycomb catalyst was prepared by a two-step impregnation method. In comparison with ceramic honeycomb catalyst with the same composition, the wire-mesh honeycomb catalyst exhibited good low-temperature activity and resistance to H2O, SO2and dust. During the60h H2O and SO2durability test (600ppm SO2+10%H2O) and40h dust exposure experiment, the wire-mesh honeycomb catalyst could provide nearly92%and90%NOX conversion, respectively. Characteration analyses of fresh and spent catalysts demonstrated that the deposition of sulfate-ammonium salts on catalyst surface was the dominant reason for the catalyst deactivation in the H2O and SO2durability test, and there was less sulfate-ammonium salts deposited on the surface of the wire-mesh honeycomb catalyst than that on the ceramic honeycomb catalyst. For the wire-mesh honeycomb catalyst, the unique three-dimensional structure was unfavorable for the high particle material deposition, which was the reason for the excellent resistance to H2O, SO2and dust.
Secondly, Fe doped Ce/TiO2catalyst was prepared by impregnation method. From the activity test results, it was found that the addition of Fe could enhance the low-temperature activity and sulfur-poisoning resistance of Ce/TiO2. The Fe-Ce/TiO2catalyst with Fe/Ti molar ratio of0.2could attain80%NOx conversion at160℃, provide above85%NOx conversion after11h SO2durability test (500ppm SO2) at250℃. The characteration results indicated that the Fe doping to Ce/TiO2could increase the amount of NH4+and adsorbed NO2on catalyst surface, and thus promte the low-temperature SCR activity.
Furthermore, the SCR reaction mechanism of the Fe-Ce/TiO2catalyst was studied. In the relatively low temperature range (<200℃), coordinated NH3and ionic NH4+sprcies as well as adsorbed NO2were involved in the SCR reaction following a Langmuir-Hinshelwood mechanism. In the relatively high temperature range (>200℃), coordinated NH3and gas-phase/weakly adsorbed NO predominated on the catalyst surface following Eley-Rideal mechanism.
Finally, Fe-Ce/TiO2/Al2O3/wire-mesh honeycomb catalyst was prepared, and its resistance to sulfur-poisoning for different SO2concentrations (100-1000ppm) was investigated. At250℃, the Fe-Ce/TiO2/Al2O3/wire-mesh honeycomb catalyst could provide approximately90%NOX conversion during100h SO2durability test (1000ppm SO2). The characteration results indicated that the sulfation of CeO2occurred preferentially during the SCR reaction in the presence of SO2, and a little sulfate-ammonium salts was formed. The sulfation of CeO2could promote conversion of Ce4+to Ce3+, resulting in the increase of chemisorbed oxygen species which might be the reason for the excellent resistance to sulfur-poisoning of the Fe-Ce/TiO2/Al2O3/wire-mesh honeycomb catalyst. The SCR reaction followed the Eley-Rideal mechanism during the SO2durability test.
引文
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