CN105709598A - Ammonium-method synchronous desulfurization and denitrification process of flue gas based on oxalic acid oxidization reduction - Google Patents
Ammonium-method synchronous desulfurization and denitrification process of flue gas based on oxalic acid oxidization reduction Download PDFInfo
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Abstract
The invention discloses an ammonium-method synchronous desulfurization and denitrification process of flue gas based on oxalic acid oxidization reduction. The ammonium-method synchronous desulfurization and denitrification process comprises the following steps: after the flue gas is pressurized, the flue gas is conveyed into a concentration tower to be in contact with a concentrated solution in the tower to react; the flue gas discharged from the concentration tower is conveyed into the middle part of an absorption tower, upward passes through a packing layer and a spraying layer to be in reversed contact with a circulating absorption solution to react, and then is discharged from a flue gas outlet; part of the concentrated solution is led out from the bottom of the concentration tower and iron is removed from the concentrated solution through an iron removing system; then the concentrated solution is conveyed into an ammonium sulfate crystallization system; after the circulating absorption solution sprayed out from the spraying layer at the upper part of the absorption tower sequentially passes through the packing layer at the upper part of the tower and then is reversed contact with the flue gas to react, the circulating absorption solution enters the bottom of the absorption tower, is conveyed to a photocatalysis regeneration reaction system through a circulating pump to be regenerated and then enters a regenerated slurry groove; and after ammonia water, a complexing agent Fe(II)EDTA, oxalic acid and ferrous sulfate are added, the mixture is used as the circulating absorption solution to be conveyed back to the spraying layer at the upper part of the absorption tower, so as to be sprayed into the tower. The ammonium-method synchronous desulfurization and denitrification process of the flue gas based on the oxalic acid oxidization reduction is simple in process, low in operation cost, low in energy consumption, simple and convenient to control, good in denitrification effect and good in quality of byproducts.
Description
Technical field
The present invention relates to the flue gas ammonia process synchronized desulfuring and denitrifying technique of a kind of field of Environment Protection, a kind of based on the redox flue gas ammonia process synchronized desulfuring and denitrifying of oxalic acid specifically.
Background technology
" 12 " period, the steel and iron industry SO of China's emphasis statistics2Discharge capacity at 2,510,000 tons/year, wherein agglomerates of sintered pellets operation SO before ferrum2Discharge capacity reaches 2,180,000 tons, accounts for more than the 87% of iron and steel enterprise's total emission volumn, to " 12 " end, sinters SO2Handling rate also only 88%.And denitration aspect, also do not carry out comprehensively.
The feature of sintering flue gas is that exhaust gas volumn is big, flue gas carries that Dust Capacity is relatively big, the discharge capacity of sulfur dioxide and concentration change is relatively big, flue-gas temperature fluctuation is big, smoke components is complicated, humidity of flue gas is big.Compared with boiler smoke, deal with more difficult, it is difficult to directly employing power plant desulfurization denitration technology, and for existing sintering (pelletizing) system, to such an extent as to existing SCR denitration technology be not properly suited for the improvement of sintering flue gas, so for the feature of sintering flue gas self, must analyze, consider comprehensively, finally work out and meet the technical matters route that sintering flue gas self is administered.If taking substep administration way, it will cause capital investment costly, the shortcomings such as plant area area is big and flue gas system is complicated.Carry out synchronizing denitration transformation being the developing direction reduced investment outlay with operating cost in existing desulphurization system.
The ammonia process of desulfurization because its desulfuration efficiency is high, invest the advantages such as low, water consumption is few, side-product can effectively utilize, non-secondary pollution and be widely used, and this method also has certain denitration effect while ensureing desulfurized effect.Du Zhen, Gao Xiang etc. have studied (NH in ammonia process of desulfurization process4)2SO3Solution absorbs NOXFeature, it is determined that SO2Existence the absorption of NO is had facilitation, it was demonstrated that the feasibility of ammonia process simultaneous SO_2 and NO removal.Owing in flue gas, NO accounts for NOX90-95%, although and NO low solubility in water causes ammonia process and has the effect of synchronized desulfuring and denitrifying, but denitration rate is low, it is impossible to reach requirement.Absorption via Chemical Complexation is a kind of method maximally efficient in wet denitration, and denitration effect is notable, and reactive adaptation is strong.At present, chelating agent is individually removed NO and has carried out careful research by Chinese scholars, absorbs the technological parameter of NO as Jing Guohua have studied Fe (II) EDTA, found that SO3 2-Can the NO that gets off of partial reduction complexation and by O2Fe (II) EDTA of oxidation, is conducive to the out of stock process of complexation.In a word, numerous achievements in research shows, the ammonia process of desulfurization and chelating agent method denitration exist binding site, it is possible to complementary not enough, it is achieved synchronized desulfuring and denitrifying.
In Absorption via Chemical Complexation, most study is exactly Fe (II) EDTA method, from 20 century 70s, Japan and some scholars of the U.S. have begun to Fe (II) EDTA method is carried out substantial amounts of research, thinking that NO is had good complexation effect by Fe (II) EDTA, denitration efficiency is high.But, Fe (II) EDTA self is also easy in by flue gas entrained O in the process of complexation NO2Aoxidized, formed NO Fe (III) EDTA without absorbing activity.Yin Qide etc. propose " Fe2+Intercalating agent complexation-iron powder reducing-acid absorbs absorption method " remove the new technology of NO in flue gas.Experiments show that, NO removal efficiency can increase along with iron powder consumption and reactor mixing speed and increase, and iron powder particle diameter is more big, and assimilation effect is more poor.At iron powder 0.8g, iron powder particle diameter is less than 0.077mm, and stir speed (S.S.) is 900r min-1, when oxygen content is 5%, obtain more than 90% NO removal efficiency.LiWang etc. adopt Fe (II) EDTA/Na2SO3Make reducing agent and absorb NO and SO simultaneously2, and Fe (II) EDTA is regenerated.Research shows there is SO2Time NO absorption rate improve 1.59 times.
For the wet ammonia process desulfurizing that sintering adopts, carry out composite realization of ammonia-Fe (II) EDTA on this basis and sinter flue gas synchronized desulfuring and denitrifying, be that a kind of flue gas multiple pollutant that sinters with application prospect works in coordination with the technology of improvement.But owing to flue gas dividing containing a certain amount of oxygen, Fe (II) the EDTA oxidation that easily will absorb in liquid, cause that denitration efficiency declines, even lose denitration ability.So the regeneration issues of denitrfying agent is the bottleneck of restriction synchronized desulfuring and denitrifying development.
Summary of the invention
The invention aims to solve above-mentioned technical problem, it is provided that a kind of technique is simple, operating cost is low, energy consumption is low, control is easy, denitration effect is good, side-product matter is measured based on oxalic acid redox flue gas ammonia process synchronized desulfuring and denitrifying technique.
Technical scheme sends into concentration tower and concentrated solution haptoreaction in tower after including flue gas supercharging, discharged by exhanst gas outlet after going out the packing layer and spraying layer and the reverse haptoreaction of circulating absorption solution passing upward through the setting of tower top in the middle part of the flue gas feeding absorption tower of concentration tower；The partial concentration liquid drawn at the bottom of concentration tower tower sends into ammonium sulfate crystallization system after iron removal system deironing, the described circulating absorption solution by the ejection of top, absorption tower spraying layer enters after sequentially passing through the packing layer on tower top and the reverse haptoreaction of flue gas and enters recycled pulp liquid bath after being delivered to the regeneration of Photocatalytic Regeneration response system by circulating pump bottom absorption tower, then is transmitted back to the spraying layer on top, absorption tower as circulating absorption solution after filling into ammonia, chelating agent Fe (II) EDTA, oxalic acid and ferrous sulfate in recycled pulp liquid bath and sprays in tower.
Controlling Fe (II) EDTA+Fe (III) EDTA total concentration in the circulating absorption solution spraying in absorption tower is 0.015～0.05mol/L, and oxalate denominationby concentration is 0.09～0.3mol/L, the pH value of circulating absorption solution is 5.0～5.5.
The liquid that absorbs entering concentration tower drawn bottom described absorption tower sends into the circulation ejection of concentration tower top with the concentrated solution of concentrated solution circulating pump extraction bottom concentration tower after mixing.
The concentrated solution entering iron removal system drawn bottom described concentration tower first sends into concentrating and precipitating pond precipitation, and the suspension bottom concentrating and precipitating pond sends into described Photocatalytic Regeneration response system, and iron removal system sent into by the clear liquor of epimere.
Described Photocatalytic Regeneration response system is the photo catalysis reactor being provided with light source.
Described iron removal system is electrolysis deironing reactor.
The present invention, in the double tower synchronized desulfuring and denitrifying technique of existing composite ammonia-Fe (II) EDTA chelating agent, adds oxalic acid to circulating absorption solution, and oxalic acid can react generation ferric oxalate and Ferrox. with the iron ion absorbed in liquid and ferrous ion.Ferric oxalate and Ferrox. are the salt that oxalate denominationby is formed with ferrum and ferrous ion.
In aqueous, when having oxygen, Ferrox. is easily oxidized to ferric oxalate.Ferric oxalate can form stable ferric oxalate complexes in aqueous, and these complex have good photochemical activity, has relatively active redox characteristic, Fe therein under irradiation under ultraviolet ray3+It is reduced into Fe2+, oxalate is oxidized and generate H under photocatalysis2O2.The Fe that photo-reduction generates2+Again with H2O2React generation OH and Fe3+, Fe3+Ferric oxalate complexes can be again formed again with oxalate denominationby.When solution exists excessive oxalate denominationby and H2O2Time, will constantly produce hydroxy radical OH, produce the quantum yield of OH free radical up to about 1.OH free radical is very strong 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 utilizes ferric oxalate in aqueous just, under photocatalysis, the NO absorbed is oxidized to nitrate anion to realize final elimination, simultaneously by oxidized Fe3+It is reduced into Fe2+, absorb Fe in liquid2+The rising of concentration, is conducive to the generation of Fe (II) EDTA, it is achieved the regeneration of chelating agent.Above-mentioned course of reaction is complicated many courses of reaction, research shows, absorb and liquid adds oxalic acid reaction generation Ferrox. in conjunction with illumination reaction, the elimination of part nitrogen oxides can either be realized, moreover it is possible to substitute iron chip filter and realize the regeneration of chelating agent Fe (II) EDTA, in present invention process, when Ferrox. and chelating agent use simultaneously, being possible not only to substitute traditional iron chip filter, it is also possible to that reduces chelating agent makes consumption, efficiency reduces the operating cost of system.
Photocatalytic Regeneration response system in the present invention is photo catalysis reactor, photo catalysis reactor available nature light by day reacts, when natural lighting condition is not enough, can opening the light source carried and carry out light-catalyzed reaction, described light source is the cancellated multilamellar light belt of arranged crosswise.Reacted circulating absorption solution is after sending into photo catalysis reactor, and circulating absorption solution mesoxalic acid iron complex issues third contact of a total solar or lunar eclipse chemical reaction at illumination condition, produces hydroxy radical OH, NO and is oxidized to nitrate anion to realize final elimination, Fe3+It is reduced into Fe2+, Fe in solution3+Concentration reduce, Fe2+Concentration raise, broken Fe3+Complexation equilibrium with EDTA, improve the concentration of Fe (II) EDTA, achieve the regeneration of Fe (II) EDTA, photo catalysis reactor is utilized to replace the iron chip filter of traditional iron filings tower, reduce deironing cost, avoid that iron filings consumption is big, absorb the dense generation from too high problem of iron ion in liquid, improve the quality of side-product.
Further, the partial concentration liquid entering iron removal system drawn bottom described concentration tower first sends into concentrating and precipitating pond precipitation, after staticly settling, the suspension bottom concentrating and precipitating pond sends into described Photocatalytic Regeneration response system, and iron removal system sent into by the clear liquor of epimere.Adopt concentrating and precipitating pond by concentrated solution concentration layering, the suspension that bottom ferric oxalate content is high sends into the regeneration of Photocatalytic Regeneration response system, the clear liquor of epimere is then sent into iron removal system and carries out deironing, both the consumption of ferrum in solution can have been reduced, the burden of iron removal system can be alleviated again, improve the de-ironing efficiency of concentrated solution, reduce the iron content in side-product.
In the present invention, in recycled pulp liquid bath, the amount of filling into of ammonia, chelating agent Fe (II) EDTA, oxalic acid and ferrous sulfate can fill into according to the requirement of Fe in circulating absorption solution (II&III) EDTA concentration, oxalate denominationby concentration and solution ph, in line with damaging, and the principle mended.
Beneficial effect:
(1) in the flue gas composite synchronized desulfuring and denitrifying technique of ammonia-Fe (II) EDTA, oxalic acid is added, oxalic acid plays the Oxidation suppressing the oxygen in flue gas to Fe (II) EDTA, while utilizing the nitrogen oxides in the multiple oxidations and photochemical reaction elimination absorption liquid that oxalic acid is raw material, substitute existing iron chip filter or electrolytic regeneration method realizes the regeneration of Fe (III) EDTA, achieve many things at one stroke.Due to oxalic acid aboundresources, with low cost be easy to get, have energy-saving and cost-reducing, reduce operating cost, the advantage making consumption and loss amount of EDTA can be reduced simultaneously.
(2) utilize concentrating and precipitating pond precipitation that concentrated solution carries out precipitated and separated, improve the response rate of ferrum, reduce the burden of iron removal system, improve the quality of side-product.
(3) adopting the inventive method that the NO absorbed can carry out oxidation to convert, denitration chelating agent carries out reducing/regenerating, desulfuration efficiency is up to more than 90%, and denitration efficiency is up to more than 50%, hence it is evident that be better than existing desulfurizing and denitrifying process.Present invention process is simple, easily operated, good reliability.
Accompanying drawing explanation
Fig. 1 present invention process flow chart.
Fig. 2 is the absorption oxidizing process schematic diagram that oxalic acid exists lower circulating absorption solution and flue gas.
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-scrubber layer, 3-iron removal system, 4-Photocatalytic Regeneration response system, 5-recycled pulp liquid bath, 6-concentrated solution sedimentation tank, 7-crystal system.
Detailed description of the invention
Embodiment:
Referring to Fig. 1, in certain flue gas desulphurization system, exhaust gas volumn is 14～16Nm about3/ h, SO2Concentration: 800～1200mg/Nm3, NOx concentration (is mainly NO): 300～400mg/Nm3.What desulfurization adopted is double tower process.Enter concentration tower 1 top after flue gas is intensified, flow from top to bottom.With the concurrent biochemical absorption reaction of concentrated solution (containing ammonia) co-current contact being sent to the ejection of concentration tower top by tower 1 circulating pump that extract out at the bottom of tower, concentrated in flow process, absorb the sulfur dioxide in flue gas and nitrogen oxides.
Physical parameter and the relevant components of concentrated solution are as follows:
PH value: 5.0～5.5；
Ammonium sulfate concentrations: 20～45% (mass percents)；
Fe (II) EDTA+Fe (III) EDTA total concentration: 0.045～0.15mol/L；
Oxalate denominationby concentration: 0.27～0.9mol/L；
Absorb liquid temp: 50-55 DEG C.
Flue gas stream in the middle part of concentration tower 1 after introduce the middle part on absorption tower 2 through connection flue, and flow through packing layer 2.1 and spraying layer 2.2 to top of tower；With the concurrent biochemical absorption reaction of the circulating absorption solution counter current contacting that tower top spraying layer 2.2 sprays (course of reaction principle is referring to Fig. 2) in flow process, absorb the sulfur dioxide in flue gas and nitrogen oxides.Flue gas enters tower top after spraying layer 2.2, and 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 percents)；
Fe (II) EDTA+Fe (III) EDTA concentration: 0.015～0.05mol/L；
Oxalate denominationby concentration: 0.09～0.3mol/L；
Absorb liquid temp: 50 DEG C.
In bottom, absorption tower, drawn circulation fluid by recycled pulp liquid pump from tower bottom and absorb liquid entrance Photocatalytic Regeneration response system (for being provided with the photo catalysis reactor of light source), sunlight can be passed through, and auxiliary light irradiates, it is circulated the light-catalyzed reaction (principle process is referring to Fig. 3) absorbing liquid:
In the solution of the saturation of the air, under acid conditionWithFurther with oxygen in water O2Reaction, ultimately forms H2O2。
2mol'sThe Fe of 1mol is generated after light-catalyzed reaction2+, consume the oxalate denominationby of 1mol, the hydroxy radical OH of 1mol, the NO that oxidative absorption gets off be provided simultaneously, owing to consuming oxalate denominationby, Fe in solution3+Reduce with oxalate denominationby concentration, Fe2+Concentration increases, and has broken the total concentration balance of Fe (II) EDTA+Fe (III) EDTA, and Fe (II) EDTA concentration increases, and Fe (III) EDTA reduces, it is achieved Fe (II) EDTA regenerates.Draw bottom absorption tower 2 per hour after 6-9L absorption liquid merges with the partial concentration liquid extracted out bottom concentration tower 1 and sprayed into by concentration tower epimere, bottom concentration tower 1, draw 2-3L serosity per hour enter concentrating and precipitating pond, 30-40 hour sedimentation time, supernatant enters iron removal system (i.e. electrolysis deironing reactor, if number of patent application is 201520886784.2, denomination of invention is " a kind of oriented flow electrolysis unit ", can also be other electrolysis reactor being principle with electrolysis deironing), the suspension that lower floor's ferric oxalate content is higher is transmitted back to Photocatalytic Regeneration response system 4.
Recycled pulp liquid bath 5 is sent into by the serosity of Photocatalytic Regeneration response system 4 Base top contact, the ammonia of consumption, chelating agent, ferrous sulfate and oxalic acid is filled into, after meeting related property parameter and the composition requirement of circulating absorption solution, to spray in absorption tower 2 by spraying layer 2.2 as circulating absorption solution in recycled pulp liquid bath 5；Concentrated solution after iron removal system deironing enters crystal system 7 and produces ammonium sulfate side-product, containing Fe (III) EDTA in remaining solution after crystallization, can the regeneration of loopback Photocatalytic Regeneration response system 4 reclaim.
Relating to other reaction such as ammonia process of desulfurization denitration, Fe (II) EDTA complexation and regenerative response in present invention process is existing popular response, and its principle, compared with technology, does not make enumeration at this.In flue gas after said method processes, NO compound removal efficiency can reach more than 50%, SO2Removal efficiency be more than 90%.
Claims (6)
1. one kind based on oxalic acid redox flue gas ammonia process synchronized desulfuring and denitrifying technique, including sending into concentration tower and concentrated solution haptoreaction in tower after flue gas supercharging, discharged by exhanst gas outlet after going out the packing layer and spraying layer and the reverse haptoreaction of circulating absorption solution passing upward through the setting of tower top in the middle part of the flue gas feeding absorption tower of concentration tower；Extension concentrated solution at the bottom of concentration tower tower sends into ammonium sulfate crystallization system after iron removal system deironing, it is characterized in that, the described circulating absorption solution by the ejection of top, absorption tower spraying layer enters after sequentially passing through the packing layer on tower top and the reverse haptoreaction of flue gas and enters recycled pulp liquid bath after being delivered to the regeneration of Photocatalytic Regeneration response system by circulating pump bottom absorption tower, then is transmitted back to the spraying layer on top, absorption tower as circulating absorption solution after filling into ammonia, chelating agent Fe (II) EDTA, oxalic acid and ferrous sulfate in recycled pulp liquid bath and sprays in tower.
2. as claimed in claim 1 based on oxalic acid redox flue gas ammonia process synchronized desulfuring and denitrifying technique, it is characterized in that, controlling Fe (II) EDTA+Fe (III) EDTA total concentration in the circulating absorption solution spraying in absorption tower is 0.015～0.05mol/L, oxalate denominationby concentration is 0.09～0.3mol/L, and the pH value of circulating absorption solution is 5.0～5.5.
3. as claimed in claim 1 or 2 based on oxalic acid redox flue gas ammonia process synchronized desulfuring and denitrifying technique, it is characterized in that, the absorbing of concentration tower that enter drawn bottom described absorption tower sends into the circulation ejection of concentration tower top by concentrated solution circulating pump after liquid mixes with the concentrated solution drawn bottom concentration tower.
4. as claimed in claim 1 based on oxalic acid redox flue gas ammonia process synchronized desulfuring and denitrifying technique, it is characterized in that, the concentrated solution entering iron removal system drawn bottom described concentration tower first sends into concentrating and precipitating pond precipitation, suspension bottom concentrating and precipitating pond sends into described Photocatalytic Regeneration response system, and iron removal system sent into by the clear liquor on top.
5. as described in claim 1 or 3 or 4 based on oxalic acid redox flue gas ammonia process synchronized desulfuring and denitrifying technique, it is characterised in that described Photocatalytic Regeneration response system is the photo catalysis reactor being provided with light source.
6. as described in claim 1 or 4 based on oxalic acid redox flue gas ammonia process synchronized desulfuring and denitrifying technique, it is characterised in that described iron removal system is electrolysis deironing reactor.
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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 |
| CN102247748A (en) * | 2011-06-30 | 2011-11-23 | 湖北省宏源药业有限公司 | Treatment method and treatment system of tail gas from glyoxylic acid production by nitric acid oxidation of glyoxal |
| 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 |
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