CN113318752A - Vanadium-tungsten-titanium system industrial denitration catalyst and preparation method and device thereof - Google Patents
Vanadium-tungsten-titanium system industrial denitration catalyst and preparation method and device thereof Download PDFInfo
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- CN113318752A CN113318752A CN202110759658.0A CN202110759658A CN113318752A CN 113318752 A CN113318752 A CN 113318752A CN 202110759658 A CN202110759658 A CN 202110759658A CN 113318752 A CN113318752 A CN 113318752A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 59
- WKXHZKXPFJNBIY-UHFFFAOYSA-N titanium tungsten vanadium Chemical compound [Ti][W][V] WKXHZKXPFJNBIY-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 82
- 238000000576 coating method Methods 0.000 claims abstract description 82
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 5
- 239000010936 titanium Substances 0.000 claims abstract description 5
- 239000000725 suspension Substances 0.000 claims description 74
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000002002 slurry Substances 0.000 claims description 24
- 229910001868 water Inorganic materials 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- 239000004576 sand Substances 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 18
- 239000002131 composite material Substances 0.000 claims description 15
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000004408 titanium dioxide Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 229910052681 coesite Inorganic materials 0.000 claims description 12
- 229910052906 cristobalite Inorganic materials 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 229910052682 stishovite Inorganic materials 0.000 claims description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 12
- 229910052905 tridymite Inorganic materials 0.000 claims description 12
- 238000005086 pumping Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002657 fibrous material Substances 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 15
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000000835 fiber Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract 1
- 230000005484 gravity Effects 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 229910052748 manganese Inorganic materials 0.000 abstract 1
- 239000011572 manganese Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- 229920001353 Dextrin Polymers 0.000 description 2
- 239000004375 Dextrin Substances 0.000 description 2
- 229910000616 Ferromanganese Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 235000019425 dextrin Nutrition 0.000 description 2
- OGUCKKLSDGRKSH-UHFFFAOYSA-N oxalic acid oxovanadium Chemical compound [V].[O].C(C(=O)O)(=O)O OGUCKKLSDGRKSH-UHFFFAOYSA-N 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 239000012494 Quartz wool Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 229920003064 carboxyethyl cellulose Polymers 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 description 1
- 229940041260 vanadyl sulfate Drugs 0.000 description 1
- 229910000352 vanadyl sulfate Inorganic materials 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8898—Manganese, technetium or rhenium containing also molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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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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- B01J37/08—Heat treatment
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
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Abstract
The invention relates to the technical field of catalyst preparation, in particular to a vanadium-tungsten-titanium system industrial denitration catalyst and a preparation method and a device thereof; the corrugated board made of fiber is used as a carrier, a first coating which takes iron, manganese and titanium as effective components and has an adsorption function is coated on the corrugated board, and then a second coating which has a function of selectively catalyzing and reducing nitrogen oxides is coated on the first coating. The vanadium-tungsten-titanium system industrial denitration catalyst has the advantages of same volume, light specific gravity, low cost and capability of adsorbing NOxThe function of the catalyst widens the low-temperature applicable temperature range of the vanadium-tungsten-titanium system catalyst.
Description
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a vanadium-tungsten-titanium system industrial denitration catalyst and a preparation method and a device thereof.
Background
NOxHas great harm to environment, is one of the main substances for forming acid rain and also forms photochemical smog in the atmosphereAnd consumption of O3Is an important factor of. And among others forms the main source in the form of combustion of fossil fuels. Such as industrial boiler, chemical industry, glass, cement, steel sintering and coking, NOxThe emission amount is huge, and the emission amount has a very high contribution value, so that the national emission standard is issued successively; for NOxEmission control, Selective Catalytic Reduction (SCR) is a widely used effective technique with the advantages of high removal efficiency, low cost, complete reaction, etc., and the core of the SCR technique is a catalyst, which directly determines the removal efficiency and emission concentration.
The catalyst of the prior SCR technology is of a medium-high temperature type, the high-efficiency temperature window is 320-420 ℃, and the catalyst has excellent NO in the temperature rangexThe removal efficiency is insufficient, but the conversion efficiency is insufficient at a lower temperature.
Disclosure of Invention
The invention aims to provide a vanadium-tungsten-titanium system industrial denitration catalyst and a preparation method and a device thereof, and aims to solve the problems that in the prior art, the SCR catalyst is of a medium-high temperature type, the high-efficiency temperature window is 320-420 ℃, and the catalyst has excellent NO in the temperature rangexThe removal efficiency is insufficient under the condition of lower temperature.
In order to achieve the purpose, the invention provides a vanadium-tungsten-titanium system industrial denitration catalyst, which comprises a first coating, a second coating and a corrugated board, wherein the first coating is coated on the surface of the corrugated board, and the second coating is coated on the surface of the first coating;
the effective components of the first coating are iron-manganese composite oxide and titanium oxide;
the effective components of the second coating are oxides of vanadium, titanium, tungsten, molybdenum and silicon;
the corrugated board is made of fiber materials.
The invention also provides a preparation method of the vanadium-tungsten-titanium system industrial denitration catalyst, which comprises the following steps:
iron-manganese composite oxide,Adding a titanium dioxide material into an aqueous solution to form a suspension, adding sol accounting for 1-5% of the total amount of the cured substances, and ball-milling by using a sand mill while controlling the granularity D90Less than 5 μm, and finally adding ionized water to obtain a first coating suspension;
adding TiO into the mixture2、WO3And SiO2Mixing and adding into ionized water, stirring uniformly to obtain a suspension, adding sol accounting for 1-5% of the total amount of cured substances, ball-milling by using a sand mill, and controlling the granularity D90Adding a pore-forming material into the suspension liquid when the particle size is less than 5 mu m, and finally adding ionized water to obtain a second coating suspension liquid;
soaking the corrugated board serving as a carrier in the first coating suspension for 10-50 s, then pumping away redundant slurry on the surface of the carrier by using a special coating negative pressure machine, drying the catalyst after coating is finished, roasting, and repeating for a plurality of times until the amount of the inner coating coated on the carrier reaches 10-50 g/L to obtain a first carrier;
and soaking the first carrier in the second coating suspension slurry, staying for 10-50 s, then pumping away redundant slurry on the surface of the carrier by using a special negative pressure coating machine, drying the catalyst after coating is finished, roasting, and repeating for several times until the amount of the inner coating coated on the carrier reaches 80-150 g/L, thereby finishing the preparation of the catalyst.
Adding a ferro-manganese composite oxide and a titanium dioxide material into an aqueous solution to form a suspension, adding a sol accounting for 1-5% of the total amount of a cured material, ball-milling by using a sand mill, and controlling the granularity D90Less than 5 μm, and finally adding ionized water to obtain a first coating suspension:
the iron-manganese composite oxide and the titanium dioxide material are sequentially as follows according to the mass ratio: 30-50% and 50-70%.
Adding a ferro-manganese composite oxide and a titanium dioxide material into an aqueous solution to form a suspension, adding a sol accounting for 1-5% of the total amount of a cured material, ball-milling by using a sand mill, and controlling the granularity D90Less than 5 μm, and finally adding ionized water to obtain a first coating suspension:
after the ionic water is added, the total amount of the oxides is guaranteed to be 10-30% of the mass ratio of the whole suspension.
Wherein, TiO is added2、WO3And SiO2Mixing and adding into ionized water, stirring uniformly to obtain a suspension, adding sol accounting for 1-5% of the total amount of cured substances, ball-milling by using a sand mill, and controlling the granularity D90And when the particle size is less than 5 mu m, adding pore-forming material into the suspension, and finally adding ionized water to obtain a second coating suspension, wherein the step of:
TiO2、WO3、SiO2the weight ratio is as follows: 70-90%, 4.5-10%, 5-10%.
Wherein, TiO is added2、WO3And SiO2Mixing and adding into ionized water, stirring uniformly to obtain a suspension, adding sol accounting for 1-5% of the total amount of cured substances, ball-milling by using a sand mill, and controlling the granularity D90And when the particle size is less than 5 mu m, adding pore-forming material into the suspension, and finally adding ionized water to obtain a second coating suspension, wherein the step of:
and finally, after the ionic water is added, the total amount of the oxides is ensured to be 25-45% of the mass ratio of the whole suspension.
The invention also provides a preparation device adopting the preparation method of the vanadium-tungsten-titanium system industrial denitration catalyst, the preparation device of the vanadium-tungsten-titanium system industrial denitration catalyst comprises a tank body, a support frame, an air cylinder, a push rod and a limiting frame, the support frame is fixedly connected with the tank body and positioned above the tank body, the air cylinder is fixedly connected with the support frame and positioned on one side of the support frame and above the tank body, the push rod is movably connected with the air cylinder and positioned below the air cylinder, the limiting frame is fixedly connected with the push rod and positioned below the push rod, the limiting frame comprises a plurality of frame body supporting bars, and each supporting bar is respectively and fixedly connected with the frame body and uniformly arranged at the bottom of the frame body at intervals.
The vanadium-tungsten-titanium system industrial denitration catalyst and the preparation method and device thereof adopt the corrugated board made of fiber material as a carrier and have high specific surface areaThe SCR reaction can be efficiently carried out, the efficiency of removing nitrogen oxides is ensured, and the bulk density is low, so that the application condition and the cost can be effectively reduced; the first coating layer with the adsorption function is coated on the corrugated board, so that NO can be widened and treatedxThe temperature window of (2) has obvious advantages for the treatment of nitrogen oxides.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of the steps of example 1 provided by the present invention.
FIG. 2 is a flow chart of the steps of example 2 provided by the present invention.
FIG. 3 is a flowchart of the steps of example 3 provided by the present invention.
FIG. 4 is a schematic structural diagram of a preparation device of a vanadium-tungsten-titanium system industrial denitration catalyst provided by the invention.
1-tank body, 2-support frame, 3-cylinder, 4-push rod, 5-limit frame, 51-frame body and 52-support strip.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The invention provides a vanadium-tungsten-titanium system industrial denitration catalyst which comprises a first coating, a second coating and a corrugated board, wherein the first coating is coated on the surface of the corrugated board, and the second coating is coated on the surface of the first coating;
the effective components of the first coating are iron-manganese composite oxide and titanium oxide;
the effective components of the second coating are oxides of vanadium, titanium, tungsten, molybdenum and silicon;
the corrugated board is made of fiber materials.
In the embodiment, the corrugated board has the size of 150mm × 150mm × 150mm and the mesh number of about 200 meshes, and the corrugated board made of fiber is used as a carrier, so that the corrugated board has the advantages of high specific surface area, capability of efficiently carrying out SCR reaction and ensuring the efficiency of removing nitrogen oxides, low stacking density and capability of effectively reducing application conditions and cost; the first coating layer with the adsorption function is coated on the corrugated board, so that NO can be widened and treatedxThe temperature window of (2) has obvious advantages for the treatment of nitrogen oxides.
Example 1, referring to fig. 1, the present invention further provides a method for manufacturing the vanadium tungsten titanium system industrial denitration catalyst, including:
s1: respectively adding materials of 30 percent and 70 percent of iron-manganese composite oxide and titanium dioxide by mass into aqueous solution to form mixed suspension, adding aluminum sol accounting for 1 percent of the total amount of cured substances, ball-milling by using a sand mill and controlling the granularity D90Adding deionized water with the particle size less than 5 microns to ensure that the total amount of the oxides accounts for 10 percent of the whole suspension liquid to obtain first coating suspension slurry;
s2: will be provided withTiO2、WO3And SiO2Respectively adding 70%, 10% and 10% of titanium dioxide, ammonium metatungstate and silica sol solution into deionized water according to the mass ratio, uniformly stirring to obtain a suspension, and simultaneously adding V2O5Dissolving vanadyl oxalate 10% in oxalic acid, heating to dissolve, adding into the suspension, stirring, adding silica sol 5% of the total amount of the cured substances, and ball milling with a sand mill to control the granularity D90Less than 5 microns, adding dextrin accounting for 1 percent of the total amount of the cured substances into the suspension, and finally adding deionized water to ensure that the content of the total amount of the oxides in the suspension is 25 percent to obtain the second coating suspension slurry;
s3: taking the corrugated board as a carrier, soaking the corrugated board in the first coating suspension liquid, staying for 10s, then pumping away redundant slurry on the surface of the carrier by using a special coating negative pressure machine, drying the catalyst at 150 ℃ for 1h after coating is finished, then roasting for 2h at 350 ℃, and repeating for a plurality of times until the amount of the inner coating coated on the carrier reaches 10g/L to obtain a first carrier;
s4: and soaking the first carrier in the second coating suspension slurry, staying for 10s, then pumping away the redundant slurry on the surface of the carrier by using a special coating negative pressure machine, drying the catalyst at 150 ℃ for 1h after the coating is finished, roasting for 2h at 450 ℃, and repeating for several times until the amount of the inner coating coated on the carrier reaches 80g/L, thereby finishing the preparation of the catalyst.
Embodiment 2, referring to fig. 2, the present invention further provides a method for manufacturing the vanadium tungsten titanium system industrial denitration catalyst, including:
s1: respectively adding materials of 40 percent and 60 percent of iron-manganese composite oxide and titanium dioxide according to the mass ratio into aqueous solution to form mixed suspension, adding alumina sol accounting for 5 percent of the total amount of cured substances, ball-milling by using a sand mill and controlling the granularity D90Adding deionized water with the particle size less than 5 microns to ensure that the total amount of the oxides accounts for 30 percent of the whole suspension liquid to obtain first coating suspension slurry;
s2: adding TiO into the mixture2、WO3And SiO2According to the mass ratio, the mixture is 80 percent,Respectively adding 7% and 8% of titanium dioxide, ammonium metatungstate and silica sol solution into deionized water, uniformly stirring to obtain suspension, and simultaneously adding V2O5Dissolving 5% ammonium metavanadate in ethanolamine, heating to dissolve, adding into the suspension, stirring, mixing, adding 10% silica sol, and ball milling with sand mill to control particle size D90Less than 5 microns, adding carboxymethyl cellulose accounting for 5 percent of the total amount of the cured substances into the suspension, and finally adding deionized water to ensure that the content of the total amount of the oxides in the suspension is 45 percent to obtain second coating suspension slurry;
s3: taking the corrugated board as a carrier, soaking the corrugated board in the first coating suspension liquid, staying for 50s, then pumping away redundant slurry on the surface of the carrier by using a special coating negative pressure machine, drying the catalyst at 100 ℃ for 3h after coating is finished, then roasting the catalyst at 400 ℃ for 2h, and repeating the steps for a plurality of times until the amount of the inner coating coated on the carrier reaches 50g/L to obtain a first carrier;
s4: and soaking the first carrier in the second coating suspension slurry, staying for 50s, then pumping away the redundant slurry on the surface of the carrier by using a special coating negative pressure machine, drying the catalyst at 100 ℃ for 3h after the coating is finished, roasting for 2h at 450 ℃, and repeating for several times until the amount of the inner coating coated on the carrier reaches 110g/L, thereby finishing the preparation of the catalyst.
s1: respectively adding 50 percent and 50 percent of materials of iron-manganese composite oxide and titanium dioxide by mass into aqueous solution to form mixed suspension, adding sol accounting for 3 percent of the total amount of cured substances, ball-milling by using a sand mill and controlling the granularity D90Adding deionized water with the particle size less than 5 microns to ensure that the total amount of the oxides accounts for 20 percent of the whole suspension liquid to obtain first coating suspension slurry;
s2: adding TiO into the mixture2、WO3And SiO2Titanium dioxide, ammonium metatungstate and silica sol solution with the mass percentages of 90%, 4.5% and 5% are respectively addedAdding into deionized water, stirring to obtain suspension, and adding V2O5Dissolving 0.5% vanadyl sulfate in oxalic acid, heating to dissolve, adding into the suspension, stirring, adding 5% of silicon-aluminum composite sol, and ball milling with a sand mill to control particle size D90Adding carboxyethyl cellulose accounting for 3% of the total amount of the cured substances into the suspension liquid, and finally adding deionized water to ensure that the content of the total amount of the oxides in the suspension liquid is 30% to obtain second coating layer suspension slurry;
s3: taking the corrugated board as a carrier, soaking the corrugated board in the first coating suspension liquid, staying for 35s, then pumping away redundant slurry on the surface of the carrier by using a special coating negative pressure machine, drying the catalyst at 120 ℃ for 2h after coating is finished, then roasting the catalyst at 400 ℃ for 1.5h, and repeating the steps for a plurality of times until the amount of the inner coating coated on the carrier reaches 30g/L to obtain a first carrier;
s4: and soaking the first carrier in the second coating suspension slurry, staying for 30s, then pumping away the redundant slurry on the surface of the carrier by using a special coating negative pressure machine, drying the catalyst at 120 ℃ for 2h after the coating is finished, roasting at 450 ℃ for 1.5h, and repeating for several times until the amount of the inner coating coated on the carrier reaches 150g/L, thereby finishing the preparation of the catalyst.
Comparative example 1: adding TiO into the mixture2、WO3And SiO2Respectively adding 70%, 10% and 10% of titanium dioxide, ammonium metatungstate and a silica sol solution into deionized water according to the mass ratio, uniformly stirring to obtain a suspension, simultaneously dissolving 10% of vanadyl oxalate into oxalic acid, heating to dissolve, then adding the obtained solution into the suspension, uniformly stirring and mixing, then adding silica sol accounting for 5% of the total amount of cured substances, ball-milling by using a sand mill to control the granularity D90 to be less than 5 mu m, then adding 1% of dextrin accounting for the total amount of the cured substances into the suspension, and finally adding deionized water to ensure that the content of the total amount of oxides in the suspension is 25% to obtain suspension slurry; soaking a corrugated paper carrier made of fiber materials in the prepared slurry, standing for 10s, then pumping away the redundant slurry on the surface of the carrier by using a special coating negative pressure machine, and placing the catalyst at 150 ℃ after coatingDrying for 1h, then roasting for 2h at 450 ℃, and repeating for several times until the amount of the outer coating layer coated on the carrier reaches 80g/L, thereby completing the preparation of the catalyst.
Catalyst fresh state activity test: the performance test of the catalyst is carried out on a continuous flowing fixed bed reactor, the prepared catalyst sample is wrapped by quartz wool on the side surface and then is put into a quartz tube reactor, 350ppm of NO and 350ppm of NH are introduced into the reactor3、14％O2、5％H2O、5％CO2By N2As equilibrium gas, the reaction space velocity is controlled to be 15000h-1The reaction temperature points were measured at 200 deg.C, 250 deg.C, 300 deg.C and 350 deg.C. Detecting the gas concentration at the outlet of the reactor by using a Fourier transform infrared spectrometer, recording data and calculating NO after the gas concentration is stablexAnd (4) conversion rate.
The test results are given in the following table:
from the above, it can be seen that the NO conversion efficiency of example 1 at several test temperature points is significantly better than that of comparative example 1, especially the conversion efficiency at 200 ℃ is improved by 9%, indicating that the catalyst prepared according to the invention broadens the NO conversionxConversion temperature window, low temperature NOxAnd (4) transformation.
Referring to fig. 4, the present invention further provides a preparation apparatus using the preparation method of the vanadium-tungsten-titanium system industrial denitration catalyst, where the preparation apparatus of the vanadium-tungsten-titanium system industrial denitration catalyst includes a tank 1, a support frame 2, a cylinder 3, a push rod 4 and a limit frame 5, the support frame 2 is fixedly connected to the tank 1 and located above the tank 1, the cylinder 3 is fixedly connected to the support frame 2 and located at one side of the support frame 2 and located above the tank 1, the push rod 4 is movably connected to the cylinder 3 and located below the cylinder 3, the limit frame 5 is fixedly connected to the push rod 4 and located below the push rod 4, the limit frame 5 includes a frame body 51 and support bars 52, the number of the support bars 52 is multiple, each support bar 52 is fixedly connected to the frame body 51, and are uniformly spaced at the bottom of the frame body 51.
In this embodiment, when soaking the operation, will the corrugated sheet is placed spacing frame 5's inside, support bar 52 is right the corrugated sheet supports, cylinder 3 passes through push rod 4 will spacing frame 5 pushes away to jar 1 is inside, until the corrugated sheet soaks in solution completely, the corrugated sheet floats in solution, through framework 51 restriction the corrugated sheet breaks away from spacing frame 5 soaks the completion back, cylinder 3 will spacing frame 5 resumes to the normal position, support bar 52 will the corrugated sheet takes out the jar body 1, for traditional centre gripping the corrugated paper soaks, and above-mentioned structure makes the corrugated sheet soaks the face more comprehensive.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A vanadium-tungsten-titanium system industrial denitration catalyst, which is characterized in that,
the vanadium-tungsten-titanium system industrial denitration catalyst comprises a first coating, a second coating and a corrugated board, wherein the first coating is coated on the surface of the corrugated board, and the second coating is coated on the surface of the first coating;
the effective components of the first coating are iron-manganese composite oxide and titanium oxide;
the effective components of the second coating are oxides of vanadium, titanium, tungsten, molybdenum and silicon;
the corrugated board is made of fiber materials.
2. The preparation method of the vanadium-tungsten-titanium system industrial denitration catalyst according to claim 1 is characterized by comprising the following steps:
oxidizing the iron-manganese composite oxide with oxygenAdding a titanium material into an aqueous solution to form a suspension, adding a sol accounting for 1-5% of the total amount of the cured substances, and ball-milling by using a sand mill while controlling the granularity D90Less than 5 μm, and finally adding ionized water to obtain a first coating suspension;
adding TiO into the mixture2、WO3And SiO2Mixing and adding into ionized water, stirring uniformly to obtain a suspension, adding sol accounting for 1-5% of the total amount of cured substances, ball-milling by using a sand mill, and controlling the granularity D90Adding a pore-forming material into the suspension liquid when the particle size is less than 5 mu m, and finally adding ionized water to obtain a second coating suspension liquid;
soaking the corrugated board serving as a carrier in the first coating suspension for 10-50 s, then pumping away redundant slurry on the surface of the carrier by using a special coating negative pressure machine, drying the catalyst after coating is finished, roasting, and repeating for a plurality of times until the amount of the inner coating coated on the carrier reaches 10-50 g/L to obtain a first carrier;
and soaking the first carrier in the second coating suspension slurry, staying for 10-50 s, then pumping away redundant slurry on the surface of the carrier by using a special negative pressure coating machine, drying the catalyst after coating is finished, roasting, and repeating for several times until the amount of the inner coating coated on the carrier reaches 80-150 g/L, thereby finishing the preparation of the catalyst.
3. The method for preparing the vanadium-tungsten-titanium system industrial denitration catalyst according to claim 2, wherein the iron-manganese composite oxide and the titanium dioxide material are added into the aqueous solution to form a suspension, a sol accounting for 1-5% of the total amount of the cured substances is added, and the sol is ball-milled by a sand mill with the particle size D controlled90Less than 5 μm, and finally adding ionized water to obtain a first coating suspension:
the iron-manganese composite oxide and the titanium dioxide material are sequentially as follows according to the mass ratio: 30-50% and 50-70%.
4. The method for preparing the vanadium-tungsten-titanium system industrial denitration catalyst according to claim 3, wherein the iron-manganese composite oxide and the titanium dioxide material are added into the aqueous solution to form the vanadium-tungsten-titanium system industrial denitration catalystAdding sol accounting for 1-5% of the total amount of the condensate into the suspension, and ball-milling the suspension by using a sand mill while controlling the granularity D90Less than 5 μm, and finally adding ionized water to obtain a first coating suspension:
after the ionic water is added, the total amount of the oxides is guaranteed to be 10-30% of the mass ratio of the whole suspension.
5. The method for preparing the vanadium-tungsten-titanium system industrial denitration catalyst according to claim 4, wherein TiO is added2、WO3And SiO2Mixing and adding into ionized water, stirring uniformly to obtain a suspension, adding sol accounting for 1-5% of the total amount of cured substances, ball-milling by using a sand mill, and controlling the granularity D90And when the particle size is less than 5 mu m, adding pore-forming material into the suspension, and finally adding ionized water to obtain a second coating suspension, wherein the step of:
TiO2、WO3and SiO2The weight ratio is as follows: 70-90%, 4.5-10%, 5-10%.
6. The method for preparing vanadium-tungsten-titanium system industrial denitration catalyst according to claim 5, wherein TiO is added2、WO3And SiO2Mixing and adding into ionized water, stirring uniformly to obtain a suspension, adding sol accounting for 1-5% of the total amount of cured substances, ball-milling by using a sand mill, and controlling the granularity D90And when the particle size is less than 5 mu m, adding pore-forming material into the suspension, and finally adding ionized water to obtain a second coating suspension, wherein the step of:
and finally, after the ionic water is added, the total amount of the oxides is ensured to be 25-45% of the mass ratio of the whole suspension.
7. The preparation apparatus using the method for preparing a vanadium tungsten titanium system industrial denitration catalyst according to claim 6,
the preparation facilities of vanadium tungsten titanium system industry denitration catalyst includes a jar body, support frame, cylinder, push rod and spacing frame, the support frame with jar body fixed connection, and be located the top of the jar body, the cylinder with support frame fixed connection, and be located one side of support frame, and be located the top of the jar body, the push rod with cylinder swing joint, and be located the below of cylinder, spacing frame with push rod fixed connection, and be located the below of push rod, spacing frame includes framework and support bar, the quantity of support bar is a plurality of, every the support bar respectively with framework fixed connection to the interval evenly set up in the bottom of framework.
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