CN102000560B - 一种用于催化净化氮氧化物的铈基复合氧化物催化剂 - Google Patents
一种用于催化净化氮氧化物的铈基复合氧化物催化剂 Download PDFInfo
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- CN102000560B CN102000560B CN201010568133.0A CN201010568133A CN102000560B CN 102000560 B CN102000560 B CN 102000560B CN 201010568133 A CN201010568133 A CN 201010568133A CN 102000560 B CN102000560 B CN 102000560B
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- catalyst
- cerium
- composite oxide
- based composite
- nitric oxide
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- 239000003054 catalyst Substances 0.000 title claims abstract description 46
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 12
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 239000002131 composite material Substances 0.000 title claims abstract description 11
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title abstract description 16
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000003197 catalytic effect Effects 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 238000000746 purification Methods 0.000 claims abstract description 6
- 238000010531 catalytic reduction reaction Methods 0.000 claims abstract description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004202 carbamide Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 230000001376 precipitating effect Effects 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 239000010937 tungsten Substances 0.000 claims abstract description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 4
- 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 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical class ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- IADRPEYPEFONML-UHFFFAOYSA-N [Ce].[W] Chemical compound [Ce].[W] IADRPEYPEFONML-UHFFFAOYSA-N 0.000 claims description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical class [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 229910052723 transition metal Inorganic materials 0.000 abstract description 5
- 150000003624 transition metals Chemical class 0.000 abstract description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 150000000703 Cerium Chemical class 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 2
- 229910021529 ammonia Inorganic materials 0.000 abstract description 2
- 239000002905 metal composite material Substances 0.000 abstract description 2
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 2
- 239000011733 molybdenum Substances 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 239000003245 coal Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000779 smoke Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 17
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 7
- 239000003546 flue gas Substances 0.000 description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种用于氨选择性催化还原氮氧化物的铈基复合氧化物催化剂及其制备方法。本发明中的催化剂是铈与钨、钼、铁中的任意一种或多种过渡金属组成的金属复合氧化物催化剂。催化剂的制备方法为均匀沉淀法，即将所需铈盐和上述任意一种或多种过渡金属所对应的盐配成混合溶液，以过量尿素作为沉淀剂，在90～95℃温度条件下连续搅拌8～15h，然后进行抽滤、洗涤、烘干和煅烧制得。本发明采用无毒无害的原料，通过简单易行的方法制备出具有催化活性高、N2生成选择性优异、操作温度窗口宽、能适应高空速反应条件等特点的铈基复合氧化物催化剂，适用于以柴油车尾气为代表的移动源和以燃煤电厂烟气为代表的固定源氮氧化物催化净化装置。
Description
技术领域
本发明应用于环境催化技术领域，涉及一种用于以柴油车尾气为代表的移动源和以燃煤电厂烟气为代表的固定源氮氧化物催化净化的铈基复合氧化物催化剂。
背景技术
氮氧化物(NOx，主要指NO和NO2)的存在会引起光化学烟雾、酸雨、温室效应和臭氧层破坏等重大环境问题，同时具有生物呼吸毒性，可对生态环境和人类健康造成巨大的危害。因此，如何有效去除NOx成为当今环境保护领域的热点问题。
随着石油资源日趋短缺，CO2减排压力增大，燃油经济性好和动力性强的柴油车越来越受到重视。与装有三效催化剂的汽油车相比，以NOx和PM为特征的尾气污染成为制约柴油车推广应用的瓶颈。柴油车尾气排放具有温度低、氧含量高、含有大量颗粒物和少量硫等特点。柴油车已成为我国机动车NOx和PM排放的主要分担者，成为机动车尾气治理中的重点和难点。目前，针对柴油机尾气NOx净化的技术方案主要有：氨类选择性催化还原NOx(NH3-SCR)、碳氢化合物选择性催化还原NOx(HC-SCR)、贮存-还原技术(NSR)、NOx和PM组合净化技术和四效催化技术等。其中，NH3-SCR被认为是最有希望全面应用于柴油车尾气净化的技术，且该技术目前已经进入了实用化阶段。
目前，NH3-SCR是国际上应用最为广泛的烟气脱硝技术。工业化应用的NH3-SCR催化剂通常是含有毒物质钒(V)的V2O5-WO3(MoO3)/TiO2催化剂。在使用过程中若V发生脱落，进入到环境中具有很大的生物毒性，且该催化剂体系具有操作温度窗口较窄、易催化烟气中的SO2转化为SO3等缺点。
因此，开发新型具有高NH3-SCR活性、宽操作温度窗口、适应高空速环境、无毒无害的非钒催化剂体系用于以柴油车尾气为代表的移动源和以燃煤电厂烟气为代表的固定源NOx的催化消除，具有非常重要的环境意义。
发明内容
为了解决现有金属氧化物催化剂体系操作温度窗口窄、低温活性差、N2选择性低、对反应空速敏感等缺点，本发明首次提供了一种新型铈基复合氧化物催化剂及其制备方法，可用作以柴油车尾气为代表的移动源和以燃煤电厂烟气为代表的固定源NOx催化净化。
本发明中的催化剂是铈与钨、钼、铁中的任意一种或多种过渡金属组成的金属复合氧化物催化剂。催化剂的制备方法为均匀沉淀法，即将所需两种金属氧化物所对应的盐配成混合溶液，其中铈盐是氯化亚铈或硝酸铈或硝酸铈铵或硫酸铈中的至少一种，各种过渡金属所对应的盐分别为钨酸铵、钼酸铵和硝酸铁，以金属元素的摩尔比计，铈和过渡金属的比例为0.2～5.0，以过量尿素作为沉淀剂，在90～95℃温度条件下连续搅拌8～15h，然后进行抽滤和洗涤，将滤饼放入烘箱中于80～120℃烘干过夜，最后经马弗炉于400～800℃空气中煅烧4～6h即制得催化剂成品。
本发明具有如下优点：
(1)操作温度窗口宽(尤其在低温区的活性好)，适用于机动车尾气温度变化幅度大的应用环境；在固定源烟气脱硝方面，有望作为低温型SCR催化剂，应用于烟气脱硫之后，以提高SCR催化剂的使用寿命；
(2)对反应空速不敏感，适用于机动车尾气净化高空速的特性，将其应用于固定源烟气脱硝时可以大幅度降低催化剂的使用量，降低成本、节约空间；
(3)具有非常优异的N2生成选择性；
(4)具有非常好的抗高温烧结能力；
(5)采用无毒组分，减少对人体健康和生态环境的危害。
具体实施方式
为了更加清晰地说明本发明，列举以下实施例，但其对本发明的范围无任何限制。
【实施例1-4】
将钨酸铵溶于草酸溶液(钨酸铵与草酸的质量比为1∶1)，并向该溶液中加入硝酸铈溶液，配制Ce/W摩尔比为0.5的溶液并混合均匀，向该溶液中加入过量尿素，并在90℃温度条件下连续搅拌12h，然后进行抽滤和洗涤，将滤饼放入烘箱中于100℃烘干过夜，最后经马弗炉于500℃空气中煅烧5h制得粉末状催化剂。将制得的催化剂压片、研碎、过筛，取40～60目备用，称为催化剂A。其它条件不变，改变Ce/W摩尔比为1.0和2.0，分别制得催化剂B和C。将催化剂B在800℃空气中煅烧1h制得催化剂D。
【实施例5】
用实施例1-4制得的铈钨复合氧化物催化剂A、B、C和D，在自制的微型固定床反应器上进行NH3选择性催化还原NOx反应活性的考察。催化剂的使用量为0.12ml，反应混合气的组成为：[NO]＝[NH3]＝500ppm，[O2]＝5％，N2作平衡气，气体总流量为500ml/min，空速为250,000h-1，反应温度150～450℃。NO和NH3及副产物N2O，NO2均利用红外气体池测定。反应结果如表1所示。
催化剂B在250,000h-1空速条件下，200～450℃的温度范围内均可实现80％以上的NOx转化率，且在N2选择性均大于97％。经过800℃高温煅烧得到的催化剂D仍可以在250,000h-1空速条件下，300～450℃的温度范围内实现80％以上的NOx转化率，且N2生成选择性均大于98％，说明该催化剂具有非常优异的抗高温烧结能力。
【实施例6】
使用催化剂B，在自制的微型固定床反应器上考察反应空速对催化剂活性的影响。催化剂的使用量分别为0.3ml、0.12ml、0.06ml，反应混合气的组成为：[NO]＝[NH3]＝500ppm，[O2]＝5％，N2作平衡气，气体总流量为500ml/min，相应空速分别为100,000h-1、250,000h-1，500,000h-1、反应温度150～450℃。NO和NH3及副产物N2O，NO2均利用红外气体池测定。反应结果如表2所示。
催化剂B在空速为100,000h-1的条件下，在200～450℃的温度范围内均可实现98％以上的NOx转化率，且N2生成选择性均大于98％，表现出了非常宽的操作温度窗口；即使在500,000h-1的高空速条件下，催化剂B仍然可以在250～450℃的温度范围内均可实现90％以上的NOx转化率，且N2选择性均大于98％，说明该催化剂具有非常优异的抗高空速反应性能。
表1不同Ce/W摩尔比及经高温煅烧后的催化剂活性评价结果
表2反应空速对催化剂B活性的影响
Claims (2)
1.一种用于氨选择性催化还原氮氧化物的铈钨复合氧化物催化剂在柴油车尾气氮氧化物催化净化中的应用，其特征在于该催化剂是采用均匀沉淀法，以过量尿素作为沉淀剂，在90～95℃温度条件下将铈元素和钨元素的摩尔比为0.2～5.0的混合溶液连续搅拌8～15h，然后进行抽滤和洗涤，将所得滤饼放入烘箱中于80～120℃烘干，最后经马弗炉于400～800℃空气中煅烧4～6h制备得到的金属复合氧化物。
2.根据权利要求1所述的应用，其特征在于催化剂制备过程中所用铈的前驱体是氯化亚铈或硝酸铈或硝酸铈铵或硫酸铈中的至少一种，所用钨的前驱体为钨酸铵。
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| Publication number | Publication date |
|---|---|
| CN102000560A (zh) | 2011-04-06 |
| US20130202513A1 (en) | 2013-08-08 |
| US9498770B2 (en) | 2016-11-22 |
| WO2012071971A1 (zh) | 2012-06-07 |
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