CN102631838B - Method for removing NO (nitric oxide) in flue gas - Google Patents

Method for removing NO (nitric oxide) in flue gas Download PDF

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CN102631838B
CN102631838B CN201110039827.XA CN201110039827A CN102631838B CN 102631838 B CN102631838 B CN 102631838B CN 201110039827 A CN201110039827 A CN 201110039827A CN 102631838 B CN102631838 B CN 102631838B
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flue gas
removes
catalyst
hours
gas
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CN102631838A (en
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齐文义
袁强
黄新龙
郝代军
秦如意
王龙延
刘淑芳
王洪彬
王少锋
胡艳芳
赵智刚
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China Petroleum and Chemical Corp
Sinopec Luoyang Guangzhou Engineering Co Ltd
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China Petroleum and Chemical Corp
Sinopec Luoyang Petrochemical Engineering Corp
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)

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Abstract

The invention discloses a method for removing NO (nitric oxide) in flue gas. Gas containing the NO flows through a reactor with the reaction temperature ranging from 400 DEG C to 800 DEG C at airspeed of 1000-10000h-1, from 10 to 40% of main catalyst, from 5 to 30% of auxiliary catalysts and from 30 to 70% of activated carbon are filled in the reactor by total weight of catalyst, and shortcomings that NO removal rate is low and a removal process is complex in the prior art are overcome.

Description

A kind of method that removes NO in flue gas
Technical field
The present invention relates to the method for NO, particularly a kind of SCR removes the method for NO in flue gas.
Background technology
At present, the method that removes NO in flue gas mainly can be divided into SCR and SNCR.SCR is under the effect of catalyst, at lower temperature, with suitable reducing agent, by NO selective reduction, is N 2; SNCR is at higher temperature, with reducing agent, by NO selective reduction, is N 2.Comparatively speaking, SCR because its operating temperature is low, it is de-that NO efficiency is high is used widely.In SCR, according to the difference of reducing agent, can be divided into again ammine selectivity catalytic reduction NO (NH 3-SCR), hydrocarbon Selective Catalytic Reduction of NO (HC-SCR) and carbon monoxide selective Reduction of NO (CO-SCR) technology.Wherein, NH 3-SCR technology is the mainstream technology of the de-NO of stationary source flue gas, be used widely abroad, and CO-SCR technology is also more and more subject to people's attention in recent years.Except above-mentioned SCR and SNCR, the de-NO of catalytic oxidation and activated coke adsorption reaction is also paid close attention to by people.USP4925825, CN1443595A, CN101496996A and document < < Environmental science and technology > > the 7th phase of 32 volumes in 2009 " FCC discarded object catalyzing N H 3the experimental study of reductive NO " etc. disclosed and take ammonia and remove the method for NO in flue gas as reducing agent; USP6379536 and USP6280607 etc. have introduced the agent that removes for FCC process NO, its essence is that utilizing the CO producing in FCC catalyst regeneration process is reducing agent, remove the NO discharge of FCC process under such removes the catalytic action of agent; USP4,828,680 disclose and in FCC catalyst, have added 0.1～10wt% carbon material, can reduce the NOx content in certain flue gas in trapping metals vanadium.USP5,015, the 362 a kind of methods that disclose catalyzed conversion NOx are the NOx method in catalyzed conversion FCC flue gas especially, adds bismuth or the bismuth oxide NOx reforming catalyst of 0.1～10wt% carbon material and 0.01～10wt% in FCC regenerator, can make the NOx in flue gas reduce by 90% left and right.DE-A-4404617 and DE-A-19600558 have disclosed take hydro carbons and removes the method for NO in flue gas as reducing agent.CN101352645A discloses a kind of catalytic oxidation denitration technique, with TiO 2or ZrO 2-TiO 2for carrier, the catalyst that Co is active component, utilizes the oxygen that in flue gas, self contains, and NO is oxidized to NO soluble in water 2after, utilize alkali liquor absorption, by removal of nitrogen oxide.CN1768902 discloses a kind of denitration of boiler smoke method, and the boiler flue low-temperature zone that is 110～150 ℃ in temperature range sprays into ozone O 3, nitric oxide NO in boiler smoke is oxidized into high valence state nitrogen oxide NO soluble in water 2, NO 3or N 2o 5, then use alkali lye water washing pan kiln gas, remove the nitrogen oxide in flue gas.CN100377763C discloses a kind of method of purifying flue gas by application of active coke, comprise that flue gas purifies in the desulfurization and denitrification reaction device consisting of two sections of moving-burden bed reactors of activated coke is housed, its flow process is: flue gas is introduced into bottom the second segment reactor from the activated coke of first paragraph reactor, the SO in adsorbing and removing flue gas are housed 2, then with NH 3or H 2after mixing with CO mist, enter the reactor that top first paragraph is added with activated coke, react and remove nitrogen oxide with activated coke wherein.
Above-mentioned, manyly also there are some defects in the method for NO in removing flue gas, the de-NO method that the ammonia of take is reducing agent, generally to using ammonia and urea or the aqueous solution of urea source as reducing agent, if the ammonia or the urea amount that use these reducing agents to inject are too much, to cause so-called ammonia to penetrate, the NOx of the ammonia brake specific exhaust emission emitting is more harmful, too much ammonia consumption may cause the generation of NOx through peroxidating, another shortcoming is, must store them, so that regular replenishment, ammonia particularly, in transportation storage process, the requirement of safety and environmental protection is very high, must cause investment and the running cost of this technology to improve, moreover its process used catalyst also can be subject to the pollution of impurity in the washing away of high concentration flue dust, wearing and tearing and flying dust, too high catalyst generation sintering, inactivation, the SO of also can making of flue-gas temperature 2existence can cause the fast-descending of catalyst activity.
The hydro carbons of take removes the NO in flue gas as reducing agent, need to be by cracking hydrocarbon; Catalytic oxidation need to be oxidized and alkali liquor absorption; Ozone oxidation needs special ozone generator, after oxidation, absorbs again; Complex process, de-NO expense are high; And in catalytic cracking process, add the problem that agent also exists the low and dilution FCC major catalyst of NO removal efficiency that removes.
Summary of the invention
A kind of method that removes NO in flue gas provided by the invention, its concrete steps are as follows:
1) by the Catalyst packing of 10%～40 % by weight major catalyst, 5%～30 % by weight cocatalyst and 30%～70 % by weight active carbon in reactor, in total catalyst weight.
2) gas that contains NO, with 1000～10000h -1air speed, preferred 3000～7000h -1air speed, by reaction temperature, be 400 ℃～800 ℃, the reactor of preferably 500 ℃～700 ℃ reacts, reacted gas is discharged;
3) in reactor, add catalyst, keep NO removal efficiency to be greater than 85%.
Described reactor of the present invention can be moving bed or fluid bed.Catalyst make-up amount, maintains the activity of catalyst reactor, keeps NO removal efficiency to be greater than 85%.
Described major catalyst is, micro-activity lower than 55, surperficial V, Ca, Na, Ni, Cu, Fe tenor be greater than 2.0 % by weight, in major catalyst gross weight, FCC dead catalyst particularly.
Described cocatalyst, prepares through following process:
1) chemical pure cerium salt and mantoquita are joined successively in the deionized water of 50～90 ℃, stir 1.5～3 hours, after dissolving completely, add boehmite, stirs 2～4 hours, then add binding agent, continue stirring 3-10 hour, obtain slurries to step 2);
2) in fire box temperature, being to step 1 under 300～400 ℃, 180～250 ℃ of plug for outlet temperature, 30～50 atmospheric pressure of pressure) slurries are dried, obtain granular substance and be dried 5～12 hours at 120～150 ℃, at 550～650 ℃, roasting is 3～12 hours, obtains intermediate product to step 3);
3) by step 2) intermediate product at Pd content, be in the aqueous citric acid solution of 2000～4000 μ g/g
Flood after 3～6 hours, then be dried 1～5 hour at 120～150 ℃, at 550～650 ℃, roasting is 3～5 hours, obtains cocatalyst.
Described cerium salt comprises chloride, nitrate, sulfate or the acylate of cerium, preferably chloride and nitrate; Described mantoquita comprises chloride, nitrate, sulfate or the acylate of copper, preferably chloride and nitrate; Described binding agent comprises the miscible glue of aluminium colloidal sol, Ludox or sial, preferably aluminium colloidal sol.
Described active carbon is that graininess, bulk density are at 0.6～1.1g/cm 3, average grain diameter is 40～80 μ m particulate materials.
A kind of method that removes NO in flue gas of the present invention is compared with prior art: owing to using the source thing that the active carbon of major catalyst and general material is reducing agent CO, CO generates and removing of NO carried out simultaneously in a reactor, thereby technique is simple, operating cost is relatively low; Simultaneously the method also has pollution, the SO of impurity in NO removal efficiency is high, range of reaction temperature is wide, catalyst is not afraid of flue dust erosive wear and flying dust 2can not affect the advantages such as its de-NO performance.
The specific embodiment
By specific embodiment, further illustrate de-NO effect of the present invention below, do not limit the scope of the invention.
Embodiment 1～6 is cocatalyst preparation example
Embodiment 1
The chemical pure level Ce (NO that 133g Tianjin BASF Chemical Co., Ltd. is produced 3) 36H 2o (purity>=95%), the chemical pure level CuCl that 205g Tianjin BASF Chemical Co., Ltd. produces 23H 2o (purity>=95%) joins in 400g, the deionized water of 70 ℃ successively, stir 2 hours, it is dissolved completely, continue to stir, the boehmite (purity>=98.5%) that adds the technical grade of 406g Shandong Aluminium Industry Co., Ltd production, stir 3 hours, then add the aluminium colloidal sol (Al of the technical grade of 256g Mengjin petrochemical plant production 2o 3butt is 19.5%) and the Ludox (SiO of the technical grade produced of 89g Mengjin petrochemical plant 2butt 28.0%), continue to stir 5 hours, obtain slurries; In fire box temperature, be that 350 ℃, 200 ℃ of outlet temperatures, atomisation pressure are at 35 atmospheric pressures, the slurries that spray drying forming obtains, by gained granular substance at 130 ℃ in drying box dry 6 hours, in Muffle furnace, roasting 7 hours at 580 ℃, obtained intermediate product.Get 200g intermediate product, the Pd content of 24g laboratory preparation is the aqueous citric acid solution of 3000 μ g/g, with distilled water diluting, adopt equi-volume process dipping 5 hours, in drying box at 130 ℃ dry 3 hours, roasting 4 hours at 580 ℃ in Muffle furnace, obtain object product A, physicochemical property is in Table 1.
Embodiment 2
The chemical pure level CeCl that 179g Tianjin BASF Chemical Co., Ltd. is produced 27H 2o (purity>=96%), the chemical pure level Cu (NO that 112g Tianjin BASF Chemical Co., Ltd. produces 3) 23H 2o (purity>=95%) joins in 400g, the deionized water of 70 ℃ successively, stir 2 hours, it is dissolved completely, continue to stir, the boehmite that adds the 393g place of production identical with embodiment 1 and grade, stirs 3 hours, then adds the aluminium colloidal sol of the 513g place of production identical with embodiment 1 and grade, remaining step, with embodiment 1, obtains intermediate product.Get 200g intermediate product, the Pd solution that 10g is identical with embodiment 1, remaining step, with embodiment 1, obtains object product B, and physicochemical property is in Table 1.
Embodiment 3
By the Ce (NO of the 66g place of production identical with embodiment 1 and grade 3) 36H 2o, the CuCl of the 68g place of production identical with embodiment 1 and grade 24H 2o, join successively in 400g, the deionized water of 70 ℃, stir 2 hours, it is dissolved completely, continue to stir, add the boehmite of the 541g place of production identical with embodiment 1 and grade, stir 3 hours, the Ludox that adds again the 179g place of production identical with embodiment 1 and grade, remaining step, with embodiment 1, obtains intermediate product.Get 200g intermediate product, the Pd solution that 3.5g is identical with embodiment 1, remaining step, with embodiment 1, obtains object product C, and physicochemical property is in Table 1.
Embodiment 4
By the Ce (NO of the 106g place of production identical with embodiment 1 and grade 3) 36H 2o, the Cu (NO of the 112g place of production identical with embodiment 1 and grade 3) 23H 2o, join successively in 400g, the deionized water of 70 ℃, stir 2 hours, it is dissolved completely, continue to stir, add the boehmite of the 440g place of production identical with embodiment 1 and grade, stir 3 hours, the aluminium colloidal sol that adds again the 513g place of production identical with embodiment 1 and grade, remaining step, with embodiment 1, obtains intermediate product.Get 200g intermediate product, the Pd solution that 14g is identical with embodiment 1, remaining step, with embodiment 1, obtains object product D, and physicochemical property is in Table 1.
Embodiment 5
By the CeCl of the 135g place of production identical with embodiment 1 and grade 27H 2o, the Cu (NO of the 48g place of production identical with embodiment 1 and grade 3) 23H 2o, join successively in 400g, the deionized water of 70 ℃, stir 2 hours, it is dissolved completely, continue to stir, add the boehmite of the 508g place of production identical with embodiment 1 and grade, stir 3 hours, the Ludox that adds again the 179g place of production identical with embodiment 1 and grade, remaining step, with embodiment 1, obtains intermediate product.Get 200g intermediate product, the Pd solution that 17g is identical with embodiment 1, remaining step, with embodiment 1, obtains object product E, and physicochemical property is in Table 1.
Embodiment 6
By the Ce (NO of the 133g place of production identical with embodiment 1 and grade 3) 36H 2o, the Cu (NO of the 160g place of production identical with embodiment 1 and grade 3) 23H 2o, join successively in 400g, the deionized water of 70 ℃, stir 2 hours, it is dissolved completely, continue to stir, add the boehmite of the 406g place of production identical with embodiment 1 and grade, stir 3 hours, the aluminium colloidal sol that adds again the 513g place of production identical with embodiment 1 and grade, remaining step, with embodiment 1, obtains intermediate product.Get 200g intermediate product, the Pd solution that 7g is identical with embodiment 1, remaining step, with embodiment 1, obtains object product F, and physicochemical property is in Table 1.
Table 1 cocatalyst physicochemical property
Embodiment 7～13 is the de-NO performance evaluation example of cocatalyst.
In being the quartz ampoule moving-burden bed reactor of 38mm, catalyst inventory 500g, internal diameter packs altogether 200gFCC dead catalyst, cocatalyst and Mixture of Activated Carbon into.FCC dead catalyst is for taking from domestic certain heavy-oil catalytic poising agent, and wherein the specific area of this poising agent is 105m 2/ g, pore volume 0.124cm 3/ g, metal Ni is 9500 μ g/g, V8700 μ g/g, Ca11500 μ g/g, Fe10380 μ g/g, Cu95 μ g/g, micro-activity 52; Active carbon is the granular active carbon of the chemical pure level of brilliance timber mill, Beijing production.During evaluation, in the situation that passing into Ar, be warming up to 630 ℃, stop Ar gas, pass into NO, O 2, SO 2, Ar gaseous mixture, in gaseous mixture, NO concentration is 2500mg/m 3, SO 2concentration is 750mg/m 3, O 2concentration is 3.7% (v), all the other are Ar, and gas flow adopts mass-flow gas meter to control, and gaseous mixture volume air speed is 6000h -1, with the portable flue gas inspection instrument of KM-9106 type, carry out the NO content in the rear gas of on-line analysis reaction, with following formula, calculate the NO of removing efficiency of the present invention:
Remove NO efficiency calculation:
X = C 1 - C 2 C 1 &times; 100 % - - - ( 1 )
In formula: X is NO removal efficiency of the present invention (%); C 1for reacting the content (mg/m of NO in rear gas 3); C 2for reacting the content (mg/m of NO in front gaseous mixture 3), the de-NO performance that table 2 is cocatalyst of the present invention.
Table 2 cocatalyst takes off NO performance
Embodiment 14～21st, and the prepared D of the embodiment of the present invention 4 of take is cocatalyst, the investigation example to catalytic component composition, reaction condition.
Embodiment 14
In moving-burden bed reactor, pack altogether 200g catalyst into, wherein FCC dead catalyst accounts for 40 % by weight, and cocatalyst accounts for 10 % by weight, and active carbon accounts for 50 % by weight.Under Ar air-flow, be warming up to 450 ℃, stop Ar gas, pass into NO, O 2, Ar gaseous mixture, in gaseous mixture, NO concentration is 2500mg/m 3, O 2concentration is 3.7% (v), all the other are Ar, and gaseous mixture air speed is 6000h -1, with the NO content in gas after multi-functional flue gas analyzer on-line analysis reaction, according to the calculating of (1) formula, removing NO efficiency is 80.6%.
Embodiment 15
Press the method for embodiment 1, the FCC dead catalyst, cocatalyst and the active carbon that add equal in quality, same ratio, under identical air speed, pass into and form identical NO mist, reaction temperature is elevated to 580 ℃, and according to the calculating of (1) formula, removing NO efficiency is 86.4%.
Embodiment 16
Press the method for embodiment 1, the FCC dead catalyst, cocatalyst and the active carbon that add equal in quality, same ratio, under identical air speed, pass into and form identical NO mist, reaction temperature is elevated to 650 ℃, and according to the calculating of (1) formula, removing NO efficiency is 94.7%.
Embodiment 17
Press the method for embodiment 1, the FCC dead catalyst, cocatalyst and the active carbon that add equal in quality, same ratio, under identical air speed, pass into and form identical NO mist, reaction temperature is elevated to 730 ℃, and according to the calculating of (1) formula, removing NO efficiency is 82.3%.
Embodiment 18
In moving-burden bed reactor, pack altogether 200g catalyst into, wherein FCC dead catalyst accounts for 45%, and cocatalyst accounts for 5%, and active carbon accounts for 50%.Under Ar air-flow, be warming up to 630 ℃, stop Ar gas, in air speed 6000 -1under, pass into and form the mist identical with embodiment 1, according to the calculating of (1) formula, removing NO efficiency is 88.5%.
Embodiment 19
In moving-burden bed reactor, pack altogether 200gFCC dead catalyst, cocatalyst and active carbon into, wherein FCC dead catalyst accounts for 35%, and cocatalyst accounts for 15%, and active carbon accounts for 50%.Under Ar air-flow, be warming up to 630 ℃, stop Ar gas, in air speed 6000 -1under, pass into and form the mist identical with embodiment 1, according to the calculating of (1) formula, removing NO efficiency is 92.6%.
Embodiment 20
In moving-burden bed reactor, pack altogether 200gFCC dead catalyst, cocatalyst and active carbon into, wherein FCC dead catalyst accounts for 35%, and cocatalyst accounts for 15%, and active carbon accounts for 50%.Under Ar air-flow, be warming up to 630 ℃, stop Ar gas, in air speed 6000 -1under, passing into mist composed as follows, NO concentration is 2500mg/m 3, SO 2concentration is 750mg/m 3, O 2concentration is 3.7% (v), all the other are Ar, calculates that to remove NO efficiency be 90.8% according to (1) formula.
Embodiment 21
In moving-burden bed reactor, pack altogether 200gFCC dead catalyst, cocatalyst and active carbon into, wherein FCC dead catalyst accounts for 35%, and cocatalyst accounts for 15%, and active carbon accounts for 50%.Under Ar air-flow, be warming up to 630 ℃, stop Ar gas, in air speed 12000 -1under, pass into and form the mist identical with embodiment 1, according to the calculating of (1) formula, removing NO efficiency is 82.6%.

Claims (12)

1. a method that removes NO in flue gas, is characterized in that, concrete steps are as follows:
1) by 10%～40 % by weight FCC dead catalyst, 5%～30 % by weight cocatalyst and 30%～70 % by weight bulk density at 0.6～1.1g/cm 3, average grain diameter is that the Catalyst packing of 40～80 μ m active carbons is in reactor, in total catalyst weight;
2) gas that contains NO, with 1000～10000h -1air speed, the moving bed or the fluidized-bed reactor that by reaction temperature, are 400 ℃～800 ℃ react, reacted gas is discharged.
2. according to a kind of method that removes NO in flue gas claimed in claim 1, it is characterized in that: in reactor, add catalyst, the active low catalyst of removal part, keeps NO removal efficiency to be greater than 85% simultaneously.
3. according to a kind of method that removes NO in flue gas claimed in claim 1, it is characterized in that: the micro-activity of described FCC dead catalyst lower than 55, surperficial V, Ca, Na, Ni, Cu, Fe tenor be greater than 2.0 % by weight, in FCC total weight.
4. according to a kind of method that removes NO in flue gas claimed in claim 1, it is characterized in that: the gas that contains NO is with 3000～7000h -1air speed pass through reactor.
5. according to a kind of method that removes NO in flue gas claimed in claim 1, it is characterized in that: the gas that contains NO, by the reactor of 500 ℃～700 ℃.
6. according to a kind of method that removes NO in flue gas claimed in claim 1, it is characterized in that: described cocatalyst, preparation method is as follows:
1) chemical pure cerium salt and mantoquita are joined successively in the deionized water of 50～90 ℃, stir 1.5～3 hours, after dissolving completely, add boehmite, stirs 2～4 hours, then add binding agent, continue stirring 3-10 hour, obtain slurries to step 2);
2) in fire box temperature, being to step 1 under 300～400 ℃, 180～250 ℃ of plug for outlet temperature, 30～50 atmospheric pressure of pressure) slurries are dried, obtain granular substance and be dried 5～12 hours at 120～150 ℃, at 550～650 ℃, roasting is 3～12 hours, obtains intermediate product to step 3);
3) by step 2) intermediate product in Pd content is the aqueous citric acid solution of 2000～4000 μ g/g, flood after 3～6 hours, then at 120～150 ℃ dry 1～5 hour, at 550～650 ℃, roasting was 3～5 hours, obtains cocatalyst.
7. according to a kind of method that removes NO in flue gas claimed in claim 6, it is characterized in that: chloride, nitrate, sulfate or acylate that described cerium salt is cerium.
8. according to a kind of method that removes NO in flue gas claimed in claim 6, it is characterized in that: described cerium salt is chloride or nitrate.
9. according to a kind of method that removes NO in flue gas claimed in claim 6, it is characterized in that: the chloride that described mantoquita is copper, nitrate, sulfate or acylate.
10. according to a kind of method that removes NO in flue gas claimed in claim 6, it is characterized in that: described mantoquita is chloride or nitrate.
11. according to a kind of method that removes NO in flue gas claimed in claim 6, it is characterized in that: described binding agent is aluminium colloidal sol, Ludox or silicon-aluminum sol.
12. according to a kind of method that removes NO in flue gas claimed in claim 6, it is characterized in that: described binding agent is aluminium colloidal sol.
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