CN110787604A - Comprehensive treatment method of sulfur-containing waste flue gas and carbide slag - Google Patents
Comprehensive treatment method of sulfur-containing waste flue gas and carbide slag Download PDFInfo
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- CN110787604A CN110787604A CN201911196324.6A CN201911196324A CN110787604A CN 110787604 A CN110787604 A CN 110787604A CN 201911196324 A CN201911196324 A CN 201911196324A CN 110787604 A CN110787604 A CN 110787604A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
- B01D53/501—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound
- B01D53/502—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound characterised by a specific solution or suspension
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/73—After-treatment of removed components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/20—Reductants
- B01D2251/206—Ammonium compounds
- B01D2251/2062—Ammonia
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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
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
Abstract
The invention relates to the technical field of flue gas treatment and purification, and particularly discloses a comprehensive treatment method of sulfur-containing waste flue gas and carbide slag. The treatment method comprises the steps of pre-spraying sulfur-containing waste flue gas by using ammonium-containing spraying liquid, and blowing air into pre-washing liquid obtained by pre-spraying to obtain purified gas and pre-washing oxidation liquid; then spraying the purified gas with dilute ammonia water to obtain tail gas reaching the standard; adding the obtained prewashing oxidation liquid into a calcium salt solution, and reacting to obtain calcium sulfate and an ammonium salt solution; adding the obtained ammonium salt solution into the carbide slag for mixing, heating for reaction to obtain ammonia gas and mixed slurry, and filtering the mixed slurry to obtain a calcium salt solution. The desulfurization efficiency of the method can reach more than 95 percent, the purity of the obtained calcium sulfate is more than 98 percent, the transfer rate of calcium in the carbide slag is more than or equal to 85 percent, and the synergistic treatment of the sulfur-containing waste flue gas and the carbide slag is realized; the method has the advantages of simple process, low cost and obvious industrial significance, and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of flue gas treatment and purification, in particular to a comprehensive treatment method of sulfur-containing waste flue gas and carbide slag.
Background
At present, a plurality of desulfurization technologies are available for flue gas, such as limestone/lime-gypsum desulfurization, magnesium oxide desulfurization, ammonia desulfurization, dual-alkali desulfurization and the like. The absorbents, desulfurization by-products, and desulfurization efficiencies and investment costs used in various flue gas desulfurization technologies vary widely.
The most common flue gas desulfurization processes used in industry are the calcium process followed by the ammonia process. The calcium method desulfurization has the advantages of rich lime resources, low cost, high desulfurization efficiency and the like, and has the defects of poor quality, low additional value and poor market prospect of the byproduct desulfurized gypsum, so that a large amount of desulfurized gypsum is accumulated, and secondary pollution is caused to the environment. The ammonia desulfurization method has the advantages of high absorption reaction speed, high absorption rate, wide application range, desulfurization and denitrification, and the like, and has the defects of high raw material cost, high storage and transportation management cost of ammonia water as a dangerous chemical, and the like.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method for cooperatively and comprehensively treating sulfur-containing waste flue gas and carbide slag, and through cooperatively treating the sulfur-containing waste flue gas and the carbide slag, the cost caused by the landfill of the carbide slag is reduced, the sulfur-containing waste flue gas is purified, and a marketable calcium sulfate product can be obtained through treatment.
In order to solve the technical problems, the invention adopts the technical scheme that: a comprehensive treatment method of sulfur-containing waste flue gas and carbide slag comprises the following steps:
(1) pre-spraying sulfur-containing waste flue gas by using ammonium-containing spraying liquid, and blowing air into pre-washing liquid obtained by pre-spraying to obtain purified gas and pre-washing oxidation liquid;
(2) spraying the purified gas obtained in the step (1) with dilute ammonia water to obtain tail gas reaching the standard;
(3) adding a calcium salt solution into the prewashing oxidation liquid obtained in the step (1), stirring for reaction, and filtering to obtain calcium sulfate and an ammonium salt solution;
(4) and (4) adding carbide slag into the ammonium salt solution obtained in the step (3), mixing, heating and reacting to obtain ammonia gas and mixed slurry, and filtering the mixed slurry to obtain a calcium salt solution.
In a preferred embodiment, in the step (1), the gas-liquid ratio of the sulfur-containing waste flue gas to the ammonium-containing spraying liquid is 0.2-2.0 m3L; the flow velocity of the sulfur-containing waste flue gas is 2-8 m/s, and the sulfur content of the sulfur-containing waste flue gas is 100-3000 mg/m3(ii) a The mass concentration of the ammonium-containing spraying liquid is 2-20%; preferably, the ammonium-containing spray liquid is ammonia water, or the ammonium-containing spray liquid is a mixed solution of ammonia water and ammonium sulfite and/or ammonium sulfate, and preferably, the ammonium-containing spray liquid is a mixed solution of ammonia water and ammonium sulfite. Parameters in the step (1) are further limited, for example, the gas-liquid ratio of the sulfur-containing waste flue gas to the ammonium-containing spray liquid is small, the selected gas-liquid ratio is small, a required spray tower liquid storage tank is enlarged, the occupied area and the equipment investment cost are increased, and if the gas-liquid ratio is too large, the absorption efficiency of sulfides in the sulfur-containing waste gas is low; for the flow velocity of the sulfur-containing waste flue gas, if the flow velocity is too low, the diameter of the required spray tower is large, the occupied area and the equipment investment cost are increased, and if the flow velocity is too high, the sulfide absorption efficiency in the sulfur-containing waste flue gas is low, and the resistance of a fan is increased; the mass concentration of the ammonium-containing spray liquid is also researched, and the phenomenon that ammonia escapes easily is found due to the fact that the concentration is too low, a required spray tower liquid storage tank is too large, the occupied area and the equipment investment cost are increased, and the concentration is too high.
Preferably, in the step (1), the volume ratio of the air to the pre-washing liquid is 60-300L/L, and the flow velocity of the air is 3-8 m/s; repeating the step for 1-4 times. The setting of the volume ratio of the air to the prewashing liquid is very critical, the oxidation of the sulfite is incomplete when the air is less, and the waste is caused when the gas-liquid ratio is high.
Preferably, in the step (2), the gas-liquid ratio of the purified gas to the diluted ammonia water is 0.2-1.0 m3L; the mass concentration of the dilute ammonia water is 0.1-3.0%; spraying the obtained solution of purified gas by using dilute ammonia waterReturning to the step (1) to be used as ammonium-containing spraying liquid. The gas-liquid ratio of the purified gas to the dilute ammonia water is limited, if the gas-liquid ratio is small, a required spray tower liquid storage tank is too large, the occupied area and the equipment investment cost are increased, and if the gas-liquid ratio is too large, the absorption efficiency of sulfides in the sulfur-containing waste gas is low; the concentration of the dilute ammonia water is low, the volume of the required equipment is large, the occupied area and the investment are increased, and the ammonia water has high concentration and is easy to cause ammonia escape. And (3) returning ammonium sulfite produced by absorbing sulfur dioxide in the purified gas by using dilute ammonia water and excessive dilute ammonia water to the step (1) for pre-spraying, reacting with sulfur dioxide in the sulfur-containing waste flue gas to generate ammonium sulfite, and oxidizing the ammonium sulfite by blown air to generate ammonium sulfate.
Preferably, in the step (3), the solid-gas ratio of the calcium salt in the calcium salt solution to the sulfur-containing waste flue gas is 1-10 g/Nm3(ii) a The mass concentration of the calcium salt solution is 2-35%; the calcium salt is one or more of calcium chloride, calcium nitrate or calcium iodide; the stirring reaction is carried out at the temperature of 5-60 ℃ for 15-60 min. The calcium salt is added, so that calcium ions in the raw material carbide slag are utilized to obtain a pure calcium sulfate product, and raw materials are provided for the next calcium salt preparation and ammonia water preparation; the dosage of calcium salt is small, and sulfate ions cannot be completely precipitated; the large amount of calcium salt causes large system circulation and high production cost; low calcium salt concentration, large equipment volume required by the system, high investment, high operation cost, overhigh calcium salt concentration and high production cost for producing calcium salt.
Preferably, in the step (4), the liquid-solid ratio of the ammonium salt solution to the carbide slag is 10-100L/kg; the carbide slag mainly comprises calcium hydroxide, wherein the mass content of the calcium hydroxide is 80-90%; the heating reaction is carried out at the temperature of 50-85 ℃ for 30-60 min. The liquid-solid ratio of the ammonium salt solution to the carbide slag has the following influence, the liquid-solid ratio is low, the utilization rate of the carbide slag is low, the liquid-solid ratio is high, and the ammonia of the ammonium salt solution is not completely discharged. The carbide slag used in the invention is mainly derived from solid waste generated in the production of polyvinyl chloride by a carbide method in a chemical plant.
Preferably, in the step (4), the ammonia gas is absorbed by water and returned to the step (2) to be used as dilute ammonia water; the obtained calcium salt solution is returned to the step (3) for use.
The method comprises the following process steps: sulfur dioxide in sulfur-containing waste flue gas generated by a coal power plant and the like reacts with ammonium ions in ammonium-containing spraying liquid to generate ammonium sulfite salt, and the ammonium sulfite salt is oxidized into stable ammonium sulfate by blown air in prewashing liquid; sulfur dioxide in the purified gas is further absorbed by dilute ammonia water to form ammonium sulfite, and tail gas reaches the standard and is discharged; stirring and reacting the prewashed oxidation liquid and the added calcium salt solution, and filtering and separating to obtain calcium sulfate and ammonium salt solution; mixing the ammonium salt solution and the carbide slag, heating and reacting, wherein the main component of the carbide slag is calcium hydroxide, ammonia gas is released by reaction, mixed slurry of calcium salt and carbide slag impurities is obtained, and the mixed slurry is filtered and separated to obtain the calcium salt solution. Taking the ammonium-containing spray liquid as ammonia water and the calcium salt solution as calcium chloride solution as an example, the reaction equation of the steps is as follows:
the desulfurization efficiency of the method can reach more than 95 percent, the purity of the obtained calcium sulfate reaches 98 percent, and the calcium sulfate can be sold as a gypsum product to create good economic benefit.
The transfer rate of calcium in the carbide slag is more than or equal to 85 percent, the utilization rate is high, the solid waste discharge amount is reduced, the cost brought by the landfill of the carbide slag is reduced, and the synergistic treatment of the sulfur-containing waste flue gas and the carbide slag is realized.
The method overcomes the defects of the existing ammonia desulphurization, does not have the problem of evaporation and drying of ammonium sulfate during the ammonia desulphurization, does not have the condition of generating a large amount of solid waste during the carbide slag desulphurization, does not have the problem of high raw material cost during the lime desulphurization, has simple process, low cost and obvious industrial significance, and is suitable for industrial production.
According to the comprehensive treatment method of the sulfur-containing waste flue gas and the carbide slag, the sulfur-containing waste flue gas and the carbide slag are subjected to synergistic treatment, so that the cost caused by carbide slag landfill is reduced. At present, the main treatment of the carbide slag is direct landfill, and related researchers also carry out research, but the carbide slag is used for sulfur fixation and soil fixation to repair roads, but certain problems exist. The carbide slag is used for sulfur fixation and desulfurization of the fire coal, so that a defogging nozzle is easy to block, the quality of the produced gypsum is low, the added value of the product is low, and the market is narrow; the carbide slag is used for soil stabilization and road repair, the application rate is low, the types of soil are various, the difference among the soils is large, the coordination work among multiple regions and multiple departments is involved, and the effective utilization of the carbide slag for soil stabilization and road repair is troublesome. The method can realize the resource utilization of the industrial solid waste carbide slag, and has obvious industrial significance.
Detailed Description
The technical solution of the present invention will be described in detail by examples.
The sulfur-containing waste flue gases used in the following examples are all from Hexaster coal electric Co Ltd of Xinjiang, and the sulfur contents of the sulfur-containing waste flue gases 1-3 are 2450mg/m3、2208mg/m3、380mg/m3(ii) a The carbide slag used in the embodiment of the invention is from Xinjiang Zhongtai chemical corporation, and mainly comprises 89.7% of calcium hydroxide, 3.5% of silicon oxide and 2.5% of aluminum oxide; the starting materials or chemicals used in the examples of the present invention are, unless otherwise specified, commercially available in a conventional manner.
Example 1
(1) Sulfur-containing waste flue gas 1 with the flow rate of 18m3At 25 deg.C, pre-spraying with mixed solution of ammonia water and ammonium sulfite (5.0 wt%), and pre-spraying at 0.15Nm in the pre-washing solution3Blowing air at a flow rate of 43mg/m to obtain purified gas (sulfur content of 43 mg/m)3) And prewashing oxidizing liquid, the flow rate of the purified gas is 18.3m3The flow rate of the prewashing oxidation liquid is 0.8L/h;
(2) spraying the purified gas obtained in the step (1) with dilute ammonia water (mass concentration is 1 percent) to obtain tail gas reaching the standard (the sulfur content is 24 mg/m)3) And the tail gas flow reaching the standard is 18.4m3/h；
(3) Adding a calcium chloride solution (with the mass concentration of 15.0%) into the prewashed oxidation liquid obtained in the step (1), carrying out stirring reaction for 1h at the temperature of 25 ℃, and filtering to obtain 145.48g of calcium sulfate (containing 36.74% of crystallized water and surface water) and 1.24L of an ammonium chloride solution (with the mass concentration of 2.9%) per hour;
(4) and (3) adding 510g of carbide slag into 10L of the ammonium chloride solution obtained in the step (3), mixing, heating and reacting at 60 ℃ for 1h to obtain ammonia gas and mixed slurry, and filtering the mixed slurry to obtain 8.3L of calcium chloride solution (the mass concentration is 3.63%).
In the step (2), the solution obtained by spraying the purified gas with the dilute ammonia water is returned to the step (1) to be used as the mixed solution of the ammonia water and the ammonium sulfite; in the step (4), ammonia gas is absorbed by water, the ammonia gas is returned to the step (2) to be used as dilute ammonia water, and the obtained calcium chloride solution is returned to the step (3) to be used.
Through detection, the desulfurization rate of the sulfur-containing waste flue gas 1 is 99.02%; the tail gas reaching the standard discharged in the step (2) reaches GB-13223-; CaSO in calcium sulfate (dry basis) obtained in step (3)4The percentage content of the compound is 99.43 percent, and Na, Al, Si and Cl are not detected; and (4) the transfer rate of Ca in the carbide slag in the step (4) is 87.75%.
Example 2
(1) Sulfur-containing waste flue gas 2 with the flow rate of 500m3Per h (gas temperature 60 ℃ C., standard volume 410Nm3H), pre-spraying with a mixed solution (with the mass concentration of 9%) of ammonia water and ammonium sulfite, and simultaneously pre-spraying the obtained pre-washing liquid at a rate of 4.0Nm3Blowing air at a flow rate of 51mg/m to obtain purified gas (sulfur content of 51 mg/m)3) And prewashing oxidizing liquid, the flow rate of the purified gas is 433Nm3The flow rate of the prewashing oxidation liquid is 13L/h;
(2) spraying the purified gas obtained in the step (1) with dilute ammonia water (the mass concentration is 4.5 percent) to obtain tail gas reaching the standard (the sulfur content is 28 mg/m)3) The tail gas flow reaching the standard is 421Nm3/h；
(3) Adding a calcium chloride solution (with the mass concentration of 30%) into the prewashed oxidation liquid obtained in the step (1), carrying out stirring reaction for 0.5h at the temperature of 30 ℃, and filtering to obtain 2.4kg of calcium sulfate (containing 34.37% of crystal water and surface water) and 17.17L of an ammonium chloride solution (with the mass concentration of 4.34%) per hour;
(4) and (3) adding 22kg of carbide slag into the 300L of ammonium chloride solution obtained in the step (3), mixing, heating and reacting for 0.6h at 75 ℃ to obtain ammonia gas and mixed slurry, and filtering the mixed slurry to obtain 235L of calcium chloride solution (the mass concentration is 5.76%).
In the step (2), the solution obtained by spraying the purified gas with the dilute ammonia water is returned to the step (1) to be used as the mixed solution of the ammonia water and the ammonium sulfite; in the step (4), ammonia gas is absorbed by water, the ammonia gas is returned to the step (2) to be used as dilute ammonia water, and the obtained calcium chloride solution is returned to the step (3) to be used.
Through detection, the desulfurization rate of the sulfur-containing waste flue gas 2 is 98.73%; the tail gas reaching the standard discharged in the step (2) reaches GB-13223-; CaSO in calcium sulfate (dry basis) obtained in step (3)4The percentage content of the compound is 99.12 percent, and Na, Al, Si and Cl are not detected; and (4) the transfer rate of Ca in the carbide slag in the step (4) is 91.46%.
Example 3
(1) The sulfur-containing waste flue gas 3 is used at a flow rate of 7360m3Per h (gas temperature 160 ℃ C., standard volume 4641Nm3H), pre-spraying with a mixed solution (mass concentration of 15%) of ammonia water and ammonium sulfite, and simultaneously pre-spraying the obtained pre-washing liquid at a rate of 8.0Nm3Blowing air at a flow rate of/h to obtain purified gas (sulfur content of 32 mg/m)3) And prewashing oxidizing liquid, the flow rate of purified gas is 4920Nm3The flow rate of the prewashing oxidation liquid is 15L/h;
(2) spraying the purified gas obtained in the step (1) with dilute ammonia water (the mass concentration is 0.5 percent) to obtain tail gas reaching the standard (the sulfur content is 14 mg/m)3) The tail gas flow reaching the standard is 4780Nm3/h；
(3) Adding a calcium nitrate solution (with the mass concentration of 20%) into the prewashed oxidation liquid obtained in the step (1), stirring and reacting for 1h at the temperature of 35 ℃, and filtering to obtain 5.6kg of calcium sulfate (containing 32.79% of crystallized water and surface water) and 24.53L of ammonium nitrate solution (with the mass concentration of 8.96%) per hour;
(4) and (3) adding 32kg of carbide slag into 400L of ammonium nitrate solution obtained in the step (3), mixing, heating and reacting for 0.6h at 85 ℃ to obtain ammonia gas and mixed slurry, and filtering the mixed slurry to obtain 320L of calcium nitrate solution (the mass concentration is 17.21%).
In the step (2), the solution obtained by spraying the purified gas with the dilute ammonia water is returned to the step (1) to be used as the mixed solution of the ammonia water and the ammonium sulfite; in the step (4), ammonia gas is absorbed by water, the ammonia gas is returned to the step (2) to be used as dilute ammonia water, and the obtained calcium nitrate solution is returned to the step (3) to be used.
Through detection, the desulfurization rate of the sulfur-containing waste flue gas 3 is 99.67%; the tail gas reaching the standard discharged in the step (2) reaches GB-13223-; CaSO in calcium sulfate (dry basis) obtained in step (3)4The percentage content of the compound is 99.32 percent, and Na, Al, Si and Cl are not detected; and (4) the transfer rate of Ca in the carbide slag in the step (4) is 86.59%.
Claims (7)
1. A comprehensive treatment method of sulfur-containing waste flue gas and carbide slag is characterized by comprising the following steps: the method comprises the following steps:
(1) pre-spraying sulfur-containing waste flue gas by using ammonium-containing spraying liquid, and blowing air into pre-washing liquid obtained by pre-spraying to obtain purified gas and pre-washing oxidation liquid;
(2) spraying the purified gas obtained in the step (1) with dilute ammonia water to obtain tail gas reaching the standard;
(3) adding a calcium salt solution into the prewashing oxidation liquid obtained in the step (1), stirring for reaction, and filtering to obtain calcium sulfate and an ammonium salt solution;
(4) and (4) adding carbide slag into the ammonium salt solution obtained in the step (3), mixing, heating and reacting to obtain ammonia gas and mixed slurry, and filtering the mixed slurry to obtain a calcium salt solution.
2. The comprehensive treatment method of sulfur-containing waste flue gas and carbide slag as claimed in claim 1, characterized in that: in the step (1), the gas-liquid ratio of the sulfur-containing waste flue gas to the ammonium-containing spraying liquid is 0.2-2.0 m3L; the flow velocity of the sulfur-containing waste flue gas is 2-8 m/s, and the sulfur content of the sulfur-containing waste flue gas is 100-3000 mg/m3(ii) a The mass concentration of the ammonium-containing spraying liquid is 2-20%; preferably, the ammonium-containing spray liquid is ammonia water, or the ammonium-containing spray liquid is a mixed solution of ammonia water and ammonium sulfite and/or ammonium sulfate, and preferably, the ammonium-containing spray liquid is a mixed solution of ammonia water and ammonium sulfite.
3. The comprehensive treatment method of sulfur-containing waste flue gas and carbide slag as claimed in claim 1, characterized in that: in the step (1), the volume ratio of the air to the pre-washing liquid is 60-300L/L; preferably, the operation of the step is repeated for 1 to 4 times.
4. The comprehensive treatment method of the sulfur-containing waste flue gas and the carbide slag according to any one of claims 1 to 3, characterized by comprising the following steps: in the step (2), the gas-liquid ratio of the purified gas to the diluted ammonia water is 0.2-1.0 m3L; the mass concentration of the dilute ammonia water is 0.1-3.0%; and (3) returning the solution obtained by spraying the purified gas by the dilute ammonia water to the step (1) to be used as ammonium-containing spraying liquid.
5. The comprehensive treatment method of sulfur-containing waste flue gas and carbide slag as claimed in claim 4, characterized in that: in the step (3), the solid-gas ratio of the calcium salt in the calcium salt solution to the sulfur-containing waste flue gas is 1-10 g/Nm3(ii) a The mass concentration of the calcium salt solution is 2-35%; the calcium salt is one or more of calcium chloride, calcium nitrate or calcium iodide; the stirring reaction is carried out at the temperature of 5-60 ℃ for 15-60 min.
6. The comprehensive treatment method of sulfur-containing waste flue gas and carbide slag as claimed in claim 5, characterized in that: in the step (4), the liquid-solid ratio of the ammonium salt solution to the carbide slag is 10-100L/kg; the carbide slag mainly comprises calcium hydroxide, wherein the mass content of the calcium hydroxide is 80-90%; the heating reaction is carried out at the temperature of 50-85 ℃ for 30-60 min.
7. The comprehensive treatment method of sulfur-containing waste flue gas and carbide slag as claimed in claim 6, characterized in that: in the step (4), the ammonia gas is absorbed by water and returns to the step (2) to be used as dilute ammonia water; the obtained calcium salt solution is returned to the step (3) for use.
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