CN103736497B - The vanadia-based SCR catalysts and preparation method thereof of nitrogen oxide in efficient process diesel engine vent gas - Google Patents
The vanadia-based SCR catalysts and preparation method thereof of nitrogen oxide in efficient process diesel engine vent gas Download PDFInfo
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Abstract
The present invention relates to a kind of novel vanadia-based SCR catalysts for nitrogen oxides treatment in diesel engine vent gas and preparation method thereof, belong to catalytic reduction method purifying motor exhaust emissions technical field.It comprises the first component: be selected from barium oxide, vanadium-erbium composite oxides and vanadium-iron compound oxide; Second component is selected from one or the combination of titanium oxide, titanium-tungsten composite oxides and titanium-Si composite oxide.The present invention is applied to diesel engine vent gas after-treatment system to be coated on cordierite honeycomb ceramic as cellular catalyst form.The invention also discloses the preparation method of this catalyst, comprise and prepare the first component by the predecessor of the first component; The first component load is coated in cordierite honeycomb ceramic surface on the second component.This catalyst has efficient catalytic performance and environment friendly.
Description
Technical field
The present invention relates to a kind of novel vanadia-based SCR catalysts for nitrogen oxides treatment in diesel engine vent gas and preparation method thereof, belong to catalytic reduction method purifying motor exhaust emissions technical field.
Background technology
NOx(is NO especially) be the most difficult pollutant removed, two kinds of different strategies are removed to NOx: as far as possible the first reduce because burning waits the NOx generated, and comprises the improvement of burning pre-treatment and combustion technology.Burning pre-treatment, mainly by denitrogenation, reduces the nitrogen content in fuel, thus reduces the growing amount of NOx in combustion process; And combustion technology is intended to improve combustibility, reduce ignition temperature, thus reduce the high temperature catalytic combustion technology of NOx emission.The current countries in the world of improvement of combustion technology are also in the research and development stage, also do not enter comprehensive practical stage.The second is after generating, then manages to be eliminated.Most important method in current improvement NOx to the process of the NOx generated.
For from moving source (such as Diesel engine, in its discharging waste gas, oxygen content typically is 5 ~ 10%) NOx that distributes, its administering method mainly contains three kinds: absorption-catalytic reduction (NOxstorage-reduction:NSR) method of the HC-SCR method using hydrocarbon compound as reducing agent, NOx and with NH
3as urea (the urea)-SCR method of reducing agent.Hydrocarbon selective reduction NOx is extensively studied, because for engine, HC compound can conveniently obtain, and containing this kind of material in usual engine exhaust.But owing to riding activity and selectivity at the operational, negative effect is more than the height of the imagination.NSR method stores with first enrichment, and the mode restoring regeneration operates.The method can realize very high NOx removal efficiency (> 85%), but the outstanding problem existed is that NSR catalyst is extremely responsive to SO2, in tail gas, the SO2 of trace also can cause catalysqt deactivation, and therefore the scope of application is still only limitted to the very low countries and regions of fuel oil sulfur content.Therefore, generally to study now and what adopt is on vanadium oxide catalysts or molecular sieve catalyst, use ammonia selective reducing NOx
Catalyst much for catalytic reduction of NOx in prior art is V
2o
5/ TiO
2system.But such catalyst at high temperature (> 600 DEG C) due to TiO
2phase transformation and active component V
2o
5sintering and volatilization, poor heat stability.
Therefore, need one to may be used for reducing NOx emission in diesel engine vent gas especially, activity is high, temperature window is wide, the Novel SCR of Heat stability is good.
Summary of the invention
For existing this deficiency of vanadia-based SCR catalysts high-temperature thermal stability difference, object of the present invention aims to provide novel vanadia-based SCR catalysts of nitrogen oxide in a kind of efficient process diesel engine vent gas and preparation method thereof, improves vanadia-based SCR catalysts high-temperature behavior.
According to technical scheme provided by the invention, the vanadia-based SCR catalysts of nitrogen oxide in process diesel engine vent gas, formula rate is as follows by weight percentage: the first component 0.1% ~ 20%; Second component 80% ~ 99.9%; First component is coated in together with second component carrier cordierite honeycomb ceramic surface;
Described first component is one or its combination of barium oxide, vanadium-erbium composite oxides and vanadium-iron compound oxide; The content of the first component for benchmark, is 0.1% ~ 20% with the first component and the second component gross weight;
Described second component is one or the combination of titanium oxide, titanium-tungsten composite oxides and titanium-Si composite oxide; The content of second component for benchmark, is 80% ~ 99.9% with the first component and second component gross weight.
Described first component is selected from V
2o
5oxide, and Fe
2o
3and Er
2o
3in one or its combination.
Described second component is TiO
2, WO
3and SiO
2three kinds of composite oxides.
Described first components based on weight percentage accounts for 5% ~ 15% of the gross weight of the first component and second component.
The vanadia-based SCR catalysts of nitrogen oxide in described process diesel engine vent gas, by weight: TiO in described second component
2it is 70 ~ 90 parts; WO
3it is 5 ~ 15 parts; SiO
2it is 5 ~ 15 parts.
The preparation method of the vanadia-based SCR catalysts of nitrogen oxide in described process diesel engine vent gas, step is as follows by weight:
(1) preparation of vanadium erbium iron complexes: first the metavanadic acid ammonia of 1 ~ 5 part is added 1 ~ 20 part of deionized water and be placed in 70 ~ 90 DEG C of water-baths and dissolve, obtain solution a;
Ferric nitrate and erbium nitrate are pressed Fe
xthe form mixing of Ery, wherein Fe
xin Ery, x is the mol ratio of iron, the mol ratio of scope to be 0 ~ 1, y be erbium, and scope is 0 ~ 1, fully obtains solution b after mixing;
Solution a is fully mixed according to weight ratio 1 ~ 2:3 ~ 6 with solution b; Then service property (quality) concentration be 25% ~ 35% ammoniacal liquor above-mentioned mixed solution to be adjusted to pH be 5 ~ 9, stir 22 ~ 26h, suction filtration, obtain filter cake, after Washing of Filter Cake is also precipitated again, 1 ~ 3h is dried at 100 ~ 400 DEG C, then roasting 1 ~ 3 hour at 200 ~ 500 DEG C, obtain the first component vanadium erbium iron complexes;
(2) preparation of coating slurries: get TiO
2, WO
3and SiO
2be followed successively by 70 ~ 90:5 ~ 15:5 ~ 15 according to mass ratio to mix, obtain second component mixture; First component and second component are mixed according to the ratio of 0.1% ~ 20%:80% ~ 99.9%, forms mixture;
Add deionized water, stir and obtain suspension, regulate the addition of deionized water, make mixture content in suspension be 10 ~ 50 parts, obtain suspension;
By suspension ball milling, control granularity D
90be less than 60 microns, obtain coating slurries;
(3) flood: cordierite honeycomb ceramic carrier be impregnated in coating slurries prepared by step (2), fully take out after dipping;
(4) dry: the cordierite honeycomb ceramic carrier after coating slurries in step (3) is dried 30 ~ 60min, at 400 ~ 600 DEG C of roasting 90 ~ 150min at 100 ~ 200 DEG C;
(5) repeat: repeat step (3) and step (4), 150 ~ 300g/L catalyst is reached to the coated weight be coated on cordierite honeycomb ceramic carrier, then at 400 ~ 600 DEG C of roasting 90 ~ 150min, the vanadia-based SCR catalysts that product efficiently processes nitrogen oxide in diesel engine vent gas is obtained.
In step (3), when cordierite honeycomb ceramic carrier impregnated in coating slurries, should 1 ~ 3s be stopped, then take out with the speed of 30 ~ 100mm/s.
The material of described cordierite honeycomb ceramic carrier is 2MgO2Al
2o
35SiO
2, the mesh order number of cordierite honeycomb ceramic carrier is 30 ~ 600 orders.
Beneficial effect of the present invention: TiO when the present invention can suppress high temperature by doped with rare-earth elements Er
2crystal formation by the transformation of anatase to rutile, thus can significantly improve the catalyst based high-temperature behavior of V, simultaneously because doped F e in the coating improves cryogenic property, thus has greatly widened the operating temperature range of catalyst, has improve catalyst activity.
Accompanying drawing explanation
Curve display monoblock type ErVO in Fig. 1
4/ TWS/ cordierite honeycomb ceramic is respectively at 650 DEG C of 2h, and 700 DEG C of 10h and 750 DEG C 10h, tri-aging states are at different temperatures to NO conversion ratio.
Curve display monoblock type Fe in Fig. 2
0.2er
0.8vO
4/ TWS/ cordierite honeycomb ceramic is respectively at 650 DEG C of 2h, and 700 DEG C of 10h and 750 DEG C 10h, tri-aging states are at different temperatures to NO conversion ratio.
Curve display monoblock type Fe in Fig. 3
0.5er
0.5vO
4/ TWS/ cordierite honeycomb ceramic is respectively at 650 DEG C of 2h, and 700 DEG C of 10h and 750 DEG C 10h, tri-aging states are at different temperatures to NO conversion ratio.
Curve display monoblock type Fe in Fig. 4
0.8er
0.2vO
4/ TWS/ cordierite honeycomb ceramic is respectively at 650 DEG C of 2h, and 700 DEG C of 10h and 750 DEG C 10h, tri-aging states are at different temperatures to NO conversion ratio.
Curve display monoblock type FeVO in Fig. 5
4/ TWS/ cordierite honeycomb ceramic is respectively at 650 DEG C of 2h, and 700 DEG C of 10h and 750 DEG C 10h, tri-aging states are at different temperatures to NO conversion ratio.
Detailed description of the invention
The following stated embodiment describes the present invention in detail.In these embodiments, unless defined otherwise, all percentages being by weight.In its floating coat, second component is TiO
2, WO
3and SiO
2three kinds of combination of oxides, to abridge, TWS represents.
Embodiment 1 prepares monoblock type ErVO
4the aging state catalyst E1 of/TWS/ cordierite honeycomb ceramic 650 DEG C:
Using 400 holes/square inch (cellspersquareinch, cpsi) cordierite honeycomb ceramic (originating from Japanese NGK) is ceramic as load.First cordierite honeycomb ceramic being cut into size is that the small cylinder of Φ 13 × 60 (mm) is for subsequent use.
The preparation method of the vanadia-based SCR catalysts of nitrogen oxide in described efficient process diesel engine vent gas, step is as follows by weight:
(1) preparation of vanadium erbium iron complexes: first by 3 parts of NH
4vO
3powder adds 15 parts of deionized waters and is placed in 80 DEG C of water-baths and dissolves, and obtains solution a;
Ferric nitrate and erbium nitrate are pressed Fe
xthe form mixing of Ery, wherein Fe
xin Ery, x is the mol ratio of iron, the mol ratio of to be 0, y be erbium, and scope is 0 ~ 1, fully obtains solution b after mixing;
Solution a is fully mixed according to weight ratio 1:3 with solution b; Then service property (quality) concentration be 25% ~ 35% ammoniacal liquor above-mentioned mixed solution to be adjusted to pH be 7.25, stir 24h, suction filtration, obtain filter cake, after also again being precipitated by Washing of Filter Cake, at 100 DEG C, dry 3h, roasting 3 hours at 200 DEG C again, obtains the first component vanadium erbium iron complexes;
(2) preparation of coating slurries: get vanadium iron compound prepared by step (1) and add in 370g deionized water, TiO
2, WO
3and SiO
2be followed successively by 70:5:5 mixing according to mass ratio, obtain second component mixture; First component and second component are mixed according to the ratio of 10%:85%, forms mixture;
Add deionized water, stir and obtain suspension, regulate the addition of deionized water, make mixture content in suspension be 35 parts, obtain suspension;
By suspension ball milling, control granularity D
90be less than 60 microns, obtain coating slurries;
(3) flood: cordierite honeycomb ceramic carrier be impregnated in coating slurries prepared by step (2), fully take out after dipping;
(4) dry: the cordierite honeycomb ceramic carrier after coating slurries in step (3) is dried 60min, at 400 DEG C of roasting 150min at 100 DEG C;
(5) repeat: repeat step (3) and step (4), 200g/L catalyst is reached to the coated weight be coated on cordierite honeycomb ceramic carrier, then at 500 DEG C of roasting 90min, the vanadia-based SCR catalysts that product efficiently processes nitrogen oxide in diesel engine vent gas is obtained.
Put into 650 DEG C by preparing gained catalyst to carry out 2h aging, pass into air with the speed of 200L/h in ageing process and be equipped with the steam of 10%, thus obtained monoblock type ErVO
4the aging state catalyst of/TWS/ cordierite honeycomb ceramic 650 DEG C.
Catalyst activity applications catalyst sample evaluation system is tested.Unstripped gas composition is: 400ppmNO; 400ppmNH
3; 6%O
2; 7%H
2o; N
2as Balance Air.Air speed is 30000h
-1.Measure the SCR activity of catalyst at different temperatures.Adopt AVLDiGS4000Light type five gas analyzer to measure each gas concentration, calculated the efficiency of DeNOx by the change in concentration situation measuring NOx in gas before and after catalyst, aging state catalyst activity test result is shown in Fig. 1.
Embodiment 2
Preparation monoblock type ErVO
4/ TWS/ cordierite honeycomb ceramic 700 DEG C aging state catalyst E2: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, make catalyst when difference is aging to put into 700 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 1.
Embodiment 3
Preparation monoblock type ErVO
4/ TWS/ cordierite honeycomb ceramic 750 DEG C aging state catalyst E3: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, make catalyst when difference is aging to put into 750 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 1.
Embodiment 4
Preparation monoblock type Fe
0.2er
0.8vO
4/ TWS/ cordierite honeycomb ceramic 650 DEG C aging state catalyst E4: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, will according to Fe when difference is Kaolinite Preparation of Catalyst
0.2the ratio of Er0.8 adds Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution, aging state catalyst activity test result is shown in Fig. 2.
Embodiment 5
Preparation monoblock type Fe
0.2er
0.8vO
4/ TWS/ cordierite honeycomb ceramic 700 DEG C aging state catalyst E5: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
0.2the ratio of Er0.8 adds Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution; Make catalyst time aging to put into 700 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 2.
Embodiment 6
Preparation monoblock type Fe
0.2er
0.8vO
4/ TWS/ cordierite honeycomb ceramic 750 DEG C aging state catalyst E6: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
0.2er
0.8ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution; Make catalyst time aging to put into 750 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 2.
Embodiment 7
Preparation monoblock type Fe
0.5er
0.5vO
4/ TWS/ cordierite honeycomb ceramic 650 DEG C aging state catalyst E7: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
0.5er
0.5ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution, aging state catalyst activity test result is shown in Fig. 3.
Embodiment 8
Preparation monoblock type Fe
0.2er
0.8vO
4/ TWS/ cordierite honeycomb ceramic 700 DEG C aging state catalyst E8: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
0.2er
0.8ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution, make catalyst time aging and put into 700 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 3.
Embodiment 9
Preparation monoblock type Fe
0.2er
0.8vO
4/ TWS/ cordierite honeycomb ceramic 750 DEG C aging state catalyst E9: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
0.2er
0.8ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution, make catalyst time aging and put into 750 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 3.
Embodiment 10
Preparation monoblock type Fe
0.8er
0.2vO
4/ TWS/ cordierite honeycomb ceramic 650 DEG C aging state catalyst E10: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
0.8er
0.2ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution, aging state catalyst activity test result is shown in Fig. 4.
Embodiment 11
Preparation monoblock type Fe
0.8er
0.2vO
4/ TWS/ cordierite honeycomb ceramic 700 DEG C aging state catalyst E11: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
0.8er
0.2ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution, make catalyst time aging and put into 700 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 4.
Embodiment 12
Preparation monoblock type Fe
0.8er
0.2vO
4/ TWS/ cordierite honeycomb ceramic 750 DEG C aging state catalyst E12: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
0.8er
0.2ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution, make catalyst time aging and put into 750 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 4.
Embodiment 13
Preparation monoblock type FeVO
4/ TWS/ cordierite honeycomb ceramic 650 DEG C aging state catalyst E13: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
1er
0ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate, is dissolved in NH in 80 DEG C of water-baths
4vO
3in solution, aging state catalyst activity test result is shown in Fig. 5.
Embodiment 14
Preparation monoblock type FeVO
4/ TWS/ cordierite honeycomb ceramic 700 DEG C aging state catalyst E14: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
1er
0ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate; Make catalyst time aging to put into 700 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 5.
Embodiment 15
Preparation monoblock type FeVO
4/ TWS/ cordierite honeycomb ceramic 750 DEG C aging state catalyst E15: concrete preparation method, aging condition are substantially identical with E1 with appreciation condition, according to Fe when difference is Kaolinite Preparation of Catalyst
1er
0ratio add Fe (NO
3)
36H
2o and Er (NO
3)
36H
2o crystalline hydrate; Make catalyst time aging to put into 750 DEG C to carry out 10h aging, aging state catalyst activity test result is shown in Fig. 5.
Claims (2)
1. process the vanadia-based SCR catalysts of nitrogen oxide in diesel engine vent gas, it is characterized in that formula rate is as follows by weight percentage: the first component is coated in together with second component carrier cordierite honeycomb ceramic surface;
Described first component is Fe
0.5er
0.5vO
4; The content of the first component for benchmark, is 5% ~ 15% with the first component and the second component gross weight;
Described second component is TiO
2, WO
3and SiO
2three kinds of combination of oxides, TiO
2, WO
3and SiO
270:5:5 is followed successively by according to mass ratio.
2. process the preparation method of the vanadia-based SCR catalysts of nitrogen oxide in diesel engine vent gas described in claim 1, it is characterized in that step is as follows by weight:
(1) preparation of vanadium erbium iron complexes: first the metavanadic acid ammonia of 1 ~ 5 part is added 1 ~ 20 part of deionized water and be placed in 70 ~ 90 DEG C of water-baths and dissolve, obtain solution a;
Ferric nitrate and erbium nitrate are pressed Fe
0.5er
0.5form mixing, obtain solution b;
Solution a is fully mixed according to weight ratio 1 ~ 2:3 ~ 6 with solution b; Then service property (quality) concentration be 25% ~ 35% ammoniacal liquor above-mentioned mixed solution to be adjusted to pH be 5 ~ 9, stir 22 ~ 26h, suction filtration, obtain filter cake, after Washing of Filter Cake is also precipitated again, 1 ~ 3h is dried at 100 ~ 400 DEG C, then roasting 1 ~ 3 hour at 200 ~ 500 DEG C, obtain the first component vanadium erbium iron complexes;
(2) preparation of coating slurries: get TiO
2, WO
3and SiO
2be followed successively by 70:5:5 mixing according to mass ratio, obtain second component mixture; First component and second component are mixed according to the ratio of 5% ~ 15%:85% ~ 95%, forms mixture;
Add deionized water, stir and obtain suspension, regulate the addition of deionized water, make mixture content in suspension be 10 ~ 50 parts, obtain suspension;
By suspension ball milling, control granularity D
90be less than 60 microns, obtain coating slurries;
(3) flood: cordierite honeycomb ceramic carrier be impregnated in coating slurries prepared by step (2), fully take out after dipping;
(4) dry: the cordierite honeycomb ceramic carrier after coating slurries in step (3) is dried 30 ~ 60min, at 400 ~ 600 DEG C of roasting 90 ~ 150min at 100 ~ 200 DEG C;
(5) repeat: repeat step (3) and step (4), 150 ~ 300g/L catalyst is reached to the coated weight be coated on cordierite honeycomb ceramic carrier, then at 400 ~ 600 DEG C of roasting 90 ~ 150min, the vanadia-based SCR catalysts that product efficiently processes nitrogen oxide in diesel engine vent gas is obtained;
In step (3), when cordierite honeycomb ceramic carrier impregnated in coating slurries, should 1 ~ 3s be stopped, then take out with the speed of 30 ~ 100mm/s.
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| CN104338545B (en) * | 2014-10-21 | 2016-05-11 | 无锡威孚环保催化剂有限公司 | A kind of efficient SCR catalyst that is applied to diesel engine vent gas purification of nitrogen oxides |
| CN106512990A (en) * | 2016-11-17 | 2017-03-22 | 徐洁 | Diesel engine exhaust gas purifying SCR catalyst |
| EP3562580A4 (en) * | 2016-12-30 | 2020-08-26 | Basf Se | An extruded honeycomb catalyst |
| CN106975477A (en) * | 2017-05-04 | 2017-07-25 | 龙岩紫荆创新研究院 | SCR denitration preparation method and catalyst |
| CN108435196A (en) * | 2018-05-02 | 2018-08-24 | 河北国创环境科技有限公司 | A kind of purifying internal combustion engine tail gas SCR denitration and preparation method |
| KR20210094092A (en) | 2018-12-14 | 2021-07-28 | 바스프 코포레이션 | Method for preparing vanadium catalyst |
| CN115739071B (en) * | 2022-11-25 | 2024-07-09 | 大唐南京环保科技有限责任公司 | Denitration catalyst and preparation method thereof |
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