CN111068707A - Low-temperature denitration catalyst, preparation method and application - Google Patents
Low-temperature denitration catalyst, preparation method and application Download PDFInfo
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- CN111068707A CN111068707A CN201811230507.0A CN201811230507A CN111068707A CN 111068707 A CN111068707 A CN 111068707A CN 201811230507 A CN201811230507 A CN 201811230507A CN 111068707 A CN111068707 A CN 111068707A
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—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
- 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
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- 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
- 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
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention belongs to the field of chemical industry, and particularly discloses a low-temperature denitration catalyst, a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing the vanadium-free impregnation liquid with a carrier, carrying out wet grinding, carrying out spray drying and roasting on the uniformly ground slurry to obtain the low-temperature denitration catalyst; wherein the vanadium-free impregnation liquid contains a precursor of manganese. The invention realizes the deep loading of the active component by dipping and wet grinding the active component and the carrier, and simultaneously replaces the conventional washing, filtering, evaporating and drying by adopting the spray drying of the slurry, thereby simplifying the preparation process and greatly reducing the secondary pollution caused by a large amount of waste water generated in the preparation process.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a low-temperature denitration catalyst, and a preparation method and application thereof.
Background
Nitrogen oxides (NOx) are one of the main atmospheric pollutants, cause acid rain and photochemical smog, cause ozone layer damage, greenhouse effect, haze and other important primitive causes in severe weather, and can harm plant growth to cause respiratory diseases of human beings. Because the social problems caused by NOx emission are increasingly obvious, the national environmental protection agency puts forward more strict requirements on NOx emission reduction, the NOx emission standard is higher and higher, the research and development of the high-efficiency nitrogen oxide removal technology have important economic significance and social value, and the popularization and application of the high-efficiency denitration technology are imperative.
Ammonia selective catalytic reduction technology (NH)3SCR) is the most effective flue gas denitration technology in commercial application at present, and is widely applied to flue gas denitration of thermal power plants. NH (NH)3The core of the SCR denitration technology is a catalyst, and the current commercial denitration catalyst is a vanadium-titanium based catalyst, and the working temperature of the catalyst is generally 300-400 ℃. The nitrogen oxides discharged by industrial kilns in China, such as glass kilns, cement kilns and the like, also account for a large part of the discharge amount of the nitrogen oxides in China, are discharge sources second only to thermal power plants, the smoke temperature of the industrial kilns is relatively low, the working temperature of the industrial kilns is mostly between 150 ℃ and 250 ℃, and catalysts with low-temperature denitration activity are needed. The ethylene steam cracking furnace is used as the technical core of the ethylene industry, and the flue gas treatment of the ethylene steam cracking furnace is also suitable for using a low-temperature denitration technology.
The existing low-temperature denitration catalyst is prepared by adopting technical methods such as dipping, precipitation and the like, the preparation process involves operations such as liquid preparation, neutralization, washing, filtration, drying and the like, the process is complicated, and particularly a large amount of waste water and waste gas can be generated to pollute the environment. Therefore, how to obtain high catalytic activity at low temperature and simplify the preparation process and reduce pollution becomes a problem of attention and improvement required in the catalyst development process.
Disclosure of Invention
The invention aims to provide a low-temperature denitration catalyst, a preparation method and application thereof.
The invention provides a preparation method of a low-temperature denitration catalyst, which comprises the following steps: mixing the vanadium-free impregnation liquid with a carrier, carrying out wet grinding, carrying out spray drying and roasting on the uniformly ground slurry to obtain the low-temperature denitration catalyst; wherein the vanadium-free impregnation liquid contains a precursor of manganese.
The second aspect of the present invention provides a low-temperature denitration catalyst prepared by the above method.
The third aspect of the invention provides an application of the low-temperature denitration catalyst in low-temperature flue gas denitration.
Compared with the prior art, the invention has the following advantages:
(1) the preparation method provided by the invention has the advantages of simple and efficient process, short production flow and reduced cost; the precursor of the active component and the carrier are conventional and easily available and can be purchased in the market.
(2) According to the invention, the active component and the carrier are impregnated and wet-ground, so that the deep loading of the active component is realized, and the prepared active component is uniform in distribution, high in denitration activity and good in stability; meanwhile, spray drying of the slurry is adopted to replace conventional washing, filtering, evaporating and drying, so that the preparation process is simplified, and secondary pollution caused by a large amount of wastewater generated in the preparation process is greatly reduced.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of a low-temperature denitration catalyst, which comprises the following steps: mixing the vanadium-free impregnation liquid with a carrier, carrying out wet grinding, carrying out spray drying and roasting on the uniformly ground slurry to obtain the low-temperature denitration catalyst; wherein the vanadium-free impregnation liquid contains a precursor of manganese.
In the invention, the low-temperature denitration catalyst takes manganese as an active component, preferably, the precursor of the manganese is soluble salt of the manganese, preferably at least one selected from manganese nitrate, manganese sulfate, manganese chloride and manganese acetate. The content of manganese is preferably 2 to 15 wt%, more preferably 5 to 10 wt%, in terms of element, based on the weight of the carrier.
Due to V2O5Has strong biological toxicity, has serious harm to the respiratory system and the skin of a human body, and the treatment of the waste vanadium catalyst is easy to cause secondary pollution. Therefore, the research and development of the denitration catalyst of the invention all adopt a vanadium-free system.
In the present invention, in the impregnation solution related to the method for preparing a denitration catalyst, the vanadium-free impregnation solution preferably further contains a precursor of a second variable valence metal element. The precursor of the second variable valence metal element is soluble salt of the second variable valence metal element, preferably at least one selected from nitrate, chloride and acetate of the second variable valence metal element, and the second variable valence metal element is preferably at least one selected from iron, copper, cerium, cobalt and nickel.
According to the present invention, in order to achieve catalytic activity of the denitration catalyst in a low temperature range, in the components for preparing the catalyst, preferably, the molar ratio of the manganese to the second valence metal is 1: 0.1 to 1, more preferably 1: 0.2-0.5.
According to the invention, in order to realize deeper loading and more uniform distribution of the impregnation liquid, the carrier is preferably at least one of titanium dioxide powder, titanium tungsten powder and titanium silicon powder.
In the invention, the grinding time is not particularly required, and the uniform grinding of the slurry can be realized, and the grinding time can be 1.0-6.0h, preferably 1.5-3.0 h. The solid-to-liquid ratio of the slurry obtained by mixing the impregnation liquid with the carrier and uniformly wet-grinding the mixture is preferably 1: 1 to 5, more preferably 1: 2-4.
According to the invention, the temperature of the spray drying is preferably 110-220 ℃, more preferably 120-170 ℃ and the time is 1.0-1.5 s.
According to the invention, the roasting temperature is preferably 400-650 ℃ and the roasting time is preferably 3-7 h.
The second aspect of the present invention provides a low-temperature denitration catalyst prepared by the above method.
The third aspect of the invention provides an application of the low-temperature denitration catalyst in low-temperature flue gas denitration.
The invention will now be further illustrated by means of specific examples.
Example 1
58.63g of manganese nitrate (117.26 g of a 50 wt% manganese nitrate aqueous solution) and 22.34g of copper chloride CuCl were weighed out separately2·2H2Placing the O in a container, adding deionized water, magnetically stirring and completely dissolving to form a steeping liquor; weighing 200g of carrier titanium dioxide, uniformly adding impregnation liquid and continuously stirring to form a solid-liquid mixture, transferring the mixture into a ball mill, adding water to adjust the solid-liquid ratio to be 1: 2, continuously grinding for 1.5h, and carrying out spray drying on the ground uniform slurry at 120 ℃ for 1.0 s. Drying stationThe obtained powder is prepared, molded and roasted for 3 hours at the temperature of 400 ℃, and the target catalyst 1 is obtained.
Example 2
52.12g of manganese nitrate (104.24 g of a 50 wt% manganese nitrate aqueous solution) and 75.88g of cerium Ce Nitrate (NO) were weighed out separately3)3·6H2Placing the O in a container, adding deionized water, magnetically stirring and completely dissolving to form a steeping liquor; weighing 200g of carrier titanium tungsten powder, uniformly adding impregnation liquid and continuously stirring to form a solid-liquid mixture, transferring the mixture into a ball mill, adding water to adjust the solid-liquid ratio to be 1: and 3, continuously grinding for 2 hours, and carrying out spray drying on the ground uniform slurry at 130 ℃ for 1.0 s. Drying the obtained powder, preparing and molding, and roasting at 450 ℃ for 4h to obtain the target catalyst 2.
Example 3
84.69g of manganese nitrate (169.38 g of a 50 wt% manganese nitrate aqueous solution) and 38.24g of iron nitrate Fe (NO) were weighed out separately3)3·9H2Placing the O in a container, adding deionized water, magnetically stirring and completely dissolving to form a steeping liquor; weighing 200g of carrier titanium dioxide, uniformly adding impregnation liquid and continuously stirring to form a solid-liquid mixture, transferring the mixture into a ball mill, adding water to adjust the solid-liquid ratio to be 1: and 4, continuously grinding for 2.5h, and carrying out spray drying on the ground uniform slurry at 160 ℃ for 1.2 s. Drying the obtained powder, preparing and molding, and roasting at 650 ℃ for 5 hours to obtain the target catalyst 3.
Example 4
39.09g of manganese nitrate (78.18 g of a 50 wt% aqueous solution of manganese nitrate) and 41.57g of CoCl were weighed out separately2·6H2Placing the O in a container, adding deionized water, magnetically stirring and completely dissolving to form a steeping liquor; weighing 200g of carrier titanium silicon powder, uniformly adding impregnation liquid and continuously stirring to form a solid-liquid mixture, transferring the mixture into a ball mill, adding water to adjust the solid-liquid ratio to be 1: 3.5, continuously grinding for 2h, and carrying out spray drying on the ground uniform slurry at 170 ℃ for 1.3 s. Drying the obtained powder, preparing and molding, and roasting at 470 ℃ for 4h to obtain the target catalyst 4.
Example 5
Are respectively provided with40.15g of manganese acetate and 40.49g of nickel nitrate Ni (NO) were weighed3)2·6H2Placing the O in a container, adding deionized water, magnetically stirring and completely dissolving to form a steeping liquor; weighing 200g of carrier titanium dioxide, uniformly adding impregnation liquid and continuously stirring to form a solid-liquid mixture, transferring the mixture into a ball mill, adding water to adjust the solid-liquid ratio to be 1: 2, continuously grinding for 1.5h, and carrying out spray drying on the ground uniform slurry at 120 ℃ for 1.0 s. Drying the obtained powder, preparing and molding, and roasting at 400 ℃ for 7h to obtain the target catalyst 5.
Test example
The catalysts 1 to 5 prepared in examples 1 to 5 were shaped and cut into a strip having a diameter of 1.5mm and a length of 3 to 5mm, and the strip was charged into a tubular SCR reactor for evaluation. The steel cylinder gas is used to simulate the composition of flue gas, and the flue gas contains NO (NOx) and O2、N2、NH3NO and NH3The concentrations are all 200vppm, O2The volume fraction is 2.5 percent, and the balance is balance gas N2The reaction space velocity is 6000h-1The gas flow and composition are regulated and controlled by a mass flow meter. A thermoelectric Thermo 42i-HL smoke gas analyzer is adopted for gas analysis, and each working condition is stable for at least 30 minutes in order to ensure the stability and accuracy of data acquisition. The results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the catalysts of examples 1-5 all have higher catalytic activity in the low temperature range of <300 ℃, especially in the range of 150 ℃ and 250 ℃, the NOx conversion rate is higher than 90%, and the catalysts exhibit excellent reaction capability. From the test results, the catalyst has the advantages of simple and efficient preparation process and reduced cost; the washing and filtering links are saved, and secondary pollution caused by a large amount of waste water generated in the preparation process is avoided; the components are easy to obtain, and the low-temperature denitration catalyst has uniform dispersion, high low-temperature denitration activity and good stability.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (12)
1. A preparation method of a low-temperature denitration catalyst is characterized by comprising the following steps: mixing the vanadium-free impregnation liquid with a carrier, carrying out wet grinding, carrying out spray drying and roasting on the uniformly ground slurry to obtain the low-temperature denitration catalyst; wherein the vanadium-free impregnation liquid contains a precursor of manganese.
2. The method of claim 1, wherein the manganese precursor is a soluble salt of manganese, preferably at least one selected from manganese nitrate, manganese sulfate, manganese chloride and manganese acetate.
3. The method according to claim 2, wherein the manganese is present in an amount of 2 to 15 wt%, preferably 5 to 10 wt%, calculated as element, based on the weight of the support.
4. The method according to claim 1, wherein the vanadium-free impregnation solution further contains a precursor of a second variable valence metal element.
5. The production method according to claim 4, wherein the precursor of the second variable valence metal element is a soluble salt of the second variable valence metal element, preferably at least one selected from a nitrate, a chloride and an acetate of the second variable valence metal element, and the second variable valence metal element is at least one selected from iron, copper, cerium, cobalt and nickel.
6. The production method according to any one of claims 1 to 5, wherein the molar ratio of the manganese to the second valence transition metal is 1: 0.1 to 1, preferably 1: 0.2-0.5.
7. The production method according to claim 1, wherein the carrier is at least one of titanium dioxide powder, titanium tungsten powder, and titanium silicon powder.
8. The method of any one of claims 1 to 7, wherein the milling time is 1.0 to 6.0h, preferably 1.5 to 3.0 h; the solid-liquid ratio of the slurry is 1: 1-5, preferably 1: 2-4.
9. The method according to any one of claims 1-7, wherein the temperature of the spray drying is 110-220 ℃, preferably 120-170 ℃, and the time is 1.0-1.5 s.
10. The preparation method according to any one of claims 1 to 7, wherein the calcination temperature is 400-650 ℃ and the calcination time is 3-7 h.
11. The low-temperature denitration catalyst prepared by the preparation method according to any one of claims 1 to 10.
12. The use of the low temperature denitration catalyst of claim 11 in low temperature flue gas denitration.
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