柴油机尾气碳烟氧化催化剂的制备与催化活性的研究
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摘要
柴油机因其循环热效率高、燃油经济性好而日益受到重视。然而柴油机排放物造成的环境污染问题也日益突出。柴油机的主要排放物碳烟，不仅对视觉和嗅觉有不良的影响，而且碳烟上常常粘附SO_2及致癌物质，对任何生物都有害。
由于碳烟颗粒的热氧化温度高达550～600℃，而柴油车的排气温度为175～400℃。为了降低碳烟燃烧温度，其中一个解决的办法就是使用以催化剂为基的DPF。在DPF中使用的催化剂应该在实际工作条件下显示出良好的活性，稳定性和耐久性。尽管世界各先进国家的科学家经过三十多年的探索和研究，但尚未找到一种像汽油机用的三效催化剂那样十分有效的碳烟氧化催化剂。
本研究分别采用浸渍法和涂覆法制备了V_2O_5-KCl和NH_4VO_3-KNO_3碳烟氧化催化剂，采用研磨混合法制备了V-ⅡA，V-Ln，Co—ⅡA，Sm-ⅡA，Ce-Zr系列碳烟氧化催化剂，采用涂覆法制备了V-ⅡA-K，Ln-K，V-Ln-K，Co-ⅡA-K，Sm-ⅡA-K，Ce-Zr-K系列碳烟氧化催化剂，采用共沉淀法、溶胶-凝胶法和高分子凝胶法制备了Ce_(0.5)Zr_(0.5)O_2碳烟氧化催化剂，采用程序升温反应控制系统(TPR)测试了催化剂的催化活性，应用TG-DSC和XRD对催化剂的结构进行了表征，采用SEM对催化剂的表面以及碳烟粒子形貌进行了观察，应用TEM对制备的Ce-Zr催化剂粉体形貌进行了观察，并采用比表面积分析仪对Ce-Zr催化剂的比表面积进行了测定。分析了催化剂的结构与催化活性之间的关系，另外还对催化剂与碳烟之间的接触模式对催化剂催化活性的影响进行了研究，并对催化剂的催化机理进行了初步探索。
采用涂覆法制备的NH_4VO_3-KNO_3催化剂的催化活性要明显高于浸渍法制备的NH_4VO_3-KNO_3催化剂的催化活性，主要是由于催化剂粉末涂覆在载体表面，形成凹凸表面，可以增大催化剂和碳烟的接触面积，因而催化活性要更高。而采用溶液浸渍的方法使催化剂进入载体组织内部，表面比较平滑，使催化剂和碳烟的接触不如涂覆法充分。
采用涂覆法制备的KNO_3催化剂的催化活性要高于KCl催化剂的催化活性，主要是因为：一方面，KNO_3的熔点较低(330℃)，熔融的KNO_3能够增强碳烟与催化剂之间的接触，另外一方面，可能的催化机制就是KNO_3是一种强氧化剂，KNO_3能够被C还原成KNO_2，KNO_2然后又能被O_2氧化成KNO_3。
对于NH_4VO_3：KNO_3=1：2催化剂来说，在主晶相KNO_3+KVO_3的协同作用下，碳烟的起始燃烧温度是362℃，催化剂的催化活性高于单一组分的KNO_3和KVO_3的催化活性。随着KNO_3含量的增加，催化剂的催化活性降低了，一方面由于KHCO_3的含量增多了，阻碍了催化剂的活性组分KNO_3和KVO_3与碳烟的接触，另一方面KVO_3相减少了，降低了与KNO_3协同作用的发挥，因此也导致了碳烟起始燃烧温度的升高。
在V-K催化剂的作用下，碳烟的起始燃烧温度较高，而且碳烟氧化速率也较慢，由于KNO_3的熔点较低，催化剂的稳定性也较差。在V-K催化剂中添加碱土金属氧化物或盐类的目的二方面是提高催化剂的稳定性，另一方面是增加催化剂中KNO_3的绝对含量，可以降低由于部分KNO_3的流失而造成的催化活性的恶化。在V-ⅡA-K系列催化剂中，在V：ⅡA：K=1：1：6催化剂的作用下，碳烟的起始燃烧温度最低。CaO和MgO的催化活性比较差，而Sr(NO_3)_2和Ba(NO_3)_2都是氧化剂，碳烟的起始燃烧温度比CaO和MgO大大降低，碳烟氧化速率也较快，其催化机制是：M(NO_3)_2+C=M(NO_2)_2+CO_2 (1) 2M(NO_2)_2+C=2MN_2O_3+CO_2 (2) 2MN_2O_3+O_2=2M(NO_2)_2 (3) M(NO_2)_2+O_2=M(NO_3)_2(M是Sr或Ba) (4)
在稀土金属氧化物催化剂中添加了KNO_3以后，催化剂的催化活性明显增强。其中稀土金属氧化物与KNO_3并没有形成化合物，而可能是一部分K~+进入到稀土金属氧化物中形成固溶体，造成晶格缺陷，促进碳烟燃烧。Ln-K催化剂的作用下，碳烟的起始燃烧温度由低到高的顺序为：Ce-K(330℃)=Pr-K(330℃)＜La-K(350℃)=Y-K(350℃)＜Sm-K(365℃)；碳烟氧化速率由快到慢的顺序为：Sm-K＞Ce-K=La-K＞Y-K＞Pr-K。在V-K催化剂中添加稀土金属氧化物，V-Ce／Pr-K=1：0.25：2催化剂的催化活性与Ce／Pr-K=1：2催化剂差不多，而V-La／Y-K=1：0.5：2催化剂的催化活性稍高于La／Y-K=1：2催化剂，V-Sm-K=1：0.5：2催化剂的催化活性明显高于Sm-K=1：2催化剂。
在所制备的Co-ⅡA-K催化剂中，接触方式对催化剂的催化活性都有影响，尤其是碳烟氧化速率受接触程度的影响较大。只有在采用研磨法制造的紧密接触的条件下，碳烟才更容易与催化剂表面的晶格氧发生反应，而采用KNO_3的熔化来制造的紧密接触条件下，碳烟氧化速率要慢一些。这主要是因为虽然KNO_3的熔化增强了碳烟与催化剂的接触，也增加了催化剂的流动性，但是熔化的KNO_3同时会连成片，反而会妨碍催化剂中几种晶相的协同作用的发挥。当Co：ⅡA：K=0.5：0.25：2时，催化剂的催化活性最高，在紧密接触与松散接触的条件下，碳烟的起始燃烧温度差不多，而碳烟氧化速率在紧密接触的条件下要快一些。Co_3O_4的催化机理是：2Co_3O_4+C=6CoO+CO_2 (5) 2CoO+C=2Co+CO (6) 2Co+O_2=2CoO (7) 6CoO+O_2=2Co_3O_4 (8)
在所制备的Sm-ⅡA-K催化剂中，Sm、ⅡA和K之间没有形成化合物，但是催化剂的催化活性较好，其中MgO／CaO／Sr(NO_3)_2／Ba(NO_3)_2提高了催化剂碳烟氧化速率，Sm_2O_3改善了冷启动性，KNO_3一方面改善了催化剂与碳烟之间的接触，另一方面本身作为氧化剂氧化碳烟。当KNO_3-Mg，KNO_3-Ca，KNO_3-Sr，和KNO_3-Ba的重量比例分别为8.41，5.78，7.57和7.36时，催化剂具有最佳的催化活性，即碳烟具有最低的起始燃烧温度318，323，332和325℃。另外在Sm-ⅡA-K催化剂的作用下，碳烟氧化速率比V-Sm-K催化剂快。
采用研磨混合法制备的Ce-Zr催化剂的催化活性要高于采用共沉淀法、溶胶凝胶法和高分子凝胶法制备的Ce-Zr-O固溶体催化剂，说明ZrO_2+CeO_2的协同催化作用大于Zr_(0.5)Ce_(0.5)O_2催化剂。无论何种制备方法制备的催化剂，在紧密接触的条件下，催化剂的催化活性都要好于在松散接触的条件，说明Ce-Zr催化剂的催化活性受接触条件的限制。尽管采用研磨混合法制备的Ce-Zr催化剂与碳烟在松散接触的条件下催化活性较差，但是在紧密接触的条件下，碳烟的起始燃烧温度甚至低于含有KNO_3的催化剂。
Diesel engines are more popular due to the relatively high thermal efficiency andfuel economy than gasoline engines. Diesel engine emissions have led to seriousenvironmental problems especially their carbon particles content. The small size ofdiesel soot particles(≤2μm) may be linked to a number of health problems by itsability to penetrate the body through the respiratory system.
The non-catalytic ignition temperature of soot generally exceeds 550℃, while thetemperature of typical exhausts is 400℃or below in light duty applications. Thecombination of traps and oxidation catalysts appears to be the most plausibleafter-treatment technique to eliminate soot particles. However, the temperature ofdiesel exhaust is in the range of 175-400℃. To lower the soot ignition temperature,one solution is using a catalyst-based DPF. The catalysts used in a catalytic DPFshould display good activity in the temperature range of diesel exhaust, and goodstability and durability under practical working conditions. Many attempts have beenmade to develop the useful catalysts that promote soot oxidation, whereas there is noeffective catalyst like three-way catalysts that can be applied in practice.
In this paper, V_2O_5-KCl and NH_4VO_3-KNO_3 catalysts have been prepared byimpregnation and coating method, V-ⅡA, V-Ln, Co-ⅡA, Sm-ⅡA, and Ce-Zrcatalysts have been produced by grinding method, V-ⅡA-K, Ln-K, V-Ln-K,Co-ⅡA-K, Sin-ⅡA-K, and Ce-Zr-K catalysts have been prepared by coating method.In addition, Ce_(0.5)Zr_(0.5)O_2 have been prepared by co-precipitation, sol-gel andpolymer-network gel methods. XRD and TG-DSC have been used to characterize the catalysts, and their catalytic activities have been evaluated by a temperatureprogrammed reaction system (TPR). The surface morphologies of catalysts and sootparticles have been observed by SEM. The morphologies of Ce-Zr catalysts powderprepared by various methods have been observed by TEM, and the BET has beenmeasured too. The relation between the structure and catalytic activity has beenanalyzed. Otherwise, the effect of contact mode between catalysts and soot on catalyticactivity has been studied, and the catalytic mechanism has been explored.
The catalytic activity of NH_4VO_3-KNO_3 catalysts prepared by coating method isbetter than those prepared by impregnation method. As the catalysts coated on thesubstrate can form accidented surface and increase the contact area between thecatalyst and the soot. However, the catalyst prepared by impregnation can enter intosubstrate and the surface is relatively smooth, which lead to poor contact between thesoot and the catalyst.
The catalytic activity of KNO_3 prepared by coating method is higher than that ofKCl. On the one hand, the melting KNO_3 can enhance the contact between the catalystand the soot as the melting point of KNO3 is 330℃; on the other hand, the probablemechanism is that one in which the nitrate is reduced to nitrite by the reaction withcarbon and that the oxygen or the nitrogen oxide oxidize the nitrite again to nitrate.
The soot onset ignition temperature is 362℃by the synergistic catalysis of KNO_3with KVO_3 for NH_4VO_3-KNO_3 catalyst with a molar ratio of 1:1, which is lower thanthat of single KNO_3 or KVO_3. The catalytic activity of NH_4VO_3-KNO_3 catalysts islowered with the increase of KNO_3 content. One reason is that the higher KHCO_3content hinders the contact between the catalyst and the soot; the other is that thesynergistic catalysis is lowered with the decrease of KVO_3.
The soot onset ignition temperature is relatively high, and soot oxidation rate isslow for V-K catalysts. In addition, the V-K catalysts are unstable due to the lowermelting point of KNO_3. The V-K catalysts added alkaline earth metal oxide or nitratecould improve the stability of catalysts, and increase the KNO_3 content avoiding thedeterioration of catalytic activity led by the loss of partial KNO_3. The catalytic activityof CaO/MgO is worse than that of Sr(NO_3)_2/Ba(NO-3)_2 which are oxidant. The catalyticmechanism of Sr(NO_3)_2/Ba(NO_3)_2 is: M(NO_3)_2+C=M(NO_2)_2+CO_2 (1) 2M(NO_2)_2+C=2MN_2O_3+CO_2 (2) 2MN_2O_3+O_2=2M(NO_2)_2 (3) M(NO_2)_2+O_2=M(NO_3)_2 (Mis SrorBa) (4)
The soot onset ignition temperature of-Ⅴ-ⅡA-K catalyst with a molar ratio of 1:1:6 is the lowest among the prepared V-ⅡA-K catalysts.
The catalytic activity is improved by adding KNO_3 to rare earth metal oxide, Thecrystal lattice defect formed by partial K~+ entering into the rare earth metal oxide canpromote the soot combustion. The soot onset ignition temperature order of Ln-Kcatalysts is as follows: Ce-K(330℃C=Pr-K(330℃)＜La-K(350℃)=Y-K(350℃)＜Sm-K(365℃). The soot oxidation rate comply to the sequence: Sm-K＞Ce-K=La-K＞Y-K＞Pr-K。
The catalytic activity of V-Ce/Pr-K catalyst with a molar ratio of 1:0.25:2 isalmost the same as that of Ce/Pr-K catalyst with a molar ratio of 1:2. The catalyticactivity of V-La/Y-K catalyst with a molar ratio of 1:0.5:2 is higher slightly than that ofLa/Y-K catalyst with a molar ratio of 1:2. The catalytic activity of V-Sm-K catalyst ishigher obviously than that of Sm-K catalyst with a molar ratio of 1:2.
The effect of contact mode between the catalyst and the soot has an importanteffect on the catalytic activity of Co-ⅡA-K catalysts, especially on the soot oxidationrate. The soot can react with crystal lattice O only in tight contact condition made bygrinding, while the soot oxidation rate becomes slow in tight contact condition madeby melting KNO_3. Although it can improve the contact condition between the soot andthe catalyst, the melting KNO_3 can encumber the synergistic catalysis of severalcrystalline phases. The catalytic activity of Co-ⅡA-K catalyst with a molar ratio of0.5:0.25:2 is the best, and the soot onset ignition temperature is almost same whetherin tight contact or in loose contact condition, while the soot oxidation rate is morerapidly in tight contact condition than that in loose contact condition. The catalyticmechanism of Co_3O_4 is: 2Co_3O4+C=6CoO+CO_2 (5) 2CoO+C=2Co+CO_2 (6) 2Co+O_2=2CoO (7) 6CoO+O_2=2Co_3O_4 (8)
The catalytic activity of Sin-ⅡA-K catalyst is good. The soot oxidation rate isquickened by adding MgO/CaO/Sr(NO_3)_2/Ba(NO_3)_2, and the cold boot performance isimproved by adding Sm_2O_3. KNO_3 can enhance the contact between catalyst and soot,and act as an oxidant. The soot onset ignition temperature is 318, 323,332, aad 325℃when the weight ratio ofKNO_3-Mg, KNO_3-Ca, KNO_3-Sr and KNO_3-Ba is 8.41, 5.78,7.57, and 7.36 respectively for Sin-ⅡA-K catalysts. In addition, the soot oxidation rateof the Sin-ⅡA-K catalysts is more rapidly than that of V-Sm-K catalysts.
The catalytic activity of Ce-Zr catalysts is higher than Zr_(0.5)Ce_(0.5)O_2 prepared byco-precipitation, sol-gel and polymer-network gel methods, wfiich shows that the synergistic catalysis of ZrO2-CeO2 is better thafi~ that of Zro.sCeo.502. The catalyticactivity of all the Ce-Zr catalysts is higher in tight contact mode than that in loosecontact mode. The soot onset ignition temperature of Ce-Zr catalyst prepared bygrinding method in tight contact condition.is lower than the catalysts containing KNO3
由于碳烟颗粒的热氧化温度高达550～600℃，而柴油车的排气温度为175～400℃。为了降低碳烟燃烧温度，其中一个解决的办法就是使用以催化剂为基的DPF。在DPF中使用的催化剂应该在实际工作条件下显示出良好的活性，稳定性和耐久性。尽管世界各先进国家的科学家经过三十多年的探索和研究，但尚未找到一种像汽油机用的三效催化剂那样十分有效的碳烟氧化催化剂。
本研究分别采用浸渍法和涂覆法制备了V_2O_5-KCl和NH_4VO_3-KNO_3碳烟氧化催化剂，采用研磨混合法制备了V-ⅡA，V-Ln，Co—ⅡA，Sm-ⅡA，Ce-Zr系列碳烟氧化催化剂，采用涂覆法制备了V-ⅡA-K，Ln-K，V-Ln-K，Co-ⅡA-K，Sm-ⅡA-K，Ce-Zr-K系列碳烟氧化催化剂，采用共沉淀法、溶胶-凝胶法和高分子凝胶法制备了Ce_(0.5)Zr_(0.5)O_2碳烟氧化催化剂，采用程序升温反应控制系统(TPR)测试了催化剂的催化活性，应用TG-DSC和XRD对催化剂的结构进行了表征，采用SEM对催化剂的表面以及碳烟粒子形貌进行了观察，应用TEM对制备的Ce-Zr催化剂粉体形貌进行了观察，并采用比表面积分析仪对Ce-Zr催化剂的比表面积进行了测定。分析了催化剂的结构与催化活性之间的关系，另外还对催化剂与碳烟之间的接触模式对催化剂催化活性的影响进行了研究，并对催化剂的催化机理进行了初步探索。
采用涂覆法制备的NH_4VO_3-KNO_3催化剂的催化活性要明显高于浸渍法制备的NH_4VO_3-KNO_3催化剂的催化活性，主要是由于催化剂粉末涂覆在载体表面，形成凹凸表面，可以增大催化剂和碳烟的接触面积，因而催化活性要更高。而采用溶液浸渍的方法使催化剂进入载体组织内部，表面比较平滑，使催化剂和碳烟的接触不如涂覆法充分。
采用涂覆法制备的KNO_3催化剂的催化活性要高于KCl催化剂的催化活性，主要是因为：一方面，KNO_3的熔点较低(330℃)，熔融的KNO_3能够增强碳烟与催化剂之间的接触，另外一方面，可能的催化机制就是KNO_3是一种强氧化剂，KNO_3能够被C还原成KNO_2，KNO_2然后又能被O_2氧化成KNO_3。
对于NH_4VO_3：KNO_3=1：2催化剂来说，在主晶相KNO_3+KVO_3的协同作用下，碳烟的起始燃烧温度是362℃，催化剂的催化活性高于单一组分的KNO_3和KVO_3的催化活性。随着KNO_3含量的增加，催化剂的催化活性降低了，一方面由于KHCO_3的含量增多了，阻碍了催化剂的活性组分KNO_3和KVO_3与碳烟的接触，另一方面KVO_3相减少了，降低了与KNO_3协同作用的发挥，因此也导致了碳烟起始燃烧温度的升高。
在V-K催化剂的作用下，碳烟的起始燃烧温度较高，而且碳烟氧化速率也较慢，由于KNO_3的熔点较低，催化剂的稳定性也较差。在V-K催化剂中添加碱土金属氧化物或盐类的目的二方面是提高催化剂的稳定性，另一方面是增加催化剂中KNO_3的绝对含量，可以降低由于部分KNO_3的流失而造成的催化活性的恶化。在V-ⅡA-K系列催化剂中，在V：ⅡA：K=1：1：6催化剂的作用下，碳烟的起始燃烧温度最低。CaO和MgO的催化活性比较差，而Sr(NO_3)_2和Ba(NO_3)_2都是氧化剂，碳烟的起始燃烧温度比CaO和MgO大大降低，碳烟氧化速率也较快，其催化机制是：M(NO_3)_2+C=M(NO_2)_2+CO_2 (1) 2M(NO_2)_2+C=2MN_2O_3+CO_2 (2) 2MN_2O_3+O_2=2M(NO_2)_2 (3) M(NO_2)_2+O_2=M(NO_3)_2(M是Sr或Ba) (4)
在稀土金属氧化物催化剂中添加了KNO_3以后，催化剂的催化活性明显增强。其中稀土金属氧化物与KNO_3并没有形成化合物，而可能是一部分K~+进入到稀土金属氧化物中形成固溶体，造成晶格缺陷，促进碳烟燃烧。Ln-K催化剂的作用下，碳烟的起始燃烧温度由低到高的顺序为：Ce-K(330℃)=Pr-K(330℃)＜La-K(350℃)=Y-K(350℃)＜Sm-K(365℃)；碳烟氧化速率由快到慢的顺序为：Sm-K＞Ce-K=La-K＞Y-K＞Pr-K。在V-K催化剂中添加稀土金属氧化物，V-Ce／Pr-K=1：0.25：2催化剂的催化活性与Ce／Pr-K=1：2催化剂差不多，而V-La／Y-K=1：0.5：2催化剂的催化活性稍高于La／Y-K=1：2催化剂，V-Sm-K=1：0.5：2催化剂的催化活性明显高于Sm-K=1：2催化剂。
在所制备的Co-ⅡA-K催化剂中，接触方式对催化剂的催化活性都有影响，尤其是碳烟氧化速率受接触程度的影响较大。只有在采用研磨法制造的紧密接触的条件下，碳烟才更容易与催化剂表面的晶格氧发生反应，而采用KNO_3的熔化来制造的紧密接触条件下，碳烟氧化速率要慢一些。这主要是因为虽然KNO_3的熔化增强了碳烟与催化剂的接触，也增加了催化剂的流动性，但是熔化的KNO_3同时会连成片，反而会妨碍催化剂中几种晶相的协同作用的发挥。当Co：ⅡA：K=0.5：0.25：2时，催化剂的催化活性最高，在紧密接触与松散接触的条件下，碳烟的起始燃烧温度差不多，而碳烟氧化速率在紧密接触的条件下要快一些。Co_3O_4的催化机理是：2Co_3O_4+C=6CoO+CO_2 (5) 2CoO+C=2Co+CO (6) 2Co+O_2=2CoO (7) 6CoO+O_2=2Co_3O_4 (8)
在所制备的Sm-ⅡA-K催化剂中，Sm、ⅡA和K之间没有形成化合物，但是催化剂的催化活性较好，其中MgO／CaO／Sr(NO_3)_2／Ba(NO_3)_2提高了催化剂碳烟氧化速率，Sm_2O_3改善了冷启动性，KNO_3一方面改善了催化剂与碳烟之间的接触，另一方面本身作为氧化剂氧化碳烟。当KNO_3-Mg，KNO_3-Ca，KNO_3-Sr，和KNO_3-Ba的重量比例分别为8.41，5.78，7.57和7.36时，催化剂具有最佳的催化活性，即碳烟具有最低的起始燃烧温度318，323，332和325℃。另外在Sm-ⅡA-K催化剂的作用下，碳烟氧化速率比V-Sm-K催化剂快。
采用研磨混合法制备的Ce-Zr催化剂的催化活性要高于采用共沉淀法、溶胶凝胶法和高分子凝胶法制备的Ce-Zr-O固溶体催化剂，说明ZrO_2+CeO_2的协同催化作用大于Zr_(0.5)Ce_(0.5)O_2催化剂。无论何种制备方法制备的催化剂，在紧密接触的条件下，催化剂的催化活性都要好于在松散接触的条件，说明Ce-Zr催化剂的催化活性受接触条件的限制。尽管采用研磨混合法制备的Ce-Zr催化剂与碳烟在松散接触的条件下催化活性较差，但是在紧密接触的条件下，碳烟的起始燃烧温度甚至低于含有KNO_3的催化剂。
Diesel engines are more popular due to the relatively high thermal efficiency andfuel economy than gasoline engines. Diesel engine emissions have led to seriousenvironmental problems especially their carbon particles content. The small size ofdiesel soot particles(≤2μm) may be linked to a number of health problems by itsability to penetrate the body through the respiratory system.
The non-catalytic ignition temperature of soot generally exceeds 550℃, while thetemperature of typical exhausts is 400℃or below in light duty applications. Thecombination of traps and oxidation catalysts appears to be the most plausibleafter-treatment technique to eliminate soot particles. However, the temperature ofdiesel exhaust is in the range of 175-400℃. To lower the soot ignition temperature,one solution is using a catalyst-based DPF. The catalysts used in a catalytic DPFshould display good activity in the temperature range of diesel exhaust, and goodstability and durability under practical working conditions. Many attempts have beenmade to develop the useful catalysts that promote soot oxidation, whereas there is noeffective catalyst like three-way catalysts that can be applied in practice.
In this paper, V_2O_5-KCl and NH_4VO_3-KNO_3 catalysts have been prepared byimpregnation and coating method, V-ⅡA, V-Ln, Co-ⅡA, Sm-ⅡA, and Ce-Zrcatalysts have been produced by grinding method, V-ⅡA-K, Ln-K, V-Ln-K,Co-ⅡA-K, Sin-ⅡA-K, and Ce-Zr-K catalysts have been prepared by coating method.In addition, Ce_(0.5)Zr_(0.5)O_2 have been prepared by co-precipitation, sol-gel andpolymer-network gel methods. XRD and TG-DSC have been used to characterize the catalysts, and their catalytic activities have been evaluated by a temperatureprogrammed reaction system (TPR). The surface morphologies of catalysts and sootparticles have been observed by SEM. The morphologies of Ce-Zr catalysts powderprepared by various methods have been observed by TEM, and the BET has beenmeasured too. The relation between the structure and catalytic activity has beenanalyzed. Otherwise, the effect of contact mode between catalysts and soot on catalyticactivity has been studied, and the catalytic mechanism has been explored.
The catalytic activity of NH_4VO_3-KNO_3 catalysts prepared by coating method isbetter than those prepared by impregnation method. As the catalysts coated on thesubstrate can form accidented surface and increase the contact area between thecatalyst and the soot. However, the catalyst prepared by impregnation can enter intosubstrate and the surface is relatively smooth, which lead to poor contact between thesoot and the catalyst.
The catalytic activity of KNO_3 prepared by coating method is higher than that ofKCl. On the one hand, the melting KNO_3 can enhance the contact between the catalystand the soot as the melting point of KNO3 is 330℃; on the other hand, the probablemechanism is that one in which the nitrate is reduced to nitrite by the reaction withcarbon and that the oxygen or the nitrogen oxide oxidize the nitrite again to nitrate.
The soot onset ignition temperature is 362℃by the synergistic catalysis of KNO_3with KVO_3 for NH_4VO_3-KNO_3 catalyst with a molar ratio of 1:1, which is lower thanthat of single KNO_3 or KVO_3. The catalytic activity of NH_4VO_3-KNO_3 catalysts islowered with the increase of KNO_3 content. One reason is that the higher KHCO_3content hinders the contact between the catalyst and the soot; the other is that thesynergistic catalysis is lowered with the decrease of KVO_3.
The soot onset ignition temperature is relatively high, and soot oxidation rate isslow for V-K catalysts. In addition, the V-K catalysts are unstable due to the lowermelting point of KNO_3. The V-K catalysts added alkaline earth metal oxide or nitratecould improve the stability of catalysts, and increase the KNO_3 content avoiding thedeterioration of catalytic activity led by the loss of partial KNO_3. The catalytic activityof CaO/MgO is worse than that of Sr(NO_3)_2/Ba(NO-3)_2 which are oxidant. The catalyticmechanism of Sr(NO_3)_2/Ba(NO_3)_2 is: M(NO_3)_2+C=M(NO_2)_2+CO_2 (1) 2M(NO_2)_2+C=2MN_2O_3+CO_2 (2) 2MN_2O_3+O_2=2M(NO_2)_2 (3) M(NO_2)_2+O_2=M(NO_3)_2 (Mis SrorBa) (4)
The soot onset ignition temperature of-Ⅴ-ⅡA-K catalyst with a molar ratio of 1:1:6 is the lowest among the prepared V-ⅡA-K catalysts.
The catalytic activity is improved by adding KNO_3 to rare earth metal oxide, Thecrystal lattice defect formed by partial K~+ entering into the rare earth metal oxide canpromote the soot combustion. The soot onset ignition temperature order of Ln-Kcatalysts is as follows: Ce-K(330℃C=Pr-K(330℃)＜La-K(350℃)=Y-K(350℃)＜Sm-K(365℃). The soot oxidation rate comply to the sequence: Sm-K＞Ce-K=La-K＞Y-K＞Pr-K。
The catalytic activity of V-Ce/Pr-K catalyst with a molar ratio of 1:0.25:2 isalmost the same as that of Ce/Pr-K catalyst with a molar ratio of 1:2. The catalyticactivity of V-La/Y-K catalyst with a molar ratio of 1:0.5:2 is higher slightly than that ofLa/Y-K catalyst with a molar ratio of 1:2. The catalytic activity of V-Sm-K catalyst ishigher obviously than that of Sm-K catalyst with a molar ratio of 1:2.
The effect of contact mode between the catalyst and the soot has an importanteffect on the catalytic activity of Co-ⅡA-K catalysts, especially on the soot oxidationrate. The soot can react with crystal lattice O only in tight contact condition made bygrinding, while the soot oxidation rate becomes slow in tight contact condition madeby melting KNO_3. Although it can improve the contact condition between the soot andthe catalyst, the melting KNO_3 can encumber the synergistic catalysis of severalcrystalline phases. The catalytic activity of Co-ⅡA-K catalyst with a molar ratio of0.5:0.25:2 is the best, and the soot onset ignition temperature is almost same whetherin tight contact or in loose contact condition, while the soot oxidation rate is morerapidly in tight contact condition than that in loose contact condition. The catalyticmechanism of Co_3O_4 is: 2Co_3O4+C=6CoO+CO_2 (5) 2CoO+C=2Co+CO_2 (6) 2Co+O_2=2CoO (7) 6CoO+O_2=2Co_3O_4 (8)
The catalytic activity of Sin-ⅡA-K catalyst is good. The soot oxidation rate isquickened by adding MgO/CaO/Sr(NO_3)_2/Ba(NO_3)_2, and the cold boot performance isimproved by adding Sm_2O_3. KNO_3 can enhance the contact between catalyst and soot,and act as an oxidant. The soot onset ignition temperature is 318, 323,332, aad 325℃when the weight ratio ofKNO_3-Mg, KNO_3-Ca, KNO_3-Sr and KNO_3-Ba is 8.41, 5.78,7.57, and 7.36 respectively for Sin-ⅡA-K catalysts. In addition, the soot oxidation rateof the Sin-ⅡA-K catalysts is more rapidly than that of V-Sm-K catalysts.
The catalytic activity of Ce-Zr catalysts is higher than Zr_(0.5)Ce_(0.5)O_2 prepared byco-precipitation, sol-gel and polymer-network gel methods, wfiich shows that the synergistic catalysis of ZrO2-CeO2 is better thafi~ that of Zro.sCeo.502. The catalyticactivity of all the Ce-Zr catalysts is higher in tight contact mode than that in loosecontact mode. The soot onset ignition temperature of Ce-Zr catalyst prepared bygrinding method in tight contact condition.is lower than the catalysts containing KNO3
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