Ba-Mn基钙钛矿及其负载型Ba/Mn/TiO_2-x （x=Al_2O_3/SiO_2/ZrO_2） NOx储存还原催化剂研究
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摘要
NOx储存还原(NSR)技术是最有前景的稀燃氮氧化物消除技术。本文系统研究了以Ba-Mn为基础的钙钛矿型和负载型NSR催化剂,采用XRD、TG-MS、BET、H_2-TPR、NOx-TPD、in-situ DRIFT等多种表征技术详细考察了催化剂的NOx储存能力、热稳定性和抗硫能力,对NOx的储存模式进行了深入研究。
采用柠檬酸络合法制备了BaMnO_3系列钙钛矿催化剂。300℃时,亚硝酸盐到硝酸盐的转化速率远大于硝酸盐和亚硝酸盐的分解速率,NOx在BaMnO_3催化剂上的NSC值最高。掺杂不同比例的B位元素Cu/Mg/Fe后发现,Cu/Mg对催化剂结构和储存性能影响不大,Fe可以进入到BaMnO_3钙钛矿晶格中,增加了氧空位,Fe掺杂比例为0.4时,催化剂对NOx的储存能力大大提高。NOx在BaMnO_3表面的吸附物种随温度和时间发生转变,Fe部分取代后不改变NOx吸附的反应历程。低温下(≤200℃),NOx在表面的吸附主要以亚硝酸盐形式存在;200℃左右,表面硝酸盐物种逐渐脱附或歧化反应生成硝酸盐;高温下(≥300℃),主要以硝酸盐形式存在。
将Ba-Mn前驱体涂覆在复合载体TiO_2-Al_2O_3、TiO_2-SiO_2和TiO_2- ZrO_2上,600℃焙烧得到催化剂TABM6、TSBM6和TZBM6。样品TABM6和TSBM6中活性组分Ba主要以BaCO_3形式存在,由于TiO_2-SiO_2酸性高于TiO_2- Al_2O_3,导致TABM6中BaCO_3的含量高于TSBM6,NOx储存量结果也相对较大。而TZBM6样品中,除了部分BaCO_3之外,还有大量的BaMnO_3钙钛矿氧化物。TZBM6样品比表面积最小,体系中BaCO_3的含量也最少,但是因为有大量的BaMnO_3钙钛矿氧化物,也具有优良的NOx储存能力,NSC值能够达到105.7μmol/g。原位漫反射红外(in-situ DRIFT)结果表明,富氧条件下吸附NOx时,TABM6和TSBM6上NOx形成硝酸盐结构,尤其是TABM6上可看到从亚硝酸盐到硝酸盐的转化过程。TZBM6上NOx的吸附与BaMnO_3类似,都生成亚硝酸盐。
800℃高温焙烧之后,TABM6和TSBM6催化剂发生烧结,活性组分Ba与载体反应生成了BaAl_2O_4和Ba_2TiSi_2O_8。TZBM6催化剂结构未发生明显变化,ZrTiO_4固溶体和BaMnO_3钙钛矿晶粒有所增长。总体上看,TZBM6的抗热稳定性最佳。
硫化后(SO_2: 200ppm),催化剂的NSC值相对于新鲜样品TABM6、TSBM6、TZBM6分别下降了52.6%、19.7%和47.6%。硫化催化剂TABM6的NOx储存量仍然最大,其次为TSBM6,TZBM6样品的再储存能力最小。TSBM6具有最好的抗硫能力,与TiO_2-SiO_2载体具有最大的酸强度有关。
采用分步浸渍法制备了Pt-Mn/Ba/TiO_2-ZrO_2催化剂。Mn负载量增加时,催化剂表面形成Mn_2O_3晶体,对催化剂氧化性能和NOx储存能力影响不大。表面高度分散的Mn物种,800℃焙烧后,一部分进入载体晶格中形成新的固溶体Mn_(0.33)Ti_(0.33)Zr_(0.33)O_(1.67)。Pt物种的分散性和存在状态对催化剂的NOx储存性能有重要影响。高温焙烧,促进了PtO_2的分散,伴随部分氧化物物种的分解形成金属态的Pt,增强了Pt和Mn物种之间的相互作用。800℃焙烧样品Pt-C1-800中,Pt的分散性最好,对NO氧化能力最好,NSC值最大。
The NOx storage and reduction (NSR) technology will be the most promising way to reduce the NOx emission from lean-burn engines. In this work, we have designed a series of NSR catalysts based on Ba-Mn, including BaMnO_3 perovskite oxides and Ba/Mn/TiO_2-X (X=Al_2O_3/SiO_2/ZrO_2) supported catalysts. Their structures and properties were characterized by the techniques of XRD, TG-MS, BET, H_2-TPR and NOx-TPD.Their NOx storage capacity, thermal stability and sulfur resistance were also investigated. The mechanism of NOx adsorbing species were discussed by in-situ DRIFT.
BaMnO_3 perovskite oxides were prepared by citric acid complexation method. At 300oC, the rate of nitrite to nitrate transformation is higher than that of nitrate and nitrite decomposition. As a result, the BaMnO_3 perovskite oxide exhibits the highest NOx uptake at 300oC. No difference in the structure and NSR activity is found in the case of partial substitution of Mn by Cu/Mg. However, Fe substitution in B site leads to generation of oxygen vacancies. The highest NOx storage capacity is achieved on BaMn_(0.6)Fe_(0.4)O_3. Adsorption and storage of NOx on BaMnO_3 proceeds in three steps: (1) the formation of nitrites at low temperature (≤200oC); (2) its transformation to nitrates at temperature higher than 200oC, but lower than 300oC; (3) the formation of nitrates at high temperature (≥300oC). On the Fe-substitution catalysts, the NOx adsorption and storage processes are similar to the BaMnO_3 catalyst.
The TABM6、TSBM6 and TZBM6 catalysts were prepared by spreading Ba-Mn precursors as a thin layer on the TiO_2-Al_2O_3, TiO_2-SiO_2 and TiO_2- ZrO_2 supports calcined at 600 oC. The NOx storage capacity depends strongly on the relative abundance of BaCO_3 phases. Compared with the TSBM6 catalyst, more active BaCO_3 phases are detected in the TABM6 catalyst due to less acidity, which results in a higher NOx storage capacity. Although the BaCO_3 concentration was relatively lower, the TZBM6 catalyst still shows a high NSC of 105.7μmol/g due to the presence of a large amount of BaMnO_3 perovskite phase. During adsorption of NOx under lean burn condition, surface nitrates are formed on the TABM6 and TSBM6 catalysts, while surface nitrites are the dominant species on the TZBM6 catalyst. The transformation of nitrites to nitrates is observed on the TABM6 catalyst by in-situ DRIFT.
Thermal aging at 800oC leads to the conversion of dispersed BaCO_3 in the TABM6 and TSBM6 catalysts to crystalline BaAl_2O_4 and Ba_2TiSi_2O_8 respectively. The TZBM6 catalyst is quite stable against thermal treatment. NOx storage capacities of TABM6、TSBM6 and TZBM6 catalysts decline by the percentages of 52.6%,19.7% and 47.6% respectively, after treated in 200ppm SO_2 atmosphere for 30 min. The order of NSC of sulfated catalysts is TABM6>TSBM6>TZBM6. The TSBM6 catalyst displays the best sulfur resistance ability due to the highest acidity of TiO_2-SiO_2 support.
The Pt-Mn/Ba/TiO_2-ZrO_2 catalysts were prepared by a successive incipient wetness impregnation using TiO_2-ZrO_2 as support. Higher Mn loading resulted in aggregation of Mn_2O_3 crystallites on TiO_2-ZrO_2 support. After calcination at 800oC, a part of Mn species diffuses into the lattice of the support and forms a new phase Mn_(0.33)Ti_(0.33)Zr_(0.33)O_(1.67). The dispersion and phase of Pt species is the key factor for the NOx storage capacity of the catalyst. As the calcinations increases, the dispersion of Pt species is higher, while some PtO_2 species decompose to Pt metal phase. The results of EXAFS and NSC measurements showed that the maximum NO conversion and NOx storage capacity were achieved on the sample Pt-C1-800 due to the highest dispersion of Pt species.
采用柠檬酸络合法制备了BaMnO_3系列钙钛矿催化剂。300℃时,亚硝酸盐到硝酸盐的转化速率远大于硝酸盐和亚硝酸盐的分解速率,NOx在BaMnO_3催化剂上的NSC值最高。掺杂不同比例的B位元素Cu/Mg/Fe后发现,Cu/Mg对催化剂结构和储存性能影响不大,Fe可以进入到BaMnO_3钙钛矿晶格中,增加了氧空位,Fe掺杂比例为0.4时,催化剂对NOx的储存能力大大提高。NOx在BaMnO_3表面的吸附物种随温度和时间发生转变,Fe部分取代后不改变NOx吸附的反应历程。低温下(≤200℃),NOx在表面的吸附主要以亚硝酸盐形式存在;200℃左右,表面硝酸盐物种逐渐脱附或歧化反应生成硝酸盐;高温下(≥300℃),主要以硝酸盐形式存在。
将Ba-Mn前驱体涂覆在复合载体TiO_2-Al_2O_3、TiO_2-SiO_2和TiO_2- ZrO_2上,600℃焙烧得到催化剂TABM6、TSBM6和TZBM6。样品TABM6和TSBM6中活性组分Ba主要以BaCO_3形式存在,由于TiO_2-SiO_2酸性高于TiO_2- Al_2O_3,导致TABM6中BaCO_3的含量高于TSBM6,NOx储存量结果也相对较大。而TZBM6样品中,除了部分BaCO_3之外,还有大量的BaMnO_3钙钛矿氧化物。TZBM6样品比表面积最小,体系中BaCO_3的含量也最少,但是因为有大量的BaMnO_3钙钛矿氧化物,也具有优良的NOx储存能力,NSC值能够达到105.7μmol/g。原位漫反射红外(in-situ DRIFT)结果表明,富氧条件下吸附NOx时,TABM6和TSBM6上NOx形成硝酸盐结构,尤其是TABM6上可看到从亚硝酸盐到硝酸盐的转化过程。TZBM6上NOx的吸附与BaMnO_3类似,都生成亚硝酸盐。
800℃高温焙烧之后,TABM6和TSBM6催化剂发生烧结,活性组分Ba与载体反应生成了BaAl_2O_4和Ba_2TiSi_2O_8。TZBM6催化剂结构未发生明显变化,ZrTiO_4固溶体和BaMnO_3钙钛矿晶粒有所增长。总体上看,TZBM6的抗热稳定性最佳。
硫化后(SO_2: 200ppm),催化剂的NSC值相对于新鲜样品TABM6、TSBM6、TZBM6分别下降了52.6%、19.7%和47.6%。硫化催化剂TABM6的NOx储存量仍然最大,其次为TSBM6,TZBM6样品的再储存能力最小。TSBM6具有最好的抗硫能力,与TiO_2-SiO_2载体具有最大的酸强度有关。
采用分步浸渍法制备了Pt-Mn/Ba/TiO_2-ZrO_2催化剂。Mn负载量增加时,催化剂表面形成Mn_2O_3晶体,对催化剂氧化性能和NOx储存能力影响不大。表面高度分散的Mn物种,800℃焙烧后,一部分进入载体晶格中形成新的固溶体Mn_(0.33)Ti_(0.33)Zr_(0.33)O_(1.67)。Pt物种的分散性和存在状态对催化剂的NOx储存性能有重要影响。高温焙烧,促进了PtO_2的分散,伴随部分氧化物物种的分解形成金属态的Pt,增强了Pt和Mn物种之间的相互作用。800℃焙烧样品Pt-C1-800中,Pt的分散性最好,对NO氧化能力最好,NSC值最大。
The NOx storage and reduction (NSR) technology will be the most promising way to reduce the NOx emission from lean-burn engines. In this work, we have designed a series of NSR catalysts based on Ba-Mn, including BaMnO_3 perovskite oxides and Ba/Mn/TiO_2-X (X=Al_2O_3/SiO_2/ZrO_2) supported catalysts. Their structures and properties were characterized by the techniques of XRD, TG-MS, BET, H_2-TPR and NOx-TPD.Their NOx storage capacity, thermal stability and sulfur resistance were also investigated. The mechanism of NOx adsorbing species were discussed by in-situ DRIFT.
BaMnO_3 perovskite oxides were prepared by citric acid complexation method. At 300oC, the rate of nitrite to nitrate transformation is higher than that of nitrate and nitrite decomposition. As a result, the BaMnO_3 perovskite oxide exhibits the highest NOx uptake at 300oC. No difference in the structure and NSR activity is found in the case of partial substitution of Mn by Cu/Mg. However, Fe substitution in B site leads to generation of oxygen vacancies. The highest NOx storage capacity is achieved on BaMn_(0.6)Fe_(0.4)O_3. Adsorption and storage of NOx on BaMnO_3 proceeds in three steps: (1) the formation of nitrites at low temperature (≤200oC); (2) its transformation to nitrates at temperature higher than 200oC, but lower than 300oC; (3) the formation of nitrates at high temperature (≥300oC). On the Fe-substitution catalysts, the NOx adsorption and storage processes are similar to the BaMnO_3 catalyst.
The TABM6、TSBM6 and TZBM6 catalysts were prepared by spreading Ba-Mn precursors as a thin layer on the TiO_2-Al_2O_3, TiO_2-SiO_2 and TiO_2- ZrO_2 supports calcined at 600 oC. The NOx storage capacity depends strongly on the relative abundance of BaCO_3 phases. Compared with the TSBM6 catalyst, more active BaCO_3 phases are detected in the TABM6 catalyst due to less acidity, which results in a higher NOx storage capacity. Although the BaCO_3 concentration was relatively lower, the TZBM6 catalyst still shows a high NSC of 105.7μmol/g due to the presence of a large amount of BaMnO_3 perovskite phase. During adsorption of NOx under lean burn condition, surface nitrates are formed on the TABM6 and TSBM6 catalysts, while surface nitrites are the dominant species on the TZBM6 catalyst. The transformation of nitrites to nitrates is observed on the TABM6 catalyst by in-situ DRIFT.
Thermal aging at 800oC leads to the conversion of dispersed BaCO_3 in the TABM6 and TSBM6 catalysts to crystalline BaAl_2O_4 and Ba_2TiSi_2O_8 respectively. The TZBM6 catalyst is quite stable against thermal treatment. NOx storage capacities of TABM6、TSBM6 and TZBM6 catalysts decline by the percentages of 52.6%,19.7% and 47.6% respectively, after treated in 200ppm SO_2 atmosphere for 30 min. The order of NSC of sulfated catalysts is TABM6>TSBM6>TZBM6. The TSBM6 catalyst displays the best sulfur resistance ability due to the highest acidity of TiO_2-SiO_2 support.
The Pt-Mn/Ba/TiO_2-ZrO_2 catalysts were prepared by a successive incipient wetness impregnation using TiO_2-ZrO_2 as support. Higher Mn loading resulted in aggregation of Mn_2O_3 crystallites on TiO_2-ZrO_2 support. After calcination at 800oC, a part of Mn species diffuses into the lattice of the support and forms a new phase Mn_(0.33)Ti_(0.33)Zr_(0.33)O_(1.67). The dispersion and phase of Pt species is the key factor for the NOx storage capacity of the catalyst. As the calcinations increases, the dispersion of Pt species is higher, while some PtO_2 species decompose to Pt metal phase. The results of EXAFS and NSC measurements showed that the maximum NO conversion and NOx storage capacity were achieved on the sample Pt-C1-800 due to the highest dispersion of Pt species.
引文
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