CN105879608A - Technology for synchronously denitrating ferrous oxalate on basis of flue gas desulfurization by aid of ammonia processes - Google Patents
Technology for synchronously denitrating ferrous oxalate on basis of flue gas desulfurization by aid of ammonia processes Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D—SEPARATION
- 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
- B01D53/46—Removing components of defined structure
- B01D53/60—Simultaneously removing sulfur oxides and nitrogen oxides
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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
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Abstract
The invention discloses a technology for synchronously denitrating ferrous oxalate on the basis of flue gas desulfurization by the aid of ammonia processes. The technology includes allowing flue gas to flow into a concentration tower, carrying out contact reaction on the flue gas and concentrated liquid in the tower, delivering flue gas from the concentration tower into the middle of an absorption tower, allowing the flue gas to upwardly flow through a packing layer and a spray layer which are arranged on the upper portion of the absorption tower, carrying out reverse contact reaction on the flue gas and circulating absorption liquid and then exhausting the flue gas from flue gas outlets; leading out partial concentrated liquid from the bottom of the concentration tower, removing iron in the partial concentrated liquid by the aid of an iron removal system, then delivering the partial concentrated liquid into an ammonium sulfate crystallization system, enabling circulating absorption liquid sprayed out of the spray layer on the upper portion of the absorption tower to sequentially flow though the packing layer on the upper portion of the tower, carrying out reverse contact reaction on the circulating absorption liquid and the flue gas, enabling the circulating absorption liquid to flow into the bottom of the absorption tower, delivering the circulating absorption liquid to a photocatalytic regeneration reaction system, regenerating circulating absorption liquid, enabling the circulating absorption liquid to flow into a regeneration slurry tank, feeding ammonia water, oxalic acid and ferrous sulfate into the regeneration slurry tank, then delivering the ammonia water, the oxalic acid and the ferrous sulfate which are used as circulating absorption liquid into the spray layer on the upper portion of the absorption tower and spraying the circulating absorption liquid into the tower. The technology has the advantages of simplicity, low running cost and energy consumption, simplicity and convenience in control, good denitrating effects and high quality of byproducts.
Description
Technical field
The present invention relates to field of Environment Protection one flue gas multiple pollutant and work in coordination with Processing tecchnics, specifically
It is that a kind of ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique.
Background technology
Smelting iron and steel industry sintering circuit is SO in addition to coal-burning power plant2With the main source of NOx,
Account for the 98% and 50% of integrated complex's total emission volumn, after sintering flue gas multiple pollutant Collaborative Control
Treatment technology is still that the key of pollution prevention.Sintering smoke characteristic is that exhaust gas volumn greatly and changes
Greatly;Dust content is big;SO2Discharge capacity and change in concentration are bigger;Cigarette temperature is low and fluctuation is big, and one
As 120~180 DEG C, low-temperature sintering technology can as little as about 80 DEG C;Complicated component;Oxygen-containing containing wet
Amount is big, respectively 15~18% and 7~13%.Three kinds of main pollutant consistence scopes are: SO2:
400~5000mg/Nm3;NOx:200~600mg/Nm3;Flue dust: 2000~6000mg/Nm3。
The most also discharge HF, HCl, various metals (Cd, Cr, Cu, Ni, Hg, Pb, Ti,
V, Zn, Mn etc.), gas chromatography (CH, PAHs, PCBs, PCDD/Fs etc.)
And the CO of volumetric concentration nearly 1%.
The above sintering smoke characteristic is also its difficulty in treatment, causes denitration mature technology SCR
Can not adapt to completely sinter flue gas with SNCR method.Complicated sintering flue gas may result in catalyst and loses
Living, produce the problems such as the escaping of ammonia, independent SCR and SNCR system produces in iron and steel enterprise
Producing higher production cost in flow process, built sintering system does not reserves enough desulphurization denitration spaces etc.
Factor, immediate constraint both denitration technologies application at sintering industry.Additionally steel industry
Industrial concentration is more and more higher, and newly-built sintering machine area is increasing, actual energy large-scale application
Little in the mature technology of sintering fume treatment.According to atmosphere pollution prevention and control requirement, sinter flue gas
Improvement multi-pollutant to be carried out Collaborative Control, therefore research and develop clean and effective, be suitable for, big flow
Multi-pollutant is worked in coordination with the sintering smoke gas treatment technology of improvement and sintering smoke pollution prevention and control is had weight
Want meaning.
In flue gas and desulfurizing and denitrifying field, sintering system is had and well adapts to by wet process
Property, just point out that Wet technique simultaneous SO_2 and NO removal is best desulfurization as far back as nineteen ninety Makansi
One of denitration technology, be a kind of have potential clean and effective, be suitable for, many pollutions of big flow
Thing works in coordination with the sintering smoke gas treatment technology of improvement, is also study hotspot and the difficult point of this area.
The most domestic about 526 sets, 7.8 ten thousand m2Knot machine flue gas has built up desulphurization system, tentatively realizes
Sintering flue gas SO2Control.But sintering device flue gas denitration engineering is considerably less in global range, only have
Denitration engineering the most only have demonstration and explore purpose.
In the aspect to sintering flue gas multiple pollutant Collaborative Control, Taiyuan Iron & Steel Corp in 2010
Two 450m2Sintering machine uses active carbon desulfurization denitration technology, is domestic first sintering cigarette
Desulfurization denitration engineering, but the regenerating active carbon after denitration rate only 33%, and desulphurization denitration and pair
The aspects such as Product recycling there is also many problems.
In Absorption via Chemical Complexation, that most study is exactly FeIIEDTA method, is used for sintering
Wet ammonia process desulfurizing, carries out ammoniacal liquor/Fe on this basisIIEDTA compounding realization sintering flue gas is same
Step desulphurization denitration, is that a kind of flue gas multiple pollutant that sinters with application prospect works in coordination with the skill of improvement
Art.But owing to flue gas dividing, easily by the Fe in absorbing liquid containing a certain amount of oxygenIIEDTA aoxidizes,
Cause denitration efficiency to decline, even lose denitration ability.So far, existing desulphurization denitration
Technique deposits problems with:
(1) flue gas ammoniacal liquor/FeIIEDTA compounds the complexing agent regeneration technology of synchronized desulfuring and denitrifying, adopts
With iron chip filter, iron filings consumption is big, and in absorbing liquid, iron concentration is too high, has both added except iron
Cost, has an effect on desulphurization denitration byproduct quality.
(2) when using electrolytic regeneration, equipment investment is big, and it is big that regeneration runs power consumption, and regeneration runs
Cost is high, and the denitration efficiency after regeneration is relatively low, less than 50%.
(3) synchronize denitration complexing agent FeIIEDTA is expensive, and consumption is relatively big, synchronizes denitration fortune
Row cost is high.
Summary of the invention
The invention aims to solve above-mentioned technical problem, it is provided that a kind of technique is simple, fortune
Row low cost, energy consumption are low, control is easy, denitration effect is good, byproduct matter is measured based on cigarette
The ferrous oxalate of the gas ammonia process of desulfurization synchronizes denitrating technique.
Technical scheme includes that flue gas enters concentration tower and concentrate haptoreaction in tower, goes out concentration tower
Flue gas send into and pass upward through packing layer that tower top arranges and spraying layer in the middle part of absorption tower and follow
Discharged by exhanst gas outlet after the reverse haptoreaction of ring absorbing liquid;The part drawn at the bottom of concentration tower tower is dense
Contracting liquid, described is sprayed by top, absorption tower except sending into ammonium sulfate crystallization system after iron through iron removal system
The circulating absorption solution of layer ejection sequentially passes through packing layer and the reverse haptoreaction of flue gas on tower top
Enter again after being delivered to the regeneration of Photocatalytic Regeneration reaction system by circulating pump bottom rear entrance absorption tower
Raw slurry tank, then in recycled pulp liquid bath, fill into conduct circulation after ammoniacal liquor, oxalic acid and ferrous sulfate
Absorbing liquid is transmitted back to the spraying layer on top, absorption tower and sprays in tower.
The circulating absorption solution mesoxalic acid concentration controlled in absorption tower is 0.09~0.3mol/L, iron
Ion+ferrous ion concentration is 0.015~0.05mol/L, and the pH value of circulating absorption solution is
5.0~5.5.
Concentrate bottom the absorbing liquid entering concentration tower drawn bottom described absorption tower and concentration tower
The circulation ejection of concentration tower top is sent into after the concentrate mixing that liquid circulating pump is drawn.
Concentrating and precipitating first sent into by the concentrate entering iron removal system drawn bottom described concentration tower
Pond is precipitated, and the suspension bottom concentrating and precipitating pond sends into described Photocatalytic Regeneration reaction system, on
Iron removal system sent into by the clarified solution of section.
Described Photocatalytic Regeneration reaction system is the photo catalysis reactor being provided with light source.
Described iron removal system removes iron reactor for electrolysis.
The present invention adds oxalic acid and sulphur to circulating absorption solution in existing double tower ammonia desulfurizing process
Acid is ferrous, and oxalic acid and the iron ion in absorbing liquid and ferrous ion react generation ferric oxalate and oxalic acid
Ferrous.Ferric oxalate and ferrous oxalate are the salt that oxalate denominationby is formed with iron and ferrous ion.
In aqueous, under conditions of having oxygen, ferrous oxalate is easily oxidized to ferric oxalate.Oxalic acid
Iron can form stable ferric oxalate complexes in aqueous, and these complex compounds have good light
Chemism, has relatively active redox characteristic under ultraviolet light irradiates.Fe therein3+
It is reduced into Fe2+, oxalate is oxidized and generate H under photocatalysis2O2.Photo-reduction is raw
The Fe become2+Again with H2O2React generation OH and Fe3+, Fe3+Again can be with oxalate denominationby
Re-form ferric oxalate complexes.As the oxalate denominationby and the H that there is excess in solution2O2Time,
To constantly produce hydroxy radical OH, produce the quantum yield of OH free radical up to about 1.
OH free radical is the strongest oxidant, can be absorbed by rapid oxidationAnd NO.
Oxalate denominationby is then constantly consumed with the carrying out of reaction, ultimately produces carbon dioxide.Inventor
Utilize ferric oxalate can produce the characteristic of OH free radical under photocatalysis, by under absorption just
The NO come is oxidized to nitrate anion to realize final removing, simultaneously by oxidized Fe3+It is reduced into
Fe2+.Fe in absorbing liquid2+The rising of concentration, is conducive to absorbing the NO in flue gas.Above-mentioned reaction
Process is complicated many courses of reaction, and research shows, adds oxalic acid reaction raw in absorbing liquid
Become ferrous oxalate to combine illumination reaction, the removing of part nitrogen oxides can either be realized.
Photocatalytic Regeneration reaction system in the present invention is photo catalysis reactor, photo catalysis reactor
May utilize nature light by day to react, in the case of natural lighting condition deficiency, can open
Opening the light source carried and carry out light-catalyzed reaction, described light source is the cancellated many of arranged crosswise
Layer light belt.Reacted absorbing liquid is being sent into after photo catalysis reactor, absorbing liquid mesoxalic acid iron network
Compound issues third contact of a total solar or lunar eclipse chemical reaction at illumination condition, produces hydroxy radical OH, is aoxidized by NO
Become nitrate anion to realize final removing, Fe3+It is reduced into Fe2+, Fe in solution3+Concentration fall
Low, Fe2+Concentration raise, it is achieved that the regeneration of ferrous oxalate.
Further, the partial concentration liquid entering iron removal system drawn bottom described concentration tower is first
Sending into concentrating and precipitating pond precipitation, after staticly settling, the suspension bottom concentrating and precipitating pond is sent into
Described Photocatalytic Regeneration reaction system, iron removal system sent into by the clarified solution of epimere.Use to concentrate and sink
Concentrate is concentrated layering by pond, shallow lake, and the suspension that bottom ferric oxalate content is high sends into Photocatalytic Regeneration
Reaction system regenerates, and the clarified solution of epimere is then sent into iron removal system and carries out except iron, both can subtract
The consumption of iron in few solution, can alleviate again the burden of iron removal system, improves imitating except iron of concentrate
Rate, reduces the iron content in byproduct.
In recycled pulp liquid bath, the amount of filling into of ammoniacal liquor, complexing agent, oxalic acid and ferrous sulfate can be according to following
Fe (II)+Fe (III) total concentration, oxalate denominationby concentration and solution ph in ring absorbing liquid
Requirement fills into, in line with damaging, and the principle mended.
Beneficial effect:
(1) in flue gas ammoniacal liquor sulfur removal technology, add ferrous oxalate, utilize ferrous oxalate
Complexing, it is achieved that synchronized desulfuring and denitrifying.
(2) due to ferric oxalate, the complexing of NO being weaker than ferrous oxalate, oxalic acid plays suppression
Dioxygen oxidation Fe in flue gas2+Effect, it is ensured that the concentration of denitration complexing agent, improve with
Step denitration effect.
(3) utilize concentrating and precipitating pond precipitation that concentrate carries out precipitated and separated, improve returning of iron
Yield and the utilization rate of oxalic acid, reduce the burden of iron removal system, improves the quality of byproduct.
(4) market of oxalic acid is with low cost is easy to get, and reduces operating cost.Oxalic acid has simultaneously
Stronger reproducibility, when electrolysis is except iron, advantageously reduces decomposition voltage, reduces fortune further
Row cost.
Accompanying drawing explanation
Fig. 1 present invention process flow chart.
Fig. 2 is circulating absorption solution and the absorption oxidizing process schematic diagram of flue gas in the presence of oxalic acid.
Fig. 3 is the regenerative response Principle of Process figure of circulating absorption solution under illumination condition.
Wherein, 1-concentration tower, 2-absorption tower, 2.1-packing layer, 2.2-spraying layer, 2-washing
Layer, 3-iron removal system, 4-Photocatalytic Regeneration reaction system, 5-recycled pulp liquid bath, 6-concentrate heavy
Pond, shallow lake, 7-crystal system.
Detailed description of the invention
Process example:
See Fig. 1, in certain flue gas desulphurization system, exhaust gas volumn about 14~16Nm3/ h, SO2Concentration:
500~800mg/Nm3, NOx concentration (predominantly NO): 300~400mg/Nm3.Desulfurization uses
Be double tower process.
Physical parameter and the relevant components of concentrate are as follows:
PH value: 5.0~5.5;
Ammonium sulfate concentrations: 20~45% (mass percent);
Fe (II)+Fe (III) total concentration: 0.045~0.15mol/L;
Concentration of oxalic acid: 0.27~0.9mol/L;
Absorbing liquid temperature: 50-55 DEG C.
Flue gas enters concentration tower 1 top, flows from top to bottom.Flow process is taken out with by the bottom of tower
The concentrate (containing ammoniacal liquor) that tower 1 circulating pump that go out, concentrated is sent to the ejection of concentration tower top is suitable
Concurrent biochemical absorption of stream contact is reacted, and absorbs the sulfur dioxide in flue gas and nitrogen oxides.
Flue gas flow in the middle part of concentration tower 1 after through connection flue introduce absorption tower 2 middle part, inhale
In receiving tower 2, flue gas flows to top of tower through packing layer 2.1 and spraying layer 2.2 from the bottom to top,
Last scrubbed layer 2.3 washs heel row further toward chimney.
Physical parameter and the relevant components of circulating absorption solution are as follows:
PH value: 5.0~5.5;
Ammonium sulfate concentrations: 5~15% (mass percent);
Fe (II)+Fe (III) total concentration: 0.015~0.05mol/L;
Concentration of oxalic acid: 0.09~0.3mol/L;
Absorbing liquid temperature: 50 DEG C.
The flue gas risen reacts with the circulating absorption solution generation chemical absorbing from top to bottom sprayed out,
Sulfur dioxide and nitrogen oxides in flue gas are absorbed;The oxygen carried due to flue gas is made
With, there is also ferrous oxidising one-tenth ferric iron in side reaction i.e. circulating absorption solution simultaneously, oxidized
The ferric iron generated reacts generation ferric oxalate further with the oxalate denominationby in circulating absorption solution
Complex compound Fe (C2O4)+、WithDeng.Owing to ferric oxalate complexes is to nitrogen oxygen
The complexing power of compound is more weak, along with the increase of the ferric amount of ferrous oxidising one-tenth, absorbing liquid
Gradually lose denitration ability.
In order to absorbing liquid is regenerated, it is ensured that denitration effect, the feeding tower drawn from tower bottom
The circulating absorption solution on top is introduced into Photocatalytic Regeneration reaction system before entering tower.In photocatalysis again
In raw reaction system, circulating absorption solution carries out the main as follows of light-catalyzed reaction:
In the solution of the saturation of the air, under acid conditionWithMolten with water further
Solve oxygen O2Reaction, ultimately forms H2O2。
2mol'sLight-catalyzed reaction, consumes the oxalate denominationby of 1mol, generates 1mol
Hydroxy radical OH, the NO that oxidative absorption gets off, generate the Fe of 1mol simultaneously2+, real
The regeneration of existing circulating absorption solution.
Absorbing liquid after regeneration enters recycled pulp liquid bath 5, refers to according to the physical property of absorbing liquid after regeneration
Mark requires to supplement ammoniacal liquor, oxalic acid and the ferrous sulfate of loss in recycled pulp liquid bath 5, then by following
Ring is pumped into the spraying layer 2.2 on top, absorption tower and sprays in tower.
The portion extracted out bottom 6-9L slurries and concentration tower 1 is drawn per hour bottom absorption tower 2
Concentrate is divided to be sprayed into by concentration tower 1 epimere, per hour by concentrating bottom concentration tower 1 after merging
Tower slurries excavationg pump is discharged 2-3L slurries and is entered concentrating and precipitating pond 6, sedimentation time 30-40
Hour, supernatant enters iron removal system 3, and (i.e. electrolysis is except iron reactor, as number of patent application is
201520886784.2, invention entitled " a kind of oriented flow electrolysis unit ", it is also possible to for it
It with electrolysis except the iron electrolysis reactor as principle), higher suspended of lower floor's ferrous oxalate content
Liquid alternative part oxalic acid joins in circulating absorption solution and is sprayed into absorption tower 2 by spraying layer 2.2
In;Ammonium sulfate byproduct is produced except the concentrate after iron enters crystal system 7 through iron removal system 3.
Claims (6)
1. ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes a denitrating technique, including flue gas
Entering concentration tower and concentrate haptoreaction in tower, the flue gas going out concentration tower is sent in the middle part of absorption tower
The packing layer passing upward through the setting of top, absorption tower inversely contacts with circulating absorption solution with spraying layer
Discharged by exhanst gas outlet after reaction;Extension concentrate at the bottom of concentration tower tower removes iron through iron removal system
Rear feeding ammonium sulfate crystallization system, it is characterised in that described by the ejection of top, absorption tower spraying layer
Circulating absorption solution sequentially pass through the packing layer on tower top and enter after the reverse haptoreaction of flue gas
Recycled pulp liquid is entered after being delivered to the regeneration of Photocatalytic Regeneration reaction system by circulating pump bottom absorption tower
Groove, then fill in recycled pulp liquid bath after ammoniacal liquor, oxalic acid and ferrous sulfate as circulating absorption solution
The spraying layer being transmitted back to top, absorption tower sprays in tower.
2. ferrous oxalate based on flue gas ammonia method desulfurizing as claimed in claim 1 synchronizes denitration
Technique, it is characterised in that control the circulating absorption solution mesoxalic acid concentration in absorption tower be 0.09~
0.3mol/L, iron ion+ferrous ion total concentration is 0.015~0.05mol/L, cyclic absorption
The pH value of liquid is 5.0~5.5.
3. ferrous oxalate based on flue gas ammonia method desulfurizing as claimed in claim 1 or 2 synchronizes
Denitrating technique, it is characterised in that the absorbing liquid entering concentration tower drawn bottom described absorption tower
The concentrate drawn with concentrate circulating pump bottom concentration tower is sent into concentration tower top after mixing and is followed
Ring spray goes out.
4. the ferrous oxalate based on flue gas ammonia method desulfurizing as described in claim 1 or 3 synchronizes
Denitrating technique, it is characterised in that the concentration entering iron removal system drawn bottom described concentration tower
Liquid first sends into concentrating and precipitating pond precipitation, and the suspension bottom concentrating and precipitating pond sends into described photocatalysis
Regenerative response system, iron removal system sent into by the clarified solution of epimere.
5. the ferrous oxalate based on flue gas ammonia method desulfurizing as described in claim 1 or 3 or 4
Synchronize denitrating technique, it is characterised in that described Photocatalytic Regeneration reaction system is to be provided with light source
Photo catalysis reactor.
6. the ferrous oxalate based on flue gas ammonia method desulfurizing as described in claim 1 or 4 synchronizes
Denitrating technique, it is characterised in that described iron removal system removes iron reactor for electrolysis.
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Cited By (1)
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CN110090548A (en) * | 2019-04-11 | 2019-08-06 | 昆明理工大学 | A kind of method that copper ashes tailing cooperates with the wet desulphurization of zinc abstraction dedusting ash and recycles zinc sulfate |
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CN105413418A (en) * | 2015-11-09 | 2016-03-23 | 武汉科技大学 | Electrolytic regeneration based simultaneous desulfurization and denitrification reaction tower |
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2016
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Patent Citations (3)
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US5840651A (en) * | 1993-11-19 | 1998-11-24 | Mitsui Mining Co., Ltd. | Process for the production of activated coke for simultaneous desulfurization and denitrification |
CN104226095A (en) * | 2014-07-30 | 2014-12-24 | 武汉悟拓科技有限公司 | Synchronous denitration process based on wet ammonia process flue gas desulfurization |
CN105413418A (en) * | 2015-11-09 | 2016-03-23 | 武汉科技大学 | Electrolytic regeneration based simultaneous desulfurization and denitrification reaction tower |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110090548A (en) * | 2019-04-11 | 2019-08-06 | 昆明理工大学 | A kind of method that copper ashes tailing cooperates with the wet desulphurization of zinc abstraction dedusting ash and recycles zinc sulfate |
CN110090548B (en) * | 2019-04-11 | 2021-11-30 | 昆明理工大学 | Method for wet desulphurization and zinc sulfate recovery of copper slag tailings and zinc smelting fly ash |
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