CN107497465A - Support type low temperature sulfuric-resisting hydrogen ammonium SCR denitration and its preparation method and application - Google Patents
Support type low temperature sulfuric-resisting hydrogen ammonium SCR denitration and its preparation method and application Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/195—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium or tantalum
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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Abstract
The invention belongs to technical field of air pollution control, specially a kind of support type low temperature sulfuric-resisting hydrogen ammonium SCR denitration and its preparation method and application.Sulfuric-resisting hydrogen ammonium SCR denitration of the present invention, its formula are M x V1‑x OPO4/TiO2, M element is Mo or W；M element and V molal quantity sum are 1；The mass fraction of active component and carrier is：Active component accounts for 1~10 part, and carrier accounts for 90~99 parts.Denitrating catalyst is prepared using infusion process in the present invention, effectively compensate for traditional V2O5‑WO3/TiO2The defects of light-off temperature is high, and temperature window is narrower, and low-temperature denitration efficiency is low, sulfur resistive water repelling property is weak.Catalyst of the present invention is tolerable to contain 0~3000mg/m simultaneously3SO2With the nitrogen oxide containing gas of 0~20 vol.% vapor, at 150~300 DEG C and 3,000~100,000h‑1Under conditions of air speed, denitration efficiency is more than 90%, and can stablize more than 80h, and the discharged nitrous oxides available for the stationary source flue gas such as glass, steel, coking coke oven control.
Description
Technical field
The invention belongs to technical field of air pollution control, and in particular to a kind of support type low temperature sulfuric-resisting hydrogen ammonium SCR takes off
Denox catalyst and its preparation method and application.
Background technology
Nitrogen oxides NO x It is（NO、NO2And N2O）One of global atmosphere pollutant main source, be cause photochemical fog,
One of the main reason for environmental problems such as acid rain, haze, depletion of the ozone layer, brought greatly to human habitat and health
Harm, thus as one of current environmental problem for being badly in need of solving.Energy resource structure of the China based on coal causes thermal power station, steel
The flue gases such as iron, metallurgy, glass, petrochemical industry, coking coke oven contain substantial amounts of NO x .In recent years, environmental protection standard in China constantly carries
Height, the emission control to nitrogen oxides is more and more stricter, and denitrification apparatus transformation largely has been carried out in coal-burning power plant, using mesh
Maximally efficient denitrating flue gas (deNO on former world x ) technology NH3- SCR and commercial effective catalyst V2O5-WO3/TiO2So that
Discharged nitrous oxides in coal-fired plant flue gas basically reach discharging standards.But at present, steel, metallurgy, glass, stone
The Industrial Boiler denitration technology such as change, coking coke oven is not yet transformed, because the flue-gas temperature of these Industrial Boilers is in 150-300
DEG C, and contain in flue gas and be higher than 300 mg/m3SO2With 20 vol.% H2O.Domestic and international commercial V at present2O5-WO3/TiO2
The denitration activity of catalyst under this condition is poor, is due to SO2In catalyst surface by V2O5It is oxidized to SO3, SO3And H2O
And NH3The material such as ammonium hydrogen sulfate or ammonium sulfate is generated, ammonium hydrogen sulfate or ammonium sulfate at this temperature are a kind of stickums, attached
In catalyst surface, be covered in active sites, block catalyst pore, catalyst denitration efficiency is declined or even is inactivated.
It is also no both at home and abroad to be directed to this kind of low temperature coal-fired flue-gas mature technology so that the emission reduction shape of this kind of consumption coal industry flue gas nitrogen oxide
Gesture is extremely serious, therefore it is significant to develop low temperature sulfuric-resisting hydrogen ammonium catalyst.
Publication No. CN102078809 A Chinese invention patent discloses a kind of low temperature suitable for 150-250 DEG C
Denitration Mn-Ti catalyst, but MnO x Easily by SO3And H2The H of O generations2SO4Poison, lose catalytic activity.Therefore, one is developed
Kind low temperature sulfuric-resisting hydrogen ammonium SCR denitration has broad application prospects.
The content of the invention
It is an object of the invention to provide one kind to possess low light-off temperature, high catalytic activity, and strong water resistant sulfur resistance is born
Load type denitrating catalyst, and its preparation method and application are provided.
Support type low temperature sulfuric-resisting hydrogen ammonium SCR denitration provided by the invention, its formula are M x V1-x OPO4/TiO2；M
Element is Mo or W；M element and V molal quantity sum are 1；The mass fraction of active component and carrier is：Active component accounts for 1~
10 parts, carrier accounts for 90~99 parts.
The present invention also provides the preparation method of above-mentioned support type low temperature sulfuric-resisting hydrogen ammonium SCR denitration, specific steps
It is as follows：
（1）Vanadium source and oxalic acid are added into deionized water, 40 ~ 90 DEG C of heating water baths, magnetic agitation to solution is in blueness；
（2）To step（1）M sources are added in solution, stir 0.5 ~ 3 h, to being completely dissolved；
（3）To step（2）Phosphorus source is added in solution, continues the h of stirring 0.5 ~ 3, it is complete to reacting；
（4）To step（3）TiO is added in solution2, ultrasonic disperse, and 60 ~ 90 DEG C of stirring in water bath are evaporated；
（5）Sample after being evaporated is placed in vacuum drying chamber and dried；
（6）Dried sample is ground to without particle, and in Muffle kiln roasting, obtains finished catalyst；
（7）Finished catalyst is granulated, 40 ~ 60 mesh sieves is crossed, that is, obtains sulfuric-resisting hydrogen ammonium SCR denitration.
Preferably, described vanadium source is V2O5Or NH4VO3, the amount for the material that described oxalic acid is put into is vanadium source input
2 ~ 4 times of the amount of matter.
Preferably, described M sources are one kind in Mo or W metal acid-salt.
Preferably, described phosphorus source is one kind in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate or ammonium phosphate.
Preferably, the vacuum of the vacuum drying chamber is -0.01 ~ -0.08 MPa, drying temperature is 80 ~ 120 DEG C,
Hold time as 8 ~ 24 h.
Preferably, described sintering temperature is 300 ~ 600 DEG C, roasting time is 6 ~ 12 h.
The advantages of support type low temperature sulfuric-resisting hydrogen ammonium SCR denitration of the present invention is：Preparation method is simple, can be effective
Make up traditional V2O5-WO3/TiO2Catalyst the defects of denitration efficiency is low at low temperature, sulfur resistive water repelling property is poor.
Catalyst of the present invention is tolerable to contain 0~3000 mg/m simultaneously3SO2With the nitrogen oxygen of 0~20 vol.% vapor
Compound flue gas, at 150~300 DEG C and 3,000~100,000 h-1Under conditions of air speed, denitration efficiency is more than 90 %, and energy
Stablize 80 more than h, the denitration process available for the discharged nitrous oxides of the stationary source flue gas such as glass, steel, coking coke oven.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.The experimental method of unreceipted actual conditions in the following example, generally according to conventional strip
Part, or according to the condition proposed by manufacturer.
Embodiment 1：
1. the preparation of catalyst：0.2 mol ammonium metavanadates are sequentially added into 500 mL deionized waters（NH4VO3）、0.48 mol
Oxalic acid dihydrate（H2C2O4·2H2O）, 60 DEG C of 0.5 h of stirring, obtain blue solution.The water of 0.11 mol tetra- is added into above-mentioned solution
Close ammonium molybdate（(NH4)6Mo7O24·4H2O）, stir 0.5 h；0.31 mol H is added into above-mentioned solution3PO4(85%), after
3 h of continuous stirring are complete to reaction；The TiO of 500 g high-specific surface areas is added into the solution2, ultrasonic disperse, 90 DEG C of stirring steamings
It is dry；Gained sample is transferred in vacuum drying chamber, the MPa of vacuum -0.07 is maintained, 120 DEG C of constant temperature, dries 12 h.Will be solid
Body is put into 700 DEG C of 6 h of roasting of Muffle furnace after being ground to no particle.It is granulated, crosses 40-60 mesh sieves, obtain low temperature support type sulfuric-resisting
Hydrogen ammonium SCR catalyst.
2. the performance test of catalyst：The catalyst for taking 0.6 g tablettings to sieve is put into fixed bed quartz tube reactor, stone
The cm of English bore=0.4, simulated flue gas is by NO, NH3、O2And N2Composition, wherein NO 1500 ppm, NH3 1500 ppm、O2 3
Vol%, the h of air speed 80,000-1, 150 ~ 300 DEG C of reaction temperature, reaction end gas NO-NO2-NO x Analyzer（Thermo 42i-
HL）On-line checking.In this test condition, the denitration efficiency of catalyst is stable in 98 more than %.
3. sulfur resistive water repelling property is tested：SO is passed through in simulated flue gas2And vapor：SO2Concentration is 1000 mg/m3, water steaming
Air volume ratio is 20 vol.%, and other test conditions are constant.In this test condition, the denitration efficiency of catalyst is still stablized
91 more than %, it was demonstrated that catalyst has stronger sulfuric-resisting hydrogen ammonium ability.
Embodiment 2：
1. the preparation of catalyst：0.2 mol ammonium metavanadates are sequentially added into 500 mL deionized waters（NH4VO3）、0.48 mol
Oxalic acid dihydrate（H2C2O4·2H2O）, 60 DEG C of 0.5 h of stirring, obtain blue solution.It is inclined that 0.067 mol is added into above-mentioned solution
Ammonium tungstate（(NH4)6H2W12O40.nH2O）, stir 0.5 h；0.31 mol H is added into above-mentioned solution3PO4(85%), continue
It is complete to reaction to stir 3 h；The TiO of 500 g high-specific surface areas is added into the solution2, ultrasonic disperse, 90 DEG C of stirrings are evaporated；
Gained sample is transferred in vacuum drying chamber, the MPa of vacuum -0.07 is maintained, 120 DEG C of constant temperature, dries 12 h.Solid is ground
700 DEG C of 6 h of roasting of Muffle furnace are put into after being milled to no particle.It is granulated, crosses 40-60 mesh sieves, obtain low temperature support type sulfuric-resisting hydrogen ammonium
SCR catalyst.
2. the performance test of catalyst：The catalyst for taking 0.6 g tablettings to sieve is put into fixed bed quartz tube reactor, stone
The cm of English bore=0.4, simulated flue gas is by NO, NH3、O2And N2Composition, wherein NO 1500 ppm, NH3 1500 ppm、O2 3
Vol%, the h of air speed 80,000-1, 150 ~ 300 DEG C of reaction temperature, reaction end gas NO-NO2-NO x Analyzer（Thermo 42i-
HL）On-line checking.In this test condition, the denitration efficiency of catalyst is stable in 96 %.
3. sulfur resistive water repelling property is tested：SO is passed through in simulated flue gas2And vapor：SO2Concentration is 1000 mg/m3, water steaming
Air volume ratio is 20 vol.%, and other test conditions are constant.In this test condition, the denitration efficiency of catalyst is still stablized
90 more than %, it was demonstrated that catalyst has stronger sulfuric-resisting hydrogen ammonium ability.
Embodiment 3：
1. the preparation of catalyst：0.1 mol vanadic anhydrides are sequentially added into 500 mL deionized waters（V2O5）、0.48 mol
Oxalic acid dihydrate（H2C2O4·2H2O）, 60 DEG C of 0.5 h of stirring, obtain orange suspension.0.11 mol is added into above-mentioned suspension
Ammonium Molybdate Tetrahydrate（(NH4)6Mo7O24·4H2O）, stir 0.5 h；0.31 mol H is added into above-mentioned solution3PO4
(85%), continue to stir 3 h to reaction completely；The TiO of 500 g high-specific surface areas is added into the solution2, ultrasonic disperse, 90 DEG C
Stirring is evaporated；Gained sample is transferred in vacuum drying chamber, the MPa of vacuum -0.07 is maintained, 120 DEG C of constant temperature, dries 12
h.By solid abrasive to without being put into 700 DEG C of Muffle furnace roasting, 6 h after particle.It is granulated, crosses 40-60 mesh sieves, obtain low temperature support type
Sulfuric-resisting hydrogen ammonium SCR catalyst.
2. the performance test of catalyst：The catalyst for taking 0.6 g tablettings to sieve is put into fixed bed quartz tube reactor, stone
The cm of English bore=0.4, simulated flue gas is by NO, NH3、O2And N2Composition, wherein NO 1500 ppm, NH3 1500 ppm、O2 3
Vol%, the h of air speed 80,000-1, 150 ~ 300 DEG C of reaction temperature, reaction end gas NO-NO2-NO x Analyzer（Thermo 42i-
HL）On-line checking.In this test condition, the denitration efficiency of catalyst is stable in 98 %.
3. sulfur resistive water repelling property is tested：SO is passed through in simulated flue gas2And vapor：SO2Concentration is 1000 mg/m3, water steaming
Air volume ratio is 20 vol.%, and other test conditions are constant.In this test condition, the denitration efficiency of catalyst is still stablized
93 more than %, it was demonstrated that catalyst has stronger sulfuric-resisting hydrogen ammonium ability.
Embodiment 4：
1. the preparation of catalyst：0.1 mol vanadic anhydrides are sequentially added into 500 mL deionized waters（V2O5）、0.48 mol
Oxalic acid dihydrate（H2C2O4·2H2O）, 60 DEG C of 0.5 h of stirring, obtain orange suspension.0.067 is added into above-mentioned suspension liquid
Mol ammonium metatungstates（(NH4)6H2W12O40.nH2O）, stir 0.5 h；0.31 mol H is added into above-mentioned solution3PO4
(85%), continue to stir 3 h to reaction completely；The TiO of 500 g high-specific surface areas is added into the solution2, ultrasonic disperse, 90 DEG C
Stirring is evaporated；Gained sample is transferred in vacuum drying chamber, the MPa of vacuum -0.07 is maintained, 120 DEG C of constant temperature, dries 12
h.By solid abrasive to without being put into 700 DEG C of Muffle furnace roasting, 6 h after particle.It is granulated, crosses 40-60 mesh sieves, obtain low temperature support type
Sulfuric-resisting hydrogen ammonium SCR catalyst.
2. the performance test of catalyst：The catalyst for taking 0.6 g tablettings to sieve is put into fixed bed quartz tube reactor, stone
The cm of English bore=0.4, simulated flue gas is by NO, NH3、O2And N2Composition, wherein NO 1500 ppm, NH3 1500 ppm、O2 3
Vol%, the h of air speed 80,000-1, 150 ~ 300 DEG C of reaction temperature, reaction end gas NO-NO2-NO x Analyzer（Thermo 42i-
HL）On-line checking.In this test condition, the denitration efficiency of catalyst is stable in 98 %.
3. sulfur resistive water repelling property is tested：SO is passed through in simulated flue gas2And vapor：SO2Concentration is 1000 mg/m3, water steaming
Air volume ratio is 20 vol.%, and other test conditions are constant.In this test condition, the denitration efficiency of catalyst is still stablized
91 more than %, it was demonstrated that catalyst has stronger sulfuric-resisting hydrogen ammonium ability.
Claims (8)
1. a kind of support type low temperature sulfuric-resisting hydrogen ammonium SCR denitration, it is characterised in that its formula is M x V1-x OPO4/TiO2；
M element is Mo or W；M element and V molal quantity sum are 1；The mass fraction of active component and carrier is：Active component accounts for 1~
10 parts, carrier accounts for 90~99 parts.
2. the preparation method of sulfuric-resisting hydrogen ammonium SCR denitration as claimed in claim 1, it is characterised in that specific steps
It is as follows：
（1）Vanadium source and oxalic acid are added into deionized water, 40 ~ 90 DEG C of heating water baths, magnetic agitation to solution is in blueness；
（2）To step（1）M sources are added in solution, stir 0.5 ~ 3 h, to being completely dissolved；
（3）To step（2）Phosphorus source is added in solution, continues the h of stirring 0.5 ~ 3, it is complete to reacting；
（4）To step（3）TiO is added in solution2, ultrasonic disperse, and be evaporated in 60 ~ 90 DEG C of stirring in water bath；
（5）Sample after being evaporated is placed in vacuum drying chamber and dried；
（6）Dried sample is ground to without particle, and in Muffle kiln roasting, obtains finished catalyst；
（7）Finished catalyst is granulated, 40 ~ 60 mesh sieves is crossed, that is, obtains sulfuric-resisting hydrogen ammonium SCR catalyst.
3. the preparation method of sulfuric-resisting hydrogen ammonium SCR denitration according to claim 2, it is characterised in that step（1）
Described in vanadium source be V2O5Or NH4VO3, the amount for the material that described oxalic acid is put into is 2 ~ 4 times of the amount of vanadium source input material.
4. the preparation method of sulfuric-resisting hydrogen ammonium SCR catalyst according to claim 2, it is characterised in that：Step（2）Middle institute
The M sources stated are one kind in Mo or W metal acid-salt.
5. the preparation method of sulfuric-resisting hydrogen ammonium SCR denitration according to claim 2, it is characterised in that：Step（3）
Described in phosphorus source be phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate or ammonium phosphate in one kind.
6. the preparation method of sulfuric-resisting hydrogen ammonium SCR denitration according to claim 2, it is characterised in that：Step
（5）Described in the vacuum of vacuum drying chamber be -0.01 ~ -0.08 MPa, drying temperature is 80 ~ 120 DEG C, hold time as 8 ~
24 h。
7. the preparation method of sulfuric-resisting hydrogen ammonium SCR denitration according to claim 2, it is characterised in that step
（6）Described in sintering temperature be 300 ~ 600 DEG C, roasting time is 6 ~ 12 h.
8. sulfuric-resisting hydrogen ammonium SCR denitration as claimed in claim 1 controls in the discharged nitrous oxides of stationary source flue gas
In application.
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| CN109603871A (en) * | 2018-11-26 | 2019-04-12 | 清华大学盐城环境工程技术研发中心 | It is a kind of using phosphorus tungsten vanadium heteropoly acid as denitrating catalyst of presoma and preparation method thereof |
| CN110665493A (en) * | 2019-09-26 | 2020-01-10 | 复旦大学 | Low-temperature ammonium bisulfate poisoning resistant denitration catalyst and preparation method thereof |
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| CN113750981A (en) * | 2021-09-26 | 2021-12-07 | 北京市科学技术研究院城市安全与环境科学研究所 | Catalyst for synergistically purifying various pollutants and preparation method thereof |
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| CN114832867A (en) * | 2021-02-02 | 2022-08-02 | 国家能源投资集团有限责任公司 | Activation method for improving low-temperature activity of honeycomb denitration catalyst |
| CN114832867B (en) * | 2021-02-02 | 2023-09-29 | 国家能源投资集团有限责任公司 | Start-up method for improving low-temperature activity of honeycomb denitration catalyst |
| CN112973766B (en) * | 2021-02-24 | 2023-05-26 | 大唐南京环保科技有限责任公司 | Preparation method of ammonium bisulfate-resistant flat-plate denitration catalyst and catalyst obtained by preparation method |
| CN112973766A (en) * | 2021-02-24 | 2021-06-18 | 大唐南京环保科技有限责任公司 | Preparation method of ammonium bisulfate-resistant flat plate type denitration catalyst and obtained catalyst |
| CN113750981A (en) * | 2021-09-26 | 2021-12-07 | 北京市科学技术研究院城市安全与环境科学研究所 | Catalyst for synergistically purifying various pollutants and preparation method thereof |
| CN114160122A (en) * | 2021-11-29 | 2022-03-11 | 长沙理工大学 | Wide-temperature-zone SCR catalyst with fly ash as matrix and capable of preventing ammonium bisulfate poisoning and preparation method and application thereof |
| CN114160122B (en) * | 2021-11-29 | 2023-12-01 | 长沙理工大学 | Ammonium bisulfate poisoning prevention wide-temperature-zone SCR catalyst taking fly ash as matrix and preparation method and application thereof |
| CN114308048A (en) * | 2021-12-31 | 2022-04-12 | 上海复翼环保科技有限公司 | Medium-low temperature ammonium bisulfate poisoning-resistant denitration catalyst and preparation method thereof |
| CN115193442A (en) * | 2022-07-17 | 2022-10-18 | 复旦大学 | Low-temperature ammonium bisulfate-resistant denitration catalyst and preparation method and application thereof |
| CN115888691A (en) * | 2022-12-02 | 2023-04-04 | 国家电投集团远达环保催化剂有限公司 | SCR denitration catalyst of gas turbine and preparation method and application thereof |
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