CN112316900A - Manganese-cerium-modified high-iron fly ash adsorbent for flue gas denitration and preparation method thereof - Google Patents
Manganese-cerium-modified high-iron fly ash adsorbent for flue gas denitration and preparation method thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
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- B01D2257/40—Nitrogen compounds
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- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
Abstract
The invention belongs to the technical field of coal ash solid waste recycling and flue gas denitration, and provides a manganese-cerium modified high-iron coal ash adsorbent for flue gas denitration and a preparation method thereof, aiming at solving the problems that a catalyst is poisoned and inactivated in the existing flue gas denitration technology, and the normal operation of a boiler system is influenced by the fact that a heating surface at the tail of a boiler is coked or blocked by adhesion. The method comprises the steps of mixing high-iron fly ash obtained by mechanically grinding, wet magnetic separation and drying raw fly ash with calcium oxide to prepare a slurry-like high-iron fly ash matrix, adding manganese nitrate and cerium nitrate, drying, roasting at high temperature, and naturally cooling to room temperature to obtain the adsorbent. The prepared adsorbent is an adsorbent for effectively removing nitrogen oxides in coal-fired flue gas in a temperature range of 260-400 ℃, and the average removal efficiency is more than or equal to 70 percent. The solid waste fly ash is used as a substrate to prepare the adsorbent for flue gas denitration, so that the treatment of waste by waste can be realized in a coal-fired power plant.
Description
Technical Field
The invention belongs to the technical field of coal ash solid waste recycling and flue gas denitration, and particularly relates to a manganese-cerium modified high-iron coal ash adsorbent for flue gas denitration and a preparation method thereof.
Background
Nitrogen oxides generated in the coal combustion process are discharged into the atmosphere to form acid rain, erode soil, destroy forests, inhibit crop growth and the like. At present, acid rain becomes one of the most harmful pollutions in China. Therefore, the control of nitrogen oxides in the flue gas is also an important link for the treatment of atmospheric pollution.
At present, the industrially mature dry-process coal-fired flue gas denitration technology is mainly selective catalytic reduction denitration (SCR), the method has high efficiency of removing nitrogen oxides, but side reaction can occur in the denitration process to generate NH with larger viscosity4HSO4The substance is easy to adhere to the denitration catalyst and the heating surface at the tail part of the boiler, so that the catalyst is inactivated, and the normal operation of a boiler system is influenced. Therefore, the development of an effective dry flue gas denitration adsorbent is imperative.
The fly ash is a solid product after coal combustion in a thermal power plant, and the main component of the fly ash is SiO2、Al2O3、CaO、Fe2O3(or Fe)3O4) And MgO, and Fe as a transition metal element has variable valence states, so that the Fe is widely applied to an active component of the denitration adsorbent, and therefore, the Fe can be fully utilized by increasing the content of the iron oxide in the fly ash. However, the existing research shows that the utilization rate of iron oxide in the original fly ash is not high due to the fact that the outer surface of the original fly ash is wrapped by a vitreous body, so that the removal and adsorption capacity is poor, therefore, in order to meet the requirements of dry denitration of flue gas of the coal-fired power plant at present, the fly ash needs to be modified appropriately to prepare a denitration adsorbent, and a pollutant treatment technology for treating wastes with processes of wastes against one another can be formed in the coal-fired power plant.
Disclosure of Invention
The invention provides a manganese-cerium modified high-iron fly ash adsorbent for flue gas denitration and a preparation method thereof, aiming at solving the problems that the poisoning and inactivation of a catalyst in the existing flue gas denitration technology, the influence on the normal operation of a boiler system due to the fact that a heating surface at the tail of a boiler is coked or blocked by adhesion, and the like.
The invention is realized by the following technical scheme: an adsorbent for flue gas denitration by manganese cerium modified high iron fly ash is prepared by mechanically grinding raw fly ash, wet magnetic separating, drying to obtain high iron fly ash, mixing with calcium oxide to obtain slurry high iron fly ash matrix, adding manganese nitrate and cerium nitrate, drying, high temperature roasting, and naturally cooling to room temperature to obtain the adsorbent.
The raw fly ash is pulverized coal furnace fly ash, wherein Fe is iron oxide and maghemite gamma-Fe is used2O3And magnetite Fe3O4Is present and the content of iron oxide is greater than 8%.
The method for preparing the manganese-cerium modified high-iron fly ash adsorbent for flue gas denitration comprises the following steps:
(1) screening raw materials: sieving the original fly ash with a 20-mesh sieve for later use;
(2) obtaining high-iron fly ash: placing the screened fly ash into a ball mill with the rotating speed of 500r/min according to the ball-to-material ratio of 1:1 for dry grinding for 3-6h, mixing the ground fly ash and deionized water according to the volume ratio of 1:5-1:10 to prepare mortar, carrying out wet magnetic separation on the mortar for 2-5 times by using a permanent magnet, and drying the fly ash subjected to magnetic separation for 8-14h at the temperature of 80-120 ℃ to obtain high-coal-ash iron powder;
(3) obtaining a slurry high-iron fly ash matrix: mixing the obtained high-iron fly ash with CaO according to the mass ratio of 6:1-3:1, uniformly mixing the mixture with deionized water according to the volume ratio of 1:5-1:15, and uniformly stirring for 8-16 hours at a constant speed of 150r/min in a water bath kettle at the temperature of 80-100 ℃ to obtain a slurry high-iron fly ash matrix;
(4) preparation of dried sample: adding Mn (NO) with a molar ratio of 15:1-5:3 into the slurry high-iron fly ash matrix3)2And Ce (NO)3)3·6H2Stirring the mixture of O at a constant speed of 150r/min for 2-6 hours, and drying the slurry at the temperature of 80-120 ℃ for 5-13 hours to obtain a dried sample;
(5) obtaining of the manganese-cerium modified high-iron fly ash adsorbent for flue gas denitration: and (3) placing the dried sample into a tube furnace, roasting for 2-4h at the temperature of 350-600 ℃ in the air atmosphere, and naturally cooling to room temperature to obtain the manganese-cerium modified high-iron fly ash adsorbent for flue gas denitration.
The permanent magnet is 12000 GS.
The method for flue gas denitration by using the manganese-cerium modified high-iron fly ash adsorbent for flue gas denitration is characterized by comprising the following steps of: the denitration agent can effectively remove NO in the coal-fired flue gas in a temperature range of 260-400 ℃. The average removal efficiency is more than or equal to 70 percent.
In the dry grinding process of the fly ash, the glass structure on the surface of the fly ash can be damaged in the mechanical ball milling process, and the iron oxide wrapped by the glass is exposed; then, in the magnetic separation process, a large amount of iron oxide is enriched to form high iron fly ash; then, in the process of CaO hydration modification, CaO reacts with Si and Al in the fly ash to generate calcium silicate hydrate, calcium aluminate hydrate and the like, so that the damage of a glass body on the surface of the fly ash is further aggravated, and the porosity of the fly ash is improved; manganese oxide and cerium oxide decomposed from the high-iron fly ash added with the manganese nitrate and the cerium nitrate in the high-temperature roasting process and iron oxide in the fly ash can form a ferro-manganese solid solution and a ferro-cerium solid solution which are main active components for removing NO; under the roasting condition of 350-. The prepared denitration agent can effectively remove NO in the coal-fired flue gas in the temperature range of 260-400 ℃. The average removal efficiency is more than or equal to 70 percent. The solid waste fly ash is used as a substrate to prepare the adsorbent for flue gas denitration, so that the treatment of waste by waste can be realized in a coal-fired power plant.
Drawings
FIG. 1 is a NO removal efficiency curve for adsorbent D of example 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments; all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: an adsorbent for flue gas denitration by manganese-cerium modified high iron fly ash, which comprises the following specific preparation method: screening raw fly ash by using a 20-mesh screen, then putting the raw fly ash into a ball mill for dry grinding for 3 hours, mixing the ground fly ash with deionized water to prepare mortar, then carrying out magnetic separation on the mortar by using a 12000GS permanent magnet for 2 times, and drying the mortar after the magnetic separation for 8 hours at the temperature of 80 ℃; obtaining high iron fly ash with iron oxide content of 16.72%; mixing 30g of high iron fly ash, 5g of CaO and 200ml of deionized water in a beaker uniformly, putting the beaker into a water bath kettle, stirring for 8 hours at the constant temperature of 95 ℃, and then adding 0.1mol of Mn (NO)3)2And 0.01mol Ce (NO)3)3·6H2And O, uniformly stirring for 2 hours to form slurry, putting the slurry into an oven, drying for 12 hours at 100 ℃, finally putting the dried sample into a tube furnace, roasting for 4 hours at 350 ℃ in air atmosphere, and naturally cooling to room temperature to obtain the high-iron fly ash adsorbent A.
The NO removal experiment is carried out at 260 ℃ with the reaction gas consisting of O2（5%）、NO（300mg/m3) And N2(balance gas) composition, the mass of the adsorbent is 2g, the experiment is stopped when the average removal efficiency is lower than 70%, and the cumulative nitrate capacity of the adsorbent in the denitration experiment is 1386 mu g/g.
Example 2: an adsorbent for flue gas denitration by manganese-cerium modified high iron fly ash, which comprises the following specific preparation method: screening raw fly ash by using a 20-mesh screen, then putting the raw fly ash into a ball mill for dry grinding for 4 hours, mixing the ground fly ash with deionized water to prepare mortar, then carrying out magnetic separation on the mortar by using a 12000GS permanent magnet for 4 times, and drying the mortar after the magnetic separation for 12 hours at the temperature of 100 ℃; obtaining high iron fly ash with the iron oxide content of 28.52%; mixing 30g of high iron fly ash, 6g of CaO and 200ml of deionized water in a beaker uniformly, putting the beaker into a water bath kettle, stirring for 12 hours at the constant temperature of 80 ℃, and then adding 0.1mol of Mn (NO)3)2And 0.02mol Ce (NO)3)3·6H2And O, uniformly stirring for 2 hours to form slurry, putting the slurry into an oven, drying for 12 hours at 100 ℃, finally putting the dried sample into a tube furnace, roasting for 2 hours at 500 ℃, and naturally cooling to room temperature to obtain the high-iron fly ash adsorbent B.
The NO removal experiment is carried out at 400 ℃ and the reaction gas is O2（5%）、NO（300mg/m3) And N2The (balance gas) composition and the mass of the adsorbent are 2g, and when the average removal efficiency is lower than 70%, the experiment is stopped, and the cumulative nitrate capacity of the adsorbent in the denitration experiment is 3024 mug/g.
Example 3: an adsorbent for flue gas denitration by manganese-cerium modified high iron fly ash, which comprises the following specific preparation method: screening raw fly ash by using a 20-mesh screen, then putting the raw fly ash into a ball mill for dry grinding for 6 hours, mixing the ground fly ash with deionized water to prepare mortar, then carrying out magnetic separation on the mortar by using a 12000GS permanent magnet for 5 times, and drying the mortar after the magnetic separation for 12 hours at the temperature of 120 ℃; obtaining high iron fly ash with 30.72 percent of iron oxide; mixing 30g of high iron fly ash, 10g of CaO and 200ml of deionized water in a beaker uniformly, putting the beaker into a water bath kettle, stirring for 16 hours at the constant temperature of 95 ℃, and then adding 0.1mol of Mn (NO)3)2And 0.03mol Ce (NO)3)3·6H2And O, uniformly stirring for 2 hours to form slurry, putting the slurry into an oven, drying for 12 hours at the temperature of 100 ℃, finally putting the dried sample into a tube furnace, roasting for 2 hours at the temperature of 550 ℃, and naturally cooling to room temperature to obtain the high-iron fly ash adsorbent C.
The NO removal experiment is carried out at 300 ℃, and the reaction gas is O2（5%）、NO（300mg/m3) And N2The (equilibrium gas) composition and the mass of the adsorbent are 2g, and when the average removal efficiency is lower than 70 percent, the experiment is stopped, and the cumulative nitrate capacity of the adsorbent in the denitration experiment is 1764 mug/g.
Example 4: an adsorbent for flue gas denitration by manganese-cerium modified high iron fly ash, which comprises the following specific preparation method: sieving raw fly ash with 20 mesh sieve, dry grinding in ball mill for 4 hr, mixing the ground fly ash with deionized water to obtain ashSlurry, then carrying out magnetic separation on the slurry for 4 times by using a 12000GS permanent magnet, and drying the slurry after the magnetic separation for 14 hours at the temperature of 100 ℃; obtaining high iron fly ash with the iron oxide content of 28.52%; mixing 30g of high iron fly ash, 6g of CaO and 200ml of deionized water in a beaker uniformly, putting the beaker into a water bath kettle, stirring for 12 hours at constant temperature of 100 ℃, and then adding 0.05mol of Mn (NO)3)2And 0.03mol Ce (NO)3)3·6H2And O, uniformly stirring for 4 hours to form slurry, drying the slurry in an oven at 80 ℃ for 5 hours, finally putting the dried sample in a tube furnace, roasting for 3 hours at 600 ℃, and naturally cooling to room temperature to obtain the high-iron fly ash adsorbent D.
The NO removal experiment is carried out at 300 ℃, and the reaction gas is O2（5%）、NO（300mg/m3) And N2(equilibrium gas) composition, the mass of the adsorbent was 2g, and the experiment was stopped when the average removal efficiency was less than 70%, and the cumulative nitrate capacity of the adsorbent in the denitration experiment was 3654. mu.g/g, as shown in FIG. 1.
Example 5: an adsorbent for flue gas denitration by manganese-cerium modified high iron fly ash, which comprises the following specific preparation method: screening raw fly ash by using a 20-mesh screen, then putting the raw fly ash into a ball mill for dry grinding for 4 hours, mixing the ground fly ash with deionized water to prepare mortar, then carrying out magnetic separation on the mortar by using a 12000GS permanent magnet for 3 times, and drying the mortar after the magnetic separation for 12 hours at the temperature of 100 ℃; obtaining high iron fly ash with the iron oxide content of 28.52%; mixing 30g of high iron fly ash, 6g of CaO and 200ml of deionized water in a beaker uniformly, putting the beaker into a water bath kettle, stirring for 12 hours at the constant temperature of 95 ℃, and then adding 0.15mol of Mn (NO)3)2And 0.01mol Ce (NO)3)3·6H2And O, uniformly stirring for 6 hours to form slurry, drying the slurry in an oven at 120 ℃ for 13 hours, finally putting the dried sample in a tube furnace, roasting at 450 ℃ for 2 hours, and naturally cooling to room temperature to obtain the high-iron fly ash adsorbent E.
The NO removal experiment is carried out at 300 ℃, and the reaction gas is O2（5%）、NO（300mg/m3) And N2(balance gas) composition, the mass of the adsorbent is 2g, the experiment is stopped when the average removal efficiency is lower than 70%, and the cumulative nitrate capacity of the adsorbent in the denitration experiment is 3150 mu g/g.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. The utility model provides a manganese cerium modifies high iron fly ash's adsorbent for flue gas denitration which characterized in that: mixing high-iron fly ash obtained by mechanically grinding, wet magnetic separation and drying raw fly ash with calcium oxide to prepare a slurry-like high-iron fly ash matrix, adding manganese nitrate and cerium nitrate, drying, roasting at high temperature, and naturally cooling to room temperature to obtain the adsorbent.
2. The manganese-cerium-modified high-iron fly ash adsorbent for flue gas denitration according to claim 1, wherein the manganese-cerium-modified high-iron fly ash adsorbent is characterized in that: the raw fly ash is pulverized coal furnace fly ash, wherein Fe is iron oxide and maghemite gamma-Fe is used2O3And magnetite Fe3O4Is present and the content of iron oxide is greater than 8%.
3. The method for preparing the manganese-cerium-modified high-iron fly ash adsorbent for flue gas denitration according to claim 1 or 2, is characterized in that: the method comprises the following steps:
(1) screening raw materials: sieving the original fly ash with a 20-mesh sieve for later use;
(2) obtaining high-iron fly ash: placing the screened fly ash into a ball mill with the rotating speed of 500r/min according to the ball-to-material ratio of 1:1 for dry grinding for 3-6h, mixing the ground fly ash and deionized water according to the volume ratio of 1:5-1:10 to prepare mortar, carrying out wet magnetic separation on the mortar for 2-5 times by using a permanent magnet, and drying the fly ash subjected to magnetic separation for 8-14h at the temperature of 80-120 ℃ to obtain high-coal-ash iron powder;
(3) obtaining a slurry high-iron fly ash matrix: mixing the obtained high-iron fly ash with CaO according to the mass ratio of 6:1-3:1, uniformly mixing the mixture with deionized water according to the volume ratio of 1:5-1:15, and uniformly stirring for 8-16 hours at a constant speed of 150r/min in a water bath kettle at the temperature of 80-100 ℃ to obtain a slurry high-iron fly ash matrix;
(4) preparation of dried sample: adding Mn (NO) with a molar ratio of 15:1-5:3 into the slurry high-iron fly ash matrix3)2And Ce (NO)3)3·6H2Stirring the mixture of O at a constant speed of 150r/min for 2-6 hours, and drying the slurry at the temperature of 80-120 ℃ for 5-13 hours to obtain a dried sample;
(5) obtaining of the manganese-cerium modified high-iron fly ash adsorbent for flue gas denitration: and (3) placing the dried sample into a tube furnace, roasting for 2-4h at the temperature of 350-600 ℃ in the air atmosphere, and naturally cooling to room temperature to obtain the manganese-cerium modified high-iron fly ash adsorbent for flue gas denitration.
4. The method for preparing the manganese-cerium-modified high-iron fly ash adsorbent for flue gas denitration according to claim 3, wherein the method comprises the following steps: the permanent magnet is 12000 GS.
5. The method for flue gas denitration by using the manganese-cerium-modified high iron fly ash adsorbent for flue gas denitration according to claim 1 or 2, characterized by comprising: the denitration agent is used for effectively removing NO in the coal-fired flue gas in a temperature range of 260-400 ℃.
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