CN113750986A - Preparation method and application of vanadium-titanium-based catalyst - Google Patents

Preparation method and application of vanadium-titanium-based catalyst Download PDF

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CN113750986A
CN113750986A CN202111225685.6A CN202111225685A CN113750986A CN 113750986 A CN113750986 A CN 113750986A CN 202111225685 A CN202111225685 A CN 202111225685A CN 113750986 A CN113750986 A CN 113750986A
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titanium dioxide
vanadium
ultrapure water
catalyst
ascorbic acid
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CN113750986B (en
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王晓祥
李伟
李蓓蕾
李素静
魏童
文渝策
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Zhejiang University ZJU
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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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Abstract

The invention discloses a preparation method and application of a vanadium-titanium based catalyst, and relates to the technical field of catalysts. Dissolving ascorbic acid in ultrapure water, stirring for 30min, dispersing 1g of titanium dioxide in 350ml of ascorbic acid aqueous solution, continuously stirring for 8h to obtain emulsion, cleaning the titanium dioxide filtered from the emulsion to be neutral by using the ultrapure water, and drying for 12h in a vacuum environment at 100 ℃ to obtain the modified rutile titanium dioxide carrier. Dissolving ammonium metavanadate in ultrapure water at the temperature of 50-70 ℃ to obtain a mixed solution, adding the modified rutile titanium dioxide carrier, stirring for 8-12 h to obtain a mixture, and drying the mixture for 12h in a vacuum environment at the temperature of 100 ℃. Calcining the dried substance for 4 hours at 550 ℃ in an air atmosphere to obtain a catalyst; thereby solving the problem of catalyst deactivation phenomenon caused by high-temperature phase change of anatase titanium dioxide which is difficult to be fundamentally solved in the prior art.

Description

Preparation method and application of vanadium-titanium-based catalyst
Technical Field
The invention relates to the technical field of catalysts, in particular to a preparation method and application of a vanadium-titanium based catalyst.
Background
TiO2Is of Al2O3And SiO2The third generation catalyst carrier begins in the seventies of the twentieth century, and the crystal forms of the third generation catalyst carrier mainly comprise anatase, brookite and rutile, wherein the anatase is the main active crystal form. Vanadium titanium catalyst (V)2O5-WO3/TiO2Or V2O5-MoO3/TiO2) Was applied in the 20 th century in Japan for the selective catalytic reduction of NH3During SCR denitration reaction, the catalyst has high-efficiency NO at 300-400 DEG CxAnd (4) conversion capacity. However, containing NOxThe flue gas/tail gas temperature change range is wide, especially under different operation conditions of the tail gas of the mobile diesel vehicle, the temperature can reach six to seven hundred degrees centigrade, and strict requirements are provided for the stability of the catalyst. When the temperature of the flue gas/tail gas is too high, the crystal structure of the catalyst is changed, the framework of the catalyst collapses, and the catalyst is permanently inactivated, so that the service life of the catalyst is greatly shortened. Since the development, vanadium-titanium catalysts have received wide attention from the industry and scientific research community: the industry has been making efforts to develop new catalysts that can replace vanadium-titanium catalysts, and the scientific research has been making efforts to provide meaningful scientific reasoning about the application and development of catalysts by analyzing the surface reaction mechanism of vanadium-titanium catalysts.
At present, there are two main methods for improving the poor thermal stability of the anatase vanadium-titanium catalyst: one is from catalyst supports, i.e. titania, generally by replacing the anatase titania support with a more stable support such as alumina, silica, etc.; in addition, the stability of the carrier can also be enhanced by adding other components in the catalyst, for example, niobium oxide and silicon oxide are doped in an anatase titanium dioxide bulk phase to realize the high-temperature stability of the carrier; the other is to replace vanadium oxide with other active metal oxides (such as iron oxide, copper oxide, etc.) to weaken the effect of anatase high temperature sintering from the active components of the catalyst. The anatase titanium dioxide is replaced by other carriers with better stability, although the defect of poor carrier stability is avoided to a certain extent, the larger specific surface area and better sulfur dioxide poisoning resistance of the anatase titanium dioxide are abandoned, and the replaced other carriers are difficult to simultaneously meet the advantages and the characteristic of good stability of the anatase. For the stability of anatase titanium dioxide enhanced by doping other metals in the carrier, the composition of the catalyst is complicated, and great difficulty is brought to mechanism research, so that the challenge is brought to the further popularization and application of the catalyst. The vanadium oxide species is replaced, so that the defect of high-temperature phase change of anatase titanium dioxide cannot be fundamentally solved, and phase change inactivation still occurs under extreme conditions.
Therefore, how to solve the problem of catalyst deactivation caused by high temperature phase transition of anatase titanium dioxide, which is difficult to be solved fundamentally in the prior art, is an important technical problem to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to provide a preparation method of a vanadium-titanium-based catalyst and an application of the vanadium-titanium-based catalyst to solve the technical problem that the deactivation phenomenon of the catalyst caused by high-temperature phase change of anatase titanium dioxide is difficult to fundamentally solve in the prior art. The technical effects that can be produced by the preferred technical scheme in the technical schemes provided by the invention are described in detail in the following.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation method and application of a vanadium-titanium based catalyst, which are characterized in that a carrier of the vanadium-titanium based catalyst is rutile titanium dioxide, the surface of the rutile titanium dioxide is modified by ascorbic acid, and ammonium metavanadate is taken as a precursor to load V on the surface of the modified carrier2O5Thereby preparing V2O5/TiO2The catalyst is prepared by the following specific preparation method:
s1, dissolving the ascorbic acid in ultrapure water, and stirring for 30min to obtain an ascorbic acid aqueous solution;
s2, dispersing 1g of titanium dioxide into 350ml of ascorbic acid aqueous solution, and continuously stirring for 8 hours to obtain emulsion;
s3, filtering the emulsion and filtering out the titanium dioxide;
s4, cleaning the titanium dioxide filtered out in the step S3 to be neutral by using the ultrapure water;
s5, drying the titanium dioxide washed to be neutral in the S4 for 12 hours in a vacuum environment at 100 ℃ to prepare a modified rutile titanium dioxide carrier;
s6, dissolving the ammonium metavanadate in the ultrapure water at the temperature of 50-70 ℃ to obtain a mixed solution;
s7, adding the modified rutile titanium dioxide carrier into the mixed solution in S6, and stirring for 8-12 h to obtain a mixture;
s8, drying the mixture in the S7 for 12 hours at 100 ℃ in a vacuum environment;
s9, calcining the dried substance in the S8 for 4h at 550 ℃ in an air atmosphere to obtain the catalyst.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the ratio of the ascorbic acid to the ultrapure water in S1 is: 1mg of the ascorbic acid corresponds to 1ml of the ultrapure water.
Further, the ammonium metavanadate and the modified rutile titanium dioxide carrier are used in amounts which meet the requirement of finally preparing V2O5/TiO2The mass fraction of V in the catalyst is 0-5%.
Further, the temperature of the ultrapure water in S6 was 60 ℃.
The catalyst prepared in the preparation method of the vanadium titanium-based catalyst is NH3Selective catalytic reduction of NOxUse in a reaction process, the NH3And said NOxThe concentration of (2) was 500 ppm.
The technical scheme provided by the application comprises the following beneficial effects:
the present invention providesIn the technical scheme, the preparation method and the application of the vanadium-titanium based catalyst are characterized in that rutile titanium dioxide is selected as a carrier of the vanadium-titanium based catalyst, the surface modification of the rutile titanium dioxide is carried out by using ascorbic acid, and ammonium metavanadate is taken as a precursor to load V on the surface of the modified carrier2O5Thereby preparing V2O5/TiO2The catalyst is prepared by the following specific preparation method: dissolving ascorbic acid in ultrapure water, stirring for 30min to obtain an ascorbic acid aqueous solution, dispersing 1g of titanium dioxide in 350ml of the ascorbic acid aqueous solution, continuously stirring for 8h to obtain an emulsion, filtering the emulsion, filtering out the titanium dioxide, cleaning the titanium dioxide filtered out in S3 to be neutral by using the ultrapure water, drying the titanium dioxide cleaned to be neutral in S4 in a vacuum environment at 100 ℃ for 12h to obtain a modified rutile titanium dioxide carrier, dissolving ammonium metavanadate in the ultrapure water at 50-70 ℃ to obtain a mixed solution, adding the modified rutile titanium dioxide carrier into the mixed solution in S6, stirring for 8h-12h to obtain a mixture, drying the mixture in S7 in the vacuum environment at 100 ℃ for 12h, and calcining the dried substance in S8 in the air atmosphere at 550 ℃ for 4h to obtain the catalyst. So arranged, the inert rutile titanium dioxide is modified to synthesize better NH3The rutile phase is a crystal phase of titanium dioxide stably existing at high temperature, anatase is easily converted into the rutile phase at high temperature, and the pure rutile phase has no reaction activity, so that the rutile phase titanium dioxide has catalytic activity while the high-temperature crystal phase of the titanium dioxide is prevented from being converted, and the defect of the high-temperature crystal phase conversion of the anatase titanium dioxide is fundamentally solved; thereby solving the problem of catalyst deactivation phenomenon caused by high-temperature phase change of anatase titanium dioxide which is difficult to be fundamentally solved in the prior art.
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 shows rutile V before and after modification2O5/TiO2Catalyst in NH3NO in SCR reactionsxComparing the conversion rate;
FIG. 2 shows rutile V before and after modification2O5/TiO2Catalyst in NH3N in SCR reaction2And (6) selective comparison.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The purpose of the present embodiment is to provide a preparation method and application of a vanadium titanium based catalyst; thereby solving the problem of catalyst deactivation phenomenon caused by high-temperature phase change of anatase titanium dioxide which is difficult to be fundamentally solved in the prior art.
Hereinafter, embodiments will be described with reference to the drawings. The embodiments described below do not limit the contents of the invention described in the claims. The entire contents of the configurations shown in the following embodiments are not limited to those required as solutions of the inventions described in the claims.
Referring to fig. 1-2, this embodiment provides a preparation method and an application of a vanadium-titanium based catalyst, in which rutile titanium dioxide is used as a carrier of the vanadium-titanium based catalyst, the rutile titanium dioxide is surface-modified with ascorbic acid, and ammonium metavanadate is used as a precursor to load V on the surface of the modified carrier2O5Thereby preparing V2O5/TiO2The catalyst is prepared by the following specific preparation method: dissolving ascorbic acid in ultrapure water, stirring for 30min to obtain ascorbic acid waterDispersing 1g of titanium dioxide into 350ml of ascorbic acid aqueous solution, continuously stirring for 8h to obtain emulsion, filtering the titanium dioxide, cleaning the titanium dioxide filtered out from S3 to be neutral by using ultrapure water, drying the titanium dioxide cleaned to be neutral in S4 in a vacuum environment at 100 ℃ for 12h to obtain a modified rutile titanium dioxide carrier, dissolving ammonium metavanadate in the ultrapure water at 50-70 ℃ to obtain a mixed solution, adding the modified rutile titanium dioxide carrier into the mixed solution in S6, stirring for 8h-12h to obtain a mixture, drying the mixture in S7 in the vacuum environment at 100 ℃ for 12h, and calcining the dried substance in S8 in an air atmosphere at 550 ℃ for 4h to obtain the catalyst.
So arranged, the inert rutile titanium dioxide is modified to synthesize better NH3The rutile phase is a crystal phase of titanium dioxide stably existing at high temperature, anatase is easily converted into the rutile phase at high temperature, and the pure rutile phase has no reaction activity, so that the rutile phase titanium dioxide has catalytic activity while the high-temperature crystal phase of the titanium dioxide is prevented from being converted, and the defect of the high-temperature crystal phase conversion of the anatase titanium dioxide is fundamentally solved; thereby solving the problem of catalyst deactivation phenomenon caused by high-temperature phase change of anatase titanium dioxide which is difficult to be fundamentally solved in the prior art.
As an alternative embodiment, the ratio of ascorbic acid to ultrapure water in S1 can be set according to the specific use environment, and in this embodiment, the ratio of ascorbic acid to ultrapure water is preferably 1mg ascorbic acid to 1ml ultrapure water.
As an alternative embodiment, the usage amounts of the ammonium metavanadate and the modified rutile titanium dioxide carrier can be set according to specific usage environments, and in this embodiment, the usage amounts of the ammonium metavanadate and the modified rutile titanium dioxide carrier should satisfy the finally obtained V2O5/TiO2The mass fraction of V in the catalyst is 0-5%.
As an alternative embodiment, the temperature of the ultrapure water in S6 can be set according to the specific use environment, and the temperature of the ultrapure water in this embodiment is preferably 60 ℃.
Application of catalyst prepared in preparation method of vanadium titanium-based catalyst in NH3Selective catalytic reduction of NOxDuring the reaction, NH in this example3And NOxIs preferably 500ppm, and is preferably 5% volume fraction O2，N2As a carrier gas, the reaction temperature is preferably 100 ℃ to 500 ℃.
NOxConversion and N2Selectivity is the investigation of NH3Two main indexes of SCR catalyst performance, as can be seen by combining FIG. 1 and FIG. 2, the modified rutile vanadium titanium catalyst has better reaction activity, and the modified vanadium titanium catalyst maintains NO less than 80% of NO in a wide temperature range of 225-425 DEG CxConversion and N of 97% or more2And (4) selectivity.
In the description of the present invention, it is to be understood that the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, are merely for convenience of description of the present invention, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (5)

1. A preparation method of a vanadium-titanium based catalyst is characterized in that a carrier of the vanadium-titanium based catalyst is rutile titanium dioxide, the surface of the rutile titanium dioxide is modified by ascorbic acid, and ammonium metavanadate is taken as a precursor on the surface of the modified carrierSurface load V2O5Thereby preparing V2O5/TiO2The catalyst is prepared by the following specific preparation method:
s1, dissolving the ascorbic acid in ultrapure water, and stirring for 30min to obtain an ascorbic acid aqueous solution;
s2, dispersing 1g of titanium dioxide into 350ml of ascorbic acid aqueous solution, and continuously stirring for 8 hours to obtain emulsion;
s3, filtering the emulsion and filtering out the titanium dioxide;
s4, cleaning the titanium dioxide filtered out in the step S3 to be neutral by using the ultrapure water;
s5, drying the titanium dioxide washed to be neutral in the S4 for 12 hours in a vacuum environment at 100 ℃ to prepare a modified rutile titanium dioxide carrier;
s6, dissolving the ammonium metavanadate in the ultrapure water at the temperature of 50-70 ℃ to obtain a mixed solution;
s7, adding the modified rutile titanium dioxide carrier into the mixed solution in S6, and stirring for 8-12 h to obtain a mixture;
s8, drying the mixture in the S7 for 12 hours at 100 ℃ in a vacuum environment;
s9, calcining the dried substance in the S8 for 4h at 550 ℃ in an air atmosphere to obtain the catalyst.
2. The method for preparing a vanadium-titanium based catalyst according to claim 1, wherein the ratio of the ascorbic acid to the ultrapure water in S1 is: 1mg of the ascorbic acid corresponds to 1ml of the ultrapure water.
3. The method for preparing a vanadium-titanium based catalyst according to claim 1, wherein the ammonium metavanadate and the modified rutile titania support are used in amounts such that V to be finally produced is satisfied2O5/TiO2The mass fraction of V in the catalyst is 0-5%.
4. The method for preparing a vanadium-titanium based catalyst according to claim 1, wherein the temperature of the ultrapure water in S6 is 60 ℃.
5. The catalyst prepared in the method for preparing a vanadium-titanium based catalyst according to any one of claims 1 to 4 in NH3Selective catalytic reduction of NOxUse in a reaction process, the NH3And the concentration of NOx is 500 ppm.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN204656555U (en) * 2014-01-14 2015-09-23 京程科技股份有限公司 Structure of vanadium oxide-titanium dioxide photocatalyst film
CN110013841A (en) * 2019-04-23 2019-07-16 上海理工大学 A kind of two dimension titanium dioxide nanosheet photocatalytic material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN204656555U (en) * 2014-01-14 2015-09-23 京程科技股份有限公司 Structure of vanadium oxide-titanium dioxide photocatalyst film
CN110013841A (en) * 2019-04-23 2019-07-16 上海理工大学 A kind of two dimension titanium dioxide nanosheet photocatalytic material and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
DIPTIPRIYA SETHI等: ""Photocatalytic destruction of Escherichia coli in water by V2O5/TiO2"", JOURNAL OF PHOTOCHEMISTRY AND PHOTOBIOLOGY B: BIOLOGY, vol. 144, pages 68 *
E. HILAL MERT等: ""Surface Modification of TiO2 with Ascorbic Acid for Heterogeneous Photocatalysis: Theory and Experiment"", J. ADV. OXID. TECHNOL., vol. 11, no. 2, pages 199 - 207 *
WEI ZHAO等: ""Ti3+ doped V2O5/TiO2 catalyst for efficient selective catalytic reduction of NOx with NH3"", JOURNAL OF COLLOID AND INTERFACE SCIENCE, vol. 581, pages 76, XP086321634, DOI: 10.1016/j.jcis.2020.07.131 *

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