CN115254199A - Low-cost denitration catalyst slurry and preparation method and application thereof - Google Patents
Low-cost denitration catalyst slurry and preparation method and application thereof Download PDFInfo
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- 239000002002 slurry Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 238000007613 slurry method Methods 0.000 title description 2
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- 239000011733 molybdenum Substances 0.000 claims abstract description 18
- 239000010936 titanium Substances 0.000 claims abstract description 18
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- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 6
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- 150000002009 diols Chemical class 0.000 claims description 4
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- 125000001664 diethylamino group Chemical group [H]C([H])([H])C([H])([H])N(*)C([H])([H])C([H])([H])[H] 0.000 claims description 3
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0219—Coating the coating containing organic compounds
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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
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0036—Grinding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention provides a low-cost denitration catalyst slurry and a preparation method and application thereof, and the low-cost denitration catalyst slurry comprises the following steps: preparing a denitration catalyst precursor, wherein the denitration catalyst precursor is prepared by mixing a tungsten source, a vanadium source, a molybdenum source, a titanium source, silica sol, ammonia water, an organic surfactant, inorganic colloid and water; and sanding or ball-milling the denitration catalyst precursor to obtain the low-cost denitration catalyst slurry. The preparation method disclosed by the invention is simple in process, short in period, safe to operate, low in cost and capable of realizing large-scale production, the prepared denitration catalyst slurry is small in particle crystal grains, high in dispersity, suspensibility and wettability, and suitable for coating porous materials with pore diameters of more than 2 micrometers, and the pore diameters of the porous materials are not easy to block during coating.
Description
Technical Field
The invention relates to the technical field of flue gas purification, in particular to low-cost denitration catalyst slurry and a preparation method and application thereof.
Background
The dust removal and denitration integrated material is a functional material formed by efficiently compounding a porous ceramic material and a nano denitration catalyst, combines the filtering principle of the porous ceramic material with the reduction and denitration mechanism of a selective catalyst, can realize the dust removal and denitration functions at the same time, can be widely applied to high-temperature flue gas purification, and is beneficial to the simplification of industrial flue gas treatment equipment and the intensification of company processes.
At present, the main methods of loading a denitration catalyst on a porous ceramic material include a sol-gel method, a coprecipitation method, an impregnation method and the like, and after loading the denitration catalyst in the pore channels or on the surfaces of the pore channels of the porous ceramic material, the denitration catalyst is subjected to heat treatment to obtain the dedusting and denitration integrated material. However, compared with the impregnation method, the sol-gel method and the coprecipitation method have the problems of complicated preparation process, long production period, high cost and the like, and the impregnation method becomes the mainstream preparation process. The impregnation method generally adopts a mode of coating denitration catalyst slurry inside or on the surface of a porous ceramic material pore channel to realize the loading of the denitration catalyst inside or on the surface of the porous ceramic material pore channel, however, the denitration catalyst slurry used for the impregnation method is not mature at present, and the problems of poor dispersibility, poor suspension property, poor wettability and the like generally exist, so that the popularization and application of the dedusting and denitration integrated material are greatly restricted; in addition, in the preparation process of the denitration catalyst slurry, spray drying or kneading is required to be sequentially carried out, heat treatment and ball milling are required to prepare a catalyst precursor, a plurality of additives are mixed, and then grinding is carried out to obtain the catalyst slurry, so that the preparation process is complex, the period is long, and the batch production cost is high.
Disclosure of Invention
In order to solve the problems, the invention provides a low-cost denitration catalyst slurry and a preparation method and application thereof, the preparation method has the advantages of simple process, short period, safe operation, lower cost and large-scale production, the prepared denitration catalyst slurry has small grain size and higher dispersibility, suspension property and wettability, is suitable for coating porous materials with the pore diameter of more than 2 mu m, and is not easy to block the pore of the porous materials during coating.
In one aspect, the invention provides a preparation method of a low-cost denitration catalyst slurry, which comprises the following steps: preparing a denitration catalyst precursor, wherein the denitration catalyst precursor is formed by mixing a tungsten source, a vanadium source, a molybdenum source, a titanium source, silica sol, ammonia water, an organic surfactant, inorganic colloid and water; and sanding or ball-milling the denitration catalyst precursor to obtain the low-cost denitration catalyst slurry.
In some embodiments of the present invention, the denitration catalyst precursor is prepared by mixing, by weight, 6 to 12 parts of a tungsten source, 10 to 15 parts of a vanadium source, 6 to 12 parts of a molybdenum source, 60 to 85 parts of a titanium source, 3 to 6 parts of silica sol, 15 to 20 parts of ammonia water, 5 to 10 parts of an organic surfactant, 0.5 to 1 part of an inorganic colloid, and 60 to 90 parts of water.
In some embodiments of the present invention, the tungsten source is ammonium metatungstate, the vanadium source is ammonium metavanadate, the molybdenum source is ammonium molybdate, and the titanium source is metatitanic acid and/or titanium dioxide. The purity of the ammonium metatungstate, the ammonium metavanadate, the ammonium molybdate, the metatitanic acid and the titanium dioxide is preferably over 98 percent.
In some embodiments of the invention, the silica sol is an alkaline silica sol, and the silica sol has a silica content of 30 to 40wt%.
In some embodiments of the invention, the organic surfactant is diethylamine or an acetylenic diol or a polyacrylic acid amine.
In some embodiments of the invention, the inorganic colloid is bentonite or magnesium aluminum silicate.
In some embodiments of the present invention, when the denitration catalyst precursor is subjected to sand grinding, the sand grinding is performed for 30-60min; and ball milling is carried out on the denitration catalyst precursor for 6-10h.
In some embodiments of the present invention, after the denitration catalyst precursor is subjected to sand grinding or ball milling, 5 to 10 parts by weight of an organic surfactant is added, and the mixture is uniformly stirred to obtain the low-cost denitration catalyst slurry.
On the other hand, the invention also provides low-cost denitration catalyst slurry which is prepared according to any one of the preparation methods.
On the other hand, the invention also provides application of the low-cost denitration catalyst slurry, and the low-cost denitration catalyst slurry is coated inside the porous material pore canal with the pore canal aperture of more than 2 mu m to obtain the dedusting and denitration integrated material.
Compared with the prior art, the invention has the following beneficial effects:
(1) The preparation method takes a tungsten source, a vanadium source, a molybdenum source, a titanium source, silica sol, ammonia water, an organic surfactant, inorganic colloid and water as raw materials, and adopts a sand grinding or ball milling process to prepare the denitration catalyst slurry. Compared with the traditional method of sequentially carrying out heat treatment and ball milling after spray drying or kneading, mixing various additives and then grinding to obtain the catalyst slurry, the method only adopts the sanding or ball milling process, has simple preparation process, short period, safe operation and lower cost, and can realize large-scale production; in the preparation process of the denitration catalyst slurry, the thermal stability is increased by adopting silica sol, an alkaline environment is provided by adopting ammonia water, and an organic surfactant and inorganic colloid (slurry stabilizer) system is adopted, so that under the combined action of the organic surfactant and the inorganic colloid, solid particles in the catalyst slurry are well dispersed, the catalyst slurry has better suspension property under lower viscosity, and is not easy to precipitate, the solid particles in the prepared denitration catalyst slurry have small crystal grains, and the prepared denitration catalyst slurry has high dispersibility, suspension property and wettability, is suitable for coating porous materials with pore diameters of more than 2 mu m, and is not easy to block pores of the porous materials during coating.
(2) The preparation method limits the formula of the precursor of the denitration catalyst to be formed by mixing 6-12 parts of tungsten source, 10-15 parts of vanadium source, 6-12 parts of molybdenum source, 60-85 parts of titanium source, 3-6 parts of silica sol, 15-20 parts of ammonia water, 5-10 parts of organic surfactant, 0.5-1 part of inorganic colloid and 60-90 parts of water, and the precursor of the denitration catalyst prepared by the formula is more beneficial to subsequent sand grinding or ball milling, and can ensure good dispersibility while ensuring particle refinement; in addition, 5-10 parts of organic surfactant is preferably added during preparation of the denitration catalyst precursor, 5-10 parts by weight of organic surfactant is added after sanding or ball milling, the organic surfactant is added twice, the addition amount of the organic surfactant is small during sanding or ball milling, the organic surfactant cannot generate heat and lose efficacy while dispersion is guaranteed, the organic surfactant is added for the second time after sanding or ball milling, dispersion is further facilitated, and the problems that the organic surfactant fails due to heating during sanding or ball milling, later-stage agglomeration and non-dispersion are caused due to the fact that the organic surfactant is large in amount during one-time addition and generates heat during sanding or ball milling are solved.
(3) The organic surfactant selected by the invention is diethylamine or alkynediol or polyacrylamide, and the inorganic colloid is bentonite or magnesium aluminum silicate. Diethylamine or alkynediol or polyacrylamide is a surfactant of small molecules, the small molecules can form an electric double layer on the surface of solid particles in the denitration catalyst slurry, under the action of charges, the particles can be better separated, and the denitration catalyst slurry is endowed with better dispersibility; the bentonite or the magnesium aluminum silicate belongs to a lamellar structure, can be combined with water to expand into a colloid with stable suspension, cannot be eroded by microorganisms, cannot deteriorate and mildew after long-term storage, and has viscosity which does not change along with temperature; the surfactant selected by the invention can be rapidly and uniformly dispersed in the whole system, surface migration can not occur, smaller molecular weight can not be scattered or damaged in the rapid dispersion process, and the surface tension is lower in static state and dynamic state.
Drawings
In order to more clearly illustrate the technical solution in the embodiment of the present invention, the drawings required to be used in the embodiment of the present invention will be described below.
Fig. 1 is a particle size distribution diagram of particles in a low-cost denitration catalyst slurry prepared by an embodiment preparation method of the present invention;
FIG. 2 is a particle size distribution diagram of a low-cost denitration catalyst slurry prepared by another preparation method according to another embodiment of the present invention;
fig. 3 is a particle size distribution diagram of a low-cost denitration catalyst slurry prepared by a preparation method according to still another embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following detailed description of various aspects of the present invention is provided with specific examples, which are only used for illustrating the present invention and do not limit the scope and spirit of the present invention.
The invention provides a preparation method of low-cost denitration catalyst slurry, which comprises the following steps: preparing a denitration catalyst precursor, wherein the denitration catalyst precursor is formed by mixing a tungsten source, a vanadium source, a molybdenum source, a titanium source, silica sol, ammonia water, an organic surfactant, inorganic colloid and water; and (3) sanding or ball-milling the denitration catalyst precursor to obtain the low-cost denitration catalyst slurry.
In the invention, the denitration catalyst precursor is prepared by mixing 6-12 parts of tungsten source, 10-15 parts of vanadium source, 6-12 parts of molybdenum source, 60-85 parts of titanium source, 3-6 parts of silica sol, 15-20 parts of ammonia water, 5-10 parts of organic surfactant, 0.5-1 part of inorganic colloid and 60-90 parts of water in parts by weight.
In the invention, the tungsten source is ammonium metatungstate, the vanadium source is ammonium metavanadate, the molybdenum source is ammonium molybdate, and the titanium source is metatitanic acid and/or titanium dioxide. Preferably, the purity of the ammonium metatungstate, the ammonium metavanadate, the ammonium molybdate, the metatitanic acid and the titanium dioxide is more than 98 percent.
In the invention, the silica sol is alkaline silica sol, and the content of silicon in the silica sol is 30-40wt%.
In the present invention, the organic surfactant is diethylamine or an acetylenic diol or a polyacrylic acid amine. The inorganic colloid is bentonite or magnesium aluminum silicate.
In the invention, when the denitration catalyst precursor is sanded, the sanding is carried out for 30-60min; and ball milling is carried out on the denitration catalyst precursor for 6-10h.
In the invention, after sand milling or ball milling is carried out on the denitration catalyst precursor, 5-10 parts by weight of organic surfactant is added, and the denitration catalyst slurry with low cost is obtained after uniform stirring.
The invention also provides a low-cost denitration catalyst slurry which is prepared according to the preparation method.
The invention also provides application of the low-cost denitration catalyst slurry prepared by the invention, and the low-cost denitration catalyst slurry prepared by the invention is coated in the porous ceramic material pore canal with the pore diameter of more than 2 mu m to obtain the dedusting and denitration integrated material.
Example 1:
the embodiment provides a preparation method of a low-cost denitration catalyst slurry, which comprises the following steps:
weighing 6 parts of tungsten source, 10 parts of vanadium source, 6 parts of molybdenum source, 60 parts of titanium source, 3 parts of silica sol, 15 parts of ammonia water, 5 parts of organic surfactant, 0.5 part of inorganic colloid and 60 parts of water in parts by weight, pouring the materials into a stirring barrel for mixing, and uniformly stirring to obtain a denitration catalyst precursor;
and (3) sanding the denitration catalyst precursor for 30-60min (preferably, sanding for 30 min) by using a sand mill, pouring the ground slurry into a stirring barrel, then adding 5 parts by weight of organic surfactant, and fully and uniformly stirring (preferably, stirring for 10 min) to obtain the low-cost denitration catalyst slurry.
In this embodiment, the tungsten source is ammonium metatungstate, the vanadium source is ammonium metavanadate, the molybdenum source is ammonium molybdate, and the titanium source is metatitanic acid. Preferably, the purity of the ammonium metatungstate, ammonium metavanadate, ammonium molybdate and metatitanic acid is more than 98%.
In this embodiment, the silica sol is an alkaline silica sol, and the silica content in the silica sol is 30 to 40wt%.
In this example, the organic surfactant was diethylamine, and the inorganic colloid was bentonite.
The present example also provides a low-cost denitration catalyst slurry, which is prepared according to the preparation method of the present example. As shown in fig. 1, a particle size distribution of the low-cost denitration catalyst slurry prepared by the preparation method of the present embodiment is shown, and it can be seen from the figure that the particle size of the low-cost denitration catalyst slurry prepared by the preparation method of the present embodiment is less than 1 μm, and D50=0.067 μm.
The embodiment also provides application of the low-cost denitration catalyst slurry prepared by the preparation method of the embodiment, and the low-cost denitration catalyst slurry prepared by the embodiment is coated inside the porous ceramic material pore canal with the pore diameter of more than 2 μm to obtain the dedusting and denitration integrated material. The low-cost denitration catalyst slurry prepared by the embodiment has small grain size, the D50 is only 0.067 mu m, the prepared low-cost denitration catalyst slurry has high dispersibility, suspension property and wettability, can be successfully coated on a porous material with the pore diameter of more than 2 mu m, is not easy to block the pore of the porous material during coating, and can be applied to preparation of dust removal and denitration integrated materials.
Example 2:
the embodiment provides a preparation method of a low-cost denitration catalyst slurry, which comprises the following steps:
weighing 8 parts of tungsten source, 12 parts of vanadium source, 8 parts of molybdenum source, 70 parts of titanium source, 5 parts of silica sol, 17 parts of ammonia water, 7 parts of organic surfactant, 0.7 part of inorganic colloid and 80 parts of water in parts by weight, and mixing to obtain a denitration catalyst precursor;
pouring the denitration catalyst precursor into a horizontal ball mill, carrying out ball milling on the denitration catalyst precursor for 6-10h (preferably, grinding for 8 h), pouring the ground slurry into a stirring barrel, then adding 7 parts by weight of organic surfactant, and fully and uniformly stirring (preferably, stirring for 10 min) to obtain the low-cost denitration catalyst slurry.
In this embodiment, the tungsten source is ammonium metatungstate, the vanadium source is ammonium metavanadate, the molybdenum source is ammonium molybdate, and the titanium source is titanium dioxide. Preferably, the purity of the ammonium metatungstate, the ammonium metavanadate, the ammonium molybdate and the titanium dioxide is more than 98 percent.
In this embodiment, the silica sol is an alkaline silica sol, and the silica content in the silica sol is 30 to 40wt%.
In this example, the organic surfactant is an acetylenic diol and the inorganic colloid is magnesium aluminum silicate.
The present example also provides a low-cost denitration catalyst slurry, which is prepared according to the preparation method of the present example. As shown in fig. 2, a particle size distribution of the low-cost denitration catalyst slurry prepared by the preparation method of the present embodiment is shown, and it can be seen from the figure that the particle size of the low-cost denitration catalyst slurry prepared by the preparation method of the present embodiment is less than 1 μm, and D50=0.063 μm.
The embodiment also provides an application of the low-cost denitration catalyst slurry prepared by the preparation method of the embodiment, and the low-cost denitration catalyst slurry prepared by the embodiment is coated inside the porous ceramic material pore channel with the pore diameter of more than 2 μm to obtain the dedusting and denitration integrated material. The low-cost denitration catalyst slurry prepared by the embodiment has small grain size, the D50 is only 0.063 mu m, and the prepared low-cost denitration catalyst slurry has high dispersibility, suspension property and wettability, can be successfully coated on a porous material with the pore diameter of more than 2 mu m, is not easy to block the pore of the porous material during coating, and can be applied to preparation of dust removal and denitration integrated materials.
Example 3:
the embodiment provides a preparation method of low-cost denitration catalyst slurry, which comprises the following steps:
weighing 12 parts of tungsten source, 15 parts of vanadium source, 12 parts of molybdenum source, 85 parts of titanium source, 6 parts of silica sol, 20 parts of ammonia water, 10 parts of organic surfactant, 1 part of inorganic colloid and 90 parts of water in parts by weight, pouring into a stirring barrel for mixing, and uniformly stirring to obtain a denitration catalyst precursor;
and (3) sanding the denitration catalyst precursor for 30-60min (preferably, grinding for 60 min) by using a sand mill, pouring the ground slurry into a stirring barrel, then adding 10 parts by weight of organic surfactant, and fully and uniformly stirring (preferably, stirring for 10 min) to obtain the low-cost denitration catalyst slurry.
In this embodiment, the tungsten source is ammonium metatungstate, the vanadium source is ammonium metavanadate, the molybdenum source is ammonium molybdate, and the titanium source is metatitanic acid and titanium dioxide. Preferably, the purity of the ammonium metatungstate, the ammonium metavanadate, the ammonium molybdate, the metatitanic acid and the titanium dioxide is more than 98 percent.
In this embodiment, the silica sol is an alkaline silica sol, and the silica content in the silica sol is 30 to 40wt%.
In this embodiment, the organic surfactant is polyacrylamide. The inorganic colloid is bentonite.
The present example also provides a low-cost denitration catalyst slurry, which is prepared according to the preparation method of the present example. As shown in fig. 3, a particle size distribution of the particles in the low-cost denitration catalyst slurry prepared by the preparation method of the present embodiment is shown, and it can be seen from the figure that the particle size of the particles in the low-cost denitration catalyst slurry prepared by the preparation method of the present embodiment is less than 1 μm, and D50=0.061 μm.
The embodiment also provides application of the low-cost denitration catalyst slurry prepared by the preparation method of the embodiment, and the low-cost denitration catalyst slurry prepared by the embodiment is coated inside the porous ceramic material pore canal with the pore diameter of more than 2 μm to obtain the dedusting and denitration integrated material. The low-cost denitration catalyst slurry prepared by the embodiment has small grain size, the D50 is only 0.061 mu m, the prepared low-cost denitration catalyst slurry has high dispersibility, suspension property and wettability, can be successfully coated on a porous material with the pore diameter of more than 2 mu m, is not easy to block the pore of the porous material during coating, and can be applied to preparation of dust removal and denitration integrated materials.
The present invention has been described in conjunction with specific embodiments which are intended to be exemplary only and are not intended to limit the scope of the invention, which is to be given the full breadth of the appended claims and any and all modifications, variations or alterations that may occur to those skilled in the art without departing from the spirit of the invention. Therefore, various equivalent changes made according to the present invention still fall within the scope covered by the present invention.
Claims (10)
1. A preparation method of low-cost denitration catalyst slurry is characterized by comprising the following steps:
preparing a denitration catalyst precursor, wherein the denitration catalyst precursor is prepared by mixing a tungsten source, a vanadium source, a molybdenum source, a titanium source, silica sol, ammonia water, an organic surfactant, inorganic colloid and water;
and sanding or ball-milling the denitration catalyst precursor to obtain the low-cost denitration catalyst slurry.
2. The preparation method according to claim 1, wherein the denitration catalyst precursor is prepared by mixing 6-12 parts by weight of a tungsten source, 10-15 parts by weight of a vanadium source, 6-12 parts by weight of a molybdenum source, 60-85 parts by weight of a titanium source, 3-6 parts by weight of a silica sol, 15-20 parts by weight of ammonia water, 5-10 parts by weight of an organic surfactant, 0.5-1 part by weight of an inorganic colloid, and 60-90 parts by weight of water.
3. The method according to claim 1, wherein the tungsten source is ammonium metatungstate, the vanadium source is ammonium metavanadate, the molybdenum source is ammonium molybdate, and the titanium source is metatitanic acid and/or titanium dioxide.
4. The method according to claim 1, wherein the silica sol is an alkaline silica sol, and the silica sol has a silica content of 30 to 40wt%.
5. The method of claim 1, wherein the organic surfactant is diethylamine or an acetylenic diol or an amine polyacrylate.
6. The method of claim 1, wherein the inorganic colloid is bentonite or magnesium aluminum silicate.
7. The preparation method according to claim 1, wherein the denitration catalyst precursor is sanded for 30-60min; and ball milling is carried out on the denitration catalyst precursor for 6-10h.
8. The preparation method of claim 1, wherein the denitration catalyst precursor is subjected to sand grinding or ball milling, 5-10 parts by weight of organic surfactant is added, and the mixture is uniformly stirred to obtain the low-cost denitration catalyst slurry.
9. A low-cost denitration catalyst slurry, characterized in that it is prepared according to the preparation method of any one of claims 1 to 8.
10. The application of the low-cost denitration catalyst slurry of claim 9, wherein the low-cost denitration catalyst slurry is coated inside a porous material pore canal with a pore canal pore diameter of more than 2 μm to obtain the dedusting and denitration integrated material.
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