CN113019356A - Method for preparing denitration catalyst by hydrothermal method - Google Patents
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- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 35
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000011258 core-shell material Substances 0.000 claims abstract description 21
- 239000004005 microsphere Substances 0.000 claims abstract description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000002378 acidificating effect Effects 0.000 claims abstract description 3
- 239000011363 dried mixture Substances 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000000047 product Substances 0.000 description 12
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000010531 catalytic reduction reaction Methods 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010420 shell particle Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000005437 stratosphere Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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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- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/404—Nitrogen oxides other than dinitrogen oxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)
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Abstract
The invention discloses a method for preparing a denitration catalyst by a hydrothermal method, which comprises the following steps: s1: adding TiO into deionized water2Ultrasonically dispersing, adjusting the pH value of the solution to be weakly acidic, adding ammonium vanadate, and magnetically stirring until the ammonium vanadate is completely dissolved to obtain a suspension A; s2, transferring the suspension A to a polytetrafluoroethylene lining hydrothermal reaction kettle for hydrothermal reaction; s3: after the hydrothermal reaction is finished, naturally cooling to room temperature, centrifugally separating the precipitate, washing the precipitate with deionized water, and drying at 80-100 ℃ for 4h e6 h; s4: transferring the dried mixture to a muffle furnace for roasting to obtain V2O5@TiO2Core-shell microspheres. The invention prepares V with controllable shell thickness2O5@TiO2Core shell microspheres, adjustable by V2O5@TiO2The shell thickness of the core-shell microsphere further regulates and controls NO conversion rate and N2The amount of O produced.
Description
Technical Field
The invention belongs to the technical field of catalytic denitration, and particularly relates to a method for preparing a denitration catalyst by a hydrothermal method.
Background
Nitrogen oxide (NOx) is the key point for emission reduction, and among the control technologies, selective catalytic reduction (selective catalytic reduction by NH)3,NH3SCR) has high denitration efficiency, mature and reliable technology and no by-product, and is a key recommended technology for NOx emission reduction. Commercial vanadium titanium catalyst is NH3Core of SCR technology, main constituent V2O5/TiO2In which TiO is2As a carrier, V2O5Is used as active component.
However, commercial vanadium-titanium catalysts are available in NH3SCR denitration product except N2In addition, some harmful by-products, such as N, are often present2O, also known as nitrous oxide, is a Greenhouse Gas (Greenhouse Gas), a monomolecular N2The Greenhouse Effect (Greenhouse Effect) is CO2298 times, the warming effect on global climate is more and more obvious. N is a radical of2O can exist stably in the atmosphere, and the O is destroyed by migration to the stratosphere3Layer of O3Lamellar voids, which subject humans and other living beings to damage from solar ultraviolet radiation.
Due to N2The activation energy required by O decomposition is higher (250kJ/mol), and no catalyst participates in N2The O decomposition reaction is difficult to proceed. At present, N2The O decomposition catalyst is mainly a noble metal supported catalyst, and the commonly used noble metals mainly comprise Pd, Pt, Ag and the like. Although the above-mentioned noble metal-supported catalyst pair N2O decomposition has a relatively high decomposition capacity, but the rarity of precious metals is not suitable for large-scale commercial application. Therefore, research and development of other NH3The SCR denitration catalytic material has important theoretical and practical significance.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method for preparing a denitration catalyst by a hydrothermal method, and preparing V with a controllable shell thickness2O5@TiO2Core shell microspheres, adjustable by V2O5@TiO2The shell thickness of the core-shell microsphere further regulates and controls NO conversion rate and N2The amount of O produced.
In order to solve the technical problems, the invention adopts a technical scheme that: a method for preparing a denitration catalyst by a hydrothermal method comprises the following steps:
s1: adding TiO into deionized water2Ultrasonically dispersing, adjusting the pH value of the solution to be weakly acidic, adding ammonium vanadate, and magnetically stirring until the ammonium vanadate is completely dissolved to obtain a suspension A;
s2, transferring the suspension A to a polytetrafluoroethylene lining hydrothermal reaction kettle for hydrothermal reaction;
s3: after the hydrothermal reaction is finished, naturally cooling to room temperature, centrifugally separating the precipitate, washing the precipitate with deionized water, and drying at 80-100 ℃ for 4-6 h;
s4: transferring the dried mixture to a muffle furnace for roasting to obtain V2O5@TiO2Core-shell microspheres.
The invention adopts a further technical scheme for solving the technical problems that:
further, the TiO2The mass ratio of the ammonium vanadate to the ammonium vanadate is 156: 1-156: 3.
Further, the pH value of the solution in the step S1 is 1.6-2.2.
Further, the hydrothermal reaction temperature of the step S2 is 100-140 ℃, and the hydrothermal reaction time is 24-36 h.
Further, the roasting temperature of the step S4 is 300-500 ℃, and the time is 1-3 h.
Further, the ultrasonic dispersion time in the step S1 is 30-40 min.
Further, the shell thickness of the core-shell microsphere of step S4 is 2 to 5 nm.
Further, the particle size of the core-shell microsphere in the step S4 is 27-30 nm.
The invention has the beneficial effects that:
1. the invention uses V2O5Is a hard template, ammonium vanadate is taken as a raw material, and a hydrothermal method is adopted to prepare V2O5@TiO2The core-shell microsphere, a special core-shell microsphere structure, can improve the effective component V2O5The specific surface area of (2) is favorable for improving the efficiency of catalytic reaction; can also be adjusted by adjusting V2O5@TiO2Method for regulating and controlling NO conversion rate and N by thickness of shell layer of core-shell microsphere2The amount of O produced;
2. after the hydrothermal reaction is finished, the product is obtained by centrifugal separation, clear liquid can be reused, no pollutant is generated, and the preparation method is simple, economic and environment-friendly;
3. the invention is in commercial V2O5Is a raw material and is beneficial to the industrial production of products.
Drawings
FIG. 1 shows the invention V2O5@TiO2A linear graph of the influence of different particle sizes (namely, different shell thicknesses) of the core-shell microspheres on the NO conversion rate is shown;
FIG. 2 shows the invention V2O5@TiO2Different particle sizes (i.e., different shell thicknesses) of core-shell microspheres vs. N2Line graph of the influence of O production.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
Example 1: a method for preparing a denitration catalyst by a hydrothermal method comprises the following steps:
s1, adding 5.00g V into 100mL deionized water2O5And ultrasonically dispersing for 30 min. Adjusting the pH value of the solution to 1.8 by using sulfuric acid, adding 0.032g of ammonium vanadate, and magnetically stirring until the ammonium vanadate is completely dissolved to obtain a suspension A;
s2, transferring the suspension A to a polytetrafluoroethylene lining hydrothermal reaction kettle, and reacting for 36h at 100 ℃.
S3, naturally cooling to room temperature, centrifugally separating the precipitate, washing the precipitate with deionized water and absolute ethyl alcohol, and drying at 100 ℃ for 6 hours;
s4, transferring the dried product to a muffle furnace, and roasting the product at 400 ℃ for 2h to obtain a product V2O5@TiO2The shell layer thickness of the core-shell microsphere is 2.5nm, and the particle size is 27.5 nm.
Example 2: a method for preparing a denitration catalyst by a hydrothermal method comprises the following steps:
s1, adding 5.00g V into 100mL deionized water2O5And carrying out ultrasonic dispersion for 40 min. Adjusting the pH value of the solution to 2.0 by using sulfuric acid, adding 0.064g of ammonium vanadate, and magnetically stirring until the ammonium vanadate is completely dissolved to obtain a suspension A;
s2, transferring the suspension A to a polytetrafluoroethylene lining hydrothermal reaction kettle, and reacting for 30h at 120 ℃.
S3, naturally cooling to room temperature, centrifugally separating precipitates, washing with deionized water and absolute ethyl alcohol, and drying at 90 ℃ for 6 hours;
s4, transferring the dried product to a muffle furnace, and roasting the product at 500 ℃ for 2h to obtain a product V2O5@TiO2The shell layer thickness of the core-shell microsphere is 3.5nm, and the particle size is 28.5 nm.
Example 3: a method for preparing a denitration catalyst by a hydrothermal method comprises the following steps:
s1, adding 5.00g V into 100mL deionized water2O5And ultrasonically dispersing for 30 min. Adjusting the pH value of the solution to 2.2 by using sulfuric acid, adding 0.096g of ammonium vanadate, and magnetically stirring until the ammonium vanadate is completely dissolved to obtain a suspension A;
s2, transferring the suspension A to a polytetrafluoroethylene lining hydrothermal reaction kettle, and reacting for 24h at 140 ℃.
S3, naturally cooling to room temperature, centrifugally separating precipitates, washing with deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 4 hours;
s4, transferring the dried product to a muffle furnace, and roasting the product at 300 ℃ for 3h to obtain a product V2O5@TiO2The shell layer thickness of the core-shell microsphere is 4.5nm, and the particle size is 29.5 nm.
V of the invention2O5@TiO2Carrying out denitration catalytic reaction on core-shell microspheres (with the shell particle sizes of 27.5nm, 28.5nm and 29.5nm) to obtain NO conversion rate and N at different temperatures2The amount of O produced.
As can be seen from the results of figures 1 and 2,v prepared by the invention2O5@TiO2The core-shell microspheres have a NO conversion rate of 90-99% and a N conversion rate of N2The amount of O produced is 30-110 ppm.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. A method for preparing a denitration catalyst by a hydrothermal method is characterized by comprising the following steps: the method comprises the following steps:
s1: adding TiO into deionized water2Ultrasonically dispersing, adjusting the pH value of the solution to be weakly acidic, adding ammonium vanadate, and magnetically stirring until the ammonium vanadate is completely dissolved to obtain a suspension A;
s2, transferring the suspension A to a polytetrafluoroethylene lining hydrothermal reaction kettle for hydrothermal reaction;
s3: after the hydrothermal reaction is finished, naturally cooling to room temperature, centrifugally separating the precipitate, washing the precipitate with deionized water, and drying at 80-100 ℃ for 4-6 h;
s4: transferring the dried mixture to a muffle furnace for roasting to obtain V2O5@TiO2Core-shell microspheres.
2. The hydrothermal method of preparing a denitration catalyst of claim 1, wherein: the TiO is2The mass ratio of the ammonium vanadate to the ammonium vanadate is 156: 1-156: 3.
3. The hydrothermal method of preparing a denitration catalyst of claim 1, wherein: the pH value of the solution in the step S1 is 1.6-2.2.
4. The hydrothermal method of preparing a denitration catalyst of claim 1, wherein: the hydrothermal reaction temperature of the step S2 is 100-140 ℃, and the hydrothermal reaction time is 24-36 h.
5. The hydrothermal method of preparing a denitration catalyst of claim 1, wherein: the roasting temperature of the step S4 is 300-500 ℃, and the time is 1-3 h.
6. The hydrothermal method of preparing a denitration catalyst of claim 1, wherein: the ultrasonic dispersion time in the step S1 is 30-40 min.
7. The hydrothermal method of preparing a denitration catalyst of claim 1, wherein: the shell thickness of the core-shell microsphere in the step S4 is 2-5 nm.
8. The hydrothermal method of preparing a denitration catalyst of claim 1, wherein: the particle size of the core-shell microsphere obtained in the step S4 is 27-30 nm.
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CN113813965A (en) * | 2021-09-28 | 2021-12-21 | 洛阳理工学院 | NH3-SCR denitration catalyst and preparation method and application thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113813965A (en) * | 2021-09-28 | 2021-12-21 | 洛阳理工学院 | NH3-SCR denitration catalyst and preparation method and application thereof |
CN113813965B (en) * | 2021-09-28 | 2023-12-08 | 洛阳理工学院 | NH 3 SCR denitration catalyst, and preparation method and application thereof |
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