CN100473456C - Catalyst for SCR denitration in boiler low-temperature fume and preparation method thereof - Google Patents
Catalyst for SCR denitration in boiler low-temperature fume and preparation method thereof Download PDFInfo
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- CN100473456C CN100473456C CNB2007100567411A CN200710056741A CN100473456C CN 100473456 C CN100473456 C CN 100473456C CN B2007100567411 A CNB2007100567411 A CN B2007100567411A CN 200710056741 A CN200710056741 A CN 200710056741A CN 100473456 C CN100473456 C CN 100473456C
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Abstract
The invention discloses a low-flue SCR denitrated catalyst and making method, which is characterized by the following: adopting active carbon fiber as carrier; leaching; setting the weight of catalyst at 1-5%; adopting manganese and cerium as main components and ferric, copper, vanadium or chromium as auxiliary elements.
Description
[technical field] the present invention relates to the nitrogen oxide of boiler low-temperature fume in the environmental technology field and handles particularly a kind of catalyst and preparation thereof.
The energy resource structure of [background technology] China is based on coal, and the coal consumption amount is also with sustainable growth.According to statistics, China's capacity of installed generator moderate heat Denso machine capacity accounts for more than 74% at present, and in a very long time in future, the coal-fired nitrogen oxides pollution that is caused is the another important environmental problem after sulfur dioxide pollution." thermal power plant's atmosphere pollutants emission standards (GB13223-2003) " that implements while in January, 2004 has been reduced to 450-1100mg/m to the highest permission concentration of emission of station boiler nitrogen oxide of the 3rd period
3Along with development economic and society, the control criterion of nitrogen oxide will be strict gradually.
At present, at stationary source NO
xControl technology mainly contains two classes: a class is the Combustion Process Control technology, is characterized in controlling NO in the combustion process
xGeneration, comprise that the selection of the type of furnace and design parameter, operation adjust and low NO
xCombustion technology is controlled the nitrogen oxide of fuel type in the combustion process, heating power type and quick three kinds of mechanism of type with this; Two classes are burning back control technology, promptly various flue gas de-NO
xTechnology is characterized in the NO that will generate in the flue gas
xBe fixed up or be reduced to N
2The nitrogen oxide control technology is a cost to reduce boiler heating power efficient generally in the stove, its denitration efficiency is not high yet, and (the SelectiveCatalytic Reduction of the selective catalytic reduction in the gas denitrifying technology behind the stove, SCR) has the efficient height, little to the transformation of boiler existing equipment, be a kind of more potential denitration technology.
Reach its maturity with the SCR technology as reducing gas such as ammonia, this technology is to utilize the selectivity of ammonia reducing agent, preferentially reacts with nitrogen oxide, and its is reduced becomes nitrogen and water.
Flue-gas temperature condition stub according to catalyst is suitable for generally uses window SCR technology can be able to be divided into according to different temperature: high temperature, middle temperature, three kinds of different SCR technologies of low temperature.The Applicable temperature that high temperature SCR generally refers to catalyst 450～600 ℃ and more than, middle temperature SCR is meant the Applicable temperature of catalyst at 320～450 ℃, and the Applicable temperature that low-temperature SCR is meant catalyst is at 120～300 ℃ or low temperature more.Commercial is that running temperature is in 320～450 ℃ middle temperature catalyst more widely at present, and this catalyst is with TiO
2Be carrier, above major catalyst or co-catalyst such as load vanadium, tungsten and molybdenum.
The position difference that middle temperature catalyst is laid according to the SCR device is divided into high ash section, low ash section and afterbody and arranges three types.Particular location promptly is installed on air preheater and ESP (electric precipitation) is preceding, before the air preheater but behind the high temperature ESP, FGD (desulfurization) three kinds of forms afterwards.Be arranged in the preceding high ash section of air preheater and ESP (electric precipitation), catalyst requires that stronger antiblocking ability is arranged, and stronger alkali resistant metal toxicity, anti-SO are arranged
2Toxicity etc.Be arranged in before the air preheater but behind the high temperature ESP, catalyst can be avoided the side effect of high dust, but still need stronger anti-SO
2Toxicity requires ESP to possess the high-temperature behavior of restraining oneself simultaneously.Be arranged in FGD middle temperature catalyst afterwards, need a large amount of flue gas reheat energy consumptions.
And low-temperature SCR catalyst can be under the lower situation of energy consumption the catalyst arrangement desulfurization after.A spot of low-temperature SCR catalyst has appearred at present both at home and abroad, as the MnO of coprecipitation preparation
x/ CeO
2Catalyst, the MnO of sol-gel or prepared by co-precipitation
x/ TiO
2, also have to be reported in this and wherein to add co-catalyst, improve poison resistance to sulfur dioxide in flue gas and water.And in the low-temperature SCR catalyst research and development at home and abroad, technical relatively that is that all right is ripe.
[summary of the invention] order of the present invention ground is to solve the above-mentioned problems in the prior art, and a kind of SCR catalyst and preparation method who is used for boiler low-temperature fume is provided.
The invention provides a kind of is carrier with the NACF, with MnO
x-CeO
2Be major catalyst, adopt infusion process,,, prepare required catalyst by conditions such as control load amount, calcining heats by suitable immersion, oven dry and calcine technology.In catalyst preparation process, also as required, containing transition metal element, the ability of raising catalyst performance and anti-sulfur dioxide and water vapour.
Component as the NACF of carrier comprises viscose base activated carbon fiber, asphalt activity carbon fiber, petroleum coke based activated carbon fiber and polyacrylonitrile radical active carbon fiber.The shape of NACF comprises NACF felt, active carbon fiber fabrics, NACF silk and NACF piece.NACF can be directly used in carrier, also can remake carrier after the peracid preliminary treatment.Being used for pretreated acid comprises: the aqueous hydrochloric acid solution of the aqueous solution of nitric acid of 10wt%～40wt% or the aqueous sulfuric acid of 10wt%～40wt% or 10wt%～40wt%.
The catalyst main component is MnO
xAnd CeO
2, wherein to account for the mass percent of the catalyst integral body that comprises NACF be 1%～15% to catalyst component.MnO
xForm can be MnO
2, Mn
3O
4, Mn
2O
3In a kind of or wherein any two or three combination.Mn/ (Mn+Ce) element mol ratio is 0.2～0.6.
The main catalytic composition of demanganization and cerium also is added with co-catalyst component in the catalyst of the present invention, co-catalyst component (M) iron or copper or vanadium or chromium element.Cocatalytic element and main catalytic element molar ratio are that M/ (M+Mn+Ce) is 0.001-0.2.
Above-mentioned Preparation of catalysts method comprises following operating procedure:
(1) preparation of carrier
Directly as carrier, or after the peracid preliminary treatment, remake carrier with NACF; The acid-treated step of NACF is: NACF carries out acidifying 1～3h in acid solution, be washed with distilled water to neutrality again, and is dry down at 80～120 ℃ at last; Acid solution is aqueous solution of nitric acid or the aqueous sulfuric acid of 10wt%～40wt% or the aqueous hydrochloric acid solution of 10wt%～40wt% of 10wt%～40wt%;
(2) load of catalyst
Quality according to the NACF carrier, the percentage that accounts for the catalyst total quality that comprises NACF by catalyst component is 1%～15%, Mn/ (Mn+Ce) element mol ratio is 0.2～0.6 requirement, calculate nitrate or the acetate or the chloride quality of required manganese cerium, nitrate or the acetate or the muriatic mixed aqueous solution of configuration manganese cerium, and add citric acid as auxiliary agent, wherein: the nitrate of citric acid, manganese cerium or acetate or muriatic mass concentration are 10%-40% in the solution; Above-mentioned carrier is placed on wherein soaks 1-3h, carry out water-bath then and dry, finish load with infusion process; Carry out drying then under 80～120 ℃, last under the atmosphere protection of nitrogen or argon gas, 250～750 ℃ of temperature lower calcination 3～10h obtain catalyst.
The nitrate or acetate or chloride or the NH that in above-mentioned (2) mixed aqueous solution in step, add co-catalyst component iron or copper or vanadium or chromium
4VO
3, with nitrate or the acetate or the chloride composition mixed aqueous solution of citric acid, manganese cerium, cocatalytic element and all catalytic elements mol ratios are that M/ (M+Mn+Ce) is 0.001-0.2.
Advantage of the present invention and good effect: in the gas-solid heterogeneous catalytic reaction, gaseous material at first is attracted to catalyst surface, finishes catalytic process then, and in general, under equal conditions, the specific area of catalyst is big more, and its catalytic capability is strong more.Adopting NACF among the present invention is carrier, has the big characteristics of specific area, to the high adsorption capacity of gaseous material.NACF has increased the sour site on its surface, NH after the peracid pre-treatment and activation
3Reducing agent obviously increases in its surperficial adsorption capacity.
The infusion process supported catalyst is a kind of simple method on carrier, compare with coprecipitation method, infusion process can convenient catalyst load on the carrier of arbitrary shape.But when load capacity was bigger, particularly when the specific area of carrier was little, catalyst was piled up at carrier surface easily, makes catalyst at high temperature occur bad phenomenon such as sintering, reunion easily like this.And NACF has abundant specific area, and is relatively good to the dispersive property of catalyst, is not easy to occur these bad phenomenon.Adopting the raw material of wood-charcoal material is carrier, and except that having preferably catalysis characteristics, raw material of wood-charcoal material itself is that sulfur trioxide also has certain inhibitory action to Sulphur Dioxide in the low-temperature SCR reaction.NACF can be felted, cloth shape etc. in addition, the quality softness, and easily braiding can be arranged in the exhaust treatment system after utilizing certain frame fixation easily, compares with grain bed, and the NACF system has the lower advantage of resistance.
The catalyst of manganese base has good low-temperature SCR characteristic, and under 250～750 ℃ of different calcining heats, manganese presents multiple oxide state, and presents different performances.When calcining heat was higher than 600 ℃, Mn oxide was mainly with Mn
2O
3Form is when calcining heat is relatively lower, mainly with MnO
2Form.Under moderate temperature, Mn
2O
3And MnO
2And Mn
3O
4All might occur.Mn
2O
3Present high selectivity but MnO
2Have more activity.
Studies show that CeO
2Catalyst not only has good low-temperature SCR catalytic activity, and has the effect of widening the reaction temperature window.CeO
2At MnO
x-CeO
2Play the effect of oxygen transmission in the composite catalyst, thereby the NO that has quickened catalyst surface is converted into NO
2Speed, and under equal conditions, NH
3Be more prone to and NO
2React.Ce belongs to rare earth element, and is abundant at the reserves of China.
Some transition metals as iron, copper, vanadium, chromium, add MnO
x-CeO
2Can play tangible synergism in the composite catalyst, not only help improving and stably catalyzed performance, inhibited to the side effect of the sulfur dioxide that exists in the flue gas and water vapour simultaneously.
The MnO of the present invention's preparation
x-CeO
2Be major catalyst, reduced the operating temperature of SCR, make in SCR technology, with NH
3During for reducing agent, can 200 ℃ being issued to higher NO removal efficiency, and sulfur dioxide and the water vapour that exists in the flue gas had stronger poison resistance.To adopt NACF be carrier in the present invention in addition, and NACF has that specific area is big, high adsorption capacity, flexible arrangement, resistance are low, and catalyst is had dispersed preferably advantage.Compared with former technology, this patent has certain advantage.
[specific embodiment]
Embodiment 1:
(1) preparation of carrier
Viscose base activated carbon fiber is placed in 30% the sulfuric acid solution and carries out acidifying 2h, be washed with distilled water to neutrality again, dry down at 80 ℃ at last.
(2) load of catalyst
Prepare 20% aqueous citric acid solution as required,, carrier is placed on wherein soaks 1h, carry out water-bath then and dry, finish load with infusion process being dissolved in this solution of the nitrate of manganese cerium.Carry out dry 12h then under 120 ℃, under the nitrogen atmosphere protection, 350 ℃ of temperature lower calcination 5h obtain catalyst at last.MnO in the catalyst
xAnd CeO
2, the mass percent that accounts for the catalyst integral body that comprises NACF is 10%, Mn/ (Mn+Ce) element mol ratio is 0.4.
(3) this catalyst is 900ppm in the NO volumetric concentration, and temperature is under 100 ℃, and oxygen concentration is 5%, and under the NH3/NO=1.0 situation, the removal efficiency of NO is 83%; In the NO volumetric concentration is 900ppm, and temperature is under 150 ℃, and oxygen concentration is 5%, NH
3Under/NO=1.0 the situation, the removal efficiency of NO is 89%.
Embodiment 2:
(1) preparation of carrier
Polyacrylonitrile radical active carbon fiber is placed in 30% the salpeter solution and carries out acidifying 2h, be washed with distilled water to neutrality again, dry down at 80 ℃ at last.
(2) load of catalyst
Prepare 20% aqueous citric acid solution as required, the nitrate of manganese cerium is dissolved in this solution, carrier is placed on wherein soaks 1h, carry out water-bath then and dry, finish load with infusion process.Carry out dry 12h then under 120 ℃, under the nitrogen atmosphere protection, 350 ℃ of temperature lower calcination 5h obtain catalyst at last.Catalyst MnO
xAnd CeO
2, the mass percent that accounts for the catalyst integral body that comprises NACF is 12%, Mn/ (Mn+Ce) element mol ratio is 0.3.
(3) this catalyst is 900ppm in the NO volumetric concentration, and temperature is under 100 ℃, and oxygen concentration is 5%, NH
3Under/NO=1.0 the situation, the removal efficiency of NO is 86%; In the NO volumetric concentration is 900ppm, and temperature is under 150 ℃, and oxygen concentration is 5%, NH
3Under/NO=1.0 the situation, the removal efficiency of NO is 93%.
Embodiment 3:
(1) preparation of carrier
The petroleum coke based active carbon fiber is placed in 20% the hydrochloric acid solution and carries out acidifying 2h, be washed with distilled water to neutrality again, dry down at 80 ℃ at last.
(2) load of catalyst
Prepare 20% aqueous citric acid solution as required, the nitrate of manganese cerium is dissolved in this solution in this aqueous solution, add NH
4VO
3, make its dissolving, carrier is placed on wherein soaks 1h, carry out water-bath then and dry, finish load with infusion process.Carry out dry 10h then under 120 ℃, under the nitrogen atmosphere protection, 550 ℃ of temperature lower calcination 5h obtain catalyst at last.Catalyst MnO
xAnd CeO
2, the mass percent that accounts for the catalyst integral body that comprises NACF is 10%, and Mn/ (Mn+Ce) element mol ratio is 0.6, and V/ (V+Mn+Ce) element mol ratio is 0.1.
(3) this catalyst is 900ppm in the NO volumetric concentration, and temperature is under 100 ℃, and oxygen concentration is 5%, NH
3Under/NO=1.0 the situation, the removal efficiency of NO is 85%; In the NO volumetric concentration is 900ppm, and temperature is under 150 ℃, and oxygen concentration is 5%, NH
3Under/NO=1.0 the situation, the removal efficiency of NO is 90%; In the NO volumetric concentration is 900ppm, and temperature is under 150 ℃, and oxygen concentration is 5%, NH
3/ NO=1.0, SO
2Concentration be 1500ppm, the removal efficiency of NO is 80%.
Embodiment 4:
(1) preparation of carrier
Viscose base activated carbon fiber is placed in 20% the sulfuric acid solution and carries out acidifying 2h, be washed with distilled water to neutrality again, dry down at 80 ℃ at last.
(2) load of catalyst
Prepare 20% aqueous citric acid solution as required, the acetate of manganese cerium is dissolved in this aqueous solution, add ferric nitrate, make its dissolving, carrier is placed on wherein soaks 1h, carry out water-bath then and dry, finish load with infusion process.Carry out dry 12h then under 120 ℃, under the nitrogen atmosphere protection, 450 ℃ of temperature lower calcination 5h obtain catalyst at last.Catalyst MnO
xAnd CeO
2, the mass percent that accounts for the catalyst integral body that comprises NACF is 10%, and Mn/ (Mn+Ce) element mol ratio is 0.6, and Fe/ (Fe+Mn+Ce) element mol ratio is 0.15.
(3) this catalyst is 900ppm in the NO volumetric concentration, and temperature is under 100 ℃, and oxygen concentration is 5%, NH
3Under/NO=1.0 the situation, the removal efficiency of NO is 82%; In the NO volumetric concentration is 900ppm, and temperature is under 150 ℃, and oxygen concentration is 5%, NH
3Under/NO=1.0 the situation, the removal efficiency of NO is 89%; In the NO volumetric concentration is 900ppm, and temperature is under 150 ℃, and oxygen concentration is 5%, NH
3/ NO=1.0, SO
2Concentration be 1500ppm, H
2O concentration is under 6% situation, and the removal efficiency of NO is 75%.
Claims (1)
1, a kind of catalyst that is used for the SCR denitration of boiler low-temperature fume is characterized in that this catalyst is carrier with the NACF, finishes the catalyst component MnO of the oxide of load manganese and cerium in its surface with infusion process
xAnd CeO
2, the percentage that catalyst component accounts for the catalyst total quality that comprises NACF is 1%～15%; MnO
xForm be MnO
2, Mn
3O
4, Mn
2O
3In a kind of or wherein two or three combination; Also be added with co-catalyst component M, M is iron or copper or vanadium or chromium element; Co-catalyst component and all catalytic elements mol ratio M/ (M+Mn+Ce) are 0.001-0.2, and Mn/ (Mn+Ce) element mol ratio is 0.2～0.6.
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