CN105749960A - 一种用于氨选择性催化还原脱除NOx的催化剂的制备方法 - Google Patents
一种用于氨选择性催化还原脱除NOx的催化剂的制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 40
- 238000010531 catalytic reduction reaction Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title abstract description 10
- 229910021529 ammonia Inorganic materials 0.000 title abstract description 5
- 239000002808 molecular sieve Substances 0.000 claims abstract description 33
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 33
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 10
- -1 iron ions Chemical class 0.000 claims abstract description 9
- 230000000694 effects Effects 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 4
- 229910001456 vanadium ion Inorganic materials 0.000 claims abstract description 4
- 238000005342 ion exchange Methods 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000009938 salting Methods 0.000 claims description 8
- 150000001768 cations Chemical class 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 238000006555 catalytic reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910001868 water Inorganic materials 0.000 claims description 5
- 229910052878 cordierite Inorganic materials 0.000 claims description 4
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 4
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 238000005341 cation exchange Methods 0.000 claims description 3
- 125000002091 cationic group Chemical group 0.000 claims description 3
- 210000002421 cell wall Anatomy 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 239000002562 thickening agent Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000009257 reactivity Effects 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- KTNUFJVOTPQPES-UHFFFAOYSA-N oxotungsten titanium vanadium Chemical group [W]=O.[Ti].[V] KTNUFJVOTPQPES-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
- B01J29/42—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing iron group metals, noble metals or copper
- B01J29/46—Iron group metals or copper
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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Abstract
本发明公开了一种用于氨选择性催化还原脱除NOx的催化剂的制备方法，以ZSM?11分子筛为催化剂载体，通过离子交换法将铜离子、铁离子、钛离子、钒离子和稀土金属阳离子负载在分子筛孔道内，构成催化反应活性位。本发明用于氨选择性催化还原脱除NOx的催化剂的制备方法，所获得的催化剂具有高温活性和水热稳定性，可以在更宽的温度区间和高空速的条件下具有高NOx转化效率，具有很好的实用性。
Description
技术领域
本发明属于NOx去除技术领域，具体涉及一种用于氨选择性催化还原脱除NOx的催化剂的制备方法。
技术背景
现有柴油机尾气脱硝催化剂的结构，基本上是以堇青石蜂窝陶瓷为结构载体，上面再涂覆具有脱硝活性的催化剂粉末。然后把整体催化剂封装到具有尿素喷射系统的催化转化器当中。当柴油发动机尾气和作为还原剂的氨气一起通过时，发生催化还原反应，也就是氨气和氮氧化物反应生产氮气和水，从而脱除掉尾气中含有的氮氧化合物，达到降低氮氧化物污染的目的。
现有催化剂主要有两种，第一种是钒钛钨氧化物催化剂，以氧化钛为载体，钒氧化物为主要活性组分，钨氧化物作为助剂则主要起提高催化剂水热稳定性的作用。但这种催化剂的缺点是钒氧化物有很大的毒性，无论在催化剂生产过程中，还是安装催化剂后，催化剂在工作时发生粉末脱落，都会给环境造成很大危害，比如粉尘吸入人体内。第二种是铜、铁、ZSM5分子筛催化剂，其中ZSM5分子筛为载体，铜和铁为活性组分。这种催化剂的缺点是催化剂工作温度区间窄，而且水热稳定性差，在实际工作中由于柴油发动机尾气中水的存在，铜和铁容易在分子筛孔道中流失，从而催化活性降低很快。
发明内容
发名目的：针对现有技术中存在的不足，本发明的目的是提供一种用于氨选择性催化还原脱除NOx的催化剂的制备方法，具有制备方法简单，成本低，获得的催化剂具有高温活性和水热稳定性，可以在更宽的温度区间和高空速的条件下具有高NOx转化效率等特点。
技术方案：为实现上述目的，本发明采用的技术方案如下：
一种用于氨选择性催化还原脱除NOx的催化剂的制备方法，以ZSM-11分子筛为催化剂载体，通过离子交换法将铜离子、铁离子、钛离子、钒离子和稀土金属阳离子负载在分子筛孔道内，构成催化反应活性位。
所述的用于氨选择性催化还原脱除NOx的催化剂的制备方法，交换的阳离子总重量与分子筛重量比为0.5~65%。
所用的离子交换法是用ZSM-11分子筛与所需交换的一种或者多种金属阳离子的盐溶液交换
所述的用于氨选择性催化还原脱除NOx的催化剂的制备方法，包括以下步骤：
1）取ZSM-11分子筛预煅烧，去除孔道和表面上的模板剂的有机物；干燥温度为50℃-200℃，干燥时间为4h-48h；煅烧温度为200℃-600℃，煅烧时间为2h-8h;
2）用ZSM-11分子筛与所需交换的一种或者多种金属阳离子的盐溶液交换；离子交换后分子筛的基本孔道结构不变；交换温度为室温到60℃、交换时间3-24h，交换小时，交换2-4次，盐溶液质量百分浓度为5-20%；
3）阳离子交换后，用去离子水洗涤，然后在50~200℃下干燥，然后在200~600℃下煅烧，从而使交换到分子筛中的阳离子稳定结合；
4）把具有催化活性的离子交换并干燥煅烧后的ZSM-11分子筛催化剂在水中分散，充分分散后加入粘合剂和增稠剂，然后涂覆到堇青石蜂窝载体上，在蜂窝载体的细小孔道壁上形成厚度几十微米的催化剂涂层。
有益效果：与现有技术相比，本发明用于氨选择性催化还原脱除NOx的催化剂的制备方法，所获得的催化剂具有高温活性和水热稳定性，可以在更宽的温度区间和高空速的条件下具有高NOx转化效率，具有很好的实用性。
具体实施方式
下面结合具体实施例对本发明做进一步说明。
实施例1
一种用于氨选择性催化还原脱除NOx的催化剂的制备方法，以ZSM-11分子筛为催化剂主要载体，通过离子交换法将铜离子、铁离子、钛离子、钒离子和稀土金属阳离子负载在分子筛孔道内，构成催化反应活性位。具体过程如下：
1）取ZSM-11分子筛预煅烧，去除孔道和表面上的模板剂的有机物；干燥温度为50℃-200℃，干燥时间为4h-48h；所述煅烧温度为200℃-600℃，煅烧时间为2h-8h。
2）用ZSM-11分子筛与所需交换的一种或者多种金属阳离子的盐溶液交换；离子交换后分子筛的基本孔道结构不变；室温到60℃下交换，交换3-24h，交换2-4次，盐溶液质量百分浓度为5-20%。
3）阳离子交换后，用去离子水洗涤，然后在50~200℃下干燥，然后在200~600℃下煅烧，从而使交换到分子筛中的阳离子稳定结合；
4）把具有催化活性的离子交换并干燥煅烧后的ZSM-11分子筛催化剂在水中分散，充分分散后加入粘合剂和增稠剂，然后涂覆到堇青石蜂窝载体上，在蜂窝载体的细小孔道壁上形成厚度几十微米的催化剂涂层。
对产品性能进行检测，结果如下表所示。
| 反应温度（℃） | 150 | 200 | 250 | 300 | 350 | 400 | 450 | 500 | 550 |
| NOx转化率（%） | 56.2 | 82.0 | 93.5 | 98.2 | 99.3 | 98.9 | 96.4 | 90.6 | 85.6 |
此外，将ZSM-11分子筛替换成钛硅分子筛，或者ZSM-11分子筛和钛硅分子筛的混合物，或ZSM-22分子筛，采用上述相同的方法制备，也能获得较好的技术效果。
Claims (4)
1.一种用于氨选择性催化还原脱除NOx的催化剂的制备方法，其特征在于，以ZSM-11分子筛为催化剂载体，通过离子交换法将铜离子、铁离子、钛离子、钒离子和稀土金属阳离子负载在分子筛孔道内，构成催化反应活性位。
2.根据权利要求1所述的用于氨选择性催化还原脱除NOx的催化剂的制备方法，其特征在于：交换的阳离子总重量与分子筛重量比为0.5~65%。
3.根据权利要求1所述的用于氨选择性催化还原脱除NOx的催化剂的制备方法，其特征在于：所用的离子交换法是用ZSM-11分子筛与所需交换的一种或者多种金属阳离子的盐溶液交换。
4.根据权利要求1所述的用于氨选择性催化还原脱除NOx的催化剂的制备方法，其特征在于，包括以下步骤：
1）取ZSM-11分子筛预煅烧，去除孔道和表面上的模板剂的有机物；干燥温度为50℃-200℃，干燥时间为4h-48h；煅烧温度为200℃-600℃，煅烧时间为2h-8h;
2）用ZSM-11分子筛与所需交换的一种或者多种金属阳离子的盐溶液交换；离子交换后分子筛的基本孔道结构不变；交换温度为室温到60℃、交换时间3-24h，交换小时，交换2-4次，盐溶液质量百分浓度为5-20%；
3）阳离子交换后，用去离子水洗涤，然后在50~200℃下干燥，然后在200~600℃下煅烧，从而使交换到分子筛中的阳离子稳定结合；
4）把具有催化活性的离子交换并干燥煅烧后的ZSM-11分子筛催化剂在水中分散，充分分散后加入粘合剂和增稠剂，然后涂覆到堇青石蜂窝载体上，在蜂窝载体的细小孔道壁上形成厚度几十微米的催化剂涂层。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3363540A1 (en) * | 2017-02-17 | 2018-08-22 | Umicore Ag & Co. Kg | Copper containing moz zeolite for selective nox reduction catalysis |
| CN108940356A (zh) * | 2018-05-29 | 2018-12-07 | 广东工业大学 | 一种Fe@ZSM-11介孔分子筛催化剂的制备方法 |
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| CN102271810A (zh) * | 2008-11-03 | 2011-12-07 | 巴斯夫公司 | 用于选择性氨氧化的双金属催化剂 |
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| US11154846B2 (en) | 2017-02-17 | 2021-10-26 | Umicore Ag & Co. Kg | Copper containing MOZ zeolite for selective NOx reduction catalysis |
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| CN108940356A (zh) * | 2018-05-29 | 2018-12-07 | 广东工业大学 | 一种Fe@ZSM-11介孔分子筛催化剂的制备方法 |
| CN108940356B (zh) * | 2018-05-29 | 2021-03-09 | 广东工业大学 | 一种Fe@ZSM-11介孔分子筛催化剂的制备方法 |
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