CN102553572A - Selective catalytic reduction (SCR) catalyst of wide active temperature window and preparation method thereof - Google Patents
Selective catalytic reduction (SCR) catalyst of wide active temperature window and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000010531 catalytic reduction reaction Methods 0.000 title description 3
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 13
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000000694 effects Effects 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- YOSLGHBNHHKHST-UHFFFAOYSA-N cerium manganese Chemical compound [Mn].[Mn].[Mn].[Mn].[Mn].[Ce] YOSLGHBNHHKHST-UHFFFAOYSA-N 0.000 claims description 8
- 150000000703 Cerium Chemical class 0.000 claims description 7
- 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 7
- 150000002696 manganese Chemical class 0.000 claims description 7
- 239000011572 manganese Substances 0.000 claims description 6
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229940071125 manganese acetate Drugs 0.000 claims description 5
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 5
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 27
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 239000007789 gas Substances 0.000 abstract description 7
- 238000000746 purification Methods 0.000 abstract description 3
- 239000004408 titanium dioxide Substances 0.000 abstract description 2
- LQWKWJWJCDXKLK-UHFFFAOYSA-N cerium(3+) manganese(2+) oxygen(2-) Chemical compound [O--].[Mn++].[Ce+3] LQWKWJWJCDXKLK-UHFFFAOYSA-N 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 231100000331 toxic Toxicity 0.000 abstract 1
- 230000002588 toxic effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 18
- 238000000227 grinding Methods 0.000 description 7
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000003245 coal Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- BZDIAFGKSAYYFC-UHFFFAOYSA-N manganese;hydrate Chemical compound O.[Mn] BZDIAFGKSAYYFC-UHFFFAOYSA-N 0.000 description 3
- 150000002823 nitrates Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 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
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 208000036142 Viral infection Diseases 0.000 description 1
- HTBAHYGLEFPCLK-UHFFFAOYSA-N [Ti].[Ce].[Mn] Chemical compound [Ti].[Ce].[Mn] HTBAHYGLEFPCLK-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000000680 avirulence Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
发明提供了一种宽活性温度窗口的SCR催化剂，用于固定源和移动源脱硝。本发明还提供了该催化剂的制备方法。该催化剂以锐钛矿型二氧化钛为载体，氧化铈和氧化锰为活性组分，氧化铈含量为催化剂质量百分含量的1-20％，氧化锰含量为催化剂质量百分含量的1-20％。本发明催化剂以锐钛矿型二氧化钛为载体，以铈锰氧化物为活性组分，不采用有毒性的活性组分V2O5，减轻了对环境的污染，具备了在较宽活性温度窗口内高效催化净化氮氧化物的性能，适应更严格的排放法规要求，在200-500℃范围内，氮氧化物的脱除率达到90％以上。该催化剂可用于净化处理固定源和移动源排放的废气中的氮氧化物，如柴油车尾气NOx处理以及固定源燃煤电厂的脱硝装置。
The invention provides an SCR catalyst with a wide activity temperature window, which is used for denitrification of stationary sources and mobile sources. The invention also provides a preparation method of the catalyst. The catalyst uses anatase titanium dioxide as a carrier, cerium oxide and manganese oxide as active components, the content of cerium oxide is 1-20% of the mass percentage of the catalyst, and the content of manganese oxide is 1-20% of the mass percentage of the catalyst . The catalyst of the present invention uses anatase-type titanium dioxide as a carrier, cerium manganese oxide as an active component, does not use toxic active component V 2 O 5 , reduces environmental pollution, and has a wide active temperature window The performance of high-efficiency catalytic purification of nitrogen oxides in the interior meets the requirements of stricter emission regulations. In the range of 200-500 ° C, the removal rate of nitrogen oxides reaches more than 90%. The catalyst can be used to purify and treat nitrogen oxides in exhaust gas emitted by stationary sources and mobile sources, such as diesel vehicle exhaust NOx treatment and denitrification devices of stationary source coal-fired power plants.
Description
Technical field
The present invention relates to catalyst technical field, relate in particular to a kind of SCR Catalysts and its preparation method of wide active temperature windows, specifically is that the cerium manganese titanium of wide active temperature windows is the SCR catalyst.
Technical background
Along with the increase day by day of development of modern industry and automobile quantity, the human NOx that in atmosphere, discharges is more and more, and NOx pollutes has become a serious day by day global problem.NOx comprises NO, NO as one of atmosphere major pollutants
2, N
2O, N
2O
3And N
2O
4Deng, mainly with NO and NO
2Form exist, wherein NO accounts for 95% of NOx total amount.The whole world enters the combustion process that derives from fossil fuels such as coal, oil, natural gas more than 90% among the NOx of atmosphere every year.It can cause greenhouse effects, depletion of the ozone layer and acid rain to form.
The NOx emission control is divided into stationary source denitrating flue gas and moving source NOx emission control.China is maximum in the world coal production and consumption state, also is that a few is one of country of main energy sources (coal accounts for more than 70% of primary energy) with coal in the world.Expectation is in 50 years from now on, and China is that main energy resource structure marked change can not take place with coal.The primary energy structures shape of this uniqueness coal-fired thermal power generation at the medium-term and long-term dominate of China power industry, this has just determined the coal-burning power plant is that main stationary source NOx emission control is still the main aspect that China administers NOx.In addition, the fast development of China's automotive industry has in recent years also brought the tail gas pollution of motor-driven vehicle problem that becomes increasingly conspicuous, and diesel vehicle NOx emission control also will be one of Future in China NOx emission control key content.
At present, (Selective Catalytic Reduction SCR) is regarded as NOx catalytic purification one of effective method the most to the SCR technology.Its principle is under the effect of catalyst, through adding the N that appropriate reductant optionally is reduced to NOx nonhazardous
2, realize the NOx catalytic eliminating, wherein the SCR of ammonia is to use gas denitrifying technology the most widely, and is regarded as and is hopeful to be applied to one of large diesel engine tail gas NOx purification techniques most.
The core of SCR technology is the catalyst that exploitation has high activity, thermally-stabilised and good durability, and being studied maximum is noble metal, metal oxide and molecular sieve catalyst, wherein, and with V
2O
5For the catalytic component based on vanadium of active component demonstrates catalytic performance preferably, and successfully drop into commercial application, this catalyst has advantages of high catalytic activity at 300-400 ℃, and has anti-preferably H
2O and SO
2Poisoning performance.But also there is certain problem in this catalyst: the one, and temperature window is narrow, only in 300-400 ℃ of scope, has greater activity, and low temperature active is poor; The 2nd, high-temperature selective and poor heat stability, accessory substance N during high temperature
2O growing amount showed increased; The 3rd, a large amount of uses of vanadium are all unfavorable to health and environment.
Summary of the invention
In order to overcome the problems referred to above that exist in the prior art; The SCR catalyst that the purpose of this invention is to provide a kind of wide active temperature windows; Be used for fixing source and moving source denitration; Have the wide characteristics of avirulence and active temperature windows, it can realize that efficient catalytic removes nitrogen oxide in 200-500 ℃ of temperature range.
Another object of the present invention provides above-mentioned wide active temperature windows SCR Preparation of catalysts method.
The SCR catalyst of wide active temperature windows of the present invention; With the anatase titanium dioxide is that carrier, cerium oxide and manganese oxide are active component; Wherein cerium oxide and manganese oxide account for the 1-20% of catalyst quality respectively, and all the other 60-98% are the carrier anatase titanium dioxide.
Said cerium oxide adds with the form of the water-soluble salt of cerium, and manganese oxide adds with the water-soluble salt form of manganese.Preferably: said cerium oxide adds with the form of cerous nitrate or cerous acetate, and said manganese oxide adds with the form of manganese nitrate or manganese acetate.
Preparation of catalysts method of the present invention is carried out according to the following steps:
1) respectively cerium salt and manganese salt are dissolved in the deionized water, wherein cerium salt calculates the 1-20% that accounts for the catalyst gross mass with cerium oxide, and manganese salt calculates the 1-20% that accounts for the catalyst gross mass with manganese oxide, then both is mixed;
2) with Detitanium-ore-type TiO
2Powder impregnation is in above-mentioned cerium manganese mixed solution, and it accounts for the 60-98% of catalyst gross mass;
3) stir 0.5-2h, 70-90 ℃ is stirred evaporate to dryness down then, places 100 ℃ of baking ovens oven dry to spend the night, roasting 3-5h in the 400-600 ℃ of air, after the grinding the SCR catalyst of wide active temperature windows.
Described cerium salt is selected from cerous nitrate or cerous acetate, and manganese salt is selected from manganese nitrate or manganese acetate.
Catalyst of the present invention is carrier with the anatase titanium dioxide, is active component with the cerium Mn oxide, does not adopt virose active component V
2O
5, alleviated pollution to environment, possessed the performance of efficient catalytic purifying nitrogen oxide in than wide active temperature windows, adapt to stricter emission regulation demands, in 200-500 ℃ of scope, removal efficiency of nitrogen oxides reaches more than 90%.This catalyst can be used for the nitrogen oxide in purified treatment stationary source and the moving source exhaust gas discharged, like the denitrification apparatus of exhaust gas from diesel vehicle NOx processing and stationary source coal-burning power plant.
Description of drawings
Fig. 1 adopts catalyst of the present invention that the typical component mist is carried out catalytic reduction graph of a relation between removal of nitrogen oxide rate and the temperature when handling.
The specific embodiment
Below in conjunction with embodiment the present invention is further specified:
The titanium dioxide that the present invention uses is homemade anatase titanium dioxide.The cerium salt that uses is cerous nitrate or cerous acetate, and the manganese salt that uses is manganese nitrate or manganese acetate.
Embodiment one
2.5227g six water cerous nitrates are dissolved in the 500ml deionized water, again 2.8191g four water acetic acid manganese are dissolved in the 500ml deionized water, two parts of solution stirring are mixed obtain solution A then.Take by weighing the 98g anatase titanium dioxide then and impregnated in the solution A, stir 2h.Stir down evaporates to dryness at 80 ℃ then, and in 100 ℃ of baking ovens dried overnight.500 ℃ of roasting 5h in Muffle furnace then, after the grinding cerium manganese content is respectively the SCR catalyst of 1% wide active temperature windows.
Embodiment two
25.2272g six water cerous nitrates are dissolved in the 500ml deionized water, again 28.1905g four water acetic acid manganese are dissolved in the 500ml deionized water, two parts of solution stirring are mixed obtain solution A then.Take by weighing the 80g anatase titanium dioxide then and impregnated in the solution A, stir 2h.Stir down evaporates to dryness at 80 ℃ then, and in 100 ℃ of baking ovens dried overnight.500 ℃ of roasting 5h in Muffle furnace then, after the grinding cerium manganese content is respectively the SCR catalyst of 10% wide active temperature windows.
Embodiment three
50.4544g six water cerous nitrates are dissolved in the 500ml deionized water, again 56.3810g four water acetic acid manganese are dissolved in the 500ml deionized water, two parts of solution stirring are mixed obtain solution A then.Take by weighing the 60g anatase titanium dioxide then and impregnated in the solution A, stir 2h.Stir down evaporates to dryness at 80 ℃ then, and in 100 ℃ of baking ovens dried overnight.500 ℃ of roasting 5h in Muffle furnace then, after the grinding cerium manganese content is respectively the SCR catalyst of 20% wide active temperature windows.
Embodiment four
2.3652g five water acetic acid ceriums are dissolved in the 500ml deionized water, again 2.8871g four water manganese nitrates are dissolved in the 500ml deionized water, two parts of solution stirring are mixed obtain solution A then.Take by weighing the 98g anatase titanium dioxide then and impregnated in the solution A, stir 2h.Stir down evaporates to dryness at 80 ℃ then, and in 100 ℃ of baking ovens dried overnight.500 ℃ of roasting 5h in Muffle furnace then, after the grinding cerium manganese content is respectively the SCR catalyst of 1% wide active temperature windows.
Embodiment five
23.6516g five water acetic acid ceriums are dissolved in the 500ml deionized water, again 28.8714 4 water manganese nitrates are dissolved in the 500ml deionized water, two parts of solution stirring are mixed obtain solution A then.Take by weighing the 80g anatase titanium dioxide then and impregnated in the solution A, stir 2h.Stir down evaporates to dryness at 80 ℃ then, and in 100 ℃ of baking ovens dried overnight.500 ℃ of roasting 5h in Muffle furnace then, after the grinding cerium manganese content is respectively the SCR catalyst of 10% wide active temperature windows.
Embodiment six
47.3032g five water acetic acid ceriums are dissolved in the 500ml deionized water, again 57.7428g four water manganese nitrates are dissolved in the 500ml deionized water, two parts of solution stirring are mixed obtain solution A then.Take by weighing the 60g anatase titanium dioxide then and impregnated in the solution A, stir 2h.Stir down evaporates to dryness at 80 ℃ then, and in 100 ℃ of baking ovens dried overnight.500 ℃ of roasting 5h in Muffle furnace then, after the grinding cerium manganese content is respectively the SCR catalyst of 20% wide active temperature windows.
Catalytic activity detects
The 1ml catalyst sample of in fixed bed reactors, packing into, and reactor put into heating furnace; Feed the NOx of 1000ppm, the NH of 1000ppm
3And 5%O
2, nitrogen is as balance gas, and air speed is 48000h
-1, purge under the room temperature and stablize 1h.Be warming up to the design temperature point, behind the stable reaction 1h, through flue gas analyzer, gather concentration data, and calculate at the NOx of this temperature spot conversion ratio.In 150-500 ℃ of (50 ℃ are the interval) temperature range, catalyst is carried out activity rating.The removal of nitrogen oxide rate of typical catalyst sample and the relation of temperature are as shown in Figure 1.As can beappreciated from fig. 1, in 250-450 ℃ of temperature range, the removal efficiency of NOx can reach more than 90%, and 300-400 ℃ temperature window than traditional catalyst has lifting by a relatively large margin, can better satisfy the needs of practical application.
Claims (5)
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Cited By (11)
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| CN102941083A (en) * | 2012-11-08 | 2013-02-27 | 环境保护部华南环境科学研究所 | Medium/low-temperature core-shell denitration catalyst and preparation method and application thereof |
| CN103638939A (en) * | 2013-11-06 | 2014-03-19 | 南京工业大学 | Composite metal sulfate series flue gas denitration catalyst and preparation method thereof |
| CN104785245A (en) * | 2015-04-03 | 2015-07-22 | 中国建筑材料科学研究总院 | Denitration catalyst, preparation method thereof as well as flue gas denitration method |
| CN105170140A (en) * | 2015-10-15 | 2015-12-23 | 天津中科先进技术研究院有限公司 | High-efficient SCR (Selective Catalytic Reduction) catalyst applicable to denitration reaction and preparation method of catalyst |
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| CN105664924A (en) * | 2016-01-13 | 2016-06-15 | 南京大学 | Denitration catalyst employing shape effect for enhancing low temperature activity, preparation method and application thereof |
| CN106111123A (en) * | 2016-06-19 | 2016-11-16 | 河北工业大学 | A kind of support type manganio composite oxides selective denitrification catalyst containing tourmaline |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102941083B (en) * | 2012-11-08 | 2015-02-18 | 环境保护部华南环境科学研究所 | Medium/low-temperature core-shell denitration catalyst and preparation method and application thereof |
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| CN103638939B (en) * | 2013-11-06 | 2016-04-13 | 南京工业大学 | Composite metal sulfate series flue gas denitration catalyst and preparation method thereof |
| CN103638939A (en) * | 2013-11-06 | 2014-03-19 | 南京工业大学 | Composite metal sulfate series flue gas denitration catalyst and preparation method thereof |
| CN104785245A (en) * | 2015-04-03 | 2015-07-22 | 中国建筑材料科学研究总院 | Denitration catalyst, preparation method thereof as well as flue gas denitration method |
| CN105170140A (en) * | 2015-10-15 | 2015-12-23 | 天津中科先进技术研究院有限公司 | High-efficient SCR (Selective Catalytic Reduction) catalyst applicable to denitration reaction and preparation method of catalyst |
| CN105363434A (en) * | 2015-11-17 | 2016-03-02 | 安徽省元琛环保科技有限公司 | Manganese based SCR catalyst for low temperature denitration and preparation method thereof |
| CN105664924A (en) * | 2016-01-13 | 2016-06-15 | 南京大学 | Denitration catalyst employing shape effect for enhancing low temperature activity, preparation method and application thereof |
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| CN109847745A (en) * | 2018-12-29 | 2019-06-07 | 安徽工业大学 | A kind of preparation method of ruthenium-based ultra-low temperature denitration catalyst |
| CN109847745B (en) * | 2018-12-29 | 2021-09-07 | 安徽工业大学 | A kind of preparation method of ruthenium-based ultra-low temperature denitration catalyst |
| CN109718767B (en) * | 2018-12-29 | 2021-09-10 | 安徽工业大学 | Ruthenium system ultralow-temperature denitration catalyst |
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Application publication date: 20120711 |