CN113634262A - Preparation method of low-temperature SCR denitration catalyst based on bubble template derivation method - Google Patents
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- 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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- 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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- 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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- B01D2251/00—Reactants
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- B01D2251/206—Ammonium compounds
- B01D2251/2062—Ammonia
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention relates to the technical field of chemical materials, and discloses a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method. The invention comprises the following steps: adding an organic complexing agent into the nitrate solution, adjusting the pH, stirring until the solution is viscous, stopping stirring, and heating the solution until flame emerges to prepare fluffy combustion powder; mixing and dissolving the prepared combustion powder and an emulsifier, adding a surfactant and a cross-linking agent after stirring, and strongly stirring until wet gel is formed; and drying and roasting the prepared wet gel to prepare the flexible catalyst with rich pore structures. The method has the advantages of low cost, strong plasticity, low density, flexible application mode and high nitrogen oxide removal rate at low temperature.
Description
Technical Field
The invention relates to the technical field of chemical materials, in particular to a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method.
Background
NOx emitted from stationary sources such as coal-fired power plants, industrial boilers, etc. is generally regarded as a major pollutant of atmospheric pollution, and excessive NOx causes a serious environmental problem such as acid rain, photochemical smog, ozone depletion, greenhouse effect, etc. Although China gradually strengthens the treatment of NOx in recent years, the total emission amount is still in a higher situation, and the work of further strengthening emission reduction is needed.
NH3Selective Catalytic Reduction (SCR) is currently the most widely used denitration technique in industry. The catalyst is used as the core of the technology, different types and different functions of catalysts are developed and applied to different fields, and among a plurality of commercial catalysts, the mixed metal oxide mainly comprising V is widely applied.
However, although the vanadium-based catalyst has high denitration performance at high temperature (300-2Conversion to SO3The ability of vanadium, the toxicity of vanadium can cause damage to the environment and the human body, and the like. More importantly, the temperature of the flue gas generated by some industries is lower (70-200 ℃), the optimal active temperature window of the catalyst is difficult to match, and the flue gas is reheated, which causes great energy consumption.
Currently, manganese-based catalysts have been widely noticed and studied for their excellent low-temperature activity and environmentally friendly characteristics, but the catalysts still have some disadvantages such as low-temperature to SO2Relatively sensitive, N at high temperature2Poor selectivity, etc. In order to further improve the performance of the manganese-based catalyst, the introduction of transition metal elements is a more common technical means. In addition, granular or powder catalysts often have an adverse effect on catalyst conversion, selectivity, and durability due to problems such as high bed resistance, uneven mass and heat transfer, and irregular flow patterns. To avoid these adverse effects, monolithic catalysts are often used industrially. In recent years, some monolithic structured catalysts utilizing various fiber/ceramic substrates (e.g., metal foams, SiC foams, ceramic sheets, and honeycomb ceramic supports) have been developed for NH3-SCR reaction.
However, the monolithic catalyst is mostly prepared by coating and dipping methods at present, and the traditional method usually faces the problems of irregular distribution of active components, poor adhesion of the surface of a fiber/ceramic substrate and adverse effects of an adhesive, difficult avoidance of falling-off of the active components after long-time operation and the like. Therefore, there is a particular need to develop non-dip coating methods that embed foam substrates with catalytically active components.
Disclosure of Invention
The invention provides a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method, which has the advantages of low cost, strong plasticity, small density, flexible application mode and high nitrogen oxide removal rate at low temperature.
The technical problem to be solved is that: the existing manganese-based catalyst has poor low-temperature activity, the preparation method of the integral catalyst is complex, the controllability is poor, and the quality stability of the prepared catalyst is poor.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention relates to a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method, which comprises the following steps:
adding an organic complexing agent into a nitrate solution, adjusting the pH value, stirring until the solution is viscous, stopping stirring, and heating the solution until flame emerges to prepare fluffy combustion powder;
step two, mixing and dissolving the combustion powder prepared in the step one with an emulsifier, adding a surfactant and a cross-linking agent after stirring, and strongly stirring until wet gel is formed;
and step three, drying and roasting the wet gel prepared in the step two to prepare the flexible catalyst with rich pore structures.
The invention relates to a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method.
The invention relates to a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method, and further, the molar ratio of total metal ions in a nitrate solution to organic carboxylic acid is 1: 1-2.5.
The invention relates to a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method, which further comprises the following steps: in the first step, the pH value is adjusted to 8-10.
The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method further comprises the step one, wherein the heating ignition temperature is 200-500 ℃, and the heating rate is controlled to be 5-30 ℃/min.
The invention relates to a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method, and further the specific preparation process of the second step comprises the following steps:
2.1, dissolving and diluting an emulsifier by deionized water, then adding combustion powder, and mechanically stirring to form sol; the mixing mass ratio of the combustion powder to the emulsifier is (1-3): 4;
2.2, adding a chemical cross-linking agent and a surfactant, and performing strong mechanical stirring until wet gel is formed; the addition amount of the chemical cross-linking agent and the surfactant is 0.5 to 3 percent of the total mass of the raw materials for forming the wet gel.
The invention relates to a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method, and further relates to a preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation methodIn step two, H is also added simultaneously2O2Adding H2O2The mass of (a) is 1 to 5% of the total mass of the raw materials forming the wet gel.
The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method further comprises the step 2.2, wherein the stirring speed of the strong mechanical stirring is 1500-3000rpm, and the stirring time is 3-10 min.
The invention relates to a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method, and further, the chemical cross-linking agent in the step 2.2 is one or more of F127, P123 or sodium dodecyl sulfate, and the surfactant is glass fiber.
The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method further comprises the following specific drying and roasting processes in the third step:
3.1, transferring the wet gel into a culture dish, and freezing and shaping by liquid nitrogen;
3.2, drying for 24-36h at the temperature of minus 40 ℃ to minus 60 ℃ in a vacuum environment;
3.3, taking out the dried gel, heating to 200 ℃, and roasting for 2-4h to obtain the flexible catalyst.
Compared with the prior art, the preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method has the following beneficial effects:
the nano powder prepared by the sol-gel-self-propagating combustion method through molecular self-assembly is loose and porous, has good dispersibility, large specific surface area, simple preparation process and high reaction rate, and saves energy.
The flexible catalyst prepared by the method has low raw material price, and the problem of falling off of active components does not exist by adopting an integrated synthesis method; meanwhile, good denitration efficiency (81 percent) can be obtained at a lower reaction temperature (60 ℃), and the catalyst has higher stability and longer service life.
The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method of the present invention is further described below with reference to the accompanying drawings.
Drawings
FIG. 1 is an electron micrograph of a catalyst prepared in preparation example 1 at 100 times magnification;
FIG. 2 is an electron micrograph of a catalyst prepared in production example 1 at 1000 times magnification;
FIG. 3 is an XRD pattern of the catalyst prepared in preparation example 1;
fig. 4 is a cyclic stress-strain curve at a maximum strain of 60% for the catalyst prepared in preparative example 1.
Detailed Description
Preparation examples
The invention relates to a preparation method of a low-temperature SCR denitration catalyst based on a bubble template derivation method, which comprises the following steps:
step one, adding an organic complexing agent into a nitrate solution, adjusting the pH value, stirring until the solution is viscous, stopping stirring, and igniting the solution until flame appears to prepare fluffy combustion powder.
In the first step, the nitrate solution is one or more of rare earth element nitrates or transition metal nitrates, a mixed solution of manganese nitrate, cerium nitrate and cobalt nitrate is used in the preparation example, and the molar ratio of the three nitrates is (10-20): 4-8): 1.
The added organic complexing agent is organic carboxylic acid, specifically one or more of citric acid, oxalic acid or stearic acid, and the molar ratio of total metal ions in the mixed nitrate to the organic carboxylic acid is 1: 1-2.5.
The specific process of adjusting the pH comprises the steps of adding a certain amount of concentrated nitric acid into a nitrate solution after an organic complexing agent is mixed, then adding concentrated ammonia water, adjusting the pH value to 8-10, stirring until the solution is viscous after the combustion condition is achieved, stopping stirring, heating and igniting to form metal oxide powder in the combustion process. The obtained metal oxide powder is nano-scale particle powder, is used as a molecular precursor, is fluffy and porous, has good dispersion performance and large specific surface area.
The ignition temperature is 200-500 ℃, and the temperature rise rate is controlled to be 5-30 ℃/min, so as to adjust the morphology and the particle size of the product in the temperature rise process.
And step two, mixing and dissolving the combustion powder prepared in the step one with an emulsifier, adding a surfactant and a cross-linking agent after stirring, and stirring strongly until a wet gel is formed. The preparation process comprises the following steps:
2.1, dissolving and diluting the emulsifier by deionized water, then adding combustion powder, and mechanically stirring for 1-2 min.
In the process, nanoparticles obtained by combustion are molecular precursors, and can form sol by mechanical stirring after being mixed with an emulsifier.
Wherein, the used emulsifier is an organic polymer, specifically polyethylene glycol and/or polyvinyl alcohol can be selected, dissolved in deionized water and stirred at about 90 ℃ until being completely dissolved; the mixing mass ratio of the combustion powder to the emulsifier is (1-3): 4.
2.2, adding a chemical cross-linking agent and a surfactant, and performing strong mechanical stirring until a wet gel is formed.
Wherein the used chemical cross-linking agent is one or more of F127, P123 or sodium dodecyl sulfate, and the surfactant is glass fiber. The addition amount of the chemical cross-linking agent and the surfactant is 0.5 to 3 percent of the total mass of the raw materials for forming the wet gel.
The multi-component gel is formed by adding the chemical cross-linking agent and the surfactant, strong stirring is assisted, gelation reaction is generated in the process, the wet gel with a porous structure is formed by foaming, the formation of the bubble aggregate and the aggregate added with the core substance is carried out simultaneously in two steps, the preparation time can be effectively shortened, and the more uniform dispersion of the combustion powder in the wet gel is ensured.
In the process, the density and the size of the air holes are adjusted by controlling the rotating speed and the stirring time of the stirrer, wherein the rotating speed is 1500-.
When the chemical cross-linking agent and the surfactant are added, H can also be added at the same time2O2Adding H2O2The mass of the foaming agent is 1 to 5 percent of the total mass of the raw materials for forming the wet gel, the foaming speed and the foaming volume can be effectively improved, and the foaming effect is effectively improvedThe aperture ratio of the finished catalyst.
And step three, drying and roasting the wet gel prepared in the step two to prepare the flexible catalyst with rich pore structures.
The specific process of drying and roasting is as follows:
3.1, transferring the wet gel into a culture dish, and freezing and shaping by liquid nitrogen;
3.2, then placing the mixture on a freeze dryer to dry for 24 to 36 hours at the temperature of minus 40 ℃ to minus 60 ℃ under the vacuum condition;
3.3, taking out the dried gel, heating to 200 ℃ at the heating rate of 1-5 ℃/min, and roasting for 2-4h at the temperature of 200 ℃ to prepare the flexible catalyst with rich pore structure.
The amount ratios of the above components are shown in tables 1 and 2, and the preparation conditions are shown in table 3.
TABLE 1 use of raw material components of combustion powders in respective production examples
| Preparation example 1 | Preparation example 2 | Preparation example 3 | Preparation example 4 | Preparation example 5 | |
| Manganese nitrate | 6g | 6g | 6g | 6g | 6g |
| Cerium nitrate | 3.5g | 3.5g | - | 8.7g | 5.8g |
| Cobalt nitrate | 0.8g | - | 0.8g | 0.97g | 0.48g |
| Citric acid | 1:1.5 | - | 1:2.5 | 1:2 | - |
| Oxalic acid | - | 1:2 | - | - | 1:2.5 |
Note: in the above table, manganese nitrate, cerium nitrate and cobalt nitrate are used in a mass dissolved in 50mL of deionized water;
citric acid or oxalic acid is the molar ratio of metal ions to organic carboxylic acid in the nitrate.
TABLE 2 use of the components of the preparation examples
| Preparation example 1 | Preparation example 2 | Preparation example 3 | Preparation example 4 | Preparation example 5 | |
| Polyvinyl alcohol | 1g | 1.5g | 1g | - | 0.5g |
| Polyethylene glycol | - | - | - | 1g | 1g |
| Burning powder | 0.75g | 0.375g | 0.75g | 0.5g | 1g |
| P123 | 0.25g | - | - | 0.5g | - |
| F127 | - | 0.5g | - | - | 0.25g |
| Sodium dodecyl sulfate | - | - | 0.5g | - | - |
| Glass fiber | 0.25g | 0.3g | 0.2g | 0.4g | 0.5g |
Note: the amounts of all components in the above table are by mass;
dissolving polyvinyl alcohol and/or polyethylene glycol in 50mL of deionized water;
the combustion powders used were those prepared in the corresponding examples in table 1.
TABLE 3 preparation conditions of the preparation examples
Note: the heating rate and heating temperature in Table 3 are the conditions of ignition after completion of the stirring in the first step;
stirring speed and stirring time are the stirring conditions of the strong mechanical stirring in the step 2.2;
the drying temperature and the drying time are the drying conditions of the vacuum freeze drying in the step 3.2;
the rate of temperature rise, firing temperature and firing time are the firing conditions in step 3.3.
The catalyst prepared in the preparation example was subjected to electron microscope scanning, wherein the surface morphology of the catalyst obtained in the preparation example 1 is shown in fig. 1 and 2.
The obtained catalyst was also subjected to X-ray diffraction, wherein the XRD pattern of the catalyst of preparation example 1 is shown in fig. 3.
The prepared catalyst was subjected to basic performance tests, and the specific test results are shown in table 4.
Wherein NOxThe test conditions of denitration efficiency are as follows: the reaction temperature is 60 ℃, the gas flow is 200mL/min, the NO concentration is 500ppm, and NH is added3Concentration 500ppm, O2Concentration of 5%, N2As balance gas, the space velocity is 10000h-1。
TABLE 4 results of performance test of flexible catalysts prepared in each preparation example
| Preparation example 1 | Preparation example 2 | Preparation example 3 | Preparation example 4 | Preparation example 5 | |
| Mass density mg/cm3 | 54 | 37 | 49 | 58 | 68 |
| Denitration efficiency% | 88.5 | 85.2 | 80.1 | 77.6 | 83 |
As can be seen from Table 4, the mass density of the catalyst obtained was from 37 to 68mg/cm3Meanwhile, the material is light in weight, is lower than other existing monolithic catalysts on the market, and has the denitration efficiency of 77.6-88.5% under the condition of lower reaction temperature (60 ℃) and is not lower than that of the existing monolithic catalysts on the market. More importantly, the preparation method is simple and easy to operate, the prepared catalyst is good in quality stability, light and soft in weight, strong in plasticity and more flexible in application mode, and the possibility of realization in the field of denitration is increased.
The prepared catalyst was subjected to a pressure test, and the compressive strain 60% test conditions were set to obtain a compressive strain curve of the catalyst prepared in each preparation example, wherein the cyclic stress-strain curve at a maximum strain of 60% in preparation example 1 is shown in fig. 4.
The compressive strain curve of fig. 4 shows almost complete recovery after 60% strain. At 60% strain, the stress was just over 1.6 kpa, showing excellent flexibility of the catalyst. The compressive stress-strain curve of the fifth cycle did not change significantly from the first cycle, demonstrating excellent elasticity of the material.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (10)
1. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method is characterized by comprising the following steps of: the method comprises the following steps:
adding an organic complexing agent into a nitrate solution, adjusting the pH value, stirring until the solution is viscous, stopping stirring, and heating the solution until flame emerges to prepare fluffy combustion powder;
step two, mixing and dissolving the combustion powder prepared in the step one with an emulsifier, adding a surfactant and a cross-linking agent after stirring, and strongly stirring until wet gel is formed;
and step three, drying and roasting the wet gel prepared in the step two to prepare the flexible catalyst with rich pore structures.
2. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method as claimed in claim 1, wherein: the nitrate solution in the first step is one or more of rare earth element nitrate or transition metal nitrate, and the organic complexing agent is organic carboxylic acid.
3. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method as claimed in claim 2, wherein: the molar ratio of the total metal ions to the organic carboxylic acid in the nitrate solution is 1: 1-2.5.
4. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method as claimed in claim 1, wherein: in the first step, the pH value is adjusted to 8-10.
5. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method as claimed in claim 1, wherein: in the first step, the heating ignition temperature is 200-.
6. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method as claimed in claim 1, wherein: the preparation process of the second step specifically comprises the following steps:
2.1, dissolving and diluting an emulsifier by deionized water, then adding combustion powder, and mechanically stirring to form sol; the mixing mass ratio of the combustion powder to the emulsifier is (1-3): 4;
2.2, adding a chemical cross-linking agent and a surfactant, and performing strong mechanical stirring until wet gel is formed; the addition amount of the chemical cross-linking agent and the surfactant is 0.5 to 3 percent of the total mass of the raw materials for forming the wet gel.
7. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method as claimed in claim 1, wherein: in step two, H is also added simultaneously2O2Adding H2O2The mass of (a) is 1 to 5% of the total mass of the raw materials forming the wet gel.
8. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method as claimed in claim 6, wherein: in the step 2.2, the stirring speed of the strong mechanical stirring is 1500-.
9. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method as claimed in claim 6, wherein: the chemical cross-linking agent in the step 2.2 is one or more of F127, P123 or sodium dodecyl sulfate, and the surfactant is glass fiber.
10. The preparation method of the low-temperature SCR denitration catalyst based on the bubble template derivation method as claimed in claim 1, wherein: the drying and roasting process in the third step is as follows:
3.1, transferring the wet gel into a culture dish, and freezing and shaping by liquid nitrogen;
3.2, in a vacuum environment, the temperature is minus 40 ℃ to minus 60 DEG CoDrying for 24-36h under C;
3.3, taking out the dried gel, heating to 200 ℃, and roasting for 2-4h to obtain the flexible catalyst.
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Application publication date: 20211112 |