CN102962074A - Denitration catalyst of wide activity temperature window as well as preparation method and application thereof - Google Patents
Denitration catalyst of wide activity temperature window as well as preparation method and application thereof Download PDFInfo
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- CN102962074A CN102962074A CN2012104699389A CN201210469938A CN102962074A CN 102962074 A CN102962074 A CN 102962074A CN 2012104699389 A CN2012104699389 A CN 2012104699389A CN 201210469938 A CN201210469938 A CN 201210469938A CN 102962074 A CN102962074 A CN 102962074A
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Abstract
The invention provides a denitration catalyst of a wide activity temperature window as well as a preparation method and application of the denitration catalyst, and belongs to the technical fields of environment catalysis and atmosphere pollution control. The composite oxide catalyst is prepared by a hydrothermal method. The denitration catalyst is characterized in that the activity temperature window is wide and has good waterproof property and good sulfur tolerance. The provided method for reducing nitric oxide comprises the following steps of: loading the catalyst in a reactor of a stationary bed; controlling the reaction temperature within the range of 150-400 DEG C; and using ammonia as a reducing agent. According to the copper-cerium-titanium composite oxide prepared by the invention, the air speed is 64000/h; and the purification efficiency of the nitric oxide is 91-99% within the range of 200-400 DEG C.
Description
Technical field
The method that the present invention relates to a kind of composite oxide catalysts and preparation thereof and utilize this catalyst selective catalyst reduction of nitrogen oxides under excess oxygen.Be applicable to stationary source and the mobile former discharging nitrogen oxide (NO such as lean-burn gasoline motor car and diesel vehicle such as coal-burning power plant, Industrial Boiler, calcining kiln
x) elimination, belong to environmental catalysis and air pollution control technique field.
Background technology
Along with the growth of energy-consuming and the increase of vehicle guaranteeding organic quantity, a large amount of Fossil fuel consumptions, nitrogen oxide emission constantly increases, and the problems such as its acid rain that causes, photochemical fog have become the global environmental problem that becomes increasingly conspicuous, therefore, NO
xEmission control become the focus of a research in the present atmosphere environmental technology field.
Ammonia SCR (Selective catalytic reduction, SCR) is considered to stationary source tail flue gas NO
xPollute one of effective method of control.The key of SCR technology is the catalyst of efficient stable.At present, the NH of industrial applications
3-SCR catalyst mainly is V
2O
5-WO
3/ TiO
2Catalyst, this catalyst has good catalytic performance in 320-400 ℃ of scope.But the problem that this catalyst exists is active constituent V
2O
5Precursor toxicity large, cause easily environmental pollution; And when flue-gas temperature was lower than 300 ℃, the denitration performance of catalyst was low.And the smog discharge temperature of boiler of power plant changes with load, even the temperature during underrun before air preheater also may be down to below 250 ℃.Existing SCR catalyst can not be applied to the flue gas condition of boiler of power plant underrun both at home and abroad.In addition, there is a large amount of industrial combustion equipments in China, comprise Industrial Boiler, calcining kiln and cement rotary kiln etc., in flue-gas temperature between air preheater and the economizer usually between 250-350 ℃, be lower than coal-fired power station boiler flue-gas temperature (320-400 ℃), therefore, the denitrating catalyst of exploitation wide temperature window can not only satisfy the NO under the different load condition of power plant
xElimination, also simultaneously can satisfy the technical need of China's industrial combustion equipment denitrating flue gas, have great importance and application prospect.
The present invention by hydro-thermal method prepared a kind of in wide temperature range to NO
xRemove well behaved NEW TYPE OF COMPOSITE oxide catalyst.
Summary of the invention
It is simple and to ammonia selective reducing NO to the purpose of this invention is to provide a kind of preparation technology
xHas high efficiency composite oxide catalysts and preparation method thereof.Concerted catalysis effect in the performance copper cerium-titanium composite oxide between each component improves the performance of catalyst, thus made a kind of environmental friendliness and in wide temperature range to NO
xWell behaved denitrating catalyst is eliminated in catalysis.
The objective of the invention is to be achieved through the following technical solutions:
The denitrating catalyst of wide active temperature windows is characterized in that: the raw material composition is expressed as Cu
xCe
yTi
1-x-yO
2, molar content 0.1≤x of Cu≤0.3 wherein, molar content 0.1≤y of Ce≤0.3, the molar content of Ti is between 0.4-0.8.
The preparation method of the denitrating catalyst of described wide active temperature windows is characterized in that: the method may further comprise the steps successively:
(1) copper nitrate and the cerous nitrate solution of preparation 0.5 ~ 1.0mol/L, the titanium sulfate solution of 1 ~ 2 mol/L;
(2) get step (1) gained copper nitrate, cerous nitrate and titanium sulfate solution, 30 ~ 50 ℃ of stirring in water bath were mixed 30 ~ 90 minutes, obtained mixed solution;
(3) step (2) gained mixed solution being added ammoniacal liquor to pH value under constantly stirring is 10, and the gained mixed liquor is transferred in the hydrothermal reaction kettle, 120 ℃ of condition hydro-thermal reactions 12 ~ 24 hours, then is down to room temperature;
(4) get step (3) gained reactant liquor suction filtration, washing was dried 12 ~ 48 hours under 120 ℃ of conditions, and then roasting 4 ~ 8 hours under 500 ℃ of conditions in Muffle furnace makes the denitrating catalyst of wide active temperature windows.
The application of the denitrating catalyst of described wide active temperature windows is characterized in that, this application process may further comprise the steps:
In the middle of fixed bed reactors, reaction temperature is controlled at 150 ~ 400 ℃ of scopes with catalyst loading; Take ammonia as reducing agent, the control total gas flow rate is at 200 ~ 400 ml/min, and air speed is 64,000 ~ 128,000 h
-1
The present invention compared with prior art has the following advantages and the high-lighting effect: do not adopt virose active component V
2O
5, by the concerted catalysis effect between performance copper cerium titanium component, Effective Raise the low-temperature denitration performance of catalyst, widened the active temperature windows of catalyst, the performance that has possessed the efficient catalytic purifying nitrogen oxide, in 200 ~ 400 ℃ of scopes, the purification efficiency of nitrogen oxide reaches 91 ~ 99%.
The specific embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
Embodiment 1:Cu
0.1Ce
0.1Ti
0.8O
2The preparation of composite oxide catalysts
A) get respectively the copper nitrate solution of 7.53ml 0.50 mol/L, the cerous nitrate solution of 7.49 ml, 0.50 mol/L and the titanium sulfate solution of 15.03 ml, 2 mol/L, 30 ℃ of stirring in water bath were mixed 30 minutes, obtained mixed solution;
B) with step a) the gained mixed solution to add ammoniacal liquor to pH value under constantly stirring be 10, the gained mixed liquor is transferred in the hydrothermal reaction kettle, 120 ℃ of condition hydro-thermal reactions 24 hours, then be down to room temperature;
C) get step b) gained reactant liquor suction filtration, washing, oven dry is 12 hours under 120 ℃ of conditions, and then roasting 6 hours under 500 ℃ of conditions in Muffle furnace makes the copper cerium and titanium compound oxide catalyst.
Embodiment 2:Cu
0.1Ce
0.3Ti
0.6O
2The preparation of composite oxide catalysts
A) get respectively the copper nitrate solution of 3.77 ml, 1.0 mol/L, the cerous nitrate solution of 11.31 ml, 1.0 mol/L and the titanium sulfate solution of 22.62 ml, 1.0 mol/L, 50 ℃ of stirring in water bath were mixed 90 minutes, obtained mixed solution;
B) with step a) the gained mixed solution to add ammoniacal liquor to pH value under constantly stirring be 10, the gained mixed liquor is transferred in the hydrothermal reaction kettle, 120 ℃ of condition hydro-thermal reactions 12 hours, then be down to room temperature;
C) get step b) gained reactant liquor suction filtration, washing, oven dry is 24 hours under 120 ℃ of conditions, and then roasting 4 hours under 500 ℃ of conditions in Muffle furnace makes the copper cerium and titanium compound oxide catalyst.
Embodiment 3:Cu
0.2Ce
0.2Ti
0.6O
2The preparation of composite oxide catalysts
A) get respectively the copper nitrate solution of 7.53ml 1.0 mol/L, the cerous nitrate solution of 7.49 ml, 1.0 mol/L and the titanium sulfate solution of 11.27 ml, 2 mol/L, 30 ℃ of stirring in water bath were mixed 60 minutes, obtained mixed solution;
B) with step a) the gained mixed solution to add ammoniacal liquor to pH value under constantly stirring be 10, the gained mixed liquor is transferred in the hydrothermal reaction kettle, 120 ℃ of condition hydro-thermal reactions 24 hours, then be down to room temperature;
C) get step b) gained reactant liquor suction filtration, washing, oven dry is 48 hours under 120 ℃ of conditions, and then roasting 8 hours under 500 ℃ of conditions in Muffle furnace makes the copper cerium and titanium compound oxide catalyst.
Embodiment 4:Cu
0.3Ce
0.1Ti
0.6O
2The preparation of composite oxide catalysts
A) get respectively the copper nitrate solution of 11.25 ml, 1.0 mol/L, the cerous nitrate solution of 3.75 ml, 1.0 mol/L and the titanium sulfate solution of 11.25 ml, 2 mol/L, 30 ℃ of stirring in water bath were mixed 60 minutes, obtained mixed solution;
B) with step a) the gained mixed solution to add ammoniacal liquor to pH value under constantly stirring be 10, the gained mixed liquor is transferred in the hydrothermal reaction kettle, 120 ℃ of condition hydro-thermal reactions 24 hours, then be down to room temperature;
C) get step b) gained reactant liquor suction filtration, washing, oven dry is 24 hours under 120 ℃ of conditions, and then roasting 4 hours under 500 ℃ of conditions in Muffle furnace makes the copper cerium and titanium compound oxide catalyst.
Embodiment 5:Cu
0.3Ce
0.3Ti
0.4O
2The preparation of composite oxide catalysts
A) get respectively the copper nitrate solution of 11.25ml 1.0 mol/L, the cerous nitrate solution of 11.25 ml, 1.0 mol/L and the titanium sulfate solution of 7.50 ml, 2 mol/L, 30 ℃ of stirring in water bath were mixed 60 minutes, obtained mixed solution;
B) with step a) the gained mixed solution to add ammoniacal liquor to pH value under constantly stirring be 10, the gained mixed liquor is transferred in the hydrothermal reaction kettle, 120 ℃ of condition hydro-thermal reactions 24 hours, then be down to room temperature;
C) get step b) gained reactant liquor suction filtration, washing, oven dry is 48 hours under 120 ℃ of conditions, and then roasting 8 hours under 500 ℃ of conditions in Muffle furnace makes the copper cerium and titanium compound oxide catalyst.
Embodiment 6(reference): Cu
0.1Ti
0.9O
2The preparation of catalyst
A) get the titanium sulfate solution of 7.53ml 0.50 mol/L copper nitrate solution and 16.91ml 2.0 mol/L, 40 ℃ of stirring in water bath mix, and obtain mixed solution;
B) with step a) the gained mixed solution to add ammoniacal liquor to pH value under constantly stirring be 10, the gained mixed liquor is transferred in the hydrothermal reaction kettle, 120 ℃ of condition hydro-thermal reactions 24 hours, then be down to room temperature;
C) get step b) gained reactant liquor suction filtration, washing, oven dry is 48 hours under 120 ℃ of conditions, and then roasting 6 hours under 500 ℃ of conditions in Muffle furnace makes the copper titanium compound oxide catalyst.
Embodiment 7(reference): Ce
0.1Ti
0.9O
2The preparation of catalyst
A) get the titanium sulfate solution of 7.49 ml, 0.50 mol/L cerous nitrate solution and 16.91ml 2.0 mol/L, 40 ℃ of stirring in water bath mix, and obtain mixed solution;
B) with step a) the gained mixed solution to add ammoniacal liquor to pH value under constantly stirring be 10, the gained mixed liquor is transferred in the hydrothermal reaction kettle, 120 ℃ of condition hydro-thermal reactions 24 hours, then be down to room temperature;
C) get step b) gained reactant liquor suction filtration, washing, oven dry is 48 hours under 120 ℃ of conditions, and then roasting 6 hours under 500 ℃ of conditions in Muffle furnace makes cerium and titanium compound oxide catalyst.
Embodiment 8: the preparation method of catalyst is identical with embodiment 1, and 0.12 gram catalyst is placed continuous fixed bed reactor, and reaction gas consists of 0.05% NO, 0.05% NH
3, 5% O
2, do Balance Air with nitrogen, the flow velocity of reaction gas is 300 ml/min, air speed is 64,000 h
-1The activity rating temperature range is 150-400 ℃, under the different temperatures, and catalyst reduction NO
xConversion ratio see Table 1.
Embodiment 9: the preparation method of catalyst is identical with embodiment 2, and 0.12 gram catalyst is placed continuous fixed bed reactor, and reaction gas consists of 0.05% NO, 0.05% NH
3, 5% O
2, do Balance Air with nitrogen, the flow velocity of reaction gas is 300 ml/min, air speed is 64,000 h
-1The activity rating temperature range is 150-400 ℃, under the different temperatures, and catalyst reduction NO
xConversion ratio see Table 1.
Embodiment 10: the preparation method of catalyst is identical with embodiment 3, and 0.12 gram catalyst is placed continuous fixed bed reactor, and reaction gas consists of 0.05% NO, 0.05% NH
3, 5% O
2, do Balance Air with nitrogen, the flow velocity of reaction gas is 300 ml/min, air speed is 64,000 h
-1The activity rating temperature range is 150-400 ℃, under the different temperatures, and catalyst reduction NO
xConversion ratio see Table 1.
Embodiment 11: the preparation method of catalyst is identical with embodiment 4, and 0.12 gram catalyst is placed continuous fixed bed reactor, and reaction gas consists of 0.05% NO, 0.05% NH
3, 5% O
2, do Balance Air with nitrogen, the flow velocity of reaction gas is 300 ml/min, air speed is 64,000 h
-1The activity rating temperature range is 150-400 ℃, under the different temperatures, and catalyst reduction NO
xConversion ratio see Table 1.
Embodiment 12: the preparation method of catalyst is identical with embodiment 5, and 0.12 gram catalyst is placed continuous fixed bed reactor, and reaction gas consists of 0.05% NO, 0.05% NH
3, 5% O
2, do Balance Air with nitrogen, the flow velocity of reaction gas is 300 ml/min, air speed is 64,000 h
-1The activity rating temperature range is 150-400 ℃, under the different temperatures, and catalyst reduction NO
xConversion ratio see Table 1.
Table 1 copper titanium, cerium titanium and copper cerium titanium catalyst activity rating result
Embodiment 13: the preparation method of catalyst is identical with embodiment 1, and 0.12 gram catalyst is placed continuous fixed bed reactor, and reaction gas consists of 0.05% NO, 0.05% NH
3, 5% O
2, 5% H
2O, 50ppm SO
2, do Balance Air with nitrogen, the flow velocity of reaction gas is 300 ml/min, air speed is 64,000 h
-1The activity rating temperature range is 150-400 ℃, under the different temperatures, and catalyst reduction NO
xConversion ratio see Table 2.
Embodiment 14: the preparation method of catalyst is identical with embodiment 2, and 0.12 gram catalyst is placed continuous fixed bed reactor, and reaction gas consists of 0.05% NO, 0.05% NH
3, 5% O
2, 5% H
2O, 50ppm SO
2, do Balance Air with nitrogen, the flow velocity of reaction gas is 300 ml/min, air speed is 64,000 h
-1The activity rating temperature range is 150-400 ℃, under the different temperatures, and catalyst reduction NO
xConversion ratio see Table 2.
Table 2 copper titanium, cerium titanium and copper cerium titanium catalyst are at water and SO
2Activity rating result during coexistence
Claims (3)
1. the denitrating catalyst of wide active temperature windows is characterized in that: raw material forms and is expressed as Cu
xCe
yTi
1-x-yO
2, molar content 0.1≤x of Cu≤0.3 wherein, molar content 0.1≤y of Ce≤0.3, the molar content of Ti is between 0.4-0.8.
2. the preparation method of the denitrating catalyst of wide active temperature windows as claimed in claim 1, it is characterized in that: the method may further comprise the steps successively:
(1) copper nitrate and the cerous nitrate solution of preparation 0.5 ~ 1.0mol/L, the titanium sulfate solution of 1 ~ 2 mol/L;
(2) get step (1) gained copper nitrate, cerous nitrate and titanium sulfate solution, 30 ~ 50 ℃ of stirring in water bath were mixed 30 ~ 90 minutes, obtained mixed solution;
(3) step (2) gained mixed solution being added ammoniacal liquor to pH value under constantly stirring is 10, and the gained mixed liquor is transferred in the hydrothermal reaction kettle, 120 ℃ of condition hydro-thermal reactions 12 ~ 24 hours, then is down to room temperature;
(4) get step (3) gained reactant liquor suction filtration, washing was dried 12 ~ 48 hours under 120 ℃ of conditions, and then roasting 4 ~ 8 hours under 500 ℃ of conditions in Muffle furnace makes the denitrating catalyst of wide active temperature windows.
3. the as claimed in claim 1 application of the denitrating catalyst of wide active temperature windows is characterized in that, this application process may further comprise the steps:
(1) with catalyst loading in the middle of fixed bed reactors, reaction temperature is controlled at 150 ~ 400 ℃ of scopes;
(2) take ammonia as reducing agent, the control total gas flow rate is at 200 ~ 400 ml/min, and air speed is 64,000 ~ 128,000 h
-1
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|---|---|---|---|---|
| CN103433040A (en) * | 2013-08-29 | 2013-12-11 | 天津大学 | Binary metal modified titanium dioxide catalyst, preparation method thereof and application of catalyst in removal of nitric oxide contained in tail gas of diesel engine |
| CN105688888A (en) * | 2016-01-14 | 2016-06-22 | 济南大学 | High-performance vanadium, cerium and titanium composite oxide catalyst for flue gas denitration and preparation method thereof |
| CN107519945A (en) * | 2017-06-08 | 2017-12-29 | 河北威达蓝海环保科技有限公司 | A kind of handling process of wide temperature range denitrating catalyst raw material |
| CN108554462A (en) * | 2018-05-14 | 2018-09-21 | 南京工业大学 | A kind of cerium tungsten titanium denitrating catalyst and its preparation method and application |
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| CN108554462A (en) * | 2018-05-14 | 2018-09-21 | 南京工业大学 | A kind of cerium tungsten titanium denitrating catalyst and its preparation method and application |
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