CN109092038B - Flue gas desulfurization and denitrification method based on coupling conversion of sodium sulfite method and circulating sodium-alkali method - Google Patents
Flue gas desulfurization and denitrification method based on coupling conversion of sodium sulfite method and circulating sodium-alkali method Download PDFInfo
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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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
- 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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- C—CHEMISTRY; METALLURGY
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/14—Preparation of sulfites
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- B01D2251/00—Reactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2251/606—Carbonates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
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- B01D2258/0283—Flue gases
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Abstract
The invention relates to a flue gas desulfurization and denitrification method based on coupling conversion of a sodium sulfite method and a circulating sodium-alkali method, which comprises the following steps of: (1) spraying oxidant into the flue gas, and oxidizing NO into NO in the oxidation unit2(ii) a (2) NO in flue gas is treated in a main absorption tower by using sodium-alkali solution2And SO2Performing synchronous absorption, and controlling the absorbed nitrogen oxides in a nitrite state by utilizing sulfite; (3) sending part of absorption liquid in the main absorption tower into a reduction tower for nitrite reduction and removal; (4) reducing nitrite in the reduction tower into nitrogen, and gradually converting sodium sulfite in the nitrogen into sodium bisulfite; (5) the SO in the reduction tower is easily introduced2The desorption tower or the neutralization/crystallization tower is used for subsequent treatment. Compared with the prior art, the invention can realize the synchronous absorption of the nitrogen oxide and the sulfur dioxide in the flue gas and can be used for absorbing the nitrogen oxide and the sulfur dioxide in the flue gas according to the sodium sulfite product and SO2The change of the market price of the product is selected from sodium sulfite or SO2Is a flue gas desulfurization process of a byproduct.
Description
Technical Field
The invention relates to the field of flue gas desulfurization and denitration, in particular to a flue gas desulfurization and denitration method based on coupling conversion of a sodium sulfite method and a circulating sodium-alkali method.
Background
Different process sections of non-ferrous metal metallurgy can produce sulfur-containing flue gas with different concentrations. When SO in flue gas2When the concentration is more than 4%, the method can be generally adoptedProducing sulfuric acid by a contact-type acid making process; when SO in flue gas2At concentrations below 2000ppm, desulfurization is often employed by discarding the desulfurization product. For the sulfur-containing flue gas with medium concentration, the adopted acid making process and the abandoned desulfurization process are not suitable. Therefore, the flue gas desulfurization process adopting the recoverable sulfur resource is compared with the purification treatment of the medium sulfur-containing flue gas.
With the continuous improvement of the environmental protection standard of China, the emission standard for controlling the nitrogen oxide in the non-ferrous metal smelting flue gas is also provided. And the application of the conventional SNCR and SCR technology in the denitration process of the non-ferrous metal smelting flue gas is limited due to the complex working condition of non-ferrous metal smelting and the high content of heavy metal in the flue gas. The method for removing the nitrogen oxides in the non-ferrous metal smelting flue gas by adopting an oxidation absorption method is a relatively suitable choice. Therefore, the process for carrying out combined desulfurization and denitrification on the non-ferrous metal smelting flue gas by adopting the absorption method has an important application prospect.
Currently, the treatment technologies of the middle-concentration sulfur-containing flue gas mainly include an ammonia method, a sodium sulfite method, a circulating sodium-alkali method, an ionic liquid method and the like, and desulfurization byproducts of the middle-concentration sulfur-containing flue gas are ammonium sulfate, sodium sulfite and SO2. Since these desulfurization by-products have large market price fluctuations, their operating costs will also vary with the market fluctuations due to the fixed associated processes and the single by-product. In the process of desulfurizing by a sodium sulfite method, the main product is sodium sulfite, and the main reaction paths are as follows:
2Na(OH)+SO2＝Na2SO3+H2O
2NaHCO3+SO2＝Na2SO3+H2O+2CO2↑
Na2CO3+SO2＝Na2SO3+CO2↑
in the process of desulfurization by a circulating sodium-alkali method, the main reaction paths are as follows:
Na2SO3+SO2+H2O＝2NaHSO3
after sodium bisulfite is heated and regenerated, high-concentration SO can be obtained2The product is as follows:
2NaHSO3＝Na2SO3+SO2↑+H2O
therefore, the product of the sodium sulfite method can further participate in the flue gas desulfurization reaction in the circulating sodium-alkali desulfurization method, and finally SO is recovered2And (5) producing the product. Therefore, the sodium sulfite process can be coupled with the circulating sodium soda process and depends on the sodium sulfite product and SO2The change of the product market price realizes the flexible adjustment of the desulphurization by-product.
In addition, the recovery type wet desulfurization method can be matched with an oxidation denitration process, but nitrite and nitrate generated by absorbing nitrogen oxide can be accumulated in the desulfurization solution, thereby affecting the quality of desulfurization byproducts. Therefore, how to organically combine the nitrogen oxide oxidation absorption with the sulfur dioxide recovery method is a problem to be solved by combining the desulfurization and denitrification technologies.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a flue gas desulfurization and denitrification method based on the coupling conversion of a sodium sulfite method and a circulating sodium-alkali method.
The purpose of the invention can be realized by the following technical scheme: a flue gas desulfurization and denitrification method based on coupling conversion of a sodium sulfite method and a circulating sodium-alkali method is characterized by comprising the following steps:
(1) spraying oxidant into the flue gas, and oxidizing NO into NO in the oxidation unit2；
(2) NO in flue gas (1) is treated in a main absorption tower by sodium-alkali solution2And SO2Performing synchronous absorption, and controlling the absorbed nitrogen oxides in a nitrite state by utilizing sulfite;
(3) when sodium sulfite and nitrite in the main absorption tower are accumulated to a certain degree, sending part of absorption liquid into a reduction tower for reduction and removal of the nitrite;
(4) extracting a certain amount of SO from the main flue after the oxidation unit2The flue gas (2) contacts the solution in the reduction tower to gradually reduce the pH value of the solution and reduce the nitrite into nitrogenGas, and gradually converting sodium sulfite in the gas into sodium bisulfite;
(5) when the sodium bisulfite conversion in the reduction column reaches a certain level, the solution (3) is transferred to SO2Heating and regenerating in a desorption tower to prepare high-concentration SO2The gas product, and sodium sulfite solution (4) obtained by desorbing and regenerating sodium bisulfite is led back to the main absorption tower to react with SO2And NO2Continuing absorption;
(6) when there is no need to recover SO2When the gas product is produced, directly introducing the solution (5) in the reduction tower into a neutralization/crystallization tower, neutralizing sodium bisulfite into sodium sulfite in a form of adding sodium alkali solution, and crystallizing to obtain a sodium sulfite product for sale;
(7) when SO regulation is required2In proportion to the sodium sulfite by-product, from SO2Extracting part of solution (6) from the sodium sulfite solution (4) obtained after the regeneration of the desorption tower, and introducing the extracted solution into a neutralization/crystallization tower to prepare a sodium sulfite product.
The oxidant in the step (1) is ozone or sodium chlorite.
And (3) the sodium alkali solution in the step (2) is one or more of a compound solution of sodium hydroxide, sodium carbonate and sodium bicarbonate.
And (3) the mass concentration of the sodium alkali solution in the main absorption tower in the step (2) is 5-30%.
And (4) leading the desulfurizing liquid in the main absorption tower out to a reduction tower to remove the accumulated nitrite in the solution for reduction by taking the first-come index as a control standard when the concentration of the nitrite in the main absorption tower in the step (3) is accumulated to be more than 0.5 percent or the pH value of the solution is less than 7.
Step (4) introducing SO2The flue gas lowers the pH of the solution in the reduction column to within the range of 3.5-6.5.
When the conversion rate of the sodium bisulfite in the reduction tower in the step (5) is more than 80 percent or the pH value of the solution is less than 3.5, the first-come index is taken as a control standard and is introduced into SO2The desorption tower or the neutralization/crystallization tower is used for subsequent treatment.
The SO2Introducing hot steam into the desorption tower to desorbPreparation of SO2The product and regenerated sodium sulfite absorption liquid.
And adding a sodium alkali solution into the neutralization/crystallization tower to neutralize sodium bisulfite and crystallize to prepare a sodium sulfite product.
Compared with the prior art, the invention has the following advantages:
1. the method can realize the synchronous absorption of the sulfur dioxide and the nitrogen oxide in the flue gas;
2. nitrite generated in the process of absorbing nitrogen oxide can be removed by a reduction denitrification method, so that the problem that the recovery of desulfurization products is influenced by the accumulation of nitrite is avoided;
3. the process is a flue gas desulfurization and denitrification method based on coupling of a sodium sulfite method and a circulating sodium-alkali method, and is based on sodium sulfite and SO on the market2Adjusting the product price to SO2When the market price is high, the process proceeds to the fifth step to produce SO2The by-products are sold. When the market price of the sodium sulfite is high, the process goes to the sixth step, and a sodium sulfite byproduct is prepared for sale.
Drawings
FIG. 1 is a schematic diagram of the process employed in the present invention. The bold arrows in the figure indicate SO2The process for desulfurization and denitrification of the by-product is carried out, and the thin arrow indicates Na2SO3Is a desulfurization and denitrification production process of byproducts.
Detailed Description
The present invention is further illustrated by the following specific examples. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.
Example 1:
as shown in fig. 1, the flue gas desulfurization and denitrification method based on the coupling of the sodium sulfite method and the circulating sodium-alkali method comprises the following steps:
first, the flue gas (the main components are NO and SO)2) In which an oxidant (ozone or sodium chlorite is selected) is sprayed to oxidize NO into NO in the oxidation unit 1012；
Secondly, the NO in the flue gas 1 is treated by sodium alkali solution (sodium hydroxide with the mass concentration of 5-30%) in the main absorption tower 1022And SO2Synchronous absorption is carried out, and the absorbed nitrogen oxides are controlled to be in a nitrite state by utilizing sulfite with higher concentration;
thirdly, when the concentration of nitrite is more than 0.5% or the pH value of the solution is less than 7 (the first-come index is used as a control standard) due to the accumulation of sodium sulfite and nitrite in the main absorption tower 102, sending part of absorption liquid into a reduction tower 103 for nitrite reduction and removal;
fourthly, a certain amount of SO-containing gas is extracted from the main flue after the oxidation unit 1012The flue gas 2 contacts the solution in the reduction tower 103, so that the pH value of the solution is gradually reduced to be within the range of 3.5-6.5, nitrite is reduced to nitrogen, and sodium sulfite in the nitrogen is gradually converted to sodium bisulfite;
fifthly, when the conversion rate of the sodium bisulfite in the reduction tower 103 is more than 80 percent or the pH value of the solution is less than 3.5 (taking the first-come index as a control standard), transferring the solution 3 to SO2Heating regeneration (with SO) in the desorption tower 1042Heating the desorption tower 104 by introducing hot steam), and preparing high-concentration SO2The gas product, and sodium sulfite solution 4 obtained by desorbing and regenerating sodium bisulfite is led back to the main absorption tower 102 for SO2And NO2Continuing absorption;
sixthly, when the SO does not need to be recovered2When the gas product is produced, the solution 5 in the reduction tower 103 is directly introduced into a neutralization/crystallization tower 105, sodium bisulfite is neutralized into sodium sulfite in a form of adding sodium alkali solution, and the sodium sulfite product is obtained by crystallization and sold;
step seven, when SO is required to be adjusted2In proportion to the sodium sulfite by-product, from SO2Extracting part of solution 6 from the sodium sulfite solution 4 obtained after the regeneration of the desorption tower 104, and introducing the extracted solution into a neutralization/crystallization tower to prepare a sodium sulfite product.
100mL of 10% sodium hydroxide was prepared. Introducing mixed gas into the absorption liquid at 30 deg.C and flow rate of 200mL/min, and mixingThe resultant gas uses nitrogen as carrier gas, O2The concentration is 10%; NO2The concentration is 300 ppm; SO (SO)2The concentration was 3000 ppm. The results show that the absorption system is on SO2The absorption efficiency of the method can reach 99 percent, and the absorbed product is sodium sulfite. And sodium-alkali absorption liquid to NO2Also has good absorption effect, the absorption efficiency can reach 90 percent, and NO is2The main absorption product of (2) is nitrite, which can indicate the SO of sodium hydroxide solution2And NO2All have better absorption efficiency and can realize the absorption of SO in the flue gas2And NO2Simultaneous absorption removal.
Example 2:
transferring the mixed solution of sodium sulfite and sodium nitrite obtained after absorbing for a certain time in 100mL of example into a new absorption experimental device, and introducing 3000ppm SO into a mixed solution absorption bottle at the temperature of 30 ℃ at the flow rate of 500mL/min2The result shows that the sodium sulfite solution can still further absorb SO in the simulated flue gas2And SO2The removal efficiency was 95%. After absorbing for a period of time, carrying out ion chromatographic analysis on the absorption liquid, and the result shows that the concentration of nitrite in the absorption liquid is remarkably reduced. No and NO are not detected in the absorption tail gas2This indicates that nitrite in the mixed absorption solution is not present as NO and NO2Is released from the mixed absorption solution after being reduced to nitrogen.
Example 3:
100mL of 10% sodium sulfite solution is prepared, and 3000ppm SO is introduced at the temperature of 30 ℃ at the flow rate of 500mL/min2By breakthrough, the product was mainly sodium bisulfite by ion analysis. Heating the saturated solution to about 150 deg.C under 0.5MPa, and blowing off with nitrogen for 60 min, and monitoring the tail gas to obtain high-concentration SO2(ii) a The absorption solution was then subjected to further ion chromatography, which indicated that a portion of the sodium bisulfate in the absorption solution had been converted to sodium sulfite at a concentration of about 50% of the sodium bisulfite in the saturated absorption solution. This indicates that part of the sodium bisulfite in the saturated absorption solution has been regenerated to sodium sulfite. After regenerationThe absorption liquid continuously reacts with SO with the concentration of 3000ppm2The gas is absorbed, and the desulfurization efficiency is still more than 99%. This indicates that the regenerated absorption liquid can be heated to recover SO2The absorption capacity of (1).
Example 4:
100mL of 10% sodium sulfite solution is prepared, and 3000ppm SO is introduced at the temperature of 30 ℃ at the flow rate of 500mL/min2To breakthrough, its starting SO2The removal efficiency was 99%. And analyzing the solution after saturated absorption by ion chromatography, wherein sulfur in the absorption solution mainly exists in a bisulfite form. To the sodium hydrogen sulfite solution, 100mL of a 10% strength sodium hydrogen carbonate solution was added and stirred for 30 minutes by passing nitrogen gas through, and it was finally determined that the sodium hydrogen sulfite in the solution was substantially converted to sodium sulfite. And (4) carrying out rotary evaporation treatment on the neutralized solution to finally obtain sodium sulfite crystals.
Claims (9)
1. A flue gas desulfurization and denitrification method based on coupling conversion of a sodium sulfite method and a circulating sodium-alkali method is characterized by comprising the following steps:
(1) spraying oxidant into the flue gas, and oxidizing NO into NO in the oxidation unit2；
(2) NO in flue gas (1) is treated in a main absorption tower by sodium-alkali solution2And SO2Performing synchronous absorption, and controlling the absorbed nitrogen oxides in a nitrite state by utilizing sulfite;
(3) when sodium sulfite and nitrite in the main absorption tower are accumulated to a certain degree, sending part of absorption liquid into a reduction tower for reduction and removal of the nitrite;
(4) extracting a certain amount of SO from the main flue after the oxidation unit2The flue gas (2) contacts the solution in the reduction tower, so that the pH value of the solution is gradually reduced, nitrite is reduced to nitrogen, and sodium sulfite in the nitrogen is gradually converted into sodium bisulfite;
(5) when the sodium bisulfite conversion in the reduction column reaches a certain level, the solution (3) is transferred to SO2Heating and regenerating in a desorption tower to prepare high-concentration SO2A gas product, andsodium sulfite solution (4) obtained by desorption and regeneration of sodium bisulfite is led back to the main absorption tower to react with SO2And NO2Continuing absorption;
(6) when there is no need to recover SO2When the gas product is produced, directly introducing the solution (5) in the reduction tower into a neutralization/crystallization tower, neutralizing sodium bisulfite into sodium sulfite in a form of adding sodium alkali solution, and crystallizing to obtain a sodium sulfite product for sale;
(7) when SO regulation is required2In proportion to the sodium sulfite by-product, from SO2Extracting part of solution (6) from the sodium sulfite solution (4) obtained after the regeneration of the desorption tower, and introducing the extracted solution into a neutralization/crystallization tower to prepare a sodium sulfite product.
2. The flue gas desulfurization and denitrification method based on coupling conversion of the sodium sulfite method and the circulating sodium-alkali method as claimed in claim 1, wherein the oxidant in step (1) is ozone or sodium chlorite.
3. The flue gas desulfurization and denitrification method based on coupling conversion of the sodium sulfite method and the circulating sodium-alkali method as claimed in claim 1, wherein the sodium-alkali solution in the step (2) is one or more of a composite solution of sodium hydroxide, sodium carbonate and sodium bicarbonate.
4. The flue gas desulfurization and denitrification method based on the coupling conversion of the sodium sulfite method and the circulating sodium-alkali method as claimed in claim 1, wherein the mass concentration of the sodium-alkali solution in the main absorption tower in the step (2) is 5-30%.
5. The flue gas desulfurization and denitrification method based on the coupling conversion of the sodium nitrite method and the circulating sodium-alkali method as claimed in claim 1, wherein the concentration of nitrite in the main absorption tower in the step (3) is accumulated to be more than 0.5% or the pH value of the solution is less than 7, and the pre-obtained index is used as a control standard, namely the desulfurization solution in the main absorption tower is led out to a reduction tower to remove the nitrite accumulated in the solution for reduction.
6. The flue gas desulfurization and denitrification method based on sodium sulfite method and circulating sodium-alkali method coupling conversion as claimed in claim 1, wherein SO is introduced in step (4)2The flue gas lowers the pH of the solution in the reduction column to within the range of 3.5-6.5.
7. The flue gas desulfurization and denitrification method based on the coupling conversion of the sodium sulfite method and the circulating sodium-alkali method as claimed in claim 1, wherein when the conversion rate of sodium bisulfite in the reduction tower in the step (5) is more than 80% or the pH value of the solution is less than 3.5, the obtained index is used as a control standard, and SO is introduced into the reduction tower2The desorption tower or the neutralization/crystallization tower is used for subsequent treatment.
8. The flue gas desulfurization and denitrification method based on coupling conversion of the sodium sulfite method and the circulating sodium-alkali method as claimed in claim 7, wherein the SO is2Introducing hot steam into the desorption tower to prepare SO by desorption2The product and regenerated sodium sulfite absorption liquid.
9. The flue gas desulfurization and denitrification method based on coupling conversion of the sodium sulfite method and the circulating sodium-alkali method as claimed in claim 7, characterized in that a sodium-alkali solution is added into the neutralization/crystallization tower to neutralize sodium bisulfite and crystallize to prepare a sodium sulfite product.
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Address after: 200030 Dongchuan Road, Minhang District, Minhang District, Shanghai Applicant after: Shanghai Jiaotong University Applicant after: Henan Yuguang Golden Plumbum Group Co., Ltd. Address before: 200030 Huashan Road, Shanghai, No. 1954, No. Applicant before: Shanghai Jiaotong University Applicant before: Henan Yuguang Golden Plumbum Group Co., Ltd. |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |