CN108554406B - 一种负载合金型碳烟氧化催化剂及其制备方法 - Google Patents
一种负载合金型碳烟氧化催化剂及其制备方法 Download PDFInfo
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 30
- 230000003647 oxidation Effects 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 15
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- 239000003446 ligand Substances 0.000 claims abstract description 9
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
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- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Natural products OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 3
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- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 3
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
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- 229910052684 Cerium Inorganic materials 0.000 claims description 2
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- -1 rare earth modified cerium-zirconium Chemical class 0.000 claims 5
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- RCFVMJKOEJFGTM-UHFFFAOYSA-N cerium zirconium Chemical group [Zr].[Ce] RCFVMJKOEJFGTM-UHFFFAOYSA-N 0.000 abstract description 13
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- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 4
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- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
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- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
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- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
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- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 description 1
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
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Abstract
一种负载合金型碳烟氧化催化剂及其制备方法,涉及大气污染物治理。包括载体与合金型活性组分,载体为铈锆复合氧化物及其轻稀土修饰体系,合金型活性组分为均质型钯银合金,合金型活性组分按质量百分比的组成为钯1%~20%,银80%~99%,总金属负载量为4%~15%。将轻稀土修饰型CeZrOx铈锆复合氧化物载体在有机酸水溶液中预浸渍后干燥,将干燥后的粉体在阳离子型钯源的水溶液中饱和浸渍,再次干燥得干燥粉体,再煅烧,冷却后的粉体浸入含有多齿配体的银离子水溶液,在搅拌下蒸干溶液,经干燥后再次煅烧;煅烧后粉体转移至管式炉中,在氢气气氛中还原;在含有水蒸汽空气气氛中水热老化处理,即得。
Description
技术领域
本发明涉及大气污染物治理,尤其是涉及一种负载合金型碳烟氧化催化剂及其制备方法。
背景技术
柴油机尾气排放的颗粒物指标日趋严格,国五重卡排放标准中30mg/kw的颗粒物(PM)低限将在国六标准中进一步下探至10mg/kw以内,轻型车的PM指标也将下降30%以上,由于受到排气再循环(EGR),选择催化还原(SCR)以及氨捕集(ASC)等还原性净化工段的限制,单纯依赖催化氧化操作(DOC)来消除还原性颗粒物的设计受到严重制约,这使得颗粒物捕集器(DPF)的安装成为柴油机颗粒物排放达标的唯一选择。颗粒捕集器是利用尺寸效应将在尾气中的颗粒物进行滤除,在使用中颗粒物不断在多孔性器壁上沉积,当累积到一定程度后,将形成附加气阻影响柴油机性能,因为碳基颗粒物系柴油机尾气颗粒排放的主要成分,所以在应用中可以通过氧化再生及清灰操作来维持颗粒捕集器正常工作。
由于碳烟颗粒的氧化温度超过600℃,而柴油机的一般排气温度仅为200~500℃,所以需要借助额外的能量才能提供所需反应温度,而借助催化剂在较低温度下促进碳烟颗粒在较低温度下实现氧化消除,则兼具可靠且节能的特点,已经成为近年来DPF设计的主要改进方向。碳烟颗粒燃烧催化剂可大致分为两类:一类是负载金属型催化剂(中国专利CN102240544A,CN102794175A,CN2013013990,CN201610069491),另一类为过渡金属复合氧化物型催化剂(中国专利CN101683616A,CN10879445A,CN101733111A,CN101623639A,CN1721066A,CN101822979A,CN101811052A,CN102658122A,CN101024182A)。负载金属型碳烟燃烧催化剂凭借其对尾气组成窗口较宽的适应性,更加适应目前多工况及多工段串联的尾气净化方案。
负载型贵金属体系的应用主要受制于贵金属组分成本偏高的短板,如果单纯通过降低负载量来摊低成本,则将导致催化剂疏松接触活性急剧下降的问题;负载银体系能够在维持较低金属成本的前提下,且通过增大负载量可有效提升催化剂的疏松接触活性,因而采用负载银体系进行的碳烟燃烧催化剂设计也陆续走进应用视野(如上所引CN2013013990,CN201610069491)。负载型银催化体系在很好地履行碳烟低温起燃活性的同时,须面临高活性的金属分散系与供氧载体之间发生强相互作用所导致氧化失活的考验,当其作用程度随高温或水热老化作用逐渐加深之后,其金属中心对分子氧的活化能力也将随之下降,造成失活,由此可见,如何在保障金属中心对分子氧活化效率的前提下,抑制其被供氧性载体所氧化以失活,是制作高稳定性负载金属型碳烟燃烧催化剂的关键所在。
发明内容
本发明的目的在于提供一种负载合金型碳烟氧化催化剂及其制备方法。
所述负载合金型碳烟氧化催化剂包括载体与合金型活性组分,所述载体为铈锆复合氧化物及其轻稀土修饰体系,所述合金型活性组分为均质型钯银合金,合金型活性组分按质量百分比的组成为钯1%~20%,银80%~99%,总金属负载量为4%~15%。
所述负载合金型碳烟氧化催化剂的组成通式为r%-PdxAg1-x/LnyZrzCe3O8-q,其中Ln为轻稀土元素La,Pr,Nd,Sm,Eu,Gd,Tb等中的至少一种,式中r%为金属组分负载质量百分比,下标x,y,z为所示组分的摩尔比例系数,x为0.01~0.2,y+z<1,氧的摩尔比例系数记为8-q,q为不定值,随催化反应进行而循环波动。
所述负载合金型碳烟氧化催化剂的合成方法,包括以下步骤:
1)将轻稀土修饰型CeZrOx铈锆复合氧化物载体在有机酸水溶液中预浸渍后,干燥,将干燥后的粉体在阳离子型钯源的水溶液中进行饱和浸渍,随后再次干燥,得干燥粉体;
在步骤1)中,所述轻稀土修饰型CeZrOx铈锆复合氧化物载体可采用固相混合法或共沉淀法制备的储氧材料,铈元素占金属原子比例的50%以上,其余元素组成不做特殊限制;所述有机酸可采用短链脂肪酸,所述短链脂肪酸可选自甲酸、乙酸、丙酸、马来酸、柠檬酸等中的一种,所述有机酸水溶液pH值可为1~2;所述干燥可在复合氧化物粉体倾入有机酸溶液后,在搅拌下进行抽空以排出内孔中气泡,随之过滤并在110℃干燥;所述阳离子型钯源可为硝酸氨钯或氨水配位处理的硝酸钯及乙酸钯等钯与配体形成带有正电荷络离子的水溶性化合物;所述饱和浸渍可采用初始润湿法以活性组分的最小溶液量完成对载体粉末的润湿;所述再次干燥的温度可为110~220℃。
2)将步骤1)所得干燥粉体在空气气氛中煅烧,冷却后的粉体浸入含有多齿配体的银离子水溶液,在搅拌下逐渐蒸干溶液,经干燥后再次在空气气氛中煅烧;
在步骤2)中,所述干燥粉体在空气气氛中煅烧可于450~600℃煅烧30~200min;所述含有多齿配体的银离子水溶液,是指在硝酸银水溶液中加入柠檬酸、苹果酸、乙二胺四乙酸、马来酸、富马酸等有机酸鳌合配体中的一种,并在络合反应完成后,以NaOH调节溶液pH为1~4;所述在搅拌下逐渐蒸干溶液,是指在通过蒸发除去大部分溶剂后,在搅拌作用下继续减压蒸馏至接近干燥;所述再次在空气气氛中煅烧可于450~600℃煅烧30~200min。
3)煅烧后粉体转移至管式炉中,在氢气气氛中还原;
在步骤3)中,所述还原的条件可为于30~150℃下还原15~60min。
4)在含有水蒸汽空气气氛中水热老化处理,即得到水热稳定化的负载合金型碳烟氧化催化剂。
在步骤4)中,所述在含有水蒸汽空气气氛中水热老化处理,可在含有水蒸汽分压0.1atm的空气气氛中于850℃水热老化处理300~600min。
降低碳烟颗粒燃烧温度的负载型银催化剂的活性评价选用热重分析仪连续监测记录在一定气氛和程序升温过程中碳烟颗粒燃烧形成气相产物后的质量变化情况,催化剂的催化氧化能力用碳烟颗粒的特征燃烧温度来表示,在催化剂作用下,碳烟颗粒的燃烧温度降低越多,则该催化剂的催化活性越好。本发明选择碳烟颗粒的起燃温度(T10)、燃烧速率最大时对应的温度(T50)和燃尽温度(T90)作为催化剂活性评价标准,它们分别表示碳烟燃烧完成10%,50%和90%对应的温度点。
本发明通过表面自催化还原的方式,对起催化氧化作用的金属中心进行合金化改造,使其在金属/载体界面上发生的强相互作用被遏制,以保持分子氧活化中心的金属态,防止其氧化失活,从而保障碳烟燃烧的催化循环中活性氧的供应,维持负载体系整体的催化效率,以获得高稳定性负载金属型碳烟燃烧催化剂。
本发明基于钯银合金对分子氧良好的活化性能,并利用钯银合金的稳定性抑制金属氧化物载体对金属活性相发生界面强相互作用而造成的失活,在所形成的整体催化剂中,在保障合金相活性中心抗氧化稳定性的基础上,通过水热处理消除载体上的活性氧的传质障碍,达到碳烟催化氧化反应抗水热失活的效果。经上线评价证实该类催化剂在碳烟燃烧应用中能够维持良好的催化氧化活性:在经水热老化处理后,疏松接触形态的碳烟燃尽温度T90可由700℃降至465℃,落在颗粒捕集器工作温度范围内。在相同的评价条件下,达到并超过已报道的各型碳烟颗粒燃烧催化剂,且制备方法简单,易于操作,适合于工业生产。
附图说明
图1为镧锆铈复合氧化物负载钯银合金催化剂上的碳烟氧化反应转化率随温度变化的关系。
具体实施方式
实施例1
在含有35g硝酸铈、3.6g硝酸镧与9.8g硝酸氧锆的混盐离子溶液中滴入氨水与碳酸氢铵的混合沉淀剂,将pH调节至8~9;采用抽滤法分去水层,滤饼经水洗涤去除硝酸根;将上述制得的混合离子碱式碳酸盐凝胶加入乙醇进行洗涤,在120℃烘干后研磨至100目以下,于900℃煅烧0.5h,降温后获得轻稀土修饰型CeZrOx铈锆复合氧化物粉末。
将5g上述轻稀土修饰型CeZrOx铈锆复合氧化物载体浸没在含有12wt.%丙酸的15mL水溶液中,震荡后抽空处理,保持浸渍1h后,再于110℃干燥处理。干燥后的粉体在含有10mg金属钯的3.7mL硝酸盐溶液(水解所产生沉淀使用氨水络合溶解)中浸渍并由浆状搅拌至凝固,随后在110℃下进行干燥;
上述5g干燥粉体在空气气氛中于600℃煅烧30min,冷却后的粉体浸入15mL含有1g苹果酸及0.85g硝酸银的水溶液(pH=1),在敞口体系中搅拌逐渐至溶剂蒸发,经干燥后再次在空气气氛中于600℃煅烧200min;
将煅烧后盛装粉末的瓷舟置于管式炉中,在5vol.%氢气(Ar平衡气)吹扫下(流速30mL/min),于60℃还原处理60min;管式炉吹扫气切换为含有水蒸汽分压约0.1atm的空气,吹扫稳定15min后,升温至850℃,连续处理600min,降温即得催化剂成品粉末。
将所述所得催化剂与碳烟颗粒按照质量比为5∶1混合,搅拌均匀,将其放入TG-209热重分析仪,在空气气氛下(空气流速为20ml/min)以10℃/min的升温速率从30℃升到800℃。将所得的失重曲线转化为转化率曲线(参见图1),T10、T50和T90的温度分别为367℃、437℃和465℃,水热处理线A造成起燃活性下降,但燃尽活性提高。
实施例2
在5g市售轻稀土修饰型CeZrOx铈锆储氧材料(Ce︰Zr︰Sm摩尔比约为3︰0.83︰0.07)中。浸没在含有10wt.%柠檬酸的15mL水溶液中,震荡后抽空处理,保持浸渍3h后,再于150℃干燥处理。干燥后的粉体在含有5mg金属钯的4.7mL硝酸氨钯水溶液中浸渍并由浆状搅拌至凝固,随后在120℃下进行干燥;
上述5g干燥粉体在空气气氛中于600℃煅烧30min,冷却后的粉体浸入15mL含有1g苹果酸及1.3g硝酸银的水溶液(pH=4),在敞口体系中搅拌逐渐至溶剂蒸发,经干燥后再次在空气气氛中于450℃煅烧30min;
将煅烧后盛装粉末的瓷舟置于管式炉中,在氢气(Ar平衡气)吹扫下(流速20mL/min),于150℃还原处理60min;管式炉吹扫气切换为含有水蒸汽分压约0.1atm的空气,吹扫稳定15min后,升温至850℃,连续处理600min,降温即得催化剂成品粉末。
将所述所得催化剂与碳烟颗粒按照质量比为5︰1混合,搅拌均匀,将其放入TG-209热重分析仪,在空气气氛下(空气流速为20ml/min)以10℃/min的升温速率从30℃升到800℃。将所得的失重曲线转化为转化率曲线,并测得T10、T50和T90的温度分别为348℃、416℃和478℃。
实施例3
在含有40g硝酸铈、3.6g硝酸钆与6.3g氯化氧锆的混盐离子溶液中滴入碳酸铵沉淀剂,将pH调节至8~9;采用抽滤法分去水层,滤饼经水洗涤去除氯离子;将上述制得的混合离子碱式碳酸盐凝胶在120℃烘干后研磨至100目以下,于750℃煅烧8h,降温后获得轻稀土修饰型CeZrOx铈锆复合氧化物粉末。
将5g上述轻稀土修饰型CeZrOx铈锆复合氧化物载体浸没在含有8wt.%柠檬酸的15mL水溶液中,震荡后抽空处理,保持浸渍1h后,再于110℃干燥处理。干燥后的粉体在含有5mg金属钯的5mL硝酸铵钯溶液中浸渍并由浆状搅拌至凝固,随后在140℃下进行干燥;
上述5g干燥粉体在空气气氛中于500℃煅烧60min,冷却后的粉体浸入15mL含有3g柠檬酸及0.5g硝酸银的水溶液(pH=1),在敞口体系中搅拌逐渐至溶剂蒸发,经干燥后再次在空气气氛中于800℃煅烧150min;
将煅烧后盛装粉末的瓷舟置于管式炉中,在1vol.%氢气(Ar平衡气)吹扫下(流速30mL/min),于50℃还原处理100min;管式炉吹扫气切换为含有水蒸汽分压约0.1atm的空气,吹扫稳定15min后,升温至850℃,连续处理600min,降温即得催化剂成品粉末。
将所述所得催化剂与碳烟颗粒按照质量比为5∶1混合,搅拌均匀,将其放入TG-209热重分析仪,在空气气氛下(空气流速为20ml/min)以10℃/min的升温速率从30℃升到800℃。将所得的失重曲线转化为转化率曲线(参见图1),T10、T50和T90的温度分别为390℃、452℃和505℃。
实施例4
在含有25g碳酸铈、1g氧化钐与2g碳酸锆的混合粉末中加入1M硝酸溶液80mL并搅拌至溶解后,滴入氨水将pH调节至8~9;在120℃烘干后研磨至100目以下,于850℃煅烧4h,降温后获得轻稀土修饰型CeZrOx铈锆复合氧化物粉末。
将5g上述轻稀土修饰型CeZrOx铈锆复合氧化物载体浸没在含有1mL甲酸的15mL水溶液中,震荡后抽空处理,保持浸渍1h后,再于110℃干燥处理。干燥后的粉体在含有2mg金属钯的5mL硝酸盐溶液(水解所产生沉淀使用氨水络合溶解)中浸渍并由浆状搅拌至凝固,随后在120℃下进行干燥;
上述5g干燥粉体在空气气氛中于600℃煅烧30min,冷却后的粉体浸入15mL含有1g乙二胺四乙酸钠及1.2g硝酸银的水溶液(pH=3.4),在敞口体系中搅拌逐渐至溶剂蒸发,经干燥后再次在空气气氛中于450℃煅烧200min;
将煅烧后盛装粉末的瓷舟置于管式炉中,在1vol.%氢气(Ar平衡气)吹扫下(流速30mL/min),于260℃还原处理15min;管式炉吹扫气切换为含有水蒸汽分压约0.1atm的空气,吹扫稳定15min后,升温至850℃,连续处理600min,降温即得催化剂成品粉末。
将所述所得催化剂与碳烟颗粒按照质量比为5∶1混合,搅拌均匀,将其放入TG-209热重分析仪,在空气气氛下(空气流速为20ml/min)以10℃/min的升温速率从30℃升到800℃。将所得的失重曲线转化为转化率曲线,并测得T10、T50和T90的温度分别为344℃、457℃和485℃。
实施例5
在含有25g氧化铈、1g七氧化四铽与2g氧化锆的混合粉末中加入氧化锆球磨罐,在行星式球磨机上研磨1h后,于850℃煅烧4h,降温后获得轻稀土修饰型CeZrOx铈锆复合氧化物粉末。
将5g上述轻稀土修饰型CeZrOx铈锆复合氧化物载体浸没在含有1g马来酸的15mL水溶液中,震荡后抽空处理,保持浸渍1h后,再于110℃干燥处理。干燥后的粉体在10mL含有5mg乙酸钯的水溶液中浸渍并由浆状搅拌至凝固,随后在120℃下进行干燥;
上述5g干燥粉体在空气气氛中于600℃煅烧30min,冷却后的粉体浸入15mL含有1g柠檬酸及1.2g硝酸银的水溶液(pH=1),在敞口体系中搅拌逐渐至溶剂蒸发,经干燥后再次在空气气氛中于650℃煅烧200min;
将煅烧后盛装粉末的瓷舟置于管式炉中,在1vol.%氢气(Ar平衡气)吹扫下(流速30mL/min),于150℃还原处理30min;管式炉吹扫气切换为含有水蒸汽分压约0.1atm的空气,吹扫稳定15min后,升温至850℃,连续处理600min,降温即得催化剂成品粉末。
将所述所得催化剂与碳烟颗粒按照质量比为5∶1混合,搅拌均匀,将其放入TG-209热重分析仪,在空气气氛下(空气流速为20ml/min)以10℃/min的升温速率从30℃升到800℃。将所得的失重曲线转化为转化率曲线,并测得T10、T50和T90的温度分别为392℃、427℃和485℃。
Claims (9)
1.一种负载合金型碳烟氧化催化剂,其特征在于包括载体与合金型活性组分,所述载体为轻稀土修饰型铈锆复合氧化物,所述合金型活性组分为均质型钯银合金,合金型活性组分按质量百分比的组成为钯1%~20%,银80%~99%,总金属负载量为4%~15%;
所述负载合金型碳烟氧化催化剂的组成通式为r%-PdxAg1-x/LnyZrzCe3O8-q,其中Ln为轻稀土元素La, Pr, Nd, Sm, Eu, Gd,Tb中至少一种,式中r%为金属组分负载质量百分比,下标x,y,z为所示组分的摩尔比例系数,x为0.01~0.2,y+z < 1,氧的摩尔比例系数记为8-q,q为不定值,随催化反应进行而循环波动;
所述负载合金型碳烟氧化催化剂的合成方法包括以下步骤:
1)将轻稀土修饰型铈锆复合氧化物载体在有机酸水溶液中预浸渍后,干燥,将干燥后的粉体在阳离子型钯源的水溶液中进行饱和浸渍,随后再次干燥,得干燥粉体;
2)将步骤1)所得干燥粉体在空气气氛中煅烧,冷却后的粉体浸入含有多齿配体的银离子水溶液,在搅拌下逐渐蒸干溶液,经干燥后再次在空气气氛中煅烧;
3)煅烧后粉体转移至管式炉中,在氢气气氛中还原;
4)在含有水蒸汽空气气氛中水热老化处理,即得到水热稳定化的负载合金型碳烟氧化催化剂。
2.如权利要求1所述负载合金型碳烟氧化催化剂的合成方法,其特征在于包括以下步骤:
1)将轻稀土修饰型铈锆复合氧化物载体在有机酸水溶液中预浸渍后,干燥,将干燥后的粉体在阳离子型钯源的水溶液中进行饱和浸渍,随后再次干燥,得干燥粉体;
2)将步骤1)所得干燥粉体在空气气氛中煅烧,冷却后的粉体浸入含有多齿配体的银离子水溶液,在搅拌下逐渐蒸干溶液,经干燥后再次在空气气氛中煅烧;
3)煅烧后粉体转移至管式炉中,在氢气气氛中还原;
4)在含有水蒸汽空气气氛中水热老化处理,即得到水热稳定化的负载合金型碳烟氧化催化剂。
3.如权利要求2所述负载合金型碳烟氧化催化剂的合成方法,其特征在于在步骤1)中,所述轻稀土修饰型铈锆复合氧化物载体采用固相混合法或共沉淀法制备的储氧材料,铈元素占金属原子比例的50%以上。
4.如权利要求2所述负载合金型碳烟氧化催化剂的合成方法,其特征在于在步骤1)中,所述有机酸采用短链脂肪酸,所述短链脂肪酸选自甲酸、乙酸、丙酸、马来酸中的一种。
5.如权利要求2所述负载合金型碳烟氧化催化剂的合成方法,其特征在于在步骤1)中,所述有机酸水溶液pH值为1~2;所述干燥是在复合氧化物粉体倾入有机酸溶液后,在搅拌下进行抽空以排出内孔中气泡,随之过滤并在110 ℃干燥。
6.如权利要求2所述负载合金型碳烟氧化催化剂的合成方法,其特征在于在步骤1)中,所述阳离子型钯源为硝酸氨钯或与氨水配位处理的硝酸钯或乙酸钯;所述饱和浸渍采用初始润湿法以活性组分的最小溶液量完成对载体粉末的润湿;所述再次干燥的温度为110~220 ℃。
7.如权利要求2所述负载合金型碳烟氧化催化剂的合成方法,其特征在于在步骤2)中,所述干燥粉体在空气气氛中煅烧是在450~600 ℃煅烧30~200 min;所述含有多齿配体的银离子水溶液,是指在硝酸银水溶液中加入柠檬酸、苹果酸、乙二胺四乙酸、马来酸、富马酸有机酸螯合配体中的一种,并在络合反应完成后,以NaOH调节溶液pH为1~4;所述在搅拌下逐渐蒸干溶液,是指在通过蒸发除去大部分溶剂后,在搅拌作用下继续减压蒸馏至接近干燥;所述再次在空气气氛中煅烧是在450~600 ℃煅烧30~200 min。
8.如权利要求2所述负载合金型碳烟氧化催化剂的合成方法,其特征在于在步骤3)中,所述还原的条件为于30~150 ℃下还原15~60 min。
9.如权利要求2所述负载合金型碳烟氧化催化剂的合成方法,其特征在于在步骤4)中,所述在含有水蒸汽空气气氛中水热老化处理,是在含有水蒸汽分压0.1 atm的空气气氛中于850 ℃水热老化处理300~600 min。
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