CN105879608B - Ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique - Google Patents

Ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique Download PDF

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CN105879608B
CN105879608B CN201610255821.9A CN201610255821A CN105879608B CN 105879608 B CN105879608 B CN 105879608B CN 201610255821 A CN201610255821 A CN 201610255821A CN 105879608 B CN105879608 B CN 105879608B
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tower
flue gas
concentration
iron
absorption
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CN105879608A (en
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吴晓琴
刘成
吴高明
张春桃
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Wuhan University of Science and Engineering WUSE
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/60Simultaneously removing sulfur oxides and nitrogen oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/73After-treatment of removed components
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77Liquid phase processes
    • B01D53/78Liquid phase processes with gas-liquid contact
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/96Regeneration, reactivation or recycling of reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2258/00Sources of waste gases
    • B01D2258/02Other waste gases
    • B01D2258/025Other waste gases from metallurgy plants

Abstract

The invention discloses a kind of, and the ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique, enter concentration tower and concentrate haptoreaction in tower including flue gas, the packing layer for passing upward through the setting of absorption tower top is sent into the middle part of absorption tower for the flue gas for going out concentration tower and spraying layer is discharged with after the reverse haptoreaction of circulating absorption solution by exhanst gas outlet;Concentration tower bottom of tower extension concentrate is through iron removal system except feeding ammonium sulfate crystallization system after iron, the circulating absorption solution by the ejection of absorption tower top spraying layer enters absorb the bottom of the tower after the packing layer on tower top and the reverse haptoreaction of flue gas and is pumped to after the regeneration of Photocatalytic Regeneration reaction system into recycled pulp liquid bath by recycling successively, then is transmitted back to as circulating absorption solution in the spraying layer penetrating tower on absorption tower top after filling into ammonium hydroxide, oxalic acid and ferrous sulfate in regenerating slurry tank.Present invention process is simple, operating cost is low, low energy consumption, control is easy, denitration effect is good, byproduct is high-quality.

Description

Ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique
Technical field
The present invention relates to a kind of flue gas multiple pollutants of field of environment protection to cooperate with Processing tecchnics, specifically a kind of to be based on flue gas The ferrous oxalate of the ammonia process of desulfurization synchronizes denitrating technique.
Background technology
Iron and steel smelting industry sintering circuit is the SO in addition to coal-burning power plant2With the main source of NOx, it is total to account for integrated complex's discharge The 98% and 50% of amount, the post-processing technology of sintering flue gas multi-pollutant Collaborative Control is still the key of pollution prevention.Sintering Smoke characteristic is that exhaust gas volumn is big and variation is big;Dust content is big;SO2Discharge capacity and concentration change greatly;Smoke temperature is low and fluctuation is big, General 120~180 DEG C, low-temperature sintering technology can be down to 80 DEG C or so;Complicated component;Oxygen-containing water capacity is big, respectively 15~ 18% and 7~13%.Three kinds of main pollutant consistences are ranging from:SO2:400~5000mg/Nm3;NOx:200~600mg/Nm3; Flue dust:2000~6000mg/Nm3.In addition HF, HCl, various metals (Cd, Cr, Cu, Ni, Hg, Pb, Ti, V, Zn, Mn are also discharged Deng), the CO of gas chromatography (CH, PAHs, PCBs, PCDD/Fs etc.) and volumetric concentration nearly 1%.
Sintering flue gas feature described above is also its difficulty in treatment, causes denitration mature technology SCR and SNCR method cannot be complete It is complete to adapt to sintering flue gas.Complicated sintering flue gas can lead to catalyst inactivation, generate the escaping of ammonia, independent SCR and SNCR systems generate higher production cost in iron and steel enterprise's production procedure, and it is empty that built sintering system does not reserve enough desulphurization denitrations Between etc. factors, immediate constraint applications of both denitration technologies in sintering industry.In addition steel industry industrial concentration is more next Higher, newly-built sintering machine area is increasing, and the mature technology that practical energy large-scale application is handled in sintering flue gas is seldom.According to Atmosphere pollution prevention and control requirement, sintering flue gas improvement will carry out multi-pollutant Collaborative Control, therefore research and develop clean and effective, be applicable in, be big The sintering flue gas Treatment process that the multi-pollutant collaboration of flow is administered is of great significance to sintering flue gas pollution prevention.
In flue gas and desulfurizing and denitrifying field, wet process has well adapting to property to sintering system, early in nineteen ninety Makansi just points out one of the desulphurization denitration technology that Wet technique simultaneous SO_2 and NO removal is best, is that a kind of tool is potential clear It is clean it is efficient, be applicable in, the multi-pollutant of big flow collaboration administer sintering flue gas Treatment process and this field research hotspot and Difficult point.
The current country about 526 sets, 7.8 ten thousand m2Knot machine flue gas has built up desulphurization system, preliminary to realize sintering flue gas SO2Control. But sintering device flue gas denitration engineering is considerably less in global range, and only denitration engineering, which also only has, demonstrates and explore purpose.
In terms of to sintering flue gas multi-pollutant Collaborative Control, two 450m of Taiyuan Iron & Steel Corp in 20102Sintering Machine uses active carbon desulfurization denitration technology, is domestic first sintering flue gas desulfurization denitration engineering, but denitrification rate only 33%, and de- There is also many problems for regenerating active carbon and byproduct recycling after sulphur denitration etc..
That most study is exactly Fe in Absorption via Chemical ComplexationIIEDTA methods, for wet ammonia process desulfurizing used by sintering, herein On the basis of carry out ammonium hydroxide/FeIIEDTA compoundings realize sintering flue gas synchronized desulfuring and denitrifying, are a kind of sintering cigarettes with application prospect The technology that the collaboration of gas multi-pollutant is administered.But due to containing a certain amount of oxygen in flue gas, easily by the Fe in absorbing liquidIIEDTA oxygen Change, causes denitration efficiency to decline, or even lose denitration ability.So far, existing desulfurizing and denitrifying process deposits problems with:
(1) flue gas ammonium hydroxide/FeIIEDTA compounds the complexing agent regeneration technology of synchronized desulfuring and denitrifying, and using iron chip filter, iron filings disappear Consumption is big, and iron concentration is excessively high in absorbing liquid, has both increased except iron cost, has an effect on desulphurization denitration byproduct quality.
(2) when using electrolytic regeneration, equipment investment is big, and regeneration operation power consumption is big, and regeneration operating cost is high, de- after regeneration Nitre is less efficient, less than 50%.
(3) denitration complexing agent Fe is synchronizedIIEDTA is expensive, and consumption is larger, and synchronous denitration operating cost is high.
Invention content
The purpose of the present invention is to solve above-mentioned technical problem, provide it is a kind of it is simple for process, operating cost is low, energy consumption Low, control simplicity, denitration effect are good, the high-quality ferrous oxalate based on flue gas ammonia method desulfurizing of byproduct synchronizes denitrating technique.
Technical solution includes that flue gas enters concentration tower and concentrate haptoreaction in tower, and the flue gas for going out concentration tower is sent into absorption Pass upward through in the middle part of tower the setting of tower top packing layer and spraying layer with after the reverse haptoreaction of circulating absorption solution by exhanst gas outlet Discharge;The partial concentration liquid that concentration tower bottom of tower is drawn is sent into ammonium sulfate crystallization system after iron removal system removes iron, described by absorbing The circulating absorption solution that tower top spraying layer sprays enters after the packing layer on tower top and the reverse haptoreaction of flue gas successively to be inhaled It receives tower bottom to be pumped to after the regeneration of Photocatalytic Regeneration reaction system into recycled pulp liquid bath by recycling, then is mended in regenerating slurry tank It is transmitted back in the spraying layer penetrating tower on absorption tower top as circulating absorption solution after entering ammonium hydroxide, oxalic acid and ferrous sulfate.
A concentration of 0.09~0.3mol/L of circulating absorption solution mesoxalic acid in absorption tower is controlled, iron ion+ferrous ion is dense Degree is 0.015~0.05mol/L, and the pH value of circulating absorption solution is 5.0~5.5.
What the absorbing liquid into concentration tower that the absorb the bottom of the tower is drawn was drawn with concentration tower bottom concentrate circulating pump Concentration tower top cycle is sent into after concentrate mixing to spray.
The concentrate into iron removal system that the concentration tower bottom is drawn first is sent into concentrating and precipitating pond precipitation, concentrating and precipitating The suspension in bottom of pond portion is sent into the Photocatalytic Regeneration reaction system, and the clarified solution of epimere is sent into iron removal system.
The Photocatalytic Regeneration reaction system is the photo catalysis reactor equipped with light source.
The iron removal system is that electrolysis removes iron reactor.
Oxalic acid and ferrous sulfate, oxalic acid and suction is added to circulating absorption solution in existing double tower ammonia desulfurizing process in the present invention Iron ion and the ferrous ion reaction received in liquid generate ferric oxalate and ferrous oxalate.Ferric oxalate and ferrous oxalate are oxalate denominationbies The salt formed with iron and ferrous ion.
In aqueous solution, ferrous oxalate is easily oxidized to ferric oxalate under conditions of having oxygen.Ferric oxalate in aqueous solution may be used Stable ferric oxalate complexes are formed, these complex compounds have good photochemical activity, have under ultraviolet light relatively living The redox characteristic of jump.Fe therein3+It is reduced into Fe2+, oxalate aoxidized under photocatalysis and generates H2O2.Light Restore the Fe generated2+Again with H2O2It reacts and generates OH and Fe3+, Fe3+Ferric oxalate can be re-formed with oxalate denominationby again Complex compound.When there are excessive oxalate denominationby and H in solution2O2When, hydroxy radical OH will be constantly generated, generates OH certainly By the quantum yield of base up to 1 or so.OH free radicals are very strong oxidants, can rapid oxidation absorbedWith NO.Oxalate denominationby is then constantly consumed with the progress of reaction, ultimately produces carbon dioxide.Inventor is exactly existed using ferric oxalate The characteristic that OH free radicals can be generated under photocatalysis, is oxidized to nitrate anion to realize final removing by the NO absorbed, The Fe that will be aoxidized simultaneously3+It is reduced into Fe2+.Fe in absorbing liquid2+The raising of concentration is conducive to absorb the NO in flue gas.It is above-mentioned anti- It is a complicated more reaction process to answer process, studies have shown that oxalic acid reaction is added in absorbing liquid generates ferrous oxalate combination light According to reaction, the removing of part nitrogen oxides can either be realized.
Photocatalytic Regeneration reaction system in the present invention is photo catalysis reactor, and photo catalysis reactor is on daytime using certainly Right light is reacted, insufficient in natural lighting condition, can be opened included light source and be carried out light-catalyzed reaction, the light Source is the multilayer optical band of the reticular structure of arranged crosswise.Absorbing liquid after reaction is after being sent into photo catalysis reactor, in absorbing liquid Ferric oxalate complexes issue third contact of a total solar or lunar eclipse chemical reaction in illumination condition, generate hydroxy radical OH, NO is oxidized to nitrate anion with reality Now final removing, Fe3+It is reduced into Fe2+, Fe in solution3+Concentration reduce, Fe2+Concentration increase, realize ferrous oxalate Regeneration.
Further, the partial concentration liquid into iron removal system that the concentration tower bottom is drawn first is sent into concentrating and precipitating pond Precipitation, after staticly settling, the suspension in concentrating and precipitating bottom of pond portion is sent into the Photocatalytic Regeneration reaction system, the clarification of epimere Liquid is sent into iron removal system.Concentrate is concentrated using concentrating and precipitating pond and is layered, oxalic acid iron content high suspension in bottom is sent into light Catalytic regeneration reaction system regenerates, and the clarified solution of epimere is then sent into iron removal system and carries out removing iron, can both reduce iron in solution Consumption, and the burden of iron removal system can be mitigated, improve the de-ironing efficiency of concentrate, reduce the iron content in byproduct.
The amount of filling into for regenerating ammonium hydroxide in slurry tank, complexing agent, oxalic acid and ferrous sulfate can be according to Fe in circulating absorption solution (II) requirement of+Fe (III) total concentration, oxalate denominationby concentration and solution ph is filled into, in line with damaging, the principle mended.
Advantageous effect:
(1) ferrous oxalate is added in flue gas ammonium hydroxide sulfur removal technology, using the complexing of ferrous oxalate, realized same Walk desulphurization denitration.
(2) ferrous oxalate is weaker than to the complexing of NO due to ferric oxalate, oxalic acid plays the dioxygen oxidation inhibited in flue gas Fe2+Effect, ensure that the concentration of denitration complexing agent, improve synchronous denitration effect.
(3) it is precipitated using concentrating and precipitating pond and precipitated and separated is carried out to concentrate, improve the rate of recovery of iron and the utilization of oxalic acid Rate reduces the burden of iron removal system, improves the quality of byproduct.
(4) market of oxalic acid is of low cost is easy to get, and reduces operating cost.Oxalic acid has stronger reproducibility simultaneously, in electricity When releasing iron, decomposition voltage is advantageously reduced, operating cost is further decreased.
Description of the drawings
Fig. 1 present invention process flow charts.
Fig. 2 is the absorption oxidation process schematic diagram of circulating absorption solution and 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 towers, the absorption towers 2-, 2.1- packing layers, 2.2- spraying layers, 2- scrubber layers, 3- iron removal systems, 4- light Catalytic regeneration reaction system, 5- regeneration slurry tank, 6- concentrating and precipitatings pond, 7- crystal systems.
Specific implementation mode
Process example:
Referring to 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 is using double tower process.
The physical parameter and relevant components of concentrate are as follows:
PH value:5.0~5.5;
Ammonium sulfate concentrations:20~45% (mass percents);
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℃.
Flue gas enters 1 top of concentration tower, flows from top to bottom.It is followed with extracted out by bottom of tower, concentrated tower 1 in flow process Ring pumps concentrate (the containing ammonium hydroxide) co-current contact sprayed toward concentration tower top concurrently biochemical absorbing reaction, absorbs in flue gas Sulfur dioxide and nitrogen oxides.
Flue gas flows to the middle part through connection flue introducing absorption tower 2 behind 1 middle part of concentration tower, and flue gas is under in absorption tower 2 Supreme to be flowed to top of tower by packing layer 2.1 and spraying layer 2.2, last washed layer 2.3 further washs heel row toward chimney.
The physical parameter and relevant components of circulating absorption solution are as follows:
PH value:5.0~5.5;
Ammonium sulfate concentrations:5~15% (mass percents);
Fe (II)+Fe (III) total concentration:0.015~0.05mol/L;
Concentration of oxalic acid:0.09~0.3mol/L;
Absorbing liquid temperature:50℃.
The flue gas of rising occurs chemical absorbing with the circulating absorption solution from top to bottom sprayed out and reacts, the titanium dioxide in flue gas Sulphur and nitrogen oxides are absorbed;Due to the oxygen effect that flue gas carries, while there is also in side reaction, that is, circulating absorption solution It is ferrous oxidising at ferric iron, generation is further reacted with the oxalate denominationby in circulating absorption solution by the ferric iron that oxidation generates Ferric oxalate complexes Fe (C2O4)+WithDeng.Complexing due to ferric oxalate complexes to nitrogen oxides Ability is weaker, and with the ferrous oxidising increase at ferric amount, absorbing liquid gradually loses denitration ability.
In order to be regenerated to absorbing liquid, ensure denitration effect, the cyclic absorption for being sent into tower top drawn from tower bottom Liquid is introduced into Photocatalytic Regeneration reaction system before entering tower.In Photocatalytic Regeneration reaction system, circulating absorption solution carries out light and urges Change the main as follows of reaction:
In the solution of the saturation of the air, under acid conditionWithFurther with oxygen in water O2Reaction, finally Form H2O2
2mol'sLight-catalyzed reaction consumes the oxalate denominationby of 1mol, generates the hydroxy radical of 1mol OH, the NO that oxidative absorption gets off, while generating the Fe of 1mol2+, realize the regeneration of circulating absorption solution.
Absorbing liquid after regeneration enters regeneration slurry tank 5, is required to recycled pulp according to the physical index of absorbing liquid after regeneration Ammonium hydroxide, oxalic acid and the ferrous sulfate of supplement loss in liquid bath 5, then be pumped by cycle the spraying layer 2.2 on absorption tower top and spray into In tower.
Per hour from 2 bottom of absorption tower draw 6-9L slurries merge with the partial concentration liquid that 1 bottom of concentration tower is extracted out after by 1 epimere of concentration tower sprays into, and it is heavy to enter concentration by concentration tower slurry discharge pump discharge 2-3L slurries from 1 bottom of concentration tower per hour Shallow lake pond 6, sedimentation time 30-40 hour, supernatant enters iron removal system 3, and (i.e. electrolysis removes iron reactor, as number of patent application is 201520886784.2, entitled " a kind of oriented flow electrolysis unit ", or other that iron is removed as principle using electrolysis Electrolysis reactor), the alternative part oxalic acid of the higher suspension of lower layer's ferrous oxalate content is added in circulating absorption solution by spraying Drenching layer 2.2 sprays into absorption tower 2;Through iron removal system 3 ammonium sulfate byproduct is produced except the concentrate after iron enters crystal system 7.

Claims (5)

1. a kind of ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique, including flue gas enters in concentration tower and tower and concentrates Liquid haptoreaction, the flue gas for going out concentration tower are sent into the middle part of absorption tower the packing layer and spraying layer for passing upward through the setting of absorption tower top It is discharged by exhanst gas outlet with after the reverse haptoreaction of circulating absorption solution;Concentration tower bottom of tower extension concentrate is removed through iron removal system Ammonium sulfate crystallization system is sent into after iron, which is characterized in that the circulating absorption solution sprayed by absorption tower top spraying layer is successively By the packing layer on tower top, by recycling, to be pumped to Photocatalytic Regeneration anti-with absorb the bottom of the tower is entered after the reverse haptoreaction of flue gas Enter recycled pulp liquid bath after answering system regeneration, then as cycle after filling into ammonium hydroxide, oxalic acid and ferrous sulfate in regenerating slurry tank The spraying layer that absorbing liquid is transmitted back to absorption tower top sprays into tower, the concentration into iron removal system that the concentration tower bottom is drawn Liquid is first sent into concentrating and precipitating pond precipitation, and the suspension in concentrating and precipitating bottom of pond portion is sent into the Photocatalytic Regeneration reaction system, epimere Clarified solution be sent into iron removal system.
2. the ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique as described in claim 1, which is characterized in that control A concentration of 0.09~0.3mol/L of circulating absorption solution mesoxalic acid in absorption tower, iron ion+ferrous ion total concentration be 0.015~ The pH value of 0.05mol/L, circulating absorption solution are 5.0~5.5.
3. the ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique as claimed in claim 1 or 2, which is characterized in that The concentrate that the absorbing liquid into concentration tower that the absorb the bottom of the tower is drawn is drawn with concentration tower bottom concentrate circulating pump mixes Concentration tower top cycle is sent into after conjunction to spray.
4. the ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique as described in claim 1, which is characterized in that described Photocatalytic Regeneration reaction system is the photo catalysis reactor equipped with light source.
5. the ferrous oxalate based on flue gas ammonia method desulfurizing synchronizes denitrating technique as described in claim 1, which is characterized in that described Iron removal system is that electrolysis removes iron reactor.
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