CN113042066B - Flue gas denitration catalyst and preparation method thereof - Google Patents

Flue gas denitration catalyst and preparation method thereof Download PDF

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CN113042066B
CN113042066B CN202110358254.0A CN202110358254A CN113042066B CN 113042066 B CN113042066 B CN 113042066B CN 202110358254 A CN202110358254 A CN 202110358254A CN 113042066 B CN113042066 B CN 113042066B
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CN113042066A (en
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刘恒芳
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Yuncheng Jinhui Chemical Co.,Ltd.
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    • 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
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    • 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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    • 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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    • B01J37/08—Heat treatment
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    • B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/342—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electric, magnetic or electromagnetic fields, e.g. for magnetic separation
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    • B01J37/349—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of flames, plasmas or lasers
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Abstract

The invention relates to a flue gas denitration catalyst and a preparation method thereof, (1) PVP fiber is prepared by adopting an electrostatic spinning process, and plasma treatment is carried out; the PVP fiber is put into a potassium permanganate solution, transferred into a reaction kettle and subjected to hydrothermal reaction to obtain PVP/MnO with a three-dimensional core-shell structure2A composite material; (2) mixing PVP/MnO2Transferring the composite material into a mixed solution containing zinc salt and ammonia water, stirring, and then placing in a high-pressure reaction kettle to obtain PVP/MnO2a/ZnO composite; dissolving the composite material in ethanol, adding nickel salt and cobalt salt, hydrothermally dripping ammonia water, and performing hydrothermal reaction to obtain PVP/MnO2/ZnO/NiCo2O4Soaking the composite material by adopting NaOH, and then calcining in air atmosphere to remove a template to obtain void/MnO2/void/NiCo2O4The composite material of (1). The catalyst has larger specific surface area, good structural stability and MnO2And NiCo2O4Has synergistic effect and better catalytic activity.

Description

Flue gas denitration catalyst and preparation method thereof
Technical Field
The invention relates to the technical field of environmental protection, and particularly relates to a flue gas denitration catalyst and a preparation method thereof.
Background
Nitrogen oxides discharged from coal-fired boilers, glass furnaces, cement furnaces and the like are one of main pollutants causing acid rain, photochemical smog and the like, cause great pollution to the atmosphere, destroy the ecological environment and damage the human health. How to effectively eliminate nitrogen oxides has become a key and difficult point of air pollution treatment at present. The Selective Catalytic Reduction (SCR) denitration technology is a flue gas denitration technology which is internationally most widely applied, has the highest market share and is most stably and reliably operated, and the principle is that NO and a reducing agent NH are reacted under the action of a catalyst3The following reactions occur: 4NH3+4NO+O2→4N2+6H2O; the core technology of the SCR technology is a catalyst, and the quality of the catalytic performance directly determines the denitration efficiency; therefore, the development of a catalyst with good catalytic performance and high stability has great significance for denitration technology.
The transition metal oxide catalytic denitration material has higher NOx catalytic performance, higher oxygen resistance compared with a noble metal catalytic material, and low cost. CN 112473682A discloses high-performance medium-low temperature NH3-SCR catalystThe preparation method of the reagent is characterized by comprising the following steps: dissolving cerous nitrate hexahydrate, ferric nitrate nonahydrate and niobium oxalate in distilled water by adopting a coprecipitation method, uniformly stirring at room temperature, dropwise adding ammonia water into the mixed solution to ensure that the mixed solution is completely precipitated, and finally aging, filtering, washing, drying and roasting in air atmosphere to prepare high-performance medium-low temperature NH3-an SCR catalyst. CN 111992214A discloses a nano hierarchical pore SiO2The @ Cu/Ni core-shell material and the preparation method and the application thereof, wherein the preparation method comprises the following steps: firstly, preparing nano-scale spherical SiO2The dispersion liquid is sequentially mixed with a copper source solution and a reducing agent to obtain brick red precipitate; then calcining the brick red precipitate to obtain the core-shell material SiO2@ Cu; finally preparing a mixture containing SiO2Mixing the dispersion of @ Cu and polyvinyl alcohol with a nickel source, and then sequentially heating, stirring, drying in an oven and calcining at high temperature to obtain the nano hierarchical pore SiO2@ Cu/Ni core-shell material.
Disclosure of Invention
Aiming at the problems of low catalytic activity, small specific surface area and poor activity of the catalyst in the prior art, the invention aims to provide void/MnO2/void/NiCo2O4The composite material flue gas denitration catalyst.
The flue gas denitration catalyst is characterized by being prepared by the following method:
(1) preparing PVP fiber by adopting an electrostatic spinning process, and carrying out plasma treatment on the PVP fiber; the PVP fiber is put into a deionized water/ethylene glycol mixed solution dissolved with potassium permanganate and transferred into a reaction kettle for hydrothermal reaction to obtain PVP/MnO with a three-dimensional core-shell structure2A composite material;
(2) mixing PVP/MnO2Transferring the composite material into a mixed solution containing zinc salt and ammonia water, stirring, and then placing in a high-pressure reaction kettle to obtain PVP/MnO2a/ZnO composite; dissolving the composite material in ethanol, adding nickel salt and cobalt salt, hydrothermally dripping ammonia water, and performing hydrothermal reaction to obtain PVP/MnO2/ZnO/NiCo2O4The composite material of (1), the composite materialSoaking by adopting NaOH, and then calcining in air atmosphere to remove the template to obtain void/MnO2/void/NiCo2O4The composite material of (1).
Preferably, the hydrothermal reaction of the steps (1) and (2) is carried out at 180 ℃ and 200 ℃ for 12-20 h;
preferably, the calcination temperature in the air is 200-300 ℃, and the calcination time is 0.5-1 h;
preferably, MnO2/ZnO/NiCo2O4The molar ratio is 1: (0.5-2): (0.5-2);
preferably, the nickel and cobalt salts are nickel and cobalt nitrates.
The technical effects are as follows:
the application firstly provides that PVP nano fiber-ZnO prepared by an electrostatic spinning process is used as a double template to prepare void/MnO with a unique three-dimensional double hollow structure2/void/NiCo2O4The composite material has larger specific surface area, and catalytic active sites, MnO, are greatly increased2And NiCo2O4The catalyst has a synergistic effect and has better catalytic activity; the preparation method has low energy consumption, little pollution, environmental protection, simplicity, convenience and rapidness, and can be used for large-scale production.
Detailed Description
Example 1
(1) Preparing PVP three-dimensional network fiber by adopting an electrostatic spinning process, and carrying out plasma treatment on the PVP three-dimensional network fiber; dissolving 0.1mol of potassium permanganate in 50ml of water/ethylene glycol mixed solution with the volume ratio of 1:1, then putting 0.5g of PVP fiber in a potassium permanganate reaction kettle, and carrying out hydrothermal reaction at 180 ℃ for 8h to obtain PVP/MnO with a three-dimensional core-shell structure2A composite material;
(2) dissolving 0.4mol of zinc nitrate in deionized water, dripping a certain amount of ammonia water, adjusting the pH to 7.8-9, and adding PVP/MnO obtained in the step (1)2The composite material is stirred and then placed in a high-pressure reaction kettle to react for 6 hours at 180 ℃ to obtain PVP/MnO2a/ZnO composite; dissolving the composite material in ethanol, adding nickel salt and cobalt salt, hydrothermally dripping ammonia water, and performing hydrothermal reaction to obtain PVP/MnO2/ZnO/NiCo2O4The composite material is soaked by NaOHThen calcining the mixture for 0.5h at 300 ℃ in an air atmosphere to remove the template to obtain void/MnO2/void/NiCo2O4The composite material of (1).
And (3) testing the catalyst: the reaction activity of the catalyst is tested in a fixed bed quartz tube reactor, the catalyst is 1g, the reaction temperature is 100-450 ℃, ammonia gas is used as a reducing agent, the total flow of gas is controlled at 300mL/min, the space velocity is 30,000 mL/g-1 h-1, the denitration efficiency is higher than 88%, and the reaction activity to N is tested2The selectivity is greater than 82%.
Example 2
(1) Preparing PVP three-dimensional network fiber by adopting an electrostatic spinning process, and carrying out plasma treatment on the PVP three-dimensional network fiber; dissolving 0.1mol of potassium permanganate in 50ml of water/ethylene glycol mixed solution with the volume ratio of 1:1, then putting 0.5g of PVP fiber in a potassium permanganate reaction kettle, and carrying out hydrothermal reaction at 180 ℃ for 8h to obtain PVP/MnO with a three-dimensional core-shell structure2A composite material;
(2) dissolving 0.4mol of zinc nitrate in deionized water, dripping a certain amount of ammonia water, adjusting the pH to 7.8-9, and adding PVP/MnO obtained in the step (1)2The composite material is stirred and then placed in a high-pressure reaction kettle to react for 6 hours at 180 ℃ to obtain PVP/MnO2a/ZnO composite; dissolving the composite material in ethanol, adding nickel salt and cobalt salt, hydrothermally dripping ammonia water, and performing hydrothermal reaction to obtain PVP/MnO2/ZnO/NiCo2O4Soaking the composite material by adopting NaOH, then calcining the composite material for 0.5h at 300 ℃ in air atmosphere to remove a template, and obtaining void/MnO2/void/NiCo2O4The composite material of (1).
And (3) testing the catalyst: the reaction activity of the catalyst is tested in a fixed bed quartz tube reactor, the catalyst is 1g, the reaction temperature is 100-450 ℃, ammonia gas is used as a reducing agent, the total flow of the gas is controlled to be 200mL/min, the space velocity is 30,000 mL/g-1 h-1, the denitration efficiency is more than 87%, and the reaction activity to N is tested2The selectivity is greater than 85%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (5)

1. The flue gas denitration catalyst is characterized by being prepared by the following method: preparing PVP fiber by adopting an electrostatic spinning process, and carrying out plasma treatment on the PVP fiber; the PVP fiber is put into a deionized water/ethylene glycol mixed solution dissolved with potassium permanganate and transferred into a reaction kettle for hydrothermal reaction to obtain PVP/MnO with a three-dimensional core-shell structure2A composite material; (2) mixing PVP/MnO2Transferring the composite material into a mixed solution containing zinc salt and ammonia water, stirring, and then placing in a high-pressure reaction kettle to obtain PVP/MnO2a/ZnO composite; dissolving the composite material in ethanol, adding nickel salt and cobalt salt, hydrothermally dripping ammonia water, and performing hydrothermal reaction to obtain PVP/MnO2/ZnO/NiCo2O4The composite material is soaked by NaOH to remove ZnO, and then calcined in air atmosphere to remove the template, so that three-dimensional reticular void/MnO is obtained2/void/NiCo2O4A double hollow core-shell composite material.
2. The flue gas denitration catalyst as claimed in claim 1, wherein the hydrothermal reaction in steps (1) and (2) is carried out at 180 ℃ and 200 ℃ for 12-20 h.
3. The flue gas denitration catalyst as claimed in claim 1, wherein the calcination temperature in air is 200-300 ℃, and the calcination time is 0.5-1 h.
4. The flue gas denitration catalyst of claim 1, wherein MnO is2/ZnO/NiCo2O4The molar ratio is 1: (0.5-2): (0.5-2).
5. The flue gas denitration catalyst of claim 1, wherein the nickel salt and the cobalt salt are nickel nitrate and cobalt nitrate.
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CN113828326B (en) * 2021-10-20 2022-04-01 烟台百川汇通科技有限公司 Flue gas denitration catalyst and preparation method thereof
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