CN105233647B - A kind of method of ammonium sulfide solution desulphurization denitration - Google Patents

A kind of method of ammonium sulfide solution desulphurization denitration Download PDF

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CN105233647B
CN105233647B CN201510592576.6A CN201510592576A CN105233647B CN 105233647 B CN105233647 B CN 105233647B CN 201510592576 A CN201510592576 A CN 201510592576A CN 105233647 B CN105233647 B CN 105233647B
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ammonium
solution
flue gas
ammonium sulfide
oxidation
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CN105233647A (en
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王学谦
王郎郎
宁平
马懿星
李林
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Kunming University of Science and Technology
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Abstract

The invention discloses a kind of method of ammonium sulfide solution desulphurization denitration, belong to flue gases purification field.The method of the invention is using ammonium sulfide solution as absorbent, absorption cleaning sulfur dioxide(SO2)And nitrogen oxides(NOx);Industrial furnace flue gas removing dust, after water-washing pre-treatment, appropriate air is blasted into flue, nitric oxide in nitrogen oxides under the conditions of low-grade fever is oxidized to nitrogen dioxide, flue gas is through two grades of absorptions of ammonium sulfide, sulfur dioxide and nitrogen oxides in gas, which are absorbed and is converted into salt, have been stayed in solution, after the completion of absorbing reaction, sulphur is recovered by filtration, filtrate is neutralized, oxidation, evaporative crystallization, drying process processing, the solid mixture of ammonium sulfate and ammonium nitrate is obtained, this mixture can be sold directly as fertilizer.Present invention process is simple, easy to operate, and denitrification efficiency is high, and cost is low, suitable for industrial applications.

Description

A kind of method of ammonium sulfide solution desulphurization denitration
Technical field
The present invention relates to a kind of method of ammonium sulfide solution desulphurization denitration, belongs to flue gases purification field.
Background technology
The energy of China is based on fire coal, and accounting for the raw coal of coal production 75% is used to directly burn, and is produced in coal combustion process Severe contamination, the sulfur dioxide of generation can cause acid rain, and nitrogen oxides is also one of acid rain Producing reason, while endangering people The health of class, can also damage the ozone layer and produce under certain condition photochemical fog etc., and coal-fired flue-gas is to cause me in a word One of greatest contamination source of state's environmental destruction.China's energy-consuming accounts for the 8% ~ 9% of the world, and the discharge capacity of sulfur dioxide is accounted for The 15.1% of the world, the sulfur dioxide that fire coal is discharged accounts for the 87% of national discharge capacity again, therefore sulfur dioxide and nitrogen oxides are dirty The problem of dye, is urgently to be resolved hurrily.Domestic coal-burning power plant, smeltery's flue gas desulfurization technique species is more, such as limestone-gypsum method, simply Wet method, sodium sulfide method, wet-type ammonia, electronic beam method etc..It is at most SCR technology that denitrating flue gas, which is applied,(SCR) With SNCR technology SNCR, the denitration reaction temperature of SCR technology is general at 280 ~ 400 DEG C, and denitration efficiency is up to 90% More than;The reaction temperature of SNCR technologies is general at 850 ~ 1100 DEG C, and denitration efficiency is medium, typically 50% or so.
At present, the desulfurization and denitrification integral technology of use is the joint of desulphurization and denitration two ways, i.e. SO mostly2And NOX Respectively handle.There are various problems in existing desulphurization denitration technology, the fixed investment of such as limestone-gypsum method is big, desulfurization Cost is high, and a large amount of gypsum of generation are difficult to processing etc.;SCR technology has that catalyst investment is big, smoke components influence is big, run into The problems such as this is high, it is high to there is reaction temperature in SNCR technologies, reducing agent with flue gas mixability is poor, denitration efficiency is low, ammonia spilling A series of problems, such as measuring big.Therefore, there is high fixed investment, operation and maintenance cost height, operation behaviour in united desulphurization denitration technology The problems such as making complicated.ZL201410290112.5 " method that flue gas desulfurization and denitrification is carried out using urea co-production technology of preparing " is carried Go out:The ammonia produced with urea co-production technology of preparing can be individually used for flue gas desulfurization and denitrification, and obtained cyanuric acid also can be independent For flue gas desulfurization and denitrification, ammonia and cyanuric acid may also be combined with while being used for desulphurization denitration, and ammonia desulfurization, ammonia takes off Nitre, cyanuric acid desulfurization, cyanuric acid denitration is all separate, and desulfurization need to be combined to progress with denitration two parts Desulphurization denitration purpose can be reached, reaction temperature also needs to control ammonia, cyanuric acid and sulfur dioxide between 500 DEG C ~ 1100 DEG C Air inlet ratio with nitrogen oxides, although improve denitrification efficiency, but complex operation, consume energy higher.ZL200710052129.7 The patent of invention of " wet ammonia flue gas cleaning technology and its system of simultaneous SO_2 and NO removal " is proposed:First make the oxidation in flue gas Nitrogen carries out oxidation reaction generation nitrogen dioxide, sulfur dioxide and nitrogen dioxide in flue gas is reacted respectively with ammoniacal liquor Ammonium sulfite, ammonium nitrate and ammonium nilrite are generated, then ammonium sulfite therein and ammonium nilrite is occurred oxidation reaction generation pair Product ammonium sulfate and ammonium nitrate, while carrying out demisting to the flue gas after desulphurization denitration, finally obtain clean flue gas, nitrogen in this invention Oxide is absorbed while can produce nitric oxide again, there is the problem of denitration efficiency is not high.Therefore a kind of operation letter is developed Single, operating cost is low, and the good technology of simultaneous SO_2 and NO removal effect is the striving direction of environmentally friendly research work.
The content of the invention
It is an object of the invention to provide a kind of ammonium sulfide solution desulfurization denitration method, industrial furnace tail gas removing dust is washed, After air oxidation pretreatment, sulfur dioxide and nitrogen oxides in two grades of ammonium sulfide solution absorption towers, absorption cleaning flue gas are passed through, Reach the purpose of tail gas cleaning discharge;Absorbing liquid is recovered by filtration after sulphur, neutralized, oxidation, evaporative crystallization and drying process The mixed fertilizer of ammonium sulfate and ammonium nitrate is obtained after processing;This method can simultaneous SO_2 and NO removal, and recycle, energy-conservation subtracted Arrange, environmental protection, the technology such as comprehensive utilization of resources is all important breakthrough.
A kind of method of ammonium sulfide solution desulphurization denitration of the present invention, specifically includes following steps:
(1)By industrial furnace flue gas after rough dusting and washing, flue-gas temperature is cooled to less than 50 DEG C;
(2)To step(1)The nitric oxide being passed through in flue gas after processing in air, nitrogen oxides is oxidized to titanium dioxide Nitrogen;
(3)The mixed solution regulation pH value of ammonium bisulfite, ATS (Ammonium thiosulphate) and ammonium nitrate is added in ammonium sulfide solution It is 10%-25% to 7 ~ 7.5 mass percent concentrations for obtaining ammonium sulfide in ammonium sulfide spray liquid, ammonium sulfide spray liquid;
(4)Will be through step(2)Flue gas after middle air oxidation and ammonium sulfide spray liquid haptoreaction, absorbing reaction process In add ammonium sulfide control absorbing liquid pH value between 5 ~ 7.5, after the completion of absorption, SO2And NOXGot off by absorption, absorbing liquid Referred to as rich solution;
(5)Rich solution, which is recovered by filtration, obtains sulphur, and ammoniacal liquor, ammonium carbonate or ammonium hydrogen carbonate regulation pH value are added in filtrate and is dropped to Less than 7.5, the ammonium bisulfite in solution is converted into ammonium sulfite;It is passed through under conditions of solution temperature is 40 DEG C ~ 80 DEG C Add mass percent under air oxidation or normal temperature to be aoxidized for 27.5%-50% hydrogen peroxide, ammonium sulfite is oxidized to sulphur Sour ammonium, ATS (Ammonium thiosulphate) is oxidized to ammonium hydrogen sulfate, and pH value can be reduced;Ammoniacal liquor, ammonium carbonate or ammonium hydrogen carbonate is added after oxidation to adjust Save pH to 6-7.
(6)By step(5)Obtained mixed liquor is concentrated by evaporation to the 30% ~ 40% of original volume in 110 DEG C ~ 120 DEG C, then at 30 DEG C ~ 40 DEG C of crystallizations, the mixture of separation dry obtained ammonium sulfate and ammonium nitrate.
It is preferred that, step(2)The amount that the air oxidation is passed through air is the 10% ~ 20% of exhaust gas volumn.
It is preferred that, step(3)The ATS (Ammonium thiosulphate) and ammonium nitrate mixed solution sulfite hydrogen ammonium, ATS (Ammonium thiosulphate) and The mass ratio of ammonium nitrate is 2:1:1~5:1:1.
When reaction starts, solution ph is larger, and H can be discharged in sulfur dioxide absorption and nitrogen oxide containing gas2S gases, In order to avoid secondary pollution, the regulation liquid that pH value is 4 ~ 7 is added into premature cure ammonium absorbing liquid, makes the pH of ammonium sulfide absorbing liquid Value is reduced to less than 7.5;Adjust the mixed solution of liquid ammonium bisulfite, ATS (Ammonium thiosulphate) and ammonium nitrate, the quality of three kinds of materials Concentration ratio is 2:1:1~5:1:1;With the progress of absorbing reaction, the pH of absorbing liquid can be reduced, when pH is reduced to 5, to Ammonium sulfide solution is added in absorbing liquid, controls the pH value of absorbing liquid in the range of 5 ~ 7.5, this scope assimilation effect is optimal; It is atomized in absorption tower by special whirlpool shower nozzle, flue gas is handled by vaporific two grades of absorption cleanings of ammonium sulfide solution, SO2And NOX Got off by absorption, absorbing liquid is referred to as rich solution, rich solution is mainly ATS (Ammonium thiosulphate), ammonium bisulfite, sulphur, ammonium sulfate and ammonium nitrate Mixed liquor.
Simultaneous SO_2 and NO removal principle of the present invention is as follows:
Absorb:Using (NH4)2S solution absorbs the SO in flue gas2And NOX, absorbing reaction process is as follows:
NO2+(NH4)2S→(NH4)2SO4+N2
SO2 + H2O → H2SO3
3NO2+H2O→ 2HNO3+NO
2NO+O2→2NO2
H2SO3 + (NH4)2S → (NH4) 2SO3 + H2S
2NO+2(NH4)2SO3→2(NH4)2SO4+N2
2HNO3+(NH4)2S → 2NH4NO3 + H2S
H2S + (NH4) 2S → 2NH4HS
2H2S + SO2 → 3S + 2H2O
2 H2S + NO2 → 2S + N2 + 2H2O
S + (NH4)2SO3 → (NH4)2S2O3
(NH4)2S2O3+2NO2+NH4OH→4(NH4)2SO4+N2
(NH4)2SO3 + 0.5O2 → (NH4)2SO4
(NH4)2SO3 + SO2 + H2O→ 2NH4HSO3
4(NH4)2SO3+2NO2→4(NH4)2SO4+N2
Neutralize:Absorbing liquid is brought out, and is recovered by filtration in sulphur, filtrate and is contained NH4HSO3, (NH4)2S2O3, (NH4)2SO4With NH4NO3, add ammoniacal liquor, ammonium carbonate or ammonium hydrogen carbonate and neutralize, make the NH in absorbing liquid4HSO3All it is transformed into (NH4)2SO3And adjust PH value is saved between 6-7.Course of reaction is as follows:
NH3 + NH4HSO3 = (NH4)2SO3
Or
NH4HCO3 + NH4HSO3 = (NH4)2SO3 + CO2 + H2O
Oxidation:Different salts are mixed with absorbing liquid, are not suitable for producing pure ammonium sulfate or ammonium nitrate products, by sulfurous Sour ammonium and ATS (Ammonium thiosulphate) are further aoxidized, and the mixed fertilizer for making ammonium sulfate and ammonium nitrate is used;Ammonium sulfite solution and sulphur The oxidation of ammonium thiosulfate has two methods:
(1)Hydrogen peroxide oxidation hydrogen peroxide oxidation will not bring other impurity into, and oxidation effectiveness is good, due to the oxygen of hydrogen peroxide The property changed is stronger, and ATS (Ammonium thiosulphate) is oxidized to ammonium hydrogen sulfate, and reaction equation is as follows:
(NH4)2SO3 + H2O2 = (NH4)2SO4 + H2O
(NH4)2S2O3 + 4H2O2 = 2NH4HSO4 + 3H2O
After the completion of oxidation reaction, because thiosulfate anion is oxidized, hydrogen radical ion is produced, the pH value of solution is reduced, now Need to add ammoniacal liquor, ammonium carbonate or ammonium hydrogen carbonate adjust pH value to 6-7 scope.
(2)Air oxidation process utilizes the oxidizable principle of ammonium sulfite, by sulfite oxidation is ammonium sulfate with air, should Contain (NH in the ammonium sulfite of method production4)2S2O3With certain catalysed oxidn, the oxidation to ammonium sulfite is favourable, instead Should be as follows:
(NH4)2SO3 + 0.5O2 = (NH4)2SO4
(NH4)2S2O3 + H2O + 2O2 = 2NH4HSO4
Air oxidation is relatively slow, need to improve the temperature of solution at 40 DEG C ~ 50 DEG C, using aerator aerating oxidation or adopts Spray mode from top to bottom with oxidizing tower to be aoxidized, that is, increase the contact area of oxygen and solution, accelerate entering for oxidation reaction OK.Ammoniacal liquor is added after oxidation, ammonium carbonate or ammonium hydrogen carbonate adjust pH value to 6-7 scope.
It is concentrated by evaporation:The mixed liquor of ammonium sulfate, ATS (Ammonium thiosulphate) and ammonium nitrate is concentrated by evaporation to substance in 110 DEG C ~ 120 DEG C Long-pending 30% ~ 40%.
Crystallization:Ammonium sulfate after concentration, ATS (Ammonium thiosulphate) and ammonium nitrate mixed liquor, which are put, is cooled to 30 DEG C ~ 40 DEG C crystallizations.Will Crystalline mother solution is centrifuged, and obtains the ammonium sulfate that water content is 3-5%, the crystallization of ATS (Ammonium thiosulphate) and ammonium nitrate, wherein thio sulphur Sour ammonium hygroscopicity is stronger, is difficult crystallization and separates out, has been partially left in concentrate, so obtained crystallization is with ammonium sulfate and nitric acid Mixture based on ammonium, concentrate can be sold as liquid fertilizer.
Advantages of the present invention:
(1)Removal efficiency is high simultaneously with sulfur dioxide for nitrogen oxides in industrial furnace flue gas, and flue gas can be with qualified discharge. The mixed fertilizer of desulfuration efficiency >=99%, denitration efficiency >=90%, byproduct sulfur purity >=98%, ammonium sulfate and ammonium nitrate is nitrogenous Amount >=20%.
(2)From the SO in flue gas during smelting2The byproducts such as sulphur and nitrogenous fertilizer are produced with NOx, denitrification efficiency is high, runs into This is low, and sulphur have with other sulphur products compared with it is widely used, it is easy to the advantages of storage and transport.Therefore, the present invention is solution Certainly flue gas during smelting purifies the key technology with utilizing, and it is suitable to industrial applications.
Embodiment
The present invention is described in further detail below by embodiment, but the scope of the present invention is not limited in described Hold.
Embodiment 1
SO in industrial furnace flue gas2And NOXRecycling method, particular content is as follows:
(1)Pending flue gas is zinc smelting flue gas in the present embodiment, and exhaust gas volumn is 30000m3Contain in/h, stove mouthful flue gas SO2:3% ~ 4%, NOX:1300~1700mg/m3, flue-gas temperature is cooled to less than 50 DEG C by flue gas during smelting removing dust after washing, drum Enter air(The amount of air is the 10% of exhaust gas volumn);
(2)By the ammonium sulfide solution that mass percent concentration is 25%, pH=7.2(ATS (Ammonium thiosulphate), ammonium bisulfite are used With the regulation of ammonium nitrate mixed liquor, the mass ratio of ammonium bisulfite, ATS (Ammonium thiosulphate) and ammonium nitrate is 3:1:1)Pass through absorption tower Whirlpool shower nozzle is atomized, and flue gas enters two-level absorption tower adverse current and fully contacted with the ammonium sulfide solution of atomization after cooling, to containing SO2With NOXThe pH value of ammonium sulfide control absorbing liquid is added during flue gas during smelting progress efficient absorption, absorbing reaction between 7.5, only Change flue gas emptying;
(3)Absorb SO2And NOXRich solution by press filtration Recovered sulphur, into filtrate add ammonium carbonate neutralized, tune PH value is saved to 6.5, air oxidation is passed through under conditions of solution temperature is 60 DEG C, oxidation completes addition ammonium hydrogen carbonate regulation pH value For 6;
(4)Solution after oxidation is concentrated by evaporation at a temperature of 115 DEG C to the 30% of original solution volume, is cooled to 30 DEG C of crystallizations, Centrifuge, produce ammonium sulfate and ammonium nitrate mixed fertilizer after drying, concentrate is used as liquid fertilizer.
By implementing SO in the above method, smoke desulfurization efficiency >=99%, denitration efficiency >=90%, exiting flue gas2Content≤ 100mg/m3;NOXContent≤100mg/m3, byproduct sulfur purity >=98%, mixed fertilizer nitrogen content >=20%.
Embodiment 2
SO in smelting lead2And NOXThe method of recycling, particular content is as follows:
(1)Pending flue gas is smelting lead in the present embodiment, and exhaust gas volumn is 10000m3Contain in/h, stove mouthful flue gas SO2:0.8% ~ 1%, NOX:1000~1300mg/m3, industrial furnace flue gas removing dust, after washing by flue-gas temperature be cooled to 50 DEG C with Under, blast air(The amount of air is the 15% of exhaust gas volumn);
(2)By the ammonium sulfide solution that mass percent concentration is 10%, pH=7.5(ATS (Ammonium thiosulphate), ammonium bisulfite are used With the regulation of ammonium nitrate mixed liquor, the mass ratio of ammonium bisulfite, ATS (Ammonium thiosulphate) and ammonium nitrate is 5:1:1)Pass through absorption tower Whirlpool shower nozzle is atomized, and flue gas enters two-level absorption tower adverse current and fully contacted with the ammonium sulfide solution of atomization after cooling, to containing SO2With NOXFlue gas during smelting carries out the pH value for adding ammonium sulfide control absorbing liquid during efficient absorption, absorbing reaction between 6, purifies Flue gas is emptied;
(3)Absorb SO2And NOXRich solution by press filtration Recovered sulphur, into filtrate add ammonium hydrogen carbonate neutralized, PH value is adjusted to 7, the solution hydrogen peroxide after neutralization(Mass percent is 48%)Oxidation, oxidation completes addition ammonium carbonate regulation PH value is 7;
(4)Solution after oxidation is concentrated by evaporation at a temperature of 110 DEG C to the 35% of original solution volume, is cooled to 35 DEG C of crystallizations, Centrifuge, produce ammonium sulfate and ammonium nitrate mixed fertilizer after drying, concentrate is used as liquid fertilizer.
By implementing SO in the above method, smoke desulfurization efficiency >=99%, denitration efficiency >=90%, exiting flue gas2Content≤ 100mg/m3;NOXContent≤100mg/m3, byproduct sulfur purity >=98%, mixed fertilizer nitrogen content >=20%.
Embodiment 3
SO in nickel fibers flue gas2And NOXThe method of recycling, particular content is as follows:
(1)Pending flue gas is nickel fibers flue gas in the present embodiment, and exhaust gas volumn is 20000m3Contain in/h, stove mouthful flue gas SO2:1% ~ 2%, NOX:900~1200mg/m3, flue-gas temperature is cooled to less than 50 DEG C after washing, blasts air by flue gas removing dust (The amount of air is the 20% of exhaust gas volumn);
(2)By the ammonium sulfide solution that mass percent concentration is 17%, pH=7(Use ATS (Ammonium thiosulphate), ammonium bisulfite and Ammonium nitrate mixed liquor is adjusted, and the mass ratio of ammonium bisulfite, ATS (Ammonium thiosulphate) and ammonium nitrate is 2:1:1)Pass through the whirlpool on absorption tower Whirlpool shower nozzle atomization, flue gas enters two-level absorption tower adverse current and fully contacted with the ammonium sulfide solution of atomization after cooling, to containing SO2And NOX The pH value of ammonium sulfide control absorbing liquid is added during flue gas during smelting progress efficient absorption, absorbing reaction between 5, purifying smoke Emptying;
(3)Absorb SO2And NOXRich solution by press filtration Recovered sulphur, into filtrate add ammoniacal liquor neutralized, regulation PH value is to 6, the solution hydrogen peroxide after neutralization(Mass percent is 32%)Oxidation, oxidation completes addition ammoniacal liquor regulation pH value and is 7.5;
(4)Solution after oxidation is concentrated by evaporation at a temperature of 120 DEG C to the 40% of original solution volume, is cooled to 40 DEG C of crystallizations, Centrifuge, produce ammonium sulfate and ammonium nitrate mixed fertilizer after drying, concentrate is used as liquid fertilizer.
By implementing SO in the above method, smoke desulfurization efficiency >=99%, denitration efficiency >=90%, exiting flue gas2Content≤ 100mg/m3;NOXContent≤100mg/m3, byproduct sulfur purity >=98%, mixed fertilizer nitrogen content >=20%.

Claims (4)

1. a kind of method of ammonium sulfide solution desulphurization denitration, it is characterised in that specifically include following steps:
(1)By industrial furnace flue gas after rough dusting and washing, flue-gas temperature is cooled to less than 50 DEG C;
(2)To step(1)Air is passed through in flue gas after processing;
(3)Ammonium bisulfite is added in ammonium sulfide solution, the mixed solution of ATS (Ammonium thiosulphate) and ammonium nitrate adjust pH value to 7 ~ 7.5 mass percent concentrations for obtaining ammonium sulfide in ammonium sulfide spray solution, ammonium sulfide spray solution are 10%-25%;
(4)Will be through step(2)Mended during flue gas and ammonium sulfide spray solution haptoreaction after middle air oxidation, absorbing reaction Plus the pH value of ammonium sulfide control absorbing liquid, between 5 ~ 7.5, after the completion of absorption, absorbing liquid is referred to as rich solution;
(5)Rich solution, which is recovered by filtration, obtains sulphur, and ammoniacal liquor, ammonium carbonate or ammonium hydrogen carbonate are added in filtrate and adjusts pH value to 6-7, so It is afterwards to be passed through under air oxidation or normal temperature that to add mass percent concentration be 27.5%- under conditions of 40 DEG C ~ 80 DEG C in solution temperature 50% hydrogen peroxide is aoxidized, and ammoniacal liquor, ammonium carbonate or ammonium hydrogen carbonate regulation pH to 6-7 are added after oxidation;
(6)By step(5)Obtained mixed liquor is concentrated by evaporation, crystallized, separating the mixing that ammonium sulfate and ammonium nitrate are obtained after drying Thing.
2. the method for ammonium sulfide solution desulphurization denitration according to claim 1, it is characterised in that:Step(2)Middle air oxygen The amount that change is passed through air is the 10% ~ 20% of exhaust gas volumn.
3. the method for ammonium sulfide solution desulphurization denitration according to claim 1, it is characterised in that:Step(3)The sulfurous The mass ratio of the mixed solution sulfite hydrogen ammonium of sour hydrogen ammonium, ATS (Ammonium thiosulphate) and ammonium nitrate, ATS (Ammonium thiosulphate) and ammonium nitrate is 2:1:1~5:1:1。
4. the method for ammonium sulfide solution desulphurization denitration according to claim 1, it is characterised in that:Step(6)Middle evaporation temperature Spend for 110 DEG C ~ 120 DEG C, crystallization temperature is 30 DEG C ~ 40 DEG C.
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