CN114849695A - Low-temperature wide-temperature active SCR denitration catalyst and preparation method thereof - Google Patents
Low-temperature wide-temperature active SCR denitration catalyst and preparation method thereof Download PDFInfo
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- CN114849695A CN114849695A CN202210690414.6A CN202210690414A CN114849695A CN 114849695 A CN114849695 A CN 114849695A CN 202210690414 A CN202210690414 A CN 202210690414A CN 114849695 A CN114849695 A CN 114849695A
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- 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
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- 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
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Abstract
The invention discloses a low-temperature wide-temperature active SCR denitration catalyst which is characterized by comprising TiO 2 As a carrier, WO 3 As an anti-poisoning component, with V 2 O 5 As an active component, Nb with strong redox ability is used as a low-temperature wide-temperature active additive element to prepare a catalyst; the said WO 3 On the support of TiO 2 In a mass fraction of 0-8%, V 2 O 5 On the support of TiO 2 The mass fraction of the additive element is 4-20%, and the molar ratio of the additive element Nb to V is 0:1-1: 0; the addition source of Nb is one or more of niobium pentoxide, niobium oxalate and industrial niobium oxalate. The low-temperature wide-temperature active SCR denitration catalyst provided by the invention is simple in preparation method, is suitable for practical application of industrial production activities, can effectively remove nitrogen oxides in flue gas and prevent nitrogen oxidesCausing harm to the environment and organisms. The denitration efficiency of the prepared catalyst can reach more than 90% at a low temperature of 180-300 ℃, and the denitration efficiency can be improved to more than 97% by doping certain Nb sources.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a low-temperature wide-temperature active SCR denitration catalyst and a preparation method thereof.
Background
The nitrogen oxide is one of main pollutants in the atmosphere, threatens biological health, has a large emission ratio of industrial nitrogen oxide, and is the most urgent emission reduction object in the atmospheric pollutants.
The Selective Catalytic Reduction (SCR) is a mature and easy-to-use method for reducing the emission of nitrogen oxides at present, and is widely applied internationally. The SCR denitration technology is characterized in that a reducing agent (ammonia, carbon monoxide and the like) and nitric oxide are introduced into a reactor together at a lower temperature range under the condition of oxygen and the action of a catalyst, and the nitric oxide in flue gas is selectively reduced into N 2 And H 2 O reduces the emission of nitrogen oxide, and the denitration efficiency can reach 80-90%. The most mature commercial SCR catalytic system is TiO 2 As a carrier, WO 3 As an anti-poisoning component, with V 2 O 5 Vanadium-based catalysts, which are active ingredients, have been widely used in the electrical industry, with operating temperatures of 300 ℃ to 400 ℃. However, industrial kilns (such as cement kilns, metallurgical furnaces for steel, coking plants, etc.) are not used in the electrical industry. The temperature of the flue gas is generally in the range of 120-300 ℃, and the flue gas conditions are more complex compared with the power industry, so that the commercial catalyst is difficult to meet the use requirements. And the low-temperature catalyst can reduce the secondary temperature rise of the flue gas as much as possible, and the cost is reduced, so the low-temperature catalyst has great practical significance for the research of the low-temperature field of the catalyst.
In order to solve the problems, the invention provides an SCR denitration catalyst and a preparation method thereof.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a low-temperature wide-temperature active SCR denitration catalyst and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: the low-temperature wide-temperature active SCR denitration catalyst is characterized by comprising TiO 2 As a carrier, WO 3 As an anti-poisoning component, with V 2 O 5 As an active component, Nb with strong oxidation-reduction capability is used as a low-temperature wide-temperature active additive element to prepare the catalyst.
Further, the method comprisesWO to 3 On the support of TiO 2 In a mass fraction of 0-8%, V 2 O 5 On the support of TiO 2 The mass fraction of the additive element is 4-20%, and the molar ratio of the additive element Nb to V is 0:1-1: 0.
Further, the addition source of Nb is one or more of niobium pentoxide, niobium oxalate and industrial niobium oxalate.
The preparation method of the low-temperature wide-temperature active SCR denitration catalyst comprises the following steps:
step 1, dissolving additives of vanadium-based salt, tungsten-based salt and different Nb sources in deionized water to obtain an active component solution;
step 2, adding TiO 2 Putting the powder into the active component solution prepared in the step 1, heating and stirring to fully and uniformly mix the active component and the carrier, and continuously volatilizing the moisture until the moisture is completely volatilized to form a dry material mass;
step 3, crushing and grinding the material mass obtained in the step 2 into powder without large particles and with uniform particles;
step 4, adding a proper amount of deionized water into the powder obtained in the step 3, kneading the powder into a mud mass with uniform hardness, putting the mud mass into a catalyst extruder, carrying out extrusion forming on the mud mass, and drying the mud mass to obtain a bar-shaped catalyst precursor blank;
and 5, calcining the blank obtained in the step 4 to obtain the low-temperature wide-temperature active SCR denitration catalyst.
Further, in step 1, the vanadium-based salt is ammonium metavanadate, and the tungsten-based salt is ammonium tungstate; in the step 2, the heating temperature is 60-120 ℃, and the heating time is 6-24 h.
Further, in step 3, the crushing and grinding comprises ball milling and mortar grinding; in the step 4, the viscosity of the prepared mud dough can be adjusted according to different extrusion equipment, and extrusion into strips is continuous and uninterrupted.
Further, in the step 5, the temperature rising rate of the blank during calcination is 2-10 ℃/min, the calcination temperature is 300-900 ℃, and the calcination time is 1-6 h.
Furthermore, the heating rate of the blank during calcination is 5 ℃/min, and the calcination temperature can be optimized to 550 ℃.
Further, the application of the low-temperature wide-temperature active SCR denitration catalyst in removing nitrogen oxides in flue gas is provided.
Further, the simulated flue gas temperature of the flue gas is 120-300 ℃, and NH in the flue gas 3 ：NO＝1:1，O 2 The content of (B) is 5 percent, and the space velocity is 20000m 3 /h。
Compared with the prior art, the invention has the advantages that: the low-temperature wide-temperature active SCR denitration catalyst provided by the invention is simple in preparation method, is suitable for practical application of industrial production activities, can effectively remove nitrogen oxides in flue gas, and prevents the nitrogen oxides from causing harm to environment and organisms. The denitration efficiency of the prepared catalyst can reach more than 90% at a low temperature of 180-300 ℃, and the denitration efficiency can be improved to more than 97% by doping certain Nb sources.
Drawings
FIG. 1 is a flow chart of the preparation of the low-temperature wide-temperature active SCR denitration catalyst provided by the invention.
FIG. 2 is a graph showing the relationship between denitration performance and temperature for different Nb source additives and different Nb contents in the embodiment of the present invention.
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings.
The following embodiments of the present invention employ a commercial standard gas (N) 2 、NH 3 、NO、O 2 ) Forming simulated smoke to simulate smoke in industry, wherein the simulated smoke is N 2 (balance gas, 99.999%), O 2 (99.999％)、NO/N 2 Standard gas (2% NO) and NH 3 /N 2 Standard gas (2% NH) 3 ) Mixing the components. The total flow rate of the flue gas is 880ml/min, wherein the total flow rate of NO is 20ml/min and NH 3 20ml/min、O 2 40ml/min、N 2 800 ml/min. . The method for measuring the denitration efficiency comprises the following steps: the prepared catalyst is placed in the middle of the quartz tube, the lower portion of the quartz tube is plugged by cotton to prevent the catalyst from falling off, the quartz tube is heated to a specific temperature, then simulated flue gas is introduced, a flue gas analyzer is used for measuring the concentration of NO at the inlet and the outlet of the quartz tube, and the denitration rate is obtained through calculation. The specific calculation formula of the denitration efficiency is as follows:
Example 1
A preparation method of a low-temperature wide-temperature active SCR denitration catalyst comprises the following steps:
3.673g of ammonium metavanadate, 1.312g of ammonium tungstate and 4.179g of niobium pentoxide were dissolved in 200ml of ionic water to obtain active component solutions, and 40g of TiO was added 2 Putting the powder into the active component solution, heating and stirring at 90 ℃ to fully and uniformly mix the active component and the carrier and volatilize water into dry material mass. And crushing the material mass by using a mortar, grinding the material mass into powder without large particles and with uniform particles, adding a proper amount of deionized water into the powder, kneading the powder into a mud mass with uniform hardness, putting the mud mass into a catalyst extruder, carrying out extrusion molding, drying to obtain a bar-shaped catalyst precursor blank, and calcining the blank at 550 ℃ for 4 hours to obtain the low-temperature wide-temperature active SCR denitration catalyst.
The obtained low-temperature wide-temperature active SCR denitration catalyst is recorded as 1Nb 1V-niobium pentoxide, wherein the molar ratio of Nb to V is 1: 1.
The denitration performance of the catalyst of the embodiment is measured by using simulated flue gas, and the denitration efficiency at different temperatures is shown in fig. 2. As can be seen from fig. 2: the denitration efficiency of the 1Nb 1V-niobium pentoxide catalyst can be stabilized at more than 90% at the temperature of 180 ℃ and 300 ℃.
3.673g of ammonium metavanadate, 1.312g of ammonium tungstate and 16.916g of niobium oxalate are respectively dissolved in 200ml of ionized water to obtain active component solutions, and 40g of TiO is added 2 Putting the powder into the active component solution, heating and stirring at 90 ℃ to fully and uniformly mix the active component and the carrier and volatilize water into dry material mass. Crushing the material mass by using a mortar, grinding the material mass into powder without large particles and with uniform particles, adding a proper amount of deionized water into the powder, kneading the powder into mud mass with uniform hardness, putting the mud mass into a catalyst extruder, carrying out extrusion molding, drying to obtain a bar-shaped catalyst precursor blank body, and drying the blank bodyAnd calcining the blank body for 4 hours at 550 ℃ to obtain the low-temperature wide-temperature active SCR denitration catalyst.
The obtained low-temperature wide-temperature active SCR denitration catalyst is recorded as 1Nb 1V-niobium oxalate, wherein the molar ratio of Nb to V is 1: 1.
The denitration performance of the catalyst of the embodiment is measured by using simulated flue gas, and the denitration efficiency at different temperatures is shown in fig. 2. As can be seen from fig. 2: the denitration efficiency of the 1Nb 1V-niobium oxalate catalyst can be stabilized at 270 ℃ at 180 ℃, and the denitration efficiency can be stabilized at 99.3% at 240 ℃ at 210 ℃.
3.673g of ammonium metavanadate, 1.312g of ammonium tungstate and 16.916g of industrial niobium oxalate are respectively dissolved in 200ml of ionized water to obtain active component solution, and 40g of TiO is added 2 Putting the powder into the active component solution, heating and stirring at 90 ℃ to fully and uniformly mix the active component and the carrier and volatilize water into dry material mass. And crushing the material mass by using a mortar, grinding the material mass into powder without large particles and with uniform particles, adding a proper amount of deionized water into the powder, kneading the powder into a mud mass with uniform hardness, putting the mud mass into a catalyst extruder, carrying out extrusion molding, drying to obtain a bar-shaped catalyst precursor blank, and calcining the blank at 550 ℃ for 4 hours to obtain the low-temperature wide-temperature active SCR denitration catalyst.
The obtained low-temperature wide-temperature active SCR denitration catalyst is recorded as 1Nb 1V-industrial niobium oxalate, wherein the molar ratio of Nb to V is 1: 1.
The denitration performance of the catalyst of the embodiment was measured by using simulated flue gas, and the denitration efficiency at different temperatures is shown in fig. 2. As can be seen from fig. 2: the denitration efficiency of the 1Nb 1V-industrial niobium oxalate catalyst can be stabilized at 300 ℃ at 210-.
The present invention and the embodiments thereof have been described above, and the description is not restrictive, and the embodiments shown in the detailed description are only a part of the embodiments of the present invention, not all embodiments, and the actual configuration is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The low-temperature wide-temperature active SCR denitration catalyst is characterized by comprising TiO 2 As a carrier, WO 3 As an anti-toxic component, with V 2 O 5 As an active component, Nb with strong oxidation-reduction capability is used as a low-temperature wide-temperature active additive element to prepare the catalyst.
2. The low-temperature wide-temperature active SCR denitration catalyst as set forth in claim 1, wherein the WO is 3 TiO as carrier 2 In a mass fraction of 0-8%, V 2 O 5 On the support of TiO 2 The mass fraction of the additive element is 4-20%, and the molar ratio of the additive element Nb to V is 0:1-1: 0.
3. The low-temperature wide-temperature active SCR denitration catalyst according to claim 1, wherein the Nb is added from one or more of niobium pentoxide, niobium oxalate and industrial niobium oxalate.
4. The low-temperature wide-temperature active SCR denitration catalyst as set forth in claim 1, which comprises the following preparation method:
step 1, dissolving additives of vanadium-based salt, tungsten-based salt and different Nb sources in deionized water to obtain an active component solution;
step 2, adding TiO 2 Putting the powder into the active component solution prepared in the step 1, heating and stirring to fully and uniformly mix the active component and the carrier, and continuously volatilizing the moisture until the moisture is completely volatilized to form a dry material mass;
step 3, crushing and grinding the material mass obtained in the step 2 into powder without large particles and with uniform particles;
step 4, adding a proper amount of deionized water into the powder obtained in the step 3, kneading the powder into a mud mass with uniform hardness, putting the mud mass into a catalyst extruder, carrying out extrusion forming on the mud mass, and drying the mud mass to obtain a bar-shaped catalyst precursor blank;
and 5, calcining the blank obtained in the step 4 to obtain the low-temperature wide-temperature active SCR denitration catalyst.
5. The low-temperature wide-temperature active SCR denitration catalyst according to claim 4, wherein in the step 1, the vanadium-based salt is ammonium metavanadate, and the tungsten-based salt is ammonium tungstate; in the step 2, the heating temperature is 60-120 ℃, and the heating time is 6-24 h.
6. The low-temperature wide-temperature active SCR denitration catalyst as set forth in claim 4, wherein in the step 3, the crushing and grinding comprises ball milling and mortar grinding; in the step 4, the viscosity of the prepared mud dough can be adjusted according to different extrusion equipment, and extrusion into strips is continuous and uninterrupted.
7. The low-temperature wide-temperature active SCR denitration catalyst as recited in claim 4, wherein in the step 5, the calcination temperature rise rate of the green body is 2-10 ℃/min, the calcination temperature is 300-900 ℃, and the calcination time is 1-6 h.
8. The low-temperature wide-temperature active SCR denitration catalyst as recited in claim 4, wherein a calcination temperature rise rate of the green body is 5 ℃/min, and a calcination temperature can be optimized to 550 ℃.
9. The low-temperature wide-temperature active SCR denitration catalyst according to any one of claims 1 to 3, wherein the low-temperature wide-temperature active SCR denitration catalyst is applied to removal of nitrogen oxides in flue gas.
10. The low-temperature wide-temperature active SCR denitration catalyst as recited in claim 9, wherein the simulated flue gas temperature of the flue gas is 120-300 ℃, and NH in the flue gas 3 ：NO＝1:1，O 2 The content of (B) is 5 percent, and the space velocity is 20000m 3 /h。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106807356A (en) * | 2017-01-24 | 2017-06-09 | 东南大学 | A kind of low temperature SCR denitration catalyst and its methods for making and using same |
| CN111203208A (en) * | 2020-01-09 | 2020-05-29 | 华侨大学 | Low-temperature vanadium titanium-based SCR denitration catalyst for promoting ABS decomposition and preparation method thereof |
| CN113457665A (en) * | 2021-06-22 | 2021-10-01 | 苏州西热节能环保技术有限公司 | Efficient low-temperature honeycomb type SCR denitration catalyst and preparation method thereof |
| US20220162970A1 (en) * | 2020-11-25 | 2022-05-26 | Hanseo University Academic Cooperation Foundation | LOW-TEMPERATURE DE-NOx CATALYST FOR TREATMENT OF EXHAUST GAS FROM STATIONARY SOURCE AND METHOD OF MANUFACTURING SAME |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106807356A (en) * | 2017-01-24 | 2017-06-09 | 东南大学 | A kind of low temperature SCR denitration catalyst and its methods for making and using same |
| CN111203208A (en) * | 2020-01-09 | 2020-05-29 | 华侨大学 | Low-temperature vanadium titanium-based SCR denitration catalyst for promoting ABS decomposition and preparation method thereof |
| US20220162970A1 (en) * | 2020-11-25 | 2022-05-26 | Hanseo University Academic Cooperation Foundation | LOW-TEMPERATURE DE-NOx CATALYST FOR TREATMENT OF EXHAUST GAS FROM STATIONARY SOURCE AND METHOD OF MANUFACTURING SAME |
| CN113457665A (en) * | 2021-06-22 | 2021-10-01 | 苏州西热节能环保技术有限公司 | Efficient low-temperature honeycomb type SCR denitration catalyst and preparation method thereof |
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