CN115041217A - Preparation method of sulfur poisoning resistant electric denitration catalyst - Google Patents
Preparation method of sulfur poisoning resistant electric denitration catalyst Download PDFInfo
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- CN115041217A CN115041217A CN202210886129.1A CN202210886129A CN115041217A CN 115041217 A CN115041217 A CN 115041217A CN 202210886129 A CN202210886129 A CN 202210886129A CN 115041217 A CN115041217 A CN 115041217A
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—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
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Abstract
The invention discloses a preparation method of a sulfur poisoning resistant electric denitration catalyst, belonging to the field of industrial flue gas SCR denitration catalysts; the preparation method comprises the following steps: s1, mixing melamine and alcohol solvent with titanium dioxide uniformly, drying and calcining to obtain melamine modified titanium dioxide; s2, designing a loading capacity according to the active components of the catalyst, dissolving the rare earth metal nitrate in water, dipping the aqueous solution of the rare earth metal nitrate into the melamine modified titanium dioxide in S1 according to an isometric dipping method, drying, and calcining to obtain the melamine modified titanium dioxide pre-loaded rare earth metal oxide; s3, according to the loading capacity of the active components of the catalyst, mixing ammonium metavanadate, ammonium metatungstate and ammonium heptamolybdate with water and monoethanolamine, heating and dissolving, then according to the proportion of equal-volume impregnation, uniformly mixing the mixed solution of vanadium, tungsten and molybdenum with the melamine modified titanium dioxide pre-loaded rare earth metal oxide obtained in the step S2, drying and calcining to obtain the denitration catalyst.
Description
Technical Field
The invention belongs to the field of preparation of industrial flue gas SCR denitration catalysts, and particularly relates to a preparation method of a sulfur poisoning resistant electric denitration catalyst.
Background
With the promotion and implementation of flue gas pollutant treatment policy in China, NO in China x The emission is being reduced year by year, but the denitration task is still difficult, and especially the denitration of the flue gas of the boiler of the coal-fired power plant is still the key point.
The flue gas denitration of coal-fired power plants commonly uses the traditional commercial V 2 O 5 -WO 3 -MoO 3 /TiO 2 The catalyst has an activity temperature window of 300-420 ℃; at present, most power plants in China are additionally provided with an SCR denitration system, but because the capacity of the power industry in China is excessive, and a thermal power generating unit adapts to deep peak regulation of a power grid in 2016 years, the traditional commercial SCR denitration catalyst (the temperature window is 300-450 ℃) cannot meet increasingly strict environmental-friendly emission requirements under the condition that the temperature of the smoke generated by peak regulation and low-load operation of the unit is reduced (as low as 250 ℃), and further NO is generated x Excessive emission and the like, and brings adverse effects to enterprises; for realizing NO operation in full load range of coal-fired power plant x Discharge reaches the standard, and needs to be matched with the traditional commercial V 2 O 5 -WO 3 -MoO 3 /TiO 2 The catalyst is adjusted in component or structure so as to adapt to load change of peak shaving of the coal-fired power plant unit.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a sulfur poisoning resistant electric denitration catalyst, and the denitration catalyst prepared by the method is suitable for denitration of flue gas of the current coal-fired power plant with wide temperature difference.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a sulfur poisoning resistant electric denitration catalyst comprises the following steps:
s1, uniformly mixing melamine and an alcohol solvent, and then adding titanium dioxide into the mixture for uniform mixing; the mixture of the three is dried and then calcined at high temperature in air atmosphere to obtain the melamine modified titanium dioxide
S2, designing a loading capacity according to the active components of the catalyst, dissolving the rare earth metal nitrate in water, then impregnating the aqueous solution of the rare earth metal nitrate into the melamine modified titanium dioxide in S1 according to an isometric impregnation method, drying the impregnated material, and calcining the dried material at a high temperature in an air atmosphere to obtain the melamine modified titanium dioxide pre-loaded rare earth metal oxide;
s3, according to the design of the loading capacity of the active components of the catalyst, mixing ammonium metavanadate, ammonium metatungstate and ammonium heptamolybdate with water and monoethanolamine, heating and dissolving, then mixing a vanadium-tungsten-molybdenum mixed solution with the melamine modified titanium dioxide pre-loaded rare earth metal oxide obtained in S2 according to the proportion of equal-volume impregnation, uniformly stirring, drying the obtained wet material, and calcining at high temperature to obtain the sulfur-resistant electric denitration catalyst.
The alcohol solvent in the S1 is ethanol, glycol or glycerol.
In the S1, the mass ratio of melamine to the alcohol solvent to the titanium dioxide is (1-5): 100: 50.
In the S1, the drying temperature is 60-200 ℃, and the drying time is 6-24 h; the calcination temperature is 450-650 ℃, and the calcination time is 6-12 h;
in the S2, the drying temperature is 100-200 ℃, and the drying time is 6-12 h; the calcination temperature is 200-400 ℃, and the calcination time is 6-12 h;
in the S3, the drying temperature is 50-100 ℃, and the drying time is 12-24 h; the calcination temperature is 450-600 ℃, and the calcination time is 6-12 h.
The rare earth metal nitrate in the S2 is cerium nitrate, lanthanum nitrate or praseodymium nitrate.
In the S2, the mass ratio of the rare earth metal nitrate to the melamine modified titanium dioxide is (1-10): 100.
In S3, the mass ratio of ammonium metavanadate, ammonium metatungstate, ammonium heptamolybdate and melamine modified titanium dioxide to the rare earth metal oxide is as follows: (0.1-1): (1-5): (1-5): 100.
in S3, the mass ratio of the melamine modified titanium dioxide pre-loaded rare earth metal oxide to the monoethanolamine is as follows: (0.05-1): 100.
the invention has the beneficial effects that:
compared with the prior preparation technology of the electric denitration catalyst, the preparation method adopted by the invention is an active component and auxiliary agent pre-loading technology, and graphitized C is formed on the surface of the carrier by using the melamine modified titanium dioxide firstly 3 N 4 Species of rare earth metal oxides and vanadium, tungsten, molybdenum metal oxides and C subsequently doped and loaded onto a support 3 N 4 Sufficient electron interaction occurs to improve the low temperature (250 ℃) activity of the catalyst, while C is present at low temperature 3 N 4 The amino groups of the species may be bound to SO 2 Selective adsorption is carried out, SO that SO is avoided 2 The migration and adsorption to the active sites improve the sulfur resistance of the catalyst at low temperature.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a graph showing denitration efficiency results of catalysts of examples 1 to 3 of the present invention under different temperature conditions;
FIG. 2 is a graph showing the results of sulfur tolerance experiments for catalysts of examples 1 to 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of a sulfur poisoning resistant electric denitration catalyst comprises the following steps:
the parts mentioned in the present example are all parts by mass;
s1, taking 5 parts of melamine and 100 parts of ethanol, fully stirring and mixing uniformly, adding 50 parts of titanium dioxide, stirring and mixing uniformly, drying by air blowing at 60 ℃ for 12 hours, and calcining at 550 ℃ for 6 hours to obtain melamine modified titanium dioxide;
s2, taking 10 parts of melamine modified titanium dioxide according to CeO 2 The doping amount is 10%, 1 part of cerium nitrate (calculated by the mass of CeO 2) is dissolved in deionized water with the volume amount required by equivalent volume impregnation, after the cerium nitrate is completely dissolved, the cerium nitrate water solution and the melamine modified titanium dioxide are uniformly mixed, then the mixture is dried at 100 ℃ for 6 hours, and finally the mixture is calcined at 300 ℃ for 9 hours to obtain the melamine modified cerium dioxide doped titanium dioxide;
s3, according to V 2 O 5 、WO 3 、MoO 3 Weighing 1 part of ammonium metavanadate, 1 part of ammonium metatungstate and 1 part of ammonium heptamolybdate (parts are calculated according to the mass of a metal oxide) according to the loading amounts of 1.0%, 1.0% and 1.0%, weighing a certain volume of deionized water according to the equal volume impregnation water absorption amount of 100 parts of titanium dioxide, adding the ammonium metavanadate, the ammonium metatungstate and the ammonium heptamolybdate into the deionized water, adding 1 part of monoethanolamine, and fully stirring to completely dissolve precursors of vanadium, tungsten and molybdenum; then, fully and uniformly mixing 100 parts of titanium dioxide obtained in the step S2 with the vanadium-tungsten-molybdenum mixed solution; drying the obtained wet material at 50 ℃ for 12h, and calcining at 600 ℃ for 6 h; and naturally cooling to obtain the sulfur-resistant electric denitration catalyst.
Example 2:
a preparation method of a sulfur poisoning resistant electric denitration catalyst comprises the following steps:
the parts mentioned in the present example are all parts by mass;
s1, taking 3 parts of melamine and 100 parts of ethylene glycol, fully stirring and mixing uniformly, then adding 50 parts of titanium dioxide, stirring and mixing uniformly, drying by air blowing at 200 ℃ for 6 hours, and then calcining at 450 ℃ for 12 hours to obtain melamine modified titanium dioxide;
s2, taking 10 parts of melamine modified titanium dioxide according to La 2 O 3 The doping amount is 1%, 0.1 part of lanthanum nitrate (by La) 2 O 3 Mass) is dissolved in deionized water with the volume required by equivalent-volume impregnation, after the solution is completely dissolved, lanthanum nitrate aqueous solution and melamine modified titanium dioxide are uniformly mixed, then the mixture is dried at 150 ℃ for 9 hours, and finally the mixture is calcined at 200 ℃ for 9 hours to obtain melamine modified lanthanum oxide doped titanium dioxide;
s3, according to V 2 O 5 、WO 3 、MoO 3 Weighing 0.5 part of ammonium metavanadate, 2.5 parts of ammonium metatungstate and 2.5 parts of ammonium heptamolybdate (parts are calculated according to the mass of metal oxide) according to the loading amounts of 0.5%, 2.5% and 2.5% respectively, weighing a certain volume of deionized water according to the equal volume impregnation water absorption amount of 100 parts of titanium dioxide, adding the ammonium metavanadate, the ammonium metatungstate and the ammonium heptamolybdate into the deionized water, adding 1 part of monoethanolamine, and fully stirring to completely dissolve precursors of vanadium, tungsten and molybdenum; then, fully and uniformly mixing 100 parts of titanium dioxide obtained in the step S2 with the vanadium-tungsten-molybdenum mixed solution; drying the obtained wet material at 75 ℃ for 18h, and calcining at 500 ℃ for 9 h; and naturally cooling to obtain the sulfur-resistant electric denitration catalyst.
Example 3:
a preparation method of a sulfur poisoning resistant electric denitration catalyst comprises the following steps:
the parts mentioned in the present example are all parts by mass;
s1, taking 1 part of melamine and 100 parts of glycerol, fully stirring and mixing uniformly, adding 50 parts of titanium dioxide, stirring and mixing uniformly, drying by blowing at 150 ℃ for 24 hours, and calcining at 650 ℃ for 9 hours to obtain melamine modified titanium dioxide;
s2, taking 10 parts of melamine modified titanium dioxide according to Pr 6 O 11 The doping amount is 5 percent, and 0.5 part of praseodymium nitrate (by Pr) is added 6 O 11 By mass) is dissolved in deionized water with the volume required by equal volume of impregnation, and after the dissolution is completed, praseodymium nitrate aqueous solution and praseodymium nitrate aqueous solution are addedUniformly mixing the melamine modified titanium dioxide, drying at 200 ℃ for 12h, and finally calcining at 400 ℃ for 6h to obtain melamine modified praseodymium oxide doped titanium dioxide;
s3, according to V 2 O 5 、WO 3 、MoO 3 Weighing 0.1 part of ammonium metavanadate, 5 parts of ammonium metatungstate and 5 parts of ammonium heptamolybdate (the parts are calculated according to the mass of metal oxides) according to the loading amounts of 0.1%, 5% and 5%, weighing deionized water with a certain volume according to the equal volume soaking water absorption amount of 100 parts of titanium dioxide, adding the ammonium metavanadate, ammonium metatungstate and ammonium heptamolybdate into the deionized water, adding 0.05 part of monoethanolamine, and fully stirring to completely dissolve precursors of vanadium, tungsten and molybdenum; then, fully and uniformly mixing 100 parts of titanium dioxide obtained in the step S2 with the vanadium-tungsten-molybdenum mixed solution; drying the obtained wet material at 100 ℃ for 24h, and calcining at 450 ℃ for 12 h; and naturally cooling to obtain the sulfur-resistant electric denitration catalyst.
As shown in fig. 1, examples 1 to 3 and the conventional commercial power SCR denitration catalyst were tested for denitration efficiency under different temperature conditions under the following test conditions: the reaction temperature is 250 ℃, 300 ℃, 350 ℃, 400 ℃, the NO concentration is 500ppm, NH 3 Concentration 500ppm, O 2 3.5 percent, Ar is balance gas, and the gas volume space velocity is 50000h -1 ；
The test results show that compared with the traditional commercial power SCR denitration catalyst, the denitration catalyst prepared in the examples 1 to 3 has obviously better denitration efficiency and wider applicable temperature range in the temperature range of 250-300 ℃.
As shown in fig. 2, sulfur resistance tests were performed on examples 1 to 3 and a conventional commercial power SCR denitration catalyst; the test conditions were: the reaction temperature was 250 ℃, the NO concentration was 500ppm, NH 3 Concentration 500ppm, SO 2 Concentration 2000ppm (when required), O 2 3.5 percent, Ar is balance gas, and the gas volume space velocity is 50000h -1 ；
The test results show that the denitration catalysts prepared in examples 1 to 3 have stronger sulfur resistance than the conventional commercial power SCR denitration catalyst.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (9)
1. The preparation method of the sulfur poisoning resistant electric denitration catalyst is characterized by comprising the following steps of:
s1, uniformly mixing melamine and an alcohol solvent, and then adding titanium dioxide into the mixture for uniform mixing; the mixture of the three is dried and then calcined at high temperature in air atmosphere to obtain the melamine modified titanium dioxide
S2, designing a loading capacity according to the active components of the catalyst, dissolving the rare earth metal nitrate in water, then impregnating the aqueous solution of the rare earth metal nitrate into the melamine modified titanium dioxide in S1 according to an isometric impregnation method, drying the impregnated material, and calcining the dried material at a high temperature in an air atmosphere to obtain the melamine modified titanium dioxide pre-loaded rare earth metal oxide;
s3, according to the loading capacity of the active components of the catalyst, mixing ammonium metavanadate, ammonium metatungstate and ammonium heptamolybdate with water and monoethanolamine, heating and dissolving, then mixing the mixed solution of vanadium, tungsten and molybdenum with the melamine modified titanium dioxide pre-loaded rare earth metal oxide obtained in the step S2 according to the proportion of equal-volume impregnation, uniformly stirring, drying the obtained wet material, and calcining at high temperature to obtain the sulfur-resistant electric denitration catalyst.
2. The method of claim 1, wherein the alcohol solvent in S1 is ethanol, ethylene glycol or glycerol.
3. The preparation method of the sulfur poisoning resistance electric denitration catalyst as claimed in claim 1, wherein in the S1, the mass ratio of melamine to the alcohol solvent to the titanium dioxide is (1-5): 100: 50.
4. the method for preparing the sulfur poisoning resistance electric denitration catalyst as claimed in claim 1, wherein in the step S1, the drying temperature is 60-200 ℃, and the drying time is 6-24 h; the calcination temperature is 450-650 ℃, and the calcination time is 6-12 h;
in the S2, the drying temperature is 100-200 ℃, and the drying time is 6-12 h; the calcination temperature is 200-400 ℃, and the calcination time is 6-12 h;
in the S3, the drying temperature is 50-100 ℃, and the drying time is 12-24 h; the calcination temperature is 450-600 ℃, and the calcination time is 6-12 h.
5. The method as claimed in claim 1, wherein the rare earth metal nitrate in S2 is cerium nitrate, lanthanum nitrate or praseodymium nitrate.
6. The preparation method of the sulfur poisoning resistance electric denitration catalyst according to claim 1, wherein in the S2, the mass ratio of the rare earth metal nitrate to the melamine modified titanium dioxide is (1-10): 100.
7. the method according to claim 1, wherein in the step S3, the mass ratio of the ammonium metavanadate, the ammonium metatungstate, the ammonium heptamolybdate and the melamine modified titanium dioxide pre-loaded rare earth metal oxide is as follows: (0.1-1): (1-5): (1-5): 100.
8. the method for preparing the sulfur poisoning resistance electric denitration catalyst according to claim 1, wherein in the S3, the mass ratio of the melamine modified titanium dioxide pre-loaded rare earth metal oxide to the monoethanolamine is as follows: (0.05-1): 100.
9. an anti-sulfur poisoning electrical denitration catalyst prepared using the method of any one of claims 1 to 8.
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| CN202210886129.1A CN115041217A (en) | 2022-07-26 | 2022-07-26 | Preparation method of sulfur poisoning resistant electric denitration catalyst |
| PCT/CN2023/105995 WO2024022073A1 (en) | 2022-07-26 | 2023-07-06 | Preparation method for sulfur poisoning-resistant electric denitration catalyst |
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| WO2024022073A1 (en) * | 2022-07-26 | 2024-02-01 | 安徽元琛环保科技股份有限公司 | Preparation method for sulfur poisoning-resistant electric denitration catalyst |
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| CN103252231B (en) * | 2013-05-02 | 2015-05-06 | 易能（马鞍山）大气治理科技有限公司 | Denitration catalyst and preparation method thereof |
| CN105817220B (en) * | 2016-05-03 | 2019-06-11 | 展宗城 | A kind of rare earth modified sulfur resistive low-temperature SCR catalyst and preparation method thereof |
| CN110508273A (en) * | 2019-07-26 | 2019-11-29 | 华侨大学 | A kind of low temperature vanadium titanium-based SCR denitration and preparation method thereof |
| WO2021226052A1 (en) * | 2020-05-06 | 2021-11-11 | Basf Corporation | Control of sox emissions during catalyst manufacture |
| CN112495369B (en) * | 2020-11-22 | 2023-03-10 | 浙江盛旺环境工程有限公司 | Medium-low temperature vanadium-tungsten titanium-based SCR denitration catalyst and preparation method thereof |
| KR102438438B1 (en) * | 2020-11-25 | 2022-09-01 | 한서대학교 산학협력단 | Low Temperature SCR Catalyst for Treating of the Exhaust Gas from a Fixed Source and Preparation Method Thereof |
| CN113522272B (en) * | 2021-08-18 | 2023-06-20 | 大唐南京环保科技有限责任公司 | Denitration catalyst and preparation method thereof |
| CN114011449A (en) * | 2021-10-14 | 2022-02-08 | 安徽元琛环保科技股份有限公司 | Method for preparing heavy/alkali metal poisoning-resistant denitration catalyst by doping modification of nitrogen-containing organic matter and modified denitration catalyst |
| CN115041217A (en) * | 2022-07-26 | 2022-09-13 | 安徽元琛环保科技股份有限公司 | Preparation method of sulfur poisoning resistant electric denitration catalyst |
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| WO2024022073A1 (en) * | 2022-07-26 | 2024-02-01 | 安徽元琛环保科技股份有限公司 | Preparation method for sulfur poisoning-resistant electric denitration catalyst |
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