CuNiTi类水滑石衍生物富氧丙烯选择性催化还原NO的研究
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摘要
随着机动车保有量的快速增加,其尾气造成的氮氧化物(NOχ)污染引起了人们的高度重视,尤其是传统三效催化剂在节约能源的贫燃发动机尾气环境中的失效问题,使富氧条件下NOχ的有效降解成为了机动车尾气脱硝领域的研究热点和重点。目前,利用尾气组分作为还原剂,采用选择性催化还原(SCR)技术对Noχ进行降解被认为是消除尾气中NOχ的有效方法。因此,开发高效的富氧SCR脱硝催化剂具有重要的理论和现实意义。
已有的研究结果表明,金属氧化物催化剂具有一定的SCR脱硝活性,且价格低廉,具有很大的应用潜力。此外,水滑石类衍生物因其高比表面积、高分散性和高稳定性的特点被用作催化剂及催化剂载体。为了获得更高的催化活性,本文对水滑石的合成方法进行了优化,采用尿素均匀共沉淀法制备了CuTi、NiTi及CuNiTi类水滑石衍生物催化剂,考察其富氧C3H6-SCR脱硝活性。通过一系列现代仪器分析手段表征催化剂的结构、探讨反应机理,研究催化剂结构与功能之间的关系,取得以下主要研究成果：
(1)共沉淀法、水热法、尿素均匀共沉淀法以及尿素水热复合法均能成功地合成水滑石。共沉淀法合成的催化剂表现为MgO和Al203的混合氧化物结构,以尿素为沉淀剂的其他三种方法合成的催化剂主要是尖晶石结构。尖晶石结构的催化剂具有更高含量的Lewis酸,其含量与催化活性成正比。尿素均匀共沉淀法合成的催化剂具有最高的Lewis酸含量,表现出最高的催化活性,是最有利于提高脱硝效率的合成方法。
(2)采用尿素均匀共沉淀法制备了CuTi类水滑石衍生物催化剂(Cu-Ti摩尔比为2、3、4和5),Cu3Ti1催化剂的催化活性最高,在270℃时,NO的转化率达到74%。随着Cu含量增加,CuTi类水滑石衍生物催化剂由钛酸铜转变为氧化铜。六方晶系的钛酸铜晶格结构中的正电荷密度远远高于单斜晶系的氧化铜,导致钛酸铜的Lewis酸含量高于氧化铜,进而表现出更高的催化活性。Cu物种在CuTi类水滑石衍生物催化剂中分别以表面分散Cu和体相Cu两种形式存在,表面分散Cu2+是反应的活性物种,体相Cu是硝酸盐的吸附位。硝酸盐、乙酸盐和甲酸盐是CuTi类水滑石衍生物催化剂富氧C3H6选择性催化还原NO反应的活性中间体。
(3)热解温度改变了CuTi类水滑石衍生物催化剂中体相Cu的结构。CuTi类水滑石在热解过程中表现出两个主要的相变过程：层问阴离子析出生成钛酸铜和钛酸铜分解生成氧化铜和金红石。450℃是类水滑石结构向钛酸铜结构转化最快的温度,该温度热解得到的催化剂以钛酸铜为主,且具有最高的比表面积、表面Lewis酸含量、表面分散Cu2+含量以及催化活性。因此,从提高催化活性的角度认为,450℃是CuTi类水滑石衍生物催化剂最佳的热解温度。
(4)采用尿素均匀共沉淀法制备了NiTi类水滑石衍生物催化剂(Ni-Ti摩尔比为0.5,1,2,和3),Ni1Til催化剂的催化活性最高,在430℃时,NO转化率和N2收率分别为77%和66%。NiTi类水滑石衍生物催化剂具有较高的比表面积,结构以锐钛矿为主。Ni在催化剂中以正二价形式存在,当Ni2+与锐钛矿之间形成了强的相互作用时,能够提高表面氧的含量且有效地控制了C3H6的活化,因而有利于富氧C3H6-SCR反应活性的提高。与CuTi类水滑石衍生物催化剂相比,NiTi类水滑石衍生物催化剂具有更高的C3H6吸附以及氧化能力。
(5)与CuTi类水滑石衍生物催化剂相比,Ni组分的引入提高了催化活性并且拓宽了反应温度窗口,这种催化活性的提高主要源于Ni组分良好的C3H6活化能力。Cu1Ni2Ti1催化剂的催化活性最高,在280℃时,NO转化率和N2收率分别为90%和84%。在富氧条件下,NO和C3H6分别被氧化生成硝酸盐和有机酸(乙酸盐和甲酸盐),硝酸盐和有机酸发生反应,最终生成无毒的N2,H2O和CO2。硝酸盐、乙酸盐和甲酸盐均是CuNiTi类水滑石衍生物催化剂富氧C3H6-SCR反应的重要中间体。Cu-Ni的同时引入提高了中间体的生成率,从而有利于催化活性的提高。
With the rapid increasing number of automobiles, growing attention is paid to pollution resulting from nitrogen oxides (NOx). Traditional three-way catalyst is no longer activitied in the lean-burn engines which are used to reduce energy consumption. Such issue has been viewed as a frotier scientific problem in the DeNOx field. Recently, selective catalytic reduction (SCR) is used as a potential method to remove NOx from these lean-burn gasoline engines using exhaust gas composition. Therefore the development of catalysts that can effecticely remove NOx under lean-burn conditions is of great importance in theoretical researches and practical applications.
Previous researches demonstrated that metal oxides catalysts possessed great promising applications due to its activities for SCR and competitive cost. In addition, hydrotalcite-derived material is considered as a promising precursor for obtaining catalyst and catalyst supporting because of its small crystallite, high surface area and high stability. To reach high catalytic preformence. in this dissertation, the synthesis method for hydrotalcite is optimized, and the CuTi. NiTi. CuNiTi hydrotalcite-derived catalyst are prepared by urea homogeneous precipitation and employed for C3H6-SCR under lean-burn conditions. Moreover, a series of modern instruments are used to characterize the structure of the catalysts, and the relationship between catalyst structures and catalytic performance is explored. The detailed works are as follows:
(1) Hydortalcites have been successfully prepared by four different methods including three strategies with urea as the base retardant, i. e., homogeneous precipitation, hydrothermal and homogeneous precipitation combined with hydrothermal. and the conventional coprecipitation. The hydortalcite-derived catalyst prepared by coprecipitation shows MgO and Al2O3mixed oxide structure, while the other three catalysts display spinel structure. The amount of Lewis acid sites on spinel is larger than that on mixed oxide, which is proportional to the catalytic activity of catalysts. The most active hydortalcite-derived catalyst with the highest amount of Lewis is synthesized by the homogeneous precipitation, which is the optimal strategy for the producing hydortalcite-derived catalyst to improving the catalytic performance for SCR.
(2) CuTi hydortalcite-derived catalysts [CuxTi1(x=2.3.4,5)] are synthesized via urea homogeneous precipitation. Among them, the Cu3Ti1catalyst presents the highest activity at 270℃and the NO conversion achieves74%. With the elevation of Cu content.the crystal structure of the catalysts varys from copper titanate to copper oxide. Compared with the monoclinic copper oxide.the hexagonal copper titanate shows higher catalytic performance due to the larger amount of Lewis acid sites and positive charge density. Cu species in the CuTi hydortalcite-derived catalysts can be primarily grouped into two categories:surface and bulk species. The surface Cu2+species is the active sites. while the bulk Cu could provide the adsorption sites for nitrates. The nitrates. acetate and formate are key intermediates for the C3H6-SCR over series CuTi hydortalcite-derived catalysts under lean-burn conditions.
(3) The various thermal decomposition temperatures change the bulk Cu structure of the CuTi hydortalcite-derived catalyst. Two phase transformations can be obtained with the increasing of the thermal decomposition temperature:one is that CuTi hydortalcite-like precursor loses the interlayer anions to produce copper titanate. and the other is that copper titanate transforms to copper oxide and rutile. The hydrotalcite-like precursor can be transformed to copper titanium oxide calcining at450℃rapidly, and the catalyst calcined at450℃displays major copper titanium crystal structure, as well as the highest surface area. amount of Lewis acid sites, amount of surface Cu2+species and catalytic activity. From the perspective of improvement for catalytic performance.450℃is the optimal thermal decomposition temperature for CuTi hydortalcite-derived catalyst.
(4) NiTi hydortalcite-derived catalysts [NixTi1(x=0.5.1.2.3)] are synthesized via urea homogeneous precipitation. Among them, the Ni1Ti1catalyst presents the highest activity at430℃and the NO conversion and N2yeild achieve77%and66%. respectively. The catalysts show high surface areas and anatase structure.Ni in these catalysts demonstrates Ni2+. which can interact with anatase to increase the content of surface oxygen and effectively control the C3H6activation. Thus, the catalytic performance can be improved. Compared with CuTi hydortalcite-derived catalysts. NiTi hydortalcite-derived catalysts possess higher capability of adsorption and oxidation for C3H6.
(5) Comperaed with the CuTi hydortalcite-derived catalysts, addition of Ni component leads to an increased catalytic activity, as well as a widened temperature widonw. Such improvement of catalytic performance can be attributed to the high activation for C3H6of Ni component. The Cu1Ni2Ti1catalyst presented the highest activity among the CuNiTi hydortalcite-derived catalysts, and the NO conversion and N2yeild achieve90%and84%. respectively. Under lean-burn conditions, the reaction started with the formation of the adsorbed nitrates via NO oxidation by O2and the products from the partial oxidation of C3H6. i.e., acetate and formate. Subsequently, nitrates reacted with acetate and formate to yield N2. CO2and H2O. The catalytic performance over CuNiTi hydortalcite-derived catalysts can be improved by introduction of Cu-Ni,which can increase the production rate of intermediate.
已有的研究结果表明,金属氧化物催化剂具有一定的SCR脱硝活性,且价格低廉,具有很大的应用潜力。此外,水滑石类衍生物因其高比表面积、高分散性和高稳定性的特点被用作催化剂及催化剂载体。为了获得更高的催化活性,本文对水滑石的合成方法进行了优化,采用尿素均匀共沉淀法制备了CuTi、NiTi及CuNiTi类水滑石衍生物催化剂,考察其富氧C3H6-SCR脱硝活性。通过一系列现代仪器分析手段表征催化剂的结构、探讨反应机理,研究催化剂结构与功能之间的关系,取得以下主要研究成果：
(1)共沉淀法、水热法、尿素均匀共沉淀法以及尿素水热复合法均能成功地合成水滑石。共沉淀法合成的催化剂表现为MgO和Al203的混合氧化物结构,以尿素为沉淀剂的其他三种方法合成的催化剂主要是尖晶石结构。尖晶石结构的催化剂具有更高含量的Lewis酸,其含量与催化活性成正比。尿素均匀共沉淀法合成的催化剂具有最高的Lewis酸含量,表现出最高的催化活性,是最有利于提高脱硝效率的合成方法。
(2)采用尿素均匀共沉淀法制备了CuTi类水滑石衍生物催化剂(Cu-Ti摩尔比为2、3、4和5),Cu3Ti1催化剂的催化活性最高,在270℃时,NO的转化率达到74%。随着Cu含量增加,CuTi类水滑石衍生物催化剂由钛酸铜转变为氧化铜。六方晶系的钛酸铜晶格结构中的正电荷密度远远高于单斜晶系的氧化铜,导致钛酸铜的Lewis酸含量高于氧化铜,进而表现出更高的催化活性。Cu物种在CuTi类水滑石衍生物催化剂中分别以表面分散Cu和体相Cu两种形式存在,表面分散Cu2+是反应的活性物种,体相Cu是硝酸盐的吸附位。硝酸盐、乙酸盐和甲酸盐是CuTi类水滑石衍生物催化剂富氧C3H6选择性催化还原NO反应的活性中间体。
(3)热解温度改变了CuTi类水滑石衍生物催化剂中体相Cu的结构。CuTi类水滑石在热解过程中表现出两个主要的相变过程：层问阴离子析出生成钛酸铜和钛酸铜分解生成氧化铜和金红石。450℃是类水滑石结构向钛酸铜结构转化最快的温度,该温度热解得到的催化剂以钛酸铜为主,且具有最高的比表面积、表面Lewis酸含量、表面分散Cu2+含量以及催化活性。因此,从提高催化活性的角度认为,450℃是CuTi类水滑石衍生物催化剂最佳的热解温度。
(4)采用尿素均匀共沉淀法制备了NiTi类水滑石衍生物催化剂(Ni-Ti摩尔比为0.5,1,2,和3),Ni1Til催化剂的催化活性最高,在430℃时,NO转化率和N2收率分别为77%和66%。NiTi类水滑石衍生物催化剂具有较高的比表面积,结构以锐钛矿为主。Ni在催化剂中以正二价形式存在,当Ni2+与锐钛矿之间形成了强的相互作用时,能够提高表面氧的含量且有效地控制了C3H6的活化,因而有利于富氧C3H6-SCR反应活性的提高。与CuTi类水滑石衍生物催化剂相比,NiTi类水滑石衍生物催化剂具有更高的C3H6吸附以及氧化能力。
(5)与CuTi类水滑石衍生物催化剂相比,Ni组分的引入提高了催化活性并且拓宽了反应温度窗口,这种催化活性的提高主要源于Ni组分良好的C3H6活化能力。Cu1Ni2Ti1催化剂的催化活性最高,在280℃时,NO转化率和N2收率分别为90%和84%。在富氧条件下,NO和C3H6分别被氧化生成硝酸盐和有机酸(乙酸盐和甲酸盐),硝酸盐和有机酸发生反应,最终生成无毒的N2,H2O和CO2。硝酸盐、乙酸盐和甲酸盐均是CuNiTi类水滑石衍生物催化剂富氧C3H6-SCR反应的重要中间体。Cu-Ni的同时引入提高了中间体的生成率,从而有利于催化活性的提高。
With the rapid increasing number of automobiles, growing attention is paid to pollution resulting from nitrogen oxides (NOx). Traditional three-way catalyst is no longer activitied in the lean-burn engines which are used to reduce energy consumption. Such issue has been viewed as a frotier scientific problem in the DeNOx field. Recently, selective catalytic reduction (SCR) is used as a potential method to remove NOx from these lean-burn gasoline engines using exhaust gas composition. Therefore the development of catalysts that can effecticely remove NOx under lean-burn conditions is of great importance in theoretical researches and practical applications.
Previous researches demonstrated that metal oxides catalysts possessed great promising applications due to its activities for SCR and competitive cost. In addition, hydrotalcite-derived material is considered as a promising precursor for obtaining catalyst and catalyst supporting because of its small crystallite, high surface area and high stability. To reach high catalytic preformence. in this dissertation, the synthesis method for hydrotalcite is optimized, and the CuTi. NiTi. CuNiTi hydrotalcite-derived catalyst are prepared by urea homogeneous precipitation and employed for C3H6-SCR under lean-burn conditions. Moreover, a series of modern instruments are used to characterize the structure of the catalysts, and the relationship between catalyst structures and catalytic performance is explored. The detailed works are as follows:
(1) Hydortalcites have been successfully prepared by four different methods including three strategies with urea as the base retardant, i. e., homogeneous precipitation, hydrothermal and homogeneous precipitation combined with hydrothermal. and the conventional coprecipitation. The hydortalcite-derived catalyst prepared by coprecipitation shows MgO and Al2O3mixed oxide structure, while the other three catalysts display spinel structure. The amount of Lewis acid sites on spinel is larger than that on mixed oxide, which is proportional to the catalytic activity of catalysts. The most active hydortalcite-derived catalyst with the highest amount of Lewis is synthesized by the homogeneous precipitation, which is the optimal strategy for the producing hydortalcite-derived catalyst to improving the catalytic performance for SCR.
(2) CuTi hydortalcite-derived catalysts [CuxTi1(x=2.3.4,5)] are synthesized via urea homogeneous precipitation. Among them, the Cu3Ti1catalyst presents the highest activity at 270℃and the NO conversion achieves74%. With the elevation of Cu content.the crystal structure of the catalysts varys from copper titanate to copper oxide. Compared with the monoclinic copper oxide.the hexagonal copper titanate shows higher catalytic performance due to the larger amount of Lewis acid sites and positive charge density. Cu species in the CuTi hydortalcite-derived catalysts can be primarily grouped into two categories:surface and bulk species. The surface Cu2+species is the active sites. while the bulk Cu could provide the adsorption sites for nitrates. The nitrates. acetate and formate are key intermediates for the C3H6-SCR over series CuTi hydortalcite-derived catalysts under lean-burn conditions.
(3) The various thermal decomposition temperatures change the bulk Cu structure of the CuTi hydortalcite-derived catalyst. Two phase transformations can be obtained with the increasing of the thermal decomposition temperature:one is that CuTi hydortalcite-like precursor loses the interlayer anions to produce copper titanate. and the other is that copper titanate transforms to copper oxide and rutile. The hydrotalcite-like precursor can be transformed to copper titanium oxide calcining at450℃rapidly, and the catalyst calcined at450℃displays major copper titanium crystal structure, as well as the highest surface area. amount of Lewis acid sites, amount of surface Cu2+species and catalytic activity. From the perspective of improvement for catalytic performance.450℃is the optimal thermal decomposition temperature for CuTi hydortalcite-derived catalyst.
(4) NiTi hydortalcite-derived catalysts [NixTi1(x=0.5.1.2.3)] are synthesized via urea homogeneous precipitation. Among them, the Ni1Ti1catalyst presents the highest activity at430℃and the NO conversion and N2yeild achieve77%and66%. respectively. The catalysts show high surface areas and anatase structure.Ni in these catalysts demonstrates Ni2+. which can interact with anatase to increase the content of surface oxygen and effectively control the C3H6activation. Thus, the catalytic performance can be improved. Compared with CuTi hydortalcite-derived catalysts. NiTi hydortalcite-derived catalysts possess higher capability of adsorption and oxidation for C3H6.
(5) Comperaed with the CuTi hydortalcite-derived catalysts, addition of Ni component leads to an increased catalytic activity, as well as a widened temperature widonw. Such improvement of catalytic performance can be attributed to the high activation for C3H6of Ni component. The Cu1Ni2Ti1catalyst presented the highest activity among the CuNiTi hydortalcite-derived catalysts, and the NO conversion and N2yeild achieve90%and84%. respectively. Under lean-burn conditions, the reaction started with the formation of the adsorbed nitrates via NO oxidation by O2and the products from the partial oxidation of C3H6. i.e., acetate and formate. Subsequently, nitrates reacted with acetate and formate to yield N2. CO2and H2O. The catalytic performance over CuNiTi hydortalcite-derived catalysts can be improved by introduction of Cu-Ni,which can increase the production rate of intermediate.
引文
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