CN110152467B - Flue gas advanced treatment method for synchronous desulfurization and denitrification by absorption method - Google Patents
Flue gas advanced treatment method for synchronous desulfurization and denitrification by absorption method Download PDFInfo
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Abstract
The invention discloses a flue gas deep treatment method for synchronous desulfurization and denitrification by an absorption method, which takes natural manganese oxide ore or synthetic nano manganese oxide added with a surfactant as NOxAnd SO2The absorption liquid realizes the purification of the flue gas. The invention relates to a method for synchronously desulfurizing and denitrating, SO2The removal rate is maintained to be more than 95 percent, the NO removal rate is maintained to be more than 80 percent, reaction products can be separated and utilized, the operation cost is low, and the method has good prospect.
Description
Technical Field
The invention belongs to the field of atmospheric pollution control engineering, and particularly relates to a wet absorption synchronous desulfurization and denitrification flue gas treatment method.
Background
A great deal of SO is generated in the high-temperature combustion process of various boilers and kilns2NOx, causes acid rain in 81.6% of cities across the country. Nitrogen oxide emissions can also lead to regional environmental pollution problems such as photochemical smog and ozone layer depletion. Technologies currently used to control nitrogen oxide emissions include Selective Catalytic Oxidation (SCO), non-selective catalytic reduction (SNCR), and Selective Catalytic Reduction (SCR). The desulfurization process mainly adopts a wet method and a semi-dry method, wherein the desulfurization process mainly adopts a calcium method and accounts for about 85 percent of the market proportion. At present, the flue gas purification process widely used in China is a combined flue gas treatment process of high-temperature SCR denitration, dust removal and wet desulphurization, on one hand, a large amount of ammonia is consumed, the risk of ammonia escape exists, and on the other hand, a large amount of desulfurized gypsum which is difficult to recycle is also byproduct. The separate and independent flue gas desulfurization and denitration technologies have the advantages of large one-time investment, high operating cost and large occupied area, and the synchronous desulfurization and denitration technology is expected to overcome the difficulties.
China is a main manganese-storing country in the world, and manganese oxide ores in the middle and western regions of Hunan, Hubei, Sichuan, Chongqing, Guangxi, Anhui, Yunnan, Gansu, Ningxia, Qinghai and the like are abundant in reserves, and in recent years, the national prospecting department finds a plurality of ultra-large manganese ore deposits in Guizhou, Guangxi and the like, and the total amount of manganese ore resources is proved to reach 13.8 hundred million tons. Although pyrolusite resources are rich in China, the quality of manganese ores is generally poor,most of the low-grade manganese ore deposit is low-grade manganese ore deposit, so that the utilization of low-grade manganese oxide ore resources in the fields of metallurgy and chemical industry is limited. The exploration and research of developing environmental engineering materials by utilizing low-grade manganese oxide ore resources have important significance on the application of the manganese ore resources and the improvement of environmental protection technology. From the existing published literature, the research work of synchronous desulfurization and denitrification by wet absorption of flue gas is available at home and abroad, and certain achievements are obtained, such as: in patent CN1843574A, sodium chlorite and an additive are used as a liquid phase absorbent, the additive is one or a combination of calcium hypochlorite, sodium bicarbonate, hydrogen peroxide, disodium hydrogen phosphate or calcium hydroxide, and under the catalysis of the additive, the oxidizability of chlorite and a series of intermediate products is greatly improved, SO is promoted2And NO, thereby greatly improving SO of the absorption liquid2、NOxAnd absorbing with a jet bubble reactor. The patent CN107744715A uses the main product ammonium sulfite in the ammonia desulphurization process as NO and SO2The absorbent of (2) solves the problem that NO is hardly soluble in water by adding CuO as an auxiliary absorbent to an absorbent by a bubbling method, but has the problem of secondary pollution such as ammonia volatilization. CN101574617B patent uses ore pulp prepared by pyrolusite and metal chelating agent as absorbent for SO in coal-fired flue gas2、NOxThe method has the advantages that the method is synchronous in absorption and removal, the metal chelating agent is used for removing polyvalent metal ions such as calcium, magnesium, lead, zinc, iron and the like in pyrolusite slurry, the problem that precipitation and scaling of the metal ions influence desulfurization interface reaction is solved, the mother liquor can utilize poor solubility of manganese sulfate and manganese nitrate at the same temperature after solid-liquid separation, the recycling of sulfur and manganese is realized, the solubility of NO in absorption liquid is not improved, and the problem of low NO removal rate exists.
When strong oxidants such as sodium chlorite and ozone are used, the former researches show that NO and SO are contained2The removal efficiency is higher, but most of the oxidants are expensive, the investment cost and the operation cost are higher, and the industrial application is difficult; if the cheap absorption liquid such as ammonium sulfite and pyrolusite pulp is used, the NO removal rate is low, generally 60-70%, and the industrial emission standard is difficult to achieve. In view of the above disadvantages, there is an urgent need for development by scientists in the field of environmental protectionA cheap and efficient wet flue gas synchronous desulfurization and denitrification method.
Disclosure of Invention
In order to avoid the defects of the prior art, the invention provides an advanced treatment method for flue gas by synchronous desulfurization and denitrification through an absorption method, aiming at realizing NO and SO with lower cost2Efficient removal of the active species.
In order to realize the purpose of the invention, the following technical scheme is adopted:
an absorption synchronous desulfurization and denitrification flue gas advanced treatment method is characterized in that:
(1) selecting manganese oxide ore or industrially synthesized nano manganese oxide, and grinding into ultrafine powder which is sieved by a 325-mesh sieve;
(2) mixing the superfine powder with water according to a mass ratio of 1: 10-40 to prepare a suspension;
(3) adding a surfactant accounting for 1-5% of the suspension by mass into the suspension, and then adjusting the pH to 2-6 by using acid to obtain an absorption liquid for synchronous desulfurization and denitrification;
(4) adding the absorption liquid into a flue gas washing and absorbing device to remove SO in the flue gas2And NOxSO after treatment2The removal rate is maintained above 95 percent, NOxThe removal rate is maintained to be more than 80 percent;
(5) to SO2The absorption liquid is regarded as invalid when the removal rate is lower than 80 percent; and (3) solid-liquid separation of the invalid absorption liquid, discarding solid substances, and evaporating and crystallizing the residual liquid to obtain manganese sulfate and manganese nitrate byproducts, or directly selling the residual liquid as a raw material of a liquid fertilizer.
Further, the manganese dioxide in the manganese oxide ore is more than 25% by mass, wherein the manganese oxide ore is at least one of manganese potassium ore, manganese calcium ore and birnessite.
Further, the manganese oxide ore is a nano mineral, and the diameter of the crystal is less than 90 nanometers.
Further, the surfactant is polyethylene glycol.
Further, the flue gas washing and absorbing device comprises, but is not limited to, a tray type, a packing type, a bubbling type, a spraying type and a spraying type washing tower.
Further, the patent CN101574617B refers to a method for obtaining manganese sulfate and manganese nitrate by-products through evaporative crystallization.
The invention has the beneficial effects that:
1. the manganese oxide ore is a natural nano mineral material, has wide source and low price, is used as an active material for wet synchronous desulfurization and denitrification, and has the function of synchronous desulfurization and denitrification. The manganese oxide is a natural oxidant and can oxidize SO in flue gas2Conversion to sulfate (equation 1):
MnO2+SO2——Mn2++SO4 2- (1)；
smaller manganese oxide particles, larger specific surface area, and SO2The higher the reactivity, the better the desulfurization effect. Manganese oxides in the manganese oxide ore are mainly nano needle-shaped particles and are coated on the surface of the clay mineral, or the needle-shaped manganese oxide particles form an interwoven structure, so that the pores among the mineral particles are developed, the porosity is high, and the reaction activity is high.
2. The surfactant used in the method has the function of stabilizing the liquid film, and can prolong the stabilization time of micro bubbles and SO in gas2、NOxReaction time with manganese oxide to accelerate SO in gas phase2、NOxMigration to liquid phase, increase of SO2、NOxAnd (4) removing efficiency.
3. Experimental research shows that the surfactant added into the absorption liquid has weak interaction with NO, so that the solubility of NO in a liquid phase is increased, the NO dissolution rate is accelerated, and the problem that NO is difficult to dissolve in the absorption process is solved, which is one of the precondition of the wet-method efficient flue gas denitration.
4. The invention discovers that the nano manganese oxide has the functions of autoxidation and catalytic oxidation of NO (equations 2 and 3), and the oxidation product is NO2Due to NO2High solubility, easy conversion to stable nitrate, NO oxidation to accelerate NO dissolution in gasHigh denitration efficiency:
MnO2+NO——Mn2++NO3 - (2)
NO+O2——NO3 - (3)。
5. the method of the invention realizes synchronous desulfurization and denitrification, and is suitable for low-temperature or flue gas purification containing toxic catalyst smoke dust. SO long as the temperature of the flue gas reaches 60 DEG C2The removal rate is more than 95%, the NO purification efficiency can reach more than 80%, and the defect of SCR denitration is overcome.
6. According to the method, manganese oxide ores can be utilized, nitrogen oxides in flue gas are recycled to be nitrates while synchronous desulfurization and denitration are realized, and manganese ores are treated to prepare manganese sulfate and manganese nitrate. Compared with SCR, the method reduces NO into useless nitrogen by ammonia, and is more environment-friendly.
Drawings
FIG. 1 is an SEM image of the manganese oxide ore used in examples 1-3, showing that: the manganese oxide is in a needle shape and is arranged in an interlaced way, and the crystal diameter is 50-90 nm.
FIG. 2 shows an experimental apparatus for simultaneous absorption, desulfurization and denitrification, wherein the reference numerals in the figure are as follows: 1-Ar gas cylinder, 2-O2Gas cylinder of/Ar, gas cylinder of 3-NO/Ar, gas cylinder of 4-SO2The device comprises an Ar gas cylinder, a 5-mass flow meter, a 6-gas mixer, a 7-pH/temperature monitor, an 8-absorption reactor, a 9-gas release head, a 10-heating magnetic stirrer, an 11-water bath, a 12-sulfuric acid drying cylinder and a 13-flue gas analyzer.
FIG. 3 is a time-dependent curve of the simultaneous desulfurization and denitrification effects of example 1, wherein the experimental conditions are as follows: [ NO ]]＝[SO2]＝1000ppm；[O2]9 percent; the mass concentration of PEG is 3%; the flow rate of flue gas is 100 mL/min; initial pH 4; the solid-to-liquid ratio is 1: 10; t-60 ℃.
FIG. 4 shows the effect of the concentration of polyethylene glycol on the desulfurization and denitrification efficiency in example 2, with the following experimental conditions: [ NO ]]＝[SO2]＝1000ppm；[O2]9 percent; the flow rate of flue gas is 100 mL/min; initial pH 4; the solid-to-liquid ratio is 1: 20; t-60 ℃.
FIG. 5 is a graph showing the effect of temperature of the absorbent solution on desulfurization and denitrification efficiencies in example 3The parts are as follows: [ NO ]]＝[SO2]＝1000ppm；[O2]9 percent; the mass concentration of PEG is 3%; the flow rate of flue gas is 100 mL/min; initial pH 3; the solid-to-liquid ratio is 1: 30.
FIG. 6 is a schematic view showing the structure of a packed absorption column in example 5, which comprises 1-shell, 2-inlet, 3-outlet, 4-porous partition, 5-wire gauze packed with metal, 6-rotary shower pipe, and 7-circulation pipe for absorption liquid.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof will be described in detail with reference to the following examples. The following is merely exemplary and illustrative of the inventive concept and various modifications, additions and substitutions of similar embodiments may be made to the described embodiments by those skilled in the art without departing from the inventive concept or exceeding the scope of the claims defined thereby.
Example 1
Selecting manganese oxide ore of Anhui somewhere, wherein the chemical composition of the ore is as follows: SiO 22，34.63％；MnO，20.91％；Fe2O3，5.58％；Al2O3，4.23％；CaO，2.21％；ZnO，1.64％；K2O，1.04％；MgO，0.65％；P2O50.56%; loss on ignition, 27.65%; others, 0.9%. The content of the manganese oxide is 26.4 percent, wherein the microscopic characteristics of the manganese oxide are shown in figure 1.
Grinding manganese oxide ore in a ball mill for 60min, and screening to obtain powder with 325 meshes. Then mixing the manganese oxide powder and water according to the mass ratio of 1:10 to prepare suspension. Adding polyethylene glycol accounting for 3 percent of the mass of the suspension into the suspension, and then adjusting the pH value of the suspension to 4 by using sulfuric acid to obtain the absorption liquid for synchronous desulfurization and denitrification.
The absorption solution was placed in a simulation experiment apparatus as shown in FIG. 2, and NO/Ar, SO was added in an amount of 0.1% by volume of NO2SO of 0.1% by volume2/Ar、O215% by volume of O2Absorption experiment (FIG. 2) for/Ar distributionThe conditions are as follows: [ NO ]]＝[SO2]＝1000ppm；[O2]9 percent; the mass concentration of PEG is 3%; the flow rate of flue gas is 100 mL/min; initial pH 4; the solid-to-liquid ratio is 1: 10; t-60 ℃. On-line detection of SO in absorbed tail gas by using flue gas analyzer2Calculating the desulfurization and denitrification efficiency and detecting Mn in the absorption liquid according to the concentration of NO2+、SO4 2-、NO3 -The concentration changes, and the reaction process is known. By detection, SO2The removal rate was maintained at 95% or more, and the NO removal rate was maintained at 80% or more (fig. 3).
Example 2
Selecting manganese oxide ore of Anhui somewhere, wherein the chemical composition of the ore is as follows: SiO 22，34.63％；MnO，20.91％；Fe2O3，5.58％；Al2O3，4.23％；CaO，2.21％；ZnO，1.64％；K2O，1.04％；MgO，0.65％；P2O50.56%; loss on ignition, 27.65%; others, 0.9%. The content of the manganese oxide is 26.4 percent, wherein the microscopic characteristics of the manganese oxide are shown in figure 1.
Grinding the manganese oxide ore in a ball mill for 30min, and screening to obtain powder with 325 meshes. Then mixing manganese oxide ore powder and water according to the mass ratio of 1:20 to prepare suspension. Adding polyethylene glycol accounting for 0%, 0.2%, 0.6%, 1.0%, 1.4%, 1.8%, 2.2%, 2.6%, 3.0%, 3.4% and 3.8% of the suspension by mass into the suspension, and then adjusting the pH of the suspension to 4 by using sulfuric acid, thereby obtaining absorption solutions with different polyethylene glycol concentrations for synchronous desulfurization and denitrification.
Respectively placing absorption liquids with different polyethylene glycol concentrations into a simulation experiment device shown in figure 2, and adding NO/Ar and SO with the volume percentage of NO of 0.1 percent2SO of 0.1% by volume2/Ar、O215% by volume of O2Absorption experiments were carried out with/Ar distribution (fig. 2) under the following experimental conditions: [ NO ]]＝[SO2]＝1000ppm；[O2]9 percent; the flow rate of flue gas is 100 mL/min; initial pH 4; the solid-to-liquid ratio is 1: 20; t-60 ℃. On-line detection of SO in absorbed tail gas by using flue gas analyzer2And calculating the desulfurization and denitrification efficiency according to the NO concentration. By detection, SO2The removal rate is maintained at 95% or more, and when 3.0% or more of polyethylene glycol is added, the NO removal rate is maintained at 80% or more (fig. 4).
Example 3
Selecting manganese oxide ore of Anhui somewhere, wherein the chemical composition of the ore is as follows: SiO 22，34.63％；MnO，20.91％；Fe2O3，5.58％；Al2O3，4.23％；CaO，2.21％；ZnO，1.64％；K2O，1.04％；MgO，0.65％；P2O50.56%; loss on ignition, 27.65%; others, 0.9%. The content of the manganese oxide is 26.4 percent, wherein the microscopic characteristics of the manganese oxide are shown in figure 1.
Grinding the manganese oxide ore in a ball mill for 30min, and screening to obtain powder with 325 meshes. And then mixing the pyrolusite powder and water according to the mass ratio of 1:30 to prepare suspension. Polyethylene glycol accounting for 3.0 percent of the mass of the suspension is added into the suspension, and then the pH value of the suspension is adjusted to 3 by using sulfuric acid, so that the absorption liquid for synchronous desulfurization and denitrification is obtained.
The absorption solution was placed in a simulation experiment apparatus as shown in FIG. 2, and NO/Ar, SO was added in an amount of 0.1% by volume of NO2SO of 0.1% by volume2/Ar、O215% by volume of O2Absorption experiments were carried out with/Ar distribution (fig. 2) under the following experimental conditions: [ NO ]]＝[SO2]＝1000ppm；[O2]9 percent; the mass concentration of PEG is 3.0%; the flow rate of flue gas is 100 mL/min; initial pH 3; the solid-liquid ratio is 1: 30; t-40, 50, 60, 70, 80 ℃. On-line detection of SO in absorbed tail gas by using flue gas analyzer2And calculating the desulfurization and denitrification efficiency according to the NO concentration. By detection, SO2The removal rate was maintained at 95% or more, and the NO removal rate was maintained at 80% or more at a temperature of 60 ℃ or more (fig. 5).
Example 4
Mixing MnSO4.H2O、KMnO4And mixing and dissolving water according to the mass ratio of 1:2:2, reacting for 60min by magnetic stirring, and centrifugally dewatering to obtain the synthetic manganese oxide.
Grinding the synthesized manganese oxide in a ball mill for 30min, and screening to obtain powder with 325 meshes. Then mixing the synthetic manganese oxide and water according to the mass ratio of 1:40 to prepare suspension. Adding polyethylene glycol accounting for 3% of the suspension by mass into the suspension, and then adjusting the pH of the suspension to 5 by using sulfuric acid to obtain the absorption liquid for synchronous desulfurization and denitrification.
The suspension was placed in a simulated experimental apparatus as shown in FIG. 2 with NO/Ar, SO at 0.1% NO by volume2SO of 0.1% by volume2/Ar、O215% by volume of O2Absorption experiments were carried out with/Ar distribution (fig. 2) under the following experimental conditions: [ NO ]]＝[SO2]＝1000ppm；[O2]9 percent; the mass concentration of PEG is 3.0%; the flow rate of flue gas is 100 mL/min; initial pH 5; the solid-to-liquid ratio is 1: 40; the temperature of the absorption liquid is maintained between 60-80 deg.C. On-line detection of SO in absorbed tail gas by using flue gas analyzer2And calculating the desulfurization and denitrification efficiency according to the NO concentration. By detection, SO2The removal rate is maintained above 95%, and the NO removal rate is maintained above 80%.
Example 5
The manganese oxide ore of a certain place is selected, and the content of the manganese oxide is 47.3 percent.
Grinding the manganese oxide ore in a ball mill for 30min, and screening to obtain powder with 325 meshes. And then mixing the pyrolusite powder and water according to the mass ratio of 1:20 to prepare suspension. Polyethylene glycol accounting for 3.0 percent of the mass of the suspension is added into the suspension, and then the pH value of the suspension is adjusted to 3 by using sulfuric acid, so that the absorption liquid for synchronous desulfurization and denitrification is obtained.
The prepared absorption liquid is circularly sprayed in the packed tower absorption device shown in figure 6, the wire mesh is wave-shaped, the wave height is 20mm, the wave length is 100mm, the diameter of the wire is 0.4mm, and the aperture is 2 mm. The flue gas of the glass kiln is taken as a processing object, the inlet temperature of the flue gas is between 120 ℃ and 180 ℃, and a flue gas analyzer is used for detecting SO in the absorbed tail gas on line2And calculating the desulfurization and denitrification efficiency according to the NO concentration. By detection, SO2The removal rate is maintained at 98 percent, and the NO removal rate is maintained above 80 percent.
Claims (4)
1. An absorption synchronous desulfurization and denitrification flue gas advanced treatment method is characterized in that:
(1) selecting manganese oxide ore or industrially synthesized nano manganese oxide, and grinding into ultrafine powder which is sieved by a 325-mesh sieve;
(2) mixing the superfine powder with water according to a mass ratio of 1: 10-40 to prepare a suspension;
(3) adding a surfactant polyethylene glycol accounting for 1-5% of the suspension by mass into the suspension, and then adjusting the pH to 2-6 with acid to obtain an absorption liquid for synchronous desulfurization and denitrification;
(4) adding the absorption liquid into a flue gas washing and absorbing device to remove SO in the flue gas2And NOxSO after treatment2The removal rate is maintained above 95 percent, NOxThe removal rate is maintained to be more than 80 percent;
(5) to SO2The absorption liquid is regarded as invalid when the removal rate is lower than 80 percent; and (3) solid-liquid separation of the invalid absorption liquid, discarding solid substances, and evaporating and crystallizing the residual liquid to obtain manganese sulfate and manganese nitrate byproducts, or directly selling the residual liquid as a raw material of a liquid fertilizer.
2. The deep treatment method for flue gas desulfurization and denitrification synchronously by an absorption method according to claim 1, characterized by comprising the following steps: the manganese dioxide content of the manganese oxide ore is more than 25% by mass, wherein the manganese oxide ore is at least one of manganese potassium ore, manganese calcium ore and birnessite.
3. The deep treatment method for flue gas desulfurization and denitrification synchronously by an absorption method according to claim 1, characterized by comprising the following steps: the manganese oxide ore is a nano mineral, and the diameter of the crystal is less than 90 nanometers.
4. The deep treatment method for flue gas desulfurization and denitrification synchronously by an absorption method according to claim 1, characterized by comprising the following steps: the flue gas washing and absorbing device comprises a tower plate type, a filling type, a bubbling type, a spraying type and a spraying type washing tower.
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| CN111272946A (en) * | 2020-03-30 | 2020-06-12 | 合肥工业大学 | Device and method for measuring content of organic carbon in industrial waste salt |
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