CN101259408A - Catalyst for removing flue gas NOx under low temperature and preparation and application - Google Patents
Catalyst for removing flue gas NOx under low temperature and preparation and application Download PDFInfo
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- CN101259408A CN101259408A CNA2008100548311A CN200810054831A CN101259408A CN 101259408 A CN101259408 A CN 101259408A CN A2008100548311 A CNA2008100548311 A CN A2008100548311A CN 200810054831 A CN200810054831 A CN 200810054831A CN 101259408 A CN101259408 A CN 101259408A
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Abstract
The invention relates to a catalyst used for removing flue gas NOx at low temperature. The weight percentage of each component is: 90.0 to 99.0 percent of active carbon fiber and 0.1 to 10.0 percent of V2O5. The active carbon fiber is dipped into a mixed solution prepared by oxalic acid and ammonium metavanadate which contains V2O5 and has a concentration of 0.000088735 to 0.0088735g/ml, then is stood for 2 to 5h under the room temperature, dried for 2 to 12h under a temperature of 40 to 60 DEG C, dried for 2 to 6h under a temperature of 100 to 120 DEG C, then is calcined for 2 to 8h in an argon atmosphere at 400 to 500 DEG C and is calcined for 2 to 5h in air of 200 to 260 DEG C to obtain the catalyst. The invention is simple to be operated, has excellent poisoning capacities of H2O resistance and SO2 resistance and improves the activity of selectively catalyzing and reducing the NOx.
Description
Affiliated field
The invention belongs to a kind of catalyst and preparation method and application of removing flue gas NOx under low temperature, is at H specifically
2O and SO
2During coexistence, the reduction of low temperature selective catalysis removes catalyst and the preparation method and application of flue gas NOx.
Background technology
Coal is the main energy sources of China, expects the year two thousand fifty will account for more than 50% of primary energy.At present the mode of utilizing of coal mainly is burning, and Coal-fired capacity accounts for the about 80% of total flow, yet has coal-firedly also produced a large amount of pollutants when providing energy for China, such as the SO more than 80% in the atmosphere
2, 60% above NO
xDeng.The atmosphere pollution serious harm ecological environment of coal smoke type influences the healthy and economic sustainable development of people, therefore controls coal-fired SO
2And NO
xDischarging be the most important thing that China builds a harmonious society.
Mainly be divided into burning neutralization burning back control two big classes for the emission control of NOx, control in the burning adopts the low nitrogen burning technology, but its removal efficiency is usually less than 50%, needs and the burning back is controlled and is used in combination.Burning back control technology be flue gas NOx to remove technology be the most effective denitration means, obtained paying close attention to widely and using, wherein most widely used is with NH
3For SCR (SCR) technology of reducing agent, promptly utilize reducing agent NH
3NOx is reduced to harmless N
2And H
2O.Bosch etc. (Catal.Today, 1988,2, the key of 369-531) pointing out the SCR technology is the catalyst of efficient stable, V
2O
5-WO
3/ TiO
2Catalyst is preferably present and most widely used industrial SCR catalyst, and the denitration rate is usually above 90%, and is stable.But still there are some problems in this type of catalyst: the one, and catalyst carrier Detitanium-ore-type TiO
2Easily crystal transfer takes place and make the preparation condition harshness, cost is higher; The 2nd, the denitration operating temperature must be higher than 350 ℃.The high-temperature operation of catalyst requires the SCR bed must be arranged in before the cleaner, and this is so that exist some problems in the configuration of whole flue gas purification system, and the high grey high-sulfur in the flue gas all can have a great impact for activity and life-span of catalyst.Therefore, research and development has the active SCR catalyst of low temperature (120-250 ℃) and not only can reduce the obstruction of flue dust and poison, and easier and existing steam generator system coupling, have important economy and practical significance, and obtain many research workers' attention in the world.
(J.Catal., 2000,195, the 268-278) V of exploitation such as a large amount of low-temperature SCR catalysts, especially Zhu been have have been researched and developed at present both at home and abroad
2O
5/ AC catalyst has high NO_x removal activity, and V
2O
5Content is being lower than 5wt%, temperature more than 180 ℃ the time, SO
2To V
2O
5/ AC catalyst has facilitation.But (Applied Catalytic B:Enviromental 2002,39 361-368) further discovers, at H Huang etc.
2O and SO
2During coexistence, this catalyst removal NOx is active to be reduced.People such as Shen Baixiong (clean coal technology, 2007,13 (1), 32-35) utilize NACF to be different from the characteristic of active carbon, researched and developed HNO
3The ACF load C eO of oxidation processes modification
2, catalyst such as MnOx; (Applied Catalytic B:Enviromental 2003,41 323-338) removes the NOx reaction with ACF for supported carrier MnOx has carried out low temperature to people such as Gregorio equally.But these people's research does not all relate to H
2O and SO
2How to affect the low temperature NO_x removal activity of catalyst during coexistence, namely do not develop at H
2O and SO
2During coexistence, has higher NO_x removal catalyst.
Summary of the invention
The object of the invention provides a kind ofly to be had at H
2O and SO
2When existing, have higher catalyst and the application thereof that removes flue gas NOx.
Catalyst of the present invention is with V
2O
5Be active component, NACF (ACF) is carrier, and each weight percentages of components is: ACF 90.0%～99.9%, V
2O
50.1%～10.0%.
The preparation method of catalyst of the present invention is immersed in ACF by the catalyst composition to contain V
2O
5Concentration is in the oxalic acid of 0.000088735-0.0088735g/ml and the mixed solution that ammonium metavanadate is made into, room temperature is placed 2-5h then, 40-60 ℃ of dry 2-12h, 100-120 ℃ of dry 2-6h, under 400-500 ℃ of argon gas atmosphere, calcine 2-5h in calcining 2-8h and 200-260 ℃ of air then, obtain the catalyst of required loading.
Application of Catalyst method of the present invention is that this catalyst is packed in the fixed bed reactors, is 120～250 ℃ in reaction temperature, and reaction pressure is a normal pressure, and reaction velocity is 500h
-1～10000h
-1Under the condition, to H
2O and SO
2There is SO
2Concentration is lower than 400ppm, H
2O concentration is lower than 3% flue gas and removes NOx.
The present invention has following advantage:
1.ACF have bigger specific area and abundant micro content, increased contact area and the effective time of multiphase gas-solid reaction, active component V
2O
5Better be scattered in the surface of catalyst, thereby improved the activity of selective catalysis reducing NOx.
2. equi-volume impregnating has simple to operately, can load on the activity of such catalysts component on the carrier of arbitrary shape easily, and dispersed catalyst than the coprecipitation preparation is more even, and active component easy-sintering is not reunited during high-temperature calcination.
3.V
2O
5Catalyst has good anti-H
2O and SO
2The ability that poisons, mainly be V after the high-temperature calcination
2O
5Form be dispersed in the surface of catalyst.
In a word, the V of the present invention's preparation
2O
5/ ACF catalyst has reduced the operating temperature of NO_x removal, and (120-250 ℃) is issued to higher denitration activity at a lower temperature.And most importantly this catalyst can be at H
2O and SO
2During coexistence, still has higher NOx removal efficiency (being higher than 60%).Selecting in addition ACF is carrier, also is a bright spot.Because the ACF specific area is big, high adsorption capacity, the form variation is so that arrange more flexible; The surface is abundant contains oxygen, and nitrogen-containing functional group can make active component and carrier have better synergy, thereby greatly improves denitration activity.So patent of the present invention was compared with former technology, had certain advantage.
The specific embodiment
Embodiment 1
1.488g viscose-based active carbon fiber is immersed in the V of 17ml
2O
5Concentration is in ammonium metavanadate/oxalic acid aqueous solution of 0.0004576g/ml, and room temperature is placed 3h then, 50 ℃ of dry 5h, and 110 ℃ of dry 5h calcine 4h in calcining 8h and 250 ℃ of air then successively under 500 ℃ of argon gas atmosphere, namely obtain mass percent and be 0.5% V
2O
5/ ACF catalyst.This catalyst is packed in the fixed bed reactors, and reaction temperature is controlled at 180 ℃, feeds the simulated flue gas NO600ppm under the normal pressure, NH
3600ppm, O
25%, balance gas N
2, reaction velocity is controlled at 1000h
-1The conversion ratio of NO is 52% during stable state.The SO that adds 300ppm simultaneously
2, 2%H
2Behind the O, the NO conversion ratio continues to be stabilized in 83%.
Embodiment 2
1.488g viscose-based active carbon fiber is immersed in the V of 17ml
2O
5Concentration is in ammonium metavanadate/oxalic acid aqueous solution of 0.004576g/ml, and room temperature is placed 3h then, 50 ℃ of dry 12h, and 110 ℃ of dry 6h namely get mass percent and are 5% V
2O
5/ ACF catalyst, this catalyst is without calcining 5h in calcining 8h and 250 ℃ of air under 500 ℃ of argon gas atmosphere, and in the fixed bed reactors of directly packing into, reaction temperature is controlled at 180 ℃, passes into the simulated flue gas NO600ppm under the normal pressure, NH
3600ppm, O
25%, Balance Air N
2, reaction velocity is controlled at 2000h
-1The conversion ratio of NO is 60% during stable state.The SO that adds 50ppm simultaneously
2, 1.2%H
2Behind the O, the NO conversion ratio continues to be stabilized in 70%.
Embodiment 3
1.488g viscose-based active carbon fiber is immersed in the V of 17ml
2O
5Concentration is in ammonium metavanadate/oxalic acid aqueous solution of 0.004576g/ml, and room temperature is placed 3h then, 50 ℃ of dry 8h, and 110 ℃ of dry 6h calcine 5h in calcining 5h and 250 ℃ of air then successively under 500 ℃ of argon gas atmosphere, namely get mass percent and be 5% V
2O
5/ ACF catalyst.This catalyst is packed in the fixed bed reactors, and reaction temperature is controlled at 180 ℃, feeds the simulated flue gas NO600ppm under the normal pressure, NH
3600ppm, O
25%, balance gas N
2, total gas flow rate is 400ml/min, reaction velocity is controlled at 2000h
-1, the conversion ratio of NO is 98% during stable state, adds the SO of 400ppm simultaneously
2, 3%H
2Behind the O, the NO conversion ratio continues to be stabilized in 80%.
Embodiment 4
1.488g viscose-based active carbon fiber is immersed in the V of 17ml
2O
5Concentration is in ammonium metavanadate/oxalic acid aqueous solution of 0.001831g/ml, and room temperature is placed 3h then, 50 ℃ of dry 4h, and 110 ℃ of dry 6h calcine 5h in calcining 8h and 250 ℃ of air then successively under 500 ℃ of argon gas atmosphere, namely get mass percent and be 2% V
2O
5/ ACF catalyst.This catalyst is packed in the fixed bed reactors, and reaction temperature is controlled at 120 ℃, feeds the simulated flue gas NO600ppm under the normal pressure, NH
3600ppm, O
25%, balance gas N
2, reaction velocity is controlled at 800h
-1, the conversion ratio of NO is 75% during stable state.Feed the SO of 200ppm simultaneously
2, 2%H
2Behind the O, the NO conversion ratio continues to be stabilized in 68%.
Embodiment 5
1.488g viscose-based active carbon fiber is immersed in the V of 17ml
2O
5Concentration is in ammonium metavanadate/oxalic acid aqueous solution of 0.0004576g/ml, and room temperature is placed 3h then, 50 ℃ of dry 2h, and 110 ℃ of dry 6h calcine 4h in calcining 8h and 250 ℃ of air then successively under 500 ℃ of argon gas atmosphere, namely obtain mass percent and be 0.5% V
2O
5/ ACF catalyst.This catalyst is packed in the fixed bed reactors, and reaction temperature is controlled at 200 ℃, feeds the simulated flue gas NO600ppm under the normal pressure, NH
3600ppm, O
25%, balance gas N
2, reaction velocity is controlled at 2000h
-1, the conversion ratio of NO is 51% during stable state.Feed the SO of 300ppm simultaneously
2, 3%H
2Behind the O, the NO conversion ratio continues to be stabilized in 75%.
Embodiment 6
1.488g viscose-based active carbon fiber is immersed in the V of 17ml
2O
5Concentration is in ammonium metavanadate/oxalic acid aqueous solution of 0.004576g/ml, and room temperature is placed 3h then, 50 ℃ of dry 7h, and 110 ℃ of dry 8h promptly get mass percent and are 5% V
2O
5/ ACF catalyst is calcined 5h in calcining 5h and 250 ℃ of air then successively under 500 ℃ of argon gas atmosphere, in the fixed bed reactors of directly packing into, reaction temperature is controlled at 150 ℃, feeds the simulated flue gas NO600ppm under the normal pressure, NH
3600ppm, O
25%, balance gas N
2, reaction velocity is controlled at 2000h
-1, the conversion ratio of NO is 96% during stable state.Feed the SO of 150ppm simultaneously
2, 2.2%H
2Behind the O, the NO conversion ratio continues to be stabilized in 84%.
Embodiment 7
1.488g viscose-based active carbon fiber is immersed in the V of 17ml
2O
5Concentration is in ammonium metavanadate/oxalic acid aqueous solution of 0.008238g/ml, and room temperature is placed 3h then, 50 ℃ of dry 12h, and 110 ℃ of dry 5h calcine 5h in calcining 5h and 250 ℃ of air then successively under 500 ℃ of argon gas atmosphere, namely obtain mass percent and be 8% V
2O
5/ ACF catalyst.This catalyst is packed in the fixed bed reactors, and reaction temperature is controlled at 200 ℃, feeds the simulated flue gas NO600ppm under the normal pressure, NH
3600ppm, O
25%, balance gas N
2, reaction velocity is controlled at 8000h
-1, the conversion ratio of NO is 97% during stable state.Feed the SO of 350ppm simultaneously
2, 2.8%H
2Behind the O, the NO conversion ratio continues to be stabilized in 82%.
Embodiment 8
1.488g viscose-based active carbon fiber is immersed in the V of 17ml
2O
5Concentration is in ammonium metavanadate/oxalic acid aqueous solution of 0.008238g/ml, and room temperature is placed 3h then, 50 ℃ of dry 12h, and 110 ℃ of dry 5h calcine 5h in calcining 5h and 250 ℃ of air then successively under 500 ℃ of argon gas atmosphere, namely obtain mass percent and be 8% V
2O
5/ ACF catalyst.This catalyst is packed in the fixed bed reactors, and reaction temperature is controlled at 250 ℃, feeds the simulated flue gas NO600ppm under the normal pressure, NH
3600ppm, O
25%, balance gas N
2, reaction velocity is controlled at 9500h
-1, the conversion ratio of NO is 98% during stable state.Feed the SO of 100ppm simultaneously
2, 2%H
2Behind the O, the NO conversion ratio continues to be stabilized in 90%.
Claims (3)
1, a kind of catalyst for removing flue gas NOx under low temperature is characterized in that catalyst is with V
2O
5Be active component, NACF is carrier, and each weight percentages of components is: NACF 90.0%～99.9%, V
2O
50.1%～10.0%.
2, a kind of Preparation of catalysts method that is used for removing flue gas NOx under low temperature as claimed in claim 1 is characterized in that comprising the steps:
Consist of NACF 90.0%～99.9%, V by catalyst
2O
50.1%～10.0%.NACF is immersed in contains V
2O
5Concentration is in the oxalic acid of 0.000088735-0.0088735g/ml and the mixed solution that ammonium metavanadate is made into, room temperature is placed 2-5h then, 40-60 ℃ of dry 2-12h, 100-120 ℃ of dry 2-6h, under 400-500 ℃ of argon gas atmosphere, calcine 2-5h in calcining 2-8h and 200-260 ℃ of air then, obtain the catalyst of required loading.
3, a kind of Application of Catalyst that is used for removing flue gas NOx under low temperature as claimed in claim 1 is characterized in that it being that catalyst is packed in the fixed bed reactors, is 120～250 ℃ in reaction temperature, and reaction pressure is a normal pressure, and reaction velocity is 500h
-1～10000h
-1Under the condition, to H
2O and SO
2There is SO
2Concentration is lower than 400ppm, H
2O concentration is lower than 3% flue gas and removes NOx.
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|---|---|---|---|
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|---|---|---|---|
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| CN104069852A (en) * | 2014-07-02 | 2014-10-01 | 宋华 | Low-temperature sulphur-resisting denitration catalyst and preparation method thereof |
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| CN113198444A (en) * | 2021-05-12 | 2021-08-03 | 昆明理工大学 | Low-temperature CO reduction denitration V/AC catalyst and preparation method and application thereof |
| CN113769534A (en) * | 2021-10-18 | 2021-12-10 | 美埃(中国)环境科技股份有限公司 | Modified active carbon method for removing nitric oxide and nitrogen dioxide gas in air |
| CN113769534B (en) * | 2021-10-18 | 2023-04-25 | 美埃(中国)环境科技股份有限公司 | Activated carbon modification method for removing nitric oxide and nitrogen dioxide gas in air |
| CN114471746A (en) * | 2022-02-15 | 2022-05-13 | 中国科学院山西煤炭化学研究所 | SCR denitration catalyst regeneration method |
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