CN103418239B - SCR method for removal of NOx by utilizing metal-organic frameworks as catalyst - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims description 8
- 239000000463 material Substances 0.000 claims abstract description 19
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims abstract description 18
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003546 flue gas Substances 0.000 claims abstract description 16
- 238000010531 catalytic reduction reaction Methods 0.000 claims abstract description 10
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 9
- 239000011593 sulfur Substances 0.000 claims abstract description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 239000013291 MIL-100 Substances 0.000 claims description 5
- 239000013206 MIL-53 Substances 0.000 claims description 5
- 239000013165 zeolitic imidazolate framework-100 Substances 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 16
- 239000002184 metal Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract description 2
- 231100000572 poisoning Toxicity 0.000 abstract description 2
- 230000000607 poisoning effect Effects 0.000 abstract description 2
- 230000009849 deactivation Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 230000009931 harmful effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- 239000013178 MIL-101(Cr) Substances 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000036619 pore blockages Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 231100000563 toxic property Toxicity 0.000 description 1
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Abstract
本发明公开了以金属有机骨架材料为催化剂用于选择性催化还原脱除氮氧化物，其利用金属有机骨架材料（MOFs）作为催化剂，NH3选择性催化还原NOx，具有抗硫性能的催化脱硝应用；烟气条件范围：400～1000ppm NOx，400～1000ppm NH3，3%～5%O2，100～500ppm SO2，10000h-1～40000h-1空速，250～350℃，催化剂的脱硝活性可达到80%以上。基于该类材料具有大的比表面积，分散有序的金属活性位点，三维通透的孔道结构，在反应过程中可有效的延缓硫酸盐沉积所导致的催化剂中毒、失活的问题，从而可实现持续高效地催化还原NOx。The invention discloses a metal organic framework material as a catalyst for selective catalytic reduction and removal of nitrogen oxides, which utilizes metal organic framework materials (MOFs) as a catalyst, NH3 selectively catalytically reduces NO x , and has sulfur-resistant catalytic Denitrification application; flue gas condition range: 400～1000ppm NO x , 400～1000ppm NH 3 , 3%～5%O 2 , 100～500ppm SO 2 , 10000h -1 ～40000h -1 space velocity, 250～350℃, catalyst The denitrification activity can reach more than 80%. Based on the fact that this type of material has a large specific surface area, dispersed and ordered metal active sites, and a three-dimensional transparent pore structure, it can effectively delay the problem of catalyst poisoning and deactivation caused by sulfate deposition during the reaction process, thereby enabling Realize continuous and efficient catalytic reduction of NO x .
Description
技术领域technical field
本发明属于烟气催化脱硝领域，涉及以金属有机骨架材料为催化剂用于选择性催化还原脱除氮氧化物。The invention belongs to the field of flue gas catalytic denitrification, and relates to the use of metal organic framework materials as catalysts for selective catalytic reduction to remove nitrogen oxides.
背景技术Background technique
氮氧化物(NOx)是重要的大气污染物之一，不仅危害动植物生长、破坏臭氧层，而且会引发酸雨、温室效应和光化学烟雾等。因此，加强氮氧化物排放的控制已被列入“十二五”规划纲要，减少氮氧化物的排放已成为现阶段关注的重点。Nitrogen oxides (NO x ) are one of the important air pollutants, which not only harm the growth of animals and plants, destroy the ozone layer, but also cause acid rain, greenhouse effect and photochemical smog. Therefore, strengthening the control of nitrogen oxide emissions has been included in the "Twelfth Five-Year Plan" outline, and reducing nitrogen oxide emissions has become the focus of attention at this stage.
目前，国内外烟气脱硝技术主要为选择性催化还原法（SCR）。商业上主要采用的V2O5/TiO2和V2O5-WO3(MoO3)/TiO2催化剂，最佳活性温度窗口在300～400℃之间，具有良好的脱硝活性和抗硫中毒性能。但是，该类催化剂还存在着一些不足：活性组分钒具有毒性，对人体健康和环境产生危害；烟气中的SO2容易被氧化为SO3，与NH3反应生成的硫酸铵盐会覆盖催化剂的活性位点、堵塞催化剂通道。因此，需要开发一种新型无钒的具有良好脱硝活性与抗硫中毒性能的催化剂。At present, the flue gas denitrification technology at home and abroad is mainly selective catalytic reduction (SCR). V 2 O 5 /TiO 2 and V 2 O 5 -WO 3 (MoO 3 )/TiO 2 catalysts that are mainly used commercially have the best activity temperature window between 300 and 400°C, and have good denitrification activity and sulfur resistance Toxic properties. However, this type of catalyst still has some disadvantages: the active component vanadium is toxic, which is harmful to human health and the environment; SO 2 in the flue gas is easily oxidized to SO 3 , and the ammonium sulfate salt formed by reacting with NH 3 will cover the Catalyst active sites, blockage of catalyst channels. Therefore, it is necessary to develop a new vanadium-free catalyst with good denitrification activity and sulfur poisoning resistance.
金属有机骨架材料（MOFs）是一种新型的具有多孔结构的功能材料，具有比表面积大，孔径可调，结构稳定等特点。利用MOFs比表面积大的优势可极大的提高催化反应过程中气体的吸附性能，结合稳定的三维孔道结构、金属位点分散有序的特点可有效的提高气相催化反应的活性。因此，以金属有机骨架材料作为脱硝催化剂将有望在二氧化硫存在的情况下同时保持良好的脱硝活性。Metal-organic frameworks (MOFs) are a new type of functional material with a porous structure, which has the characteristics of large specific surface area, adjustable pore size, and stable structure. Taking advantage of the large specific surface area of MOFs can greatly improve the gas adsorption performance during the catalytic reaction process, combined with the stable three-dimensional pore structure and the dispersed and orderly characteristics of metal sites can effectively improve the activity of gas-phase catalytic reactions. Therefore, the use of metal-organic frameworks as denitration catalysts is expected to maintain good denitration activity in the presence of sulfur dioxide.
专利申请号为201010235033.6的专利文件公开了一种以金属有机骨架材料为载体的低温SCR脱硝催化剂，通过负载过渡金属组分在低空速下其低温脱硝活性达到80%，但是在其应用实例中仅以MIL-101(Cr)为载体，其脱硝活性由负载的过渡金属实现，并未考察以金属有机骨架材料作为催化剂的脱硝性能。专利申请号为200710046923.0的专利文件公开了一种烟气脱硝多孔有机催化剂，在250℃时，NOx的脱除率为85%，由于其催化剂以腐殖酸为载体，V2O5为活性组分，对人体和环境具有危害作用，且在实例应用中未考虑SO2对催化剂的影响。专利申请号为201210113884.2的专利文件公开了一种负载型铁基复合氧化物催化剂，在实例应用过程中，200℃的中温烟气条件下，可以达到90％的NOx脱除效率，但未提及抗硫的性能。针对以上催化剂应用的不足，可将金属有机骨架材料作为脱硝催化剂，开发一种具有良好的抗硫性能的选择性催化还原脱除NOx的方法。The patent document with the patent application number 201010235033.6 discloses a low-temperature SCR denitration catalyst supported by a metal-organic framework material, and its low-temperature denitration activity reaches 80% at low space velocity by loading transition metal components, but in its application examples only With MIL-101(Cr) as the carrier, its denitrification activity is achieved by the supported transition metals, and the denitrification performance of metal-organic framework materials as catalysts has not been investigated. The patent document with the patent application number 200710046923.0 discloses a porous organic catalyst for flue gas denitrification. At 250°C, the removal rate of NOx is 85%. Since the catalyst uses humic acid as the carrier and V 2 O 5 as the active Components, which have harmful effects on human body and environment, and the influence of SO2 on the catalyst was not considered in the example application. The patent document with the patent application number 201210113884.2 discloses a supported iron-based composite oxide catalyst, which can achieve a NOx removal efficiency of 90% under a medium-temperature flue gas condition of 200°C in an example application process, but does not mention and sulfur resistance. In view of the shortcomings of the above catalyst applications, metal-organic framework materials can be used as denitration catalysts to develop a selective catalytic reduction method for NOx removal with good sulfur resistance.
发明内容Contents of the invention
针对现存的脱硝催化剂存在的含有对人体和环境有害的活性组分钒，普遍的抗硫性能不佳的问题，本发明旨在开发一种以金属有机骨架材料为脱硝催化剂，利用NH3选择性催化还原NOx的应用方法。Aiming at the problem that existing denitrification catalysts contain vanadium, an active component harmful to human body and environment, and generally have poor sulfur resistance performance, the present invention aims to develop a metal organic framework material as a denitration catalyst, using NH Selective Application method of catalytic reduction of NOx .
以金属有机骨架材料为催化剂的选择性催化还原脱除NOx，利用金属有机骨架材料作为催化剂，NH3选择性催化还原NOx，具有抗硫性能的催化脱硝应用技术；具体技术方案如下：Selective catalytic reduction removal of NO x using metal organic framework materials as catalysts, using metal organic framework materials as catalysts, NH 3 selective catalytic reduction of NO x , catalytic denitrification application technology with anti-sulfur performance; specific technical solutions are as follows:
烟气条件范围：400～1000ppm NOx，400～1000ppm NH3，3%～5%O2，100～500ppm SO2，10000h-1～40000h-1空速，250～350℃,脱硝效率可达到80%以上。Flue gas condition range: 400～1000ppm NOx , 400～1000ppm NH 3 , 3%～5%O 2 , 100～500ppm SO 2 , 10000h -1 ～40000h -1 space velocity, 250～350℃, the denitrification efficiency can reach More than 80%.
所述的金属有机骨架材料为MIL-100（Fe）、MIL-53（Fe）或ZIF-100（Co）。The metal organic framework material is MIL-100 (Fe), MIL-53 (Fe) or ZIF-100 (Co).
本发明利用上述的MOFs材料作为脱硝催化剂，是基于该类材料中含有大量且分散有序的金属活性位点，在SCR反应过程中可作为酸性位点有效的吸附NH3，促进NOx的还原。在SO2存在下，因MOFs催化剂具有大的比表面积，三维通透的孔道结构，因而可有效的延缓硫酸盐沉积所导致的孔道堵塞、金属活性位点覆盖的问题，从而可实现在含硫烟气中高效的催化还原NOx。The present invention uses the above-mentioned MOFs material as a denitration catalyst, based on the fact that this type of material contains a large number of dispersed and orderly metal active sites, which can be used as acidic sites to effectively adsorb NH 3 during the SCR reaction process and promote the reduction of NO x . In the presence of SO 2 , because the MOFs catalyst has a large specific surface area and a three-dimensional transparent pore structure, it can effectively delay the problems of pore blockage and metal active site coverage caused by sulfate deposition, so that it can be realized in sulfur-containing Efficient catalytic reduction of NO x in flue gas.
具体实施方式Detailed ways
下面通过实施例对本发明做进一步说明。The present invention will be further described below by embodiment.
本发明应用的MOFs催化剂包括MIL-100（Fe）、MIL-53（Fe）以及ZIF-100（Co）三种材料，通过水热合成的制备方法得到的材料经压片、研磨、过筛等过程，得到40～100目的催化剂置于固定床反应器中，在不同的模拟烟气条件下，评价催化剂的活性。The MOFs catalyst used in the present invention includes three materials: MIL-100 (Fe), MIL-53 (Fe) and ZIF-100 (Co). The materials obtained by the preparation method of hydrothermal synthesis are pressed into tablets, ground, sieved, etc. In the process, 40-100 mesh catalysts were obtained and placed in a fixed-bed reactor, and the activity of the catalyst was evaluated under different simulated flue gas conditions.
实施例1，将MIL-100（Fe）催化剂装填于固定床反应器内，经实验研究表明，在模拟烟气条件下，空速保持在30000h-1，NOx=NH3=1000ppm，4%O2，在270℃时，脱硝活性可以达到90%。Example 1, the MIL-100 (Fe) catalyst was packed in a fixed bed reactor. Experimental research showed that under simulated flue gas conditions, the space velocity was maintained at 30000h -1 , NO x =NH 3 =1000ppm, 4% O 2 , at 270°C, the denitrification activity can reach 90%.
实施例2，将MIL-53（Fe）催化剂装填于固定床反应器内，在模拟烟气条件下，空速保持在35000h-1，NOx=NH3=600ppm，5%O2，通过实验研究表明，在275℃时，脱硝活性可以达到80%以上。Example 2, the MIL-53 (Fe) catalyst was packed in a fixed bed reactor, under simulated flue gas conditions, the space velocity was maintained at 35000h -1 , NO x =NH 3 =600ppm, 5%O 2 , through the experiment Studies have shown that at 275°C, the denitrification activity can reach more than 80%.
实施例3，将ZIF-100（Co）催化剂装填于固定床反应器内，在模拟烟气条件下，空速保持在20000h-1，NOx=NH3=400ppm，3%O2，通过实验研究表明，在285℃时，脱硝活性可以达到80%以上。Example 3, the ZIF-100 (Co) catalyst was packed in a fixed bed reactor, under simulated flue gas conditions, the space velocity was maintained at 20000h -1 , NO x =NH 3 =400ppm, 3%O 2 , through the experiment Studies have shown that at 285°C, the denitrification activity can reach more than 80%.
实施例4，将MIL-100（Fe）催化剂装填于固定床反应器内，在模拟烟气条件下，空速保持在40000h-1，NOx=NH3=800ppm，4%O2，同时通入500ppm SO2，通过实验研究表明，在275℃时，脱硝活性可以达到85%以上。Example 4, the MIL-100 (Fe) catalyst was packed in a fixed-bed reactor, under simulated flue gas conditions, the space velocity was maintained at 40000h -1 , NO x =NH 3 =800ppm, 4%O 2 , and at the same time Adding 500ppm SO 2 , experimental research shows that at 275°C, the denitrification activity can reach more than 85%.
实施例5，将MIL-53（Fe）催化剂装填于固定床反应器内，在模拟烟气条件下，空速保持在40000h-1，NOx=NH3=500ppm，3%O2，同时通入200ppm SO2，通过实验研究表明，在280℃时，脱硝活性可以达到80%以上。Example 5, the MIL-53 (Fe) catalyst was packed in a fixed bed reactor, under simulated flue gas conditions, the space velocity was maintained at 40000h -1 , NO x =NH 3 =500ppm, 3%O 2 , and at the same time Adding 200ppm SO 2 , the experimental research shows that the denitrification activity can reach more than 80% at 280°C.
实施例6，将ZIF-100（Co）催化剂装填于固定床反应器内，在模拟烟气条件下，空速保持在10000h-1，NOx=NH3=800ppm，4%O2，同时通入100ppmSO2，在290℃时，脱硝活性可达到80%以上。Example 6, the ZIF-100 (Co) catalyst was packed in a fixed-bed reactor, under simulated flue gas conditions, the space velocity was maintained at 10000h -1 , NO x =NH 3 =800ppm, 4%O 2 , and at the same time Adding 100ppmSO 2 , at 290℃, the denitrification activity can reach more than 80%.
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| CN103752168A (en) * | 2014-01-10 | 2014-04-30 | 大连理工大学 | Application method for MIL-100(Fe) catalyst in NH3-SCR (Selective Catalytic Reduction) reaction |
| WO2017216012A1 (en) | 2016-06-13 | 2017-12-21 | Basf Se | CATALYST COMPOSITE AND USE THEREOF IN THE SELECTIVE CATALYTIC REDUCTION OF NOx |
| CN106345523B (en) * | 2016-09-18 | 2018-09-14 | 华南理工大学 | A kind of low-temperature denitration catalyst and preparation method thereof based on carbonization MOFs |
| CN106391117A (en) * | 2016-09-22 | 2017-02-15 | 山东理工大学 | Method for removing mercury in flue gas by means of porous metal and organic framework material catalyst |
| CN106622380B (en) * | 2016-12-27 | 2019-02-22 | 五邑大学 | A kind of denitration catalyst and its preparation method and application |
| CN107086313B (en) * | 2017-05-24 | 2019-11-15 | 北京化工大学 | A kind of iron, cobalt, nitrogen co-doped carbon catalyst and its preparation method and application |
| CN107185593A (en) * | 2017-06-05 | 2017-09-22 | 上海电力学院 | A kind of SCR denitration of resistant to potassium poisoning and preparation method thereof |
| CN108704472A (en) * | 2018-05-28 | 2018-10-26 | 上海大学 | The method of metal-organic framework polymer treatment nitrogen oxides and volatile organic contaminant |
| CN110787840B (en) * | 2019-11-06 | 2022-10-14 | 中国科学院过程工程研究所 | Bimetallic MOFs catalyst and preparation method and application thereof |
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