CN107511158A - Denitrating catalyst of low temperature water resistant sulfur resistive and its preparation method and application - Google Patents
Denitrating catalyst of low temperature water resistant sulfur resistive 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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- B01D53/34—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 denitrating catalyst of low temperature water resistant sulfur resistive and its preparation method and application.Denitrating catalyst of the present invention is using titanium dioxide as carrier, with the one or more in barium oxide, vanadium phosphorus oxide and cerium oxide for active component, with the one or more in molybdenum oxide, tungsten oxide, nickel oxide and Zirconium oxide for auxiliary agent, cosolvent and dispersant are used as using oxalic acid.The catalyst effectively reduces the reduction of specific surface area of catalyst in roasting process, significantly improves denitration efficiency, and solve the problems, such as traditional catalytic component based on vanadium due in the presence low temperature of water and sulphur cytotoxic activity drastically decline.Denitrating catalyst of the present invention is in 150~300 DEG C and 5,000~150,000h‑1Under conditions of air speed, denitration efficiency is stable more than 93%, N2Selectivity is higher than 95%, has strong sulfur resistive water resistant ability, and the discharged nitrous oxides especially suitable for flue gases such as glass, steel, coking coke ovens control.
Description
Technical field
The invention belongs to technical field of air pollution control, and in particular to a kind of denitrating catalyst of low temperature water resistant sulfur resistive and
Its preparation method and application.
Background technology
With the fast development of economic society, energy-consuming is also in sustainable growth.China is current second potential energy in the world
Source producing country and country of consumption, leading present situation is accounted for consumption of coal in energy consumption structure and is difficult to change within following quite long-term
Become.Consumption of coal causes air pollution due to coal combustion, causes the discharge of a large amount of pernicious gases, such as nitrogen oxides.
Nitrogen oxide emission is added in performance assessment criteria first during " 12 ", and " production nitrogen is big for thermal power plant, cement plant etc.
Family " is also gradually paid close attention to by country, and the emission control of nitrogen oxides just shows effect.2006-2015, China's nitrogen oxides row
Put total amount and present and rise then stabilization or even downward trend.Even in 2015, discharged nitrous oxides total amount was still high
Up to more than 2,000 ten thousand tons, denitration is imperative.
Nitrogen oxides control aspect, mainly there are low burn burning technology and denitrating flue gas.According to national economy sustainable development
It is required that country is more and more stricter to emission request limitation, only reduces and discharge by low burn burning technology, discharge mark far can not be reached
Standard, denitrating flue gas are then generally using the method for reducing discharged nitrous oxides.Wherein SCR is that definitely main flow is also business at present
Change the most successful gas denitrifying technology, be universally acknowledged maximally effective when the removal efficiency for requiring nitrogen oxides is more than 50%
Denitration technology, its floor space is small, is advantageous to be transformed in original flow, while simple to operate, technology maturation.Restrict
Principal element in SCR denitration technology is catalyst, and its expense can account for half of SCR system initial outlay or so.Catalyst
Fine or not only relation denitration effect, and influence its own life-span, so as to influence SCR follow-up operation cost.
Current commercial vanadium titanium denitrating catalyst(V2O5/TiO2)In middle-temperature section(350-450℃)Catalytic performance is superior.Largely
Industrial Boiler, such as coke oven flue gas, steel, cement, glass, petrochemical industry, nitric acid production industry, because temperature is relatively low, cause not
High temperature denitrating catalyst can directly be used.New type low temperature denitrating catalyst is developed, and keeps the height of low-temperature denitration catalyst living
Property, high stability, sulfur resistive water-resistance be badly in need of solve difficult point.
In recent years, research finds that manganese-based catalyst has higher activity in low-temperature SCR reaction, but mixed gas is few
SO existing for amount2The activity for destroying catalyst can be had a strong impact on.SO under low temperature2It is oxidized to SO3, can be anti-with catalytically-active materials
Stable sulphate cpd should be generated so that catalyst loses activity, or is having H2O's and NH3The difficult decomposition of reaction generation
Avtive spot of ammonium hydrogen sulfate or ammonium sulfate blocking catalyst etc. so that catalyst is difficult to play preferable clean-up effect.With this
Meanwhile the narrow stable performance that also limit catalyst activity of catalyst activity temperature window.Therefore a kind of low temperature bar is developed
Have the catalyst of efficient sulfur resistive water resistant and denitration performance significant under part.
The content of the invention
It is an object of the invention to provide a kind of denitrating catalyst of new type low temperature water resistant sulfur resistive and preparation method thereof, and solve
The problem of certainly traditional vanadium titanium catalyst low temperature sulfur poisoning and water intoxication inactivate, realize the nitrogen of the flue gases such as glass, steel, coking coke oven
Emissions of oxides controls.
The denitrating catalyst of new type low temperature water resistant sulfur resistive provided by the invention, is made up of carrier, active component and auxiliary agent, its
The percentage by weight of component opposite carrier is as follows:Active component is 1 ~ 40%, and auxiliary agent accounts for 1 ~ 20%;Wherein, the carrier is dioxy
Change titanium, the active component is the one or more in barium oxide, phosphorus barium oxide and cerium oxide, and the auxiliary agent is tungsten oxygen
One or more in compound, molybdenum oxide, nickel oxide and Zirconium oxide.
The preparation method of the denitrating catalyst of described low temperature water resistant sulfur resistive provided by the invention, is comprised the following steps that:
Step 1:One or more in a certain amount of vanadic salts and cerium oxide are dissolved in a certain amount of deionized water with oxalic acid
In, heating, which is sufficiently stirred, to be disperseed to form mixed liquor;
Step 2:By solution, stirring in one or more addition step 1 in a certain amount of tungsten salt, molybdenum salt, nickel salt and zirconates
Dissolving;
Step 3:By solution, stirring and dissolving in a certain amount of phosphatic one or more addition step 2;
Step 3:A certain amount of titania support is added into solution in step 3,60 ~ 100 DEG C of stirrings are evaporated;
Step 4:Collection is evaporated product and is calcined 2 ~ 6 hours at 250 ~ 650 DEG C, obtains finished catalyst.
In the present invention, the vanadic salts is the one or more in ammonium metavanadate, vanadyl oxalate and vanadic sulfate, in its solution
The concentration of v element is 0.001 ~ 0.1mol/L;The phosphate is in phosphoric acid, ammonium phosphate, ammonium dihydrogen phosphate and diammonium hydrogen phosphate
One or more, the concentration of P elements is 0.001 ~ 0.1mol/L in its solution;The cerium salt is cerous nitrate, cerium chloride and sulphur
One or more in sour cerium, the concentration of Ce elements is 0.001 ~ 1.0mol/L in its solution;The tungsten salt is ammonium metatungstate, secondary
One or more in ammonium tungstate, sodium tungstate and potassium tungstate, the concentration of wolfram element is 0.001 ~ 1.0mol/L in its solution;It is described
Molybdenum salt be ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate and ammonium octamolybdate in one or more, the concentration of its Molybdenum in Solution element
For 0.001 ~ 1.0mol/L;Concentration of oxalic acid is 2-4 times of v element concentration;The nickel salt is nickel nitrate, nickel acetate or nickel chloride
In one or more, the concentration of nickel element is 0.001 ~ 1.0mol/L in its solution;The zirconates is zirconium nitrate, oxychlorination
One or more in zirconium, acetic acid zirconium or zirconium sulfate, the concentration of zr element is 0.001 ~ 1.0mol/L in its solution.
The denitrating catalyst of low temperature water resistant sulfur resistive provided by the invention, on the one hand effectively reduce catalyst ratio in roasting process
The reduction of surface area, significantly improves denitration efficiency, on the other hand solves traditional catalytic component based on vanadium because the presence of water and sulphur is low
The problem of middle benefit gas cytotoxic activity drastically declines.Its advantage is:With 100 ~ 150m2/ g specific surface area, at 150~300 DEG C and 5,
000~150,000h-1Under conditions of air speed, denitration efficiency is stable more than 95%, N2Selectivity is higher than 95%, and containing 0~
3000mg/m3SO2With 5% ~ 20% H2More than 85%, N is still kept under O nitrogen oxide containing gas2Selectivity is higher than 90%, tool
There is strong sulfur resistive water resistant ability, the discharged nitrous oxides especially suitable for the stationary source flue gas such as glass, steel, coking coke oven control.
Embodiment
The present invention is described in further detail below by specific embodiment.It should be understood that these embodiments are only used for
The bright present invention rather than limitation the scope of the present invention.The experimental method of unreceipted actual conditions, is generally pressed in the following example
More solito condition, or according to the condition proposed by manufacturer.
Embodiment 1:
1. the preparation of catalyst:Sequentially added into 200 mL deionized waters 0.01mol ammonium metavanadates, 0.03mol oxalic acid and
The water cerous nitrates of 0.03mol six, it is sufficiently stirred and disperses to form mixed liquor;Be separately added into again 0.005mol ammonium heptamolybdates and
0.01mol ammonium phosphate, stirring and dissolving are uniform;Then 10g titania supports are added into above-mentioned mixed liquor, 80 DEG C of stirrings are evaporated;
Collection is evaporated product and is calcined 3 hours at 500 DEG C, obtains finished catalyst.
2. the performance test of catalyst:Specific surface area of catalyst is 120 m2/ g, automatically compared by Tristar II 3020
Surface area and pore analysis instrument are tested to obtain.The catalyst for taking 0.5 g to prepare is put into fixed bed quartz tube reactor, quartz ampoule
The cm of internal diameter=0.8, simulated flue gas is by NO, NH3、O2And N2Composition, wherein NO 1000 ppm, NH31000 ppm、O23 %, air speed
40,000 h-1, 150 ~ 300 DEG C of reaction temperature, reaction end gas Antaris IGS gas analyzer on-line checkings.In the test
Under the conditions of, the denitration efficiency of catalyst is stable in 95 more than %, N2Selectivity is more than 96%.
3. catalyst sulfur resistive water repelling property is tested:SO is additionally added in simulated flue gas2So that SO2Concentration is 500 mg/m3,
It is simultaneously extra to add H2O so that H2O volume fraction is 20%, and other test conditions are constant.In this test condition, catalyst
Denitration efficiency still stablize in 92 more than %, N2Selectivity is more than 94%.
Embodiment 2:
1. the preparation of catalyst:0.01mol ammonium metavanadates, 0.04mol oxalic acid are sequentially added into 200 mL deionized waters, is filled
Divide and be dispersed with stirring to form mixed liquor;0.002mol ammonium metatungstates, 0.01mol nickel nitrates and 0.01mol phosphoric acid are separately added into again, are stirred
Mix and be uniformly dissolved;Then 10g titania supports are added into above-mentioned mixed liquor, 80 DEG C of stirrings are evaporated;Collection be evaporated product and
350 DEG C are calcined 3 hours, obtain finished catalyst.
2. the performance test of catalyst:Specific surface area of catalyst is 145 m2/ g, automatically compared by Tristar II 3020
Surface area and pore analysis instrument are tested to obtain.The catalyst for taking 0.5 g to prepare is put into fixed bed quartz tube reactor, quartz ampoule
The cm of internal diameter=0.8, simulated flue gas is by NO, NH3、O2And N2Composition, wherein NO 500 ppm, NH3500 ppm、O23 %, air speed
30,000 h-1, 150 ~ 300 DEG C of reaction temperature, reaction end gas Antaris IGS gas analyzer on-line checkings.In the test
Under the conditions of, the denitration efficiency of catalyst is stable in 97 more than %, N2Selectivity is more than 96%.
3. catalyst sulfur resistive water repelling property is tested:SO is additionally added in simulated flue gas2So that SO2Concentration is 1,500 mg/
m3, while additionally add H2O so that H2O volume fraction is 10%, and other test conditions are constant.In this test condition, it is catalyzed
The denitration efficiency of agent is still stablized in 90 more than %, N2Selectivity is more than 92%.
Embodiment 3:
1. the preparation of catalyst:Sequentially added into 200 mL deionized waters 0.01mol ammonium metavanadates, 0.03mol oxalic acid and
The water cerous nitrates of 0.005mol six, it is sufficiently stirred and disperses to form mixed liquor;0.002mol sodium tungstates, 0.01mol are separately added into again
Zirconium sulfate and 0.01mol ammonium dihydrogen phosphates, stirring and dissolving are uniform;Then 10g titania supports are added into above-mentioned mixed liquor, 80
DEG C stirring is evaporated;Collection is evaporated product and is calcined 3 hours at 550 DEG C, obtains finished catalyst.
2. the performance test of catalyst:Specific surface area of catalyst is 105 m2/ g, automatically compared by Tristar II 3020
Surface area and pore analysis instrument are tested to obtain.The catalyst for taking 0.5 g to prepare is put into fixed bed quartz tube reactor, quartz ampoule
The cm of internal diameter=0.8, simulated flue gas is by NO, NH3、O2And N2Composition, wherein NO 1500 ppm, NH31500 ppm、O23 %, air speed
50,000 h-1, 150 ~ 300 DEG C of reaction temperature, reaction end gas Antaris IGS gas analyzer on-line checkings.In the test
Under the conditions of, the denitration efficiency of catalyst is stable in 96 more than %, N2Selectivity is more than 94%.
3. catalyst sulfur resistive water repelling property is tested:SO is additionally added in simulated flue gas2So that SO2Concentration is 500 mg/m3,
It is simultaneously extra to add H2O so that H2O volume fraction is 10%, and other test conditions are constant.In this test condition, catalyst
Denitration efficiency still stablize in 92 more than %, N2Selectivity is more than 90%.
Embodiment 4:
1. the preparation of catalyst:0.01mol vanadyl oxalates, 0.02mol oxalic acid are sequentially added into 200 mL deionized waters, is filled
Divide and be dispersed with stirring to form mixed liquor;0.02mol ammonium heptamolybdates, 0.0005mol ammonium metatungstates and 0.01mol phosphoric acid are separately added into again
Ammonium, stirring and dissolving are uniform;Then 10g titania supports are added into above-mentioned mixed liquor, 80 DEG C of stirrings are evaporated;Collection is evaporated product
And be calcined 3 hours at 350 DEG C, obtain finished catalyst.
2. the performance test of catalyst:Specific surface area of catalyst is 140 m2/ g, automatically compared by Tristar II 3020
Surface area and pore analysis instrument are tested to obtain.The catalyst for taking 0.5 g to prepare is put into fixed bed quartz tube reactor, quartz ampoule
The cm of internal diameter=0.8, simulated flue gas is by NO, NH3、O2And N2Composition, wherein NO 1000 ppm, NH31000 ppm、O23 %, air speed
30,000 h-1, 150 ~ 300 DEG C of reaction temperature, reaction end gas Antaris IGS gas analyzer on-line checkings.In the test
Under the conditions of, the denitration efficiency of catalyst is stable in 95 more than %, N2Selectivity is more than 93%.
3. catalyst sulfur resistive water repelling property is tested:SO is additionally added in simulated flue gas2So that SO2Concentration is 1,000 mg/
m3, while additionally add H2O so that H2O volume fraction is 15%, and other test conditions are constant.In this test condition, it is catalyzed
The denitration efficiency of agent is still stablized in 92 more than %, N2Selectivity is more than 95%.
Embodiment 5:
1. the preparation of catalyst:0.01mol vanadic sulfates, 0.02mol oxalic acid are sequentially added into 200 mL deionized waters, is filled
Divide and be dispersed with stirring to form mixed liquor;0.01mol ammonium tetramolybdates, 0.01mol zirconium nitrates and 0.01mol phosphoric acid hydrogen two are separately added into again
Ammonium, stirring and dissolving are uniform;Then 10g titania supports are added into above-mentioned mixed liquor, 90 DEG C of stirrings are evaporated;Collection is evaporated product
And be calcined 3 hours at 400 DEG C, obtain finished catalyst.
2. the performance test of catalyst:Specific surface area of catalyst is 115 m2/ g, automatically compared by Tristar II 3020
Surface area and pore analysis instrument are tested to obtain.The catalyst for taking 0.5 g to prepare is put into fixed bed quartz tube reactor, quartz ampoule
The cm of internal diameter=0.8, simulated flue gas is by NO, NH3、O2And N2Composition, wherein NO 1500 ppm, NH31500 ppm、O23 %, air speed
40,000 h-1, 150 ~ 300 DEG C of reaction temperature, reaction end gas Antaris IGS gas analyzer on-line checkings.In the test
Under the conditions of, the denitration efficiency of catalyst is stable in 93 more than %, N2Selectivity is more than 94%.
3. catalyst sulfur resistive water repelling property is tested:SO is additionally added in simulated flue gas2So that SO2Concentration is 1,500 mg/
m3, while additionally add H2O so that H2O volume fraction is 20%, and other test conditions are constant.In this test condition, it is catalyzed
The denitration efficiency of agent is still stablized in 90 more than %, N2Selectivity is more than 92%.
Claims (5)
1. a kind of denitrating catalyst of low temperature water resistant sulfur resistive, it is characterised in that be made up of carrier, active component and auxiliary agent, its group
Split-phase is as follows to vehicle weight percentage:Active component is 1 ~ 40%, and auxiliary agent accounts for 1 ~ 20%;Wherein, the carrier is titanium dioxide,
The active component be barium oxide, phosphorus barium oxide and cerium oxide in one or more, the auxiliary agent be tungsten oxide,
One or more in molybdenum oxide, nickel oxide and Zirconium oxide.
2. the preparation method of the denitrating catalyst of low temperature water resistant sulfur resistive as claimed in claim 1, it is characterised in that specific steps
It is as follows:
Step 1:One or more in vanadic salts and cerium oxide are dissolved in deionized water with oxalic acid, heating is sufficiently stirred point
Dissipate and form mixed liquor;
Step 2:By the one or more in tungsten salt, molybdenum salt, nickel salt and zirconates, add in the solution that step 1 is prepared, stirring is molten
Solution;
Step 3:By phosphatic one or more, add in the solution that step 2 is prepared, stirring and dissolving;
Step 3:Titania support is added in step 3 in preparing, 60 ~ 100 DEG C of stirrings are evaporated;
Step 4:Collection is evaporated product and is calcined 2 ~ 6 hours at 250 ~ 650 DEG C, obtains finished catalyst.
3. the preparation method of the denitrating catalyst of low temperature water resistant sulfur resistive according to claim 2, it is characterised in that the vanadium
Salt is the one or more in ammonium metavanadate, vanadyl oxalate and vanadic sulfate, in its solution the concentration of v element for 0.001 ~
0.1mol/L;The phosphate be phosphoric acid, ammonium phosphate, ammonium dihydrogen phosphate and diammonium hydrogen phosphate in one or more, its solution
The concentration of middle P elements is 0.001 ~ 0.1mol/L;The cerium salt is the one or more in cerous nitrate, cerium chloride and cerous sulfate,
The concentration of Ce elements is 0.001 ~ 1.0mol/L in its solution;The tungsten salt is ammonium metatungstate, ammonium paratungstate, sodium tungstate and wolframic acid
One or more in potassium, the concentration of wolfram element is 0.001 ~ 1.0mol/L in its solution;The molybdenum salt is ammonium dimolybdate, four molybdenums
One or more in sour ammonium, ammonium heptamolybdate and ammonium octamolybdate, the concentration of its Molybdenum in Solution element is 0.001 ~ 1.0mol/L;Institute
Nickel salt is stated as the one or more in nickel nitrate, nickel acetate or nickel chloride, in its solution the concentration of nickel element for 0.001 ~
1.0mol/L;The zirconates is the one or more in zirconium nitrate, zirconium oxychloride, acetic acid zirconium or zirconium sulfate, zirconium in its solution
The concentration of element is 0.001 ~ 1.0mol/L.
4. the preparation method of the denitrating catalyst of low temperature water resistant sulfur resistive according to claim 2, it is characterised in that oxalic acid exists
Concentration in solution is 2-4 times of vanadic salts.
5. the denitrating catalyst of low temperature water resistant sulfur resistive as claimed in claim 1 controls in the discharged nitrous oxides of stationary source flue gas
In application.
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