CN114904520A - 一种低nh3生成量三效催化剂及其制备方法 - Google Patents
一种低nh3生成量三效催化剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及催化技术应用和与大气污染治理有关的环保领域，特别涉及一种低NH3生成量三效催化剂及其制备方法。该三效催化剂由载体和涂层材料组成；所述涂层材料由贵金属活性组分和催化材料组成；所述贵金属活性组分包括第一贵金属活性组分和第二贵金属活性组分；所述第一贵金属活性组分为包含Ru的组合物；所述第二贵金属活性组分为包含Pt、Pd和Rh的组合物；或为包含Pd和Rh的组合物。通过在涂层材料中添加金属钌或钌的氧化物，提高了TWC的N2选择性，降低了TWC副产物NH3生成量，从源头上降低了NH3生成量，并且部分生成的NH3在Ru催化剂上分解为N2和H2，避免了采用AOC净化TWC生成的副产物NH3，提供了一种新的有效地解决NH3排放超标问题的方案。
Description
技术领域
本发明涉及催化技术应用和与大气污染治理有关的环保领域，特别涉及一种低NH3生成量三效催化剂及其制备方法。
背景技术
采用当量比燃烧的汽车，通常在排气管上加装三效催化剂(Three Way Catalyst，简称TWC)，净化尾气中的碳氢化合物(Hydrocarbon，简称HC)、氮氧化物(NOx)和一氧化碳(CO)。汽车安装尾气净化催化剂的目的是将CO、HC和NOx等三种主要污染物转化为CO2、N2和H2O等对人体无害的物质，同时要避免产生新的有害物质。汽车在不同工况运行时，尾气中污染物浓度、流量、温度和空燃比等波动较大，TWC通常会发生多个主反应和副反应。其中部分主反应和副反应(主反应：CO+H2O→CO2+H2，HC+H2O→CO2+H2；副反应：NO+H2→NH3+H2O，CO+NO+H2→NH3+H2O)会导致TWC上生成新的污染物NH3。NH3是一种无色有刺激性恶臭的气体，对人体的皮肤、眼睛和呼吸器官有一定的伤害。GB17691-2018《重型柴油车污染物排放限值及测量方法(中国第六阶段)》规定汽车尾气排放的NH3不超过10ppm。
文献(Applied Thermal Engineering 130(2018)1363–1372)报道了一款安装TWC的重型天然气发动机(当量比燃烧)NH3排放量，WHTC(World Harmonized TransientCycle，全球统一瞬态测试循环)试验，超过80％的工况，NH3排放量超过100ppm，最高超过450ppm；稳态13工况点试验，13个工况中有11个工况，NH3排放量超过100ppm，最高超过300ppm。文献(Atmospheric Environment 97(2014)43-53)对比验证了7款安装TWC的轻型汽油车(当量比燃烧)，NEDC(New European Driving Cycle，新标欧洲循环测试)试验结果显示，NH3排放量最高108ppm，最低6ppm，不同汽车NH3排放差异较大，主要和汽车排放控制系统及后处理催化剂相关。文献(Science of the Total Environment 616–617(2018)774–784)对比了安装DOC+DPF的柴油车(稀薄燃烧)和安装了TWC的天然气车(当量比燃烧)，不同测试循环时NH3排放量，结果显示，柴油车NH3排放量均低于10mg/km，但天然气车NH3排放量13-24mg/km，当量比燃烧的天然气车NH3排放量显著高于稀薄燃烧的柴油车。以上文献表明，安装TWC的当量比燃烧汽车，NH3排放较高是普遍现象，需要通过安装其它净化NH3的催化剂或通过降低TWC NH3生成量(提高TWC N2选择性)解决安装TWC的当量燃烧汽车NH3排放超标的问题。中国专利(CN109225316 A)介绍了一种TWC+AOC(Ammonia Oxidation Catalyst，氨氧化催化剂，简称AOC)，通过AOC净化TWC生成的副产物NH3。TWC+AOC实现高效净化CO、HC和NOx，同时可以将NH3排放降至10ppm以下。该技术路线在国内国六重型天然气车上广泛应用。通过AOC可以解决安装TWC的当量燃烧汽车NH3排放超标问题，但增加AOC后，发动机后处理系统的标定难度增加、尾气净化催化转化器体积增大和成本有一定幅度提高。
发明内容
本发明的目的在于：针对现有技术存在的通过AOC可以解决安装TWC的当量燃烧汽车NH3排放超标问题，但增加AOC后，发动机后处理系统的标定难度增加、尾气净化催化转化器体积增大和成本有一定幅度提高的问题，提供一种低NH3生成量三效催化剂。该催化剂，通过在TWC中加入钌金属或者钌氧化物，提高TWC的N2选择性，降低NH3生成量。该方案是新的更有效地解决NH3排放超标的技术方案。
为了实现上述目的，本发明采用的技术方案为：
一种低NH3生成量三效催化剂，由载体和涂层材料组成；
所述涂层材料由贵金属活性组分和催化材料组成；
所述贵金属活性组分包括第一贵金属活性组分和第二贵金属活性组分；
所述第一贵金属活性组分为包含Ru的组合物；
所述第二贵金属活性组分为包含Pt、Pd和Rh的组合物；或所述第二贵金属活性组分为包含Pd和Rh的组合物。
本发明低NH3生成量三效催化剂，通过在涂层材料中添加金属钌(Ru)和/或者钌的氧化物，提高了TWC的N2选择性，抑制了TWC副产物NH3生成量。从源头上降低了NH3生成量，并且部分生成的NH3在Ru催化剂上分解为N2和H2，促使NH3生成量大幅度降低，降低了催化转化器体积和成本，更有效地解决NH3排放超标的问题。其中的铂、钯和铑为常用的三效催化剂的贵金属。
作为本发明的优选方案，以单质计，Ru的含量为1～100g/ft3。
当钌的含量在1～100g/ft3范围内时，NH3生成量均低于10ppm，NH3生成量很低，表现出高N2选择性。
作为本发明的优选方案，以单质计，Ru的含量为5～40g/ft3。
随着钌的含量的增加，NH3生成量逐步降低，当钌的含量过高时，生产成本增加。在上述范围内时，在表现出高N2选择性的同时，降低了成本。
当钌的含量不为0时，均能起到降低NH3生成量的作用。随着钌含量的增加，NH3生成量越低。钌的含量取值为0.05、0.1、0.2、0.3、0.5、0.8、1、2、2.5、3、5、10、20、25、30、40、50等数值，单位为g/ft3。
作为本发明的优选方案，所述Ru的组合物中包含金属钌和/或钌的氧化物。
第二贵金属活性组分的含量、比例，涂层上载量等，为商用TWC的常规用量。
作为本发明的优选方案，所述催化材料包含储氧材料和氧化铝材料。
作为本发明的优选方案，所述储氧材料包含CeO2，CeO2-ZrO2，CeO2-ZrO2-Y2O3，CeO2-ZrO2-La2O3，CeO2-ZrO2-La2O3-Y2O3CeO2-ZrO2-La2O3-Pr2O3，CeO2-ZrO2-La2O3-Nd2O3的至少一种。
作为本发明的优选方案，所述氧化铝材料包含纯氧化铝；La、Ce等改性氧化铝中的至少一种。
作为本发明的优选方案，所述载体为陶瓷载体或者金属载体。所述陶瓷载体为堇青石陶瓷载体。
本发明还提供一种如上所述的低NH3生成量三效催化剂的制备方法，包括如下步骤，
S1，涂层材料的制备；
将第一贵金属活性组分的盐溶液和第二贵金属活性组分的盐溶液负载到催化材料上；经干燥焙烧后，得到涂层材料；
S2，涂层材料浆料制备；
将涂层材料、水、粘结剂混合，球磨制浆，得到涂层材料浆料；
S3，制备三效催化剂；
将涂层材料浆料涂覆与载体上，经干燥焙烧后，得到三效催化剂。
本发明的制备方法是将Ru和其它贵金属活性组分一起负载到储氧材料和氧化铝上，然后干燥焙烧固化，最后制浆涂覆至堇青石陶瓷载体或者金属载体上。
综上所述，由于采用了上述技术方案，本发明的有益效果是：
1、本发明的低NH3生成量三效催化剂，通过添加金属钌，其中Ru的含量为1～100g/ft3，更优选为Ru的含量为5～40g/ft3，提升了TWC的N2选择性，与现有的三效催化器相比，在能够实现高效净化当量比燃烧汽车尾气中CO/HC/NOx的同时，NH3生成量也大幅降低，避免了采用AOC等方式去除生成的NH3，降低了催化转化器的体积。
2、本发明采用的三效催化剂的制备方法，避免了使用多种催化剂混合制备的方式，工艺更为简便，该制备方法为传统的汽车尾气净化催化剂制备工艺，大大降低了生产成本，更易工艺放大和产业化。
附图说明
图1是本发明对比例和实施例制备的催化剂对CO转化效率曲线。图1中，C1-1和C2-1是对比例1和对比例2催化剂，C3-1、C4-1和C5-1是实施例1、实施例2和实施例3催化剂。
图2是本发明对比例和实施例制备的催化剂对HC(CH4)转化效率曲线。图2中，C1-1和C2-1是对比例1和实施例2催化剂，C3-1、C4-1和C5-1是实施例1、实施例2和实施例3催化剂。
图3是本发明对比例和实施例制备的催化剂对NOx(NO)转化效率曲线。图3中，C1-1和C2-1是对比例1和实施例2催化剂，C3-1、C4-1和C5-1是实施例1、实施例2和实施例3催化剂。
图4是本发明对比例和实施例制备的催化剂不同LambdaNH3生成量。图4中，C1-1和C2-1是对比例1和实施例2催化剂，C3-1、C4-1和C5-1是实施例1、实施例2和实施例3催化剂。
具体实施方式
下面结合附图，对本发明作详细的说明。
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。
对比例1
S1，涂层材料的制备；
将Pd(NO3)2和Rh(NO3)2溶液，以浸渍法负载到Al2O3和CeO2-ZrO2材料上，80℃干燥6h，500℃焙烧2h，得到涂层材料，记为M1。
S2，涂层材料浆料制备；
将M1和水、粘结剂混合，得到涂层材料浆料，记为N1。
S3，制备三效催化剂；
将N1涂覆至堇青石陶瓷载体上，载体尺寸Φ25.4*101.6/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pd、Rh总含量35g/ft3，Pd、Rh比例为9：1。制备好的催化剂记为C1-1。
将N1涂覆至堇青石陶瓷载体上，载体尺寸Φ304.8*152.4/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pd、Rh总含量35g/ft3，Pd、Rh比例为9：1。制备好的催化剂记为C1-2。
对比例2
S1，涂层材料的制备；
将Pt(NO3)2、Pd(NO3)2和Rh(NO3)2溶液，以浸渍法负载到La-Al2O3和CeO2-ZrO2材料上，80℃干燥6h，500℃焙烧2h，得到涂层材料，记为M2。
S2，涂层材料浆料制备；
将M2与水、粘结剂混合，得到涂层材料浆料，记为N2。
S3，制备三效催化剂；
将N2涂覆至堇青石陶瓷载体上，载体尺寸Φ25.4*101.6/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pt、Pd、Rh总含量35g/ft3，Pt、Pd、Rh比例为3：6：1。制备好的催化剂记为C2-1。
将N2涂覆至堇青石陶瓷载体上，载体尺寸Φ304.8*152.4/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pt、Pd、Rh总含量35g/ft3，Pt、Pd、Rh比例为3：6：1。制备好的催化剂记为C2-2。
实施例1
S1，涂层材料的制备；
将Pd(NO3)2、Rh(NO3)2和Ru(NO3)2溶液，以浸渍法负载到Al2O3和CeO2-ZrO2材料上，80℃干燥6h，500℃焙烧2h，得到涂层材料，记为M3。
S2，涂层材料浆料制备；
将M3与水、粘结剂混合，得到涂层材料浆料，记为N3。
S3，制备三效催化剂；
将N3涂覆至堇青石陶瓷载体上，载体尺寸Φ25.4*101.6/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pd、Rh总含量35g/ft3，Pd、Rh比例为9：1，Ru含量为5g/ft3。制备好的催化剂记为C3-1。
将N3涂覆至堇青石陶瓷载体上，载体尺寸Φ304.8*152.4/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pd、Rh总含量35g/ft3，Pd、Rh比例为9：1，Ru含量为5g/ft3。制备好的催化剂记为C3-2。
实施例2
S1，涂层材料的制备；
将Pt(NO3)2、Pd(NO3)2、Rh(NO3)2和Ru(NO3)2溶液，浸渍法负载到La-Al2O3和CeO2-ZrO2材料上，80℃干燥6h，500℃焙烧2h，得到涂层材料，记为M4。
S2，涂层材料浆料制备；
将M4与水、粘结剂混合，得到涂层材料浆料，记为N4。
S3，制备三效催化剂；
将N4涂覆至堇青石陶瓷载体上，载体尺寸Φ25.4*101.6/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pt、Pd、Rh总含量35g/ft3，Pt、Pd、Rh比例为3：6：1，Ru含量为20g/ft3。制备好的催化剂记为C4-1。
将N4涂覆至堇青石陶瓷载体上，载体尺寸Φ304.8*152.4/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pt、Pd、Rh总含量35g/ft3，Pt、Pd、Rh比例为3：6：1，Ru含量为20g/ft3。制备好的催化剂记为C4-2。
实施例3
S1，涂层材料的制备；
将Pt(NO3)2、Pd(NO3)2、Rh(NO3)2和Ru(NO3)2溶液，以浸渍法负载到La-Al2O3和CeO2-ZrO2材料上，80℃干燥6h，500℃焙烧2h，得到涂层材料，记为M5。
S2，涂层材料浆料制备；
将M5与水、粘结剂混合，得到涂层材料浆料，记为N5。
S3，制备三效催化剂；
将N5涂覆至堇青石陶瓷载体上，载体尺寸Φ25.4*101.6/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pt、Pd、Rh总含量35g/ft3，Pt、Pd、Rh比例为3：6：1，Ru含量为40g/ft3。制备好的催化剂记为C5-1。
将N5涂覆至堇青石陶瓷载体上，载体尺寸Φ304.8*152.4/400cpsi。经80℃干燥6h，500℃焙烧2h，涂覆量200g/L，Pt、Pd、Rh总含量35g/ft3，Pt、Pd、Rh比例为3：6：1，Ru含量为40g/ft3。制备好的催化剂记为C5-2。
试验例1
将上述对比例和实施例中得到的催化剂C1-1、C2-1、C3-1、C4-1和C5-1在汽车尾气小样模拟装置上进行活性评价试验，试验条件如下：
模拟气氛：HC(CH4):1000ppm；CO:4000ppm；NO:1000ppm；O2:3500ppm；H2O:10％；CO2:10％；N2为平衡气，空速40000h-1(根据TWC的体积计算的空速)。本发明专利采用结构最稳定的CH4代表汽车尾气中的HC；采用NO代表汽车尾气中的NOx(含NO和NO2等NOx)。催化剂在模拟气氛下，测试300-600℃(汽车尾气主要温度区间)各催化剂对CO、CH4和NO的转化效率。
图1、图2和图3分别是对比例1、对比例2、实施例1、实施例2和实施例3对应的催化剂C1-1、C2-1、C3-1、C4-1和C5-1对CO、CH4和NO三种污染物的转化效率曲线。
图1结果显示，对比例和实施例对CO都有很高的转化效率，性能差异不大。
图2结果显示，对于CH4的起燃温度性能，实施例1较对比例1活性略有降低；实施例2和对比例2活性基本相当；实施例3较实施例2略有提升。以上结果表明，按本发明专利制备工艺和催化材料制备的TWC，金属Ru的添加对PtPdRh型和PdRh型活性影响规律不一致，PdRh型TWC活性略有抑制，PtPdRh型TWC活性几乎没有影响，甚至随着Ru添加量的增加，PtPdRh型TWC的活性还略有提升。
图3结果显示，各实施例和对比例对NO的起燃温度性能影响特点和CH4的规律一致。
试验例2
将对比例和实施例中得到的催化剂C1-1、C2-1、C3-1、C4-1和C5-1在汽车尾气小样模拟装置上验证不同lambdaNH3生成量(N2选择性)，试验条件如下：
模拟气氛：HC(CH4):1000ppm；CO:4000ppm；NO:1000ppm；H2O:10％；CO2:10％；N2为平衡气，空速40000h-1(根据TWC的体积计算的空速)；O2含量根据Lambda值确定。本发明专利采用结构最稳定的CH4代表汽车尾气中的HC；采用NO代表汽车尾气中的NOx(含NO和NO2等NOx)。催化剂在模拟气氛下，测试500℃(此温度为TWC NH3生成量相对较高的温度，同时汽车尾气平均排温也在此附近，选择该温度试验较有代表性)，各对比例和实施例在不同Lambda时NH3生成量。Lambda为当量空燃比。
图4是对比例1、对比例2、实施例1、实施例2和实施例3对应的催化剂C1-1、C2-1、C3-1、C4-1和C5-1在lambda值0.93-1.05时NH3的生成量。图4中五条曲线从上到下依次对应C1-1、C2-1、C3-1、C4-1和C5-1。
图4结果显示，实施例较对比例NH3生成量均大幅降低，说明金属Ru的添加，对催化剂NH3生成量降低效果显著。实施例3相较实施例1和实施例2，在lambda小于1时，NH3生成量又有一定幅度降低，这说明，Ru的添加量对NH3生成量也有影响，在一定添加范围内，随Ru添加量的提高，NH3生成量会小幅降低。
试验例3
将上述对比例和实施例得到的催化剂C1-2、C2-2、C3-2、C4-2和C5-2在重型当量比燃烧的燃气机发动机台架，按照GB17691-2016《重型柴油车污染物排放限值及测量方法(中国第六阶段)》中规定的测试方法，验证了WHTC测试循环工况，对比例和实施对CO、HC(CH4)、NOx和NH3的排放值。
表1是对比例1、对比例2、实施例1、实施例2和实施例3对应的催化剂C1-2、C2-2、C3-2、C4-2和C5-2按WHTC循环工况测试的CO、HC(CH4)、NOx和NH3的排放值。
表1对比例和实施例发动机台架WHTC试验各污染物排放值
表1结果显示，实施例和对比例对CO、HC(CH4)和NOx三种污染物均净化至国六限值的50％以内，表现出非常高的污染物净化效率。对比例1和对比例2NH3生成量是国六限值的3倍以上，排放超标；实施例1、实施例2和实施例3NH3生成量均低于10ppm，NH3生成量很低，表现出高N2选择性。以上结果表明，实施例1、实施例2和实施例3对CO、CH4和NOx高效净化的同时，NH3排放大幅降低，N2选择性大幅提高。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (9)
1.一种三效催化剂，由载体和涂层材料组成；所述涂层材料由贵金属活性组分和催化材料组成；其特征在于，
所述贵金属活性组分包括第一贵金属活性组分和第二贵金属活性组分；
所述第一贵金属活性组分为包含Ru的组合物；
所述第二贵金属活性组分为包含Pt、Pd和Rh的组合物；或所述第二贵金属活性组分为包含Pd和Rh的组合物。
2.根据权利要求1所述的三效催化剂，其特征在于，以单质计，Ru的含量为1～100g/ft3。
3.根据权利要求2所述的三效催化剂，其特征在于，以单质计，Ru的含量为5～40g/ft3。
4.根据权利要求1所述的三效催化剂，其特征在于，所述Ru的组合物中包含金属钌和/或钌的氧化物。
5.根据权利要求1所述的三效催化剂，其特征在于，所述催化材料包含储氧材料和氧化铝材料。
6.根据权利要求5所述的三效催化剂，其特征在于，所述储氧材料包含CeO2，CeO2-ZrO2，CeO2-ZrO2-Y2O3，CeO2-ZrO2-La2O3，CeO2-ZrO2-La2O3-Y2O3，CeO2-ZrO2-La2O3-Pr2O3，CeO2-ZrO2-La2O3-Nd2O3的至少一种。
7.根据权利要求5所述的三效催化剂，其特征在于，所述氧化铝材料包含纯氧化铝；La、Ce等改性氧化铝中的至少一种。
8.根据权利要求1所述的三效催化剂，其特征在于，所述载体为陶瓷载体或者金属载体。
9.一种如权利要求1-8任一所述的三效催化剂的制备方法，其特征在于，包括如下步骤，
S1，涂层材料的制备；将第一贵金属活性组分的盐溶液和第二贵金属活性组分的盐溶液负载到催化材料上；经干燥焙烧后，得到涂层材料；
S2，涂层材料浆料制备；将涂层材料、水、粘结剂混合，球磨制浆，得到涂层材料浆料；
S3，制备三效催化剂；将涂层材料浆料涂覆与载体上，经干燥焙烧后，得到三效催化剂。
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| US20020049137A1 (en) * | 2000-07-27 | 2002-04-25 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Composite oxide, process for producing the same, catalyst for purifying exhaust gas, and process for producing the same |
| EP1254712A1 (en) * | 2001-05-05 | 2002-11-06 | OMG AG & Co. KG | A noble metal-containing supported catalyst and a process for its preparation |
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| CN117654567B (zh) * | 2024-01-31 | 2024-05-07 | 中汽研汽车检验中心（天津）有限公司 | 一种Pt-Ru三效催化剂及其制备方法 |
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