CN110237837B - Preparation method of fluidized bed denitration catalyst - Google Patents
Preparation method of fluidized bed denitration catalyst Download PDFInfo
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- CN110237837B CN110237837B CN201810536035.5A CN201810536035A CN110237837B CN 110237837 B CN110237837 B CN 110237837B CN 201810536035 A CN201810536035 A CN 201810536035A CN 110237837 B CN110237837 B CN 110237837B
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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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- 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
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- 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
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The invention discloses a preparation method of a fluidized bed denitration catalyst, which comprises the procedures of raw material preparation, precursor synthesis, catalyst synthesis, water washing, drying and calcination. The produced catalyst can keep high flux and low pressure drop of the flue gas SCR denitration device, and has high desulfurization efficiency and low cost.
Description
Technical Field
The invention relates to the field of inorganic synthetic denitration agents, in particular to a preparation method of a fluidized bed denitration catalyst.
Background
With the development of industrialization in China, the pollution of the air environment is more and more serious, the problem of environmental protection gradually draws social attention, and environmental regulations are continuously perfected. It has been determined that fuel combustion is the primary cause of the rise in atmospheric NOx levels.
The denitration technology is one of the most efficient NOx control measures in recent years, the existing mature denitration method comprises an absorption method and a catalysis method, and the SCR (Selective catalytic reduction) technology is widely adopted to treat chimney tail gas of thermal power plants, incineration plants and the like and diesel vehicle tail gas due to the advantages of high efficiency, high selectivity, economy, easy operation and the like. The catalyst used in chimney tail gas of thermal power plants and incineration plants is generally honeycomb catalyst, and because the chimney tail gas has a large amount of dust, the efficiency of the catalyst is reduced due to the blockage of the honeycomb pore channels with the time. At present, the research is more than that of a powder catalyst, but the powder catalyst has the defects of large pressure drop, easiness in purging, small mechanical strength and the like, and cannot be directly applied to industrialization.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a fluidized bed denitration catalyst, and the produced catalyst can keep high flux and low pressure drop of a flue gas SCR denitration device, and has high desulfurization efficiency and low cost.
In order to achieve the purpose, the technical scheme adopted by the invention is to provide a preparation method of a fluidized bed denitration catalyst, which comprises the following steps:
s1, raw material preparation: preparing sodium silicate into aqueous solution containing 10-15wt% of silicon dioxide; preparing sulfuric acid into 30-40% wt aqueous solution; preparing sodium tungstate into an aqueous solution containing 10-15wt% of tungsten trioxide; preparing titanyl sulfate into an aqueous solution containing 5-10wt% of titanium dioxide for later use;
s2, precursor synthesis: adding a sodium silicate aqueous solution containing silicon dioxide into a reaction tank, stirring, simultaneously adding a sulfuric acid aqueous solution until the pH is 4-5, and then stirring; heating the slurry after reaction to 50-60 ℃, and preserving heat; the PH value of the solution is adjusted to 4-5, and the solution is heated to 50-60 ℃, so that the stability of the precursor can be maintained to the maximum extent;
s3, catalyst synthesis: adding titanium dioxide-containing titanyl sulfate aqueous solution into the material prepared in the step S2, stirring uniformly, adding tungsten trioxide-containing sodium tungstate aqueous solution, adjusting the pH value to 7-8 after adding, heating to 70-80 ℃, and preserving heat, wherein the mass ratio of titanium dioxide to tungsten trioxide to silicon dioxide is 1: 4-5, so that the catalytic activity is optimal;
s4, washing: washing the material prepared in the step S3 with water until the conductivity of the washing water is below 300 mu S/cm;
s5, drying: drying and granulating the material prepared in the step S4;
s6, calcining: and calcining the dried material obtained in the step S5 at the temperature of 400-450 ℃ for 1-2 hours to obtain the denitration catalyst.
Specifically, in step S2, after the sodium silicate aqueous solution is added into the reaction tank, the sodium silicate aqueous solution is stirred at the speed of 100-100 rpm at 20-30 ℃, the sulfuric acid aqueous solution is added at the speed of 50-100ml/min, and the heat preservation time is 20-30 minutes. The precursor can be controlled under the conditions of lower temperature, higher stirring speed and lower feeding speed, and the precursor does not have a gel state.
Specifically, in step S3, the speed of adding the aqueous solution of sodium tungstate containing tungsten trioxide is 50-100ml/min, so that the aqueous solution of sodium tungstate containing tungsten trioxide is mixed more uniformly, and the heat preservation time is 1-2 hours, so that the hydrolysis of sodium tungstate is more complete.
Specifically, in step S5, the operation temperature of drying and granulation is 200 ℃ at the inlet and 250 ℃ at the outlet, and the drying efficiency can be improved by 90-100 ℃; the average particle size is 150-200 mu m, so that the fluidization performance of the fluidized bed is better.
The invention has the beneficial effects that: the carrier for forming the catalyst is essentially a silica gel carrier with a space three-dimensional structure and has porosity. The spatial distribution of the active components of the catalyst is more uniform. Therefore, the denitration catalyst prepared by the invention has the advantages of high efficiency, low cost, easy industrialization and the like, and can keep high flux and low pressure drop of the flue gas SCR denitration device.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
S1, raw material preparation: preparing 1000g of sodium silicate aqueous solution containing 10wt% of silicon dioxide, preparing 250g of sodium tungstate aqueous solution containing 10wt% of tungsten trioxide, preparing 500g of titanyl sulfate aqueous solution containing 5wt% of titanium dioxide, and preparing 30 wt% of sulfuric acid aqueous solution for later use;
s2, precursor synthesis: adding the prepared sodium silicate aqueous solution into a reaction tank, starting stirring at the speed of 100 rpm at the temperature of 30 ℃, adding a sulfuric acid aqueous solution at the speed of 100ml/min until the pH value is 4.2, stirring for 30 minutes, heating to 50 ℃, and keeping the temperature for 30 minutes;
s3, catalyst synthesis: and (3) adding 500g of titanyl sulfate aqueous solution into the material prepared in the step S2, stirring uniformly, adding 250g of sodium tungstate aqueous solution at the speed of 100ml/min, adjusting the pH value to 7.5 by using ammonia water after the addition is finished, heating to 80 ℃, and keeping the temperature for 2 hours.
S4, washing: washing the material prepared in the step S3 until the conductivity of the washing water is below 300 mu S/cm, wherein the washing water is qualified; for water washing, the water washing equipment adopted in this embodiment is a plate-and-frame press, and certainly, other water washing equipment such as a centrifuge can be adopted, which is not a limitation to the protection scope of the present invention, as long as the material is washed with water until the conductivity is 300 μ S/cm;
s5, drying: drying and granulating the material prepared in the step S4, wherein the operation temperature is 225 ℃ at the inlet, 100 ℃ at the outlet, and the average particle size is 200 mu m; in this example, spray drying was used for drying granulation, but other methods may be used.
S6, calcining: and (4) calcining the material dried in the step S5 at 400 ℃ for 2 hours to prepare the fluidized bed denitration catalyst.
Example 2
S1, raw material preparation: preparing 1000g of aqueous solution containing 12 wt% of silicon dioxide, preparing 250g of aqueous solution containing 12 wt% of tungsten trioxide by using sodium tungstate, preparing 375g of aqueous solution containing 8 wt% of titanium dioxide by using titanyl sulfate, and preparing aqueous solution containing 33 wt% of sulfuric acid for later use;
s2, precursor synthesis: adding the prepared sodium silicate aqueous solution into a reaction tank, starting stirring at the speed of 75 rpm at the temperature of 25 ℃, adding a sulfuric acid aqueous solution at the speed of 100ml/min until the pH value is 4.5, stirring for 35 minutes, heating to 55 ℃, and keeping the temperature for 30 minutes;
s3, catalyst synthesis: and adding 375g of titanyl sulfate aqueous solution into the material prepared in the step S2, stirring uniformly, adding 250g of sodium tungstate aqueous solution at the speed of 80ml/min, adjusting the pH to 7.8 after the addition is finished, heating to 75 ℃, and keeping the temperature for 1.5 hours.
S4, washing: washing the material prepared in the step S3 until the conductivity of the washing water is below 300 mu S/cm, wherein the washing water is qualified; for water washing, the water washing equipment adopted in this embodiment is a plate-and-frame press, and certainly, other water washing equipment such as a centrifuge can be adopted, which is not a limitation to the protection scope of the present invention, as long as the material is washed with water until the conductivity is 300 μ S/cm;
s5, drying: drying and granulating the material prepared in the step S4 by spray drying, wherein the operation temperature is 250 ℃ at the inlet, 100 ℃ at the outlet and the average particle size is 180 mu m; in this embodiment, spray drying is adopted for drying granulation, but other methods can be adopted;
s6, calcining: and (4) calcining the dried material obtained in the step S5 at 425 ℃ for 1.5 hours to obtain the fluidized bed denitration catalyst.
Example 3
S1, raw material preparation: preparing 1000g of aqueous solution containing 15wt% of silicon dioxide, preparing 200g of aqueous solution containing 15wt% of tungsten trioxide from sodium tungstate, preparing 300g of aqueous solution containing 10wt% of titanium dioxide from titanyl sulfate, and preparing 40wt% of sulfuric acid aqueous solution for later use;
s2, precursor synthesis: adding the prepared sodium silicate aqueous solution into a reaction tank, starting stirring at the speed of 75 rpm at the temperature of 25 ℃, adding a sulfuric acid aqueous solution at the speed of 100ml/min until the pH value is 4.5, stirring for 35 minutes, heating to 55 ℃, and keeping the temperature for 30 minutes;
s3, catalyst synthesis: and adding 375g of titanyl sulfate aqueous solution into the material prepared in the step S2, stirring uniformly, adding 250g of sodium tungstate aqueous solution at the speed of 80ml/min, adjusting the pH to 7.8 after the addition is finished, heating to 70 ℃, and keeping the temperature for 1.5 hours.
S4, washing: washing the material prepared in the step S3 until the conductivity of the washing water is below 300 mu S/cm, wherein the washing water is qualified; for water washing, the water washing equipment adopted in this embodiment is a plate-and-frame press, and certainly, other water washing equipment such as a centrifuge can be adopted, which is not a limitation to the protection scope of the present invention, as long as the material is washed with water until the conductivity is 300 μ S/cm;
s5, drying: drying and granulating the material prepared in the step S4 by spray drying, wherein the operation temperature is 250 ℃ at the inlet, 100 ℃ at the outlet and the average particle size is 150 mu m; in this embodiment, spray drying is adopted for drying granulation, but other methods can be adopted;
s6, calcining: and (4) calcining the material dried in the step S5 at 400 ℃ for 2 hours to prepare the fluidized bed denitration catalyst.
Table 1 shows the performance tests of the catalysts obtained in examples 1 to 3.
| Examples | Bulk specific gravity g/ml | Average particle diameter μm | Denitration efficiency% |
| 1 | 0.67 | 200 | 65.0 |
| 2 | 0.61 | 180 | 66.2 |
| 3 | 0.59 | 150 | 64.5 |
TABLE 1
The above embodiments are merely illustrative of the preferred embodiments of the present invention, and not restrictive, and various changes and modifications to the technical solutions of the present invention may be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are intended to fall within the scope of the present invention defined by the appended claims.
Claims (4)
1. A preparation method of a fluidized bed denitration catalyst is characterized by comprising the following steps:
s1, raw material preparation: preparing sodium silicate into 10-15wt% of aqueous solution calculated by silicon dioxide; preparing sulfuric acid into 30-40wt% aqueous solution; preparing sodium tungstate into an aqueous solution with the weight percent of 10-15 percent in terms of tungsten trioxide; titanyl sulfate is prepared into 5 to 10 weight percent aqueous solution calculated by titanium dioxide for standby;
s2, precursor synthesis: adding a sodium silicate aqueous solution into a reaction tank, stirring, simultaneously adding a sulfuric acid aqueous solution until the pH is =4-5, and stirring; heating the slurry after reaction to 50-60 ℃, and preserving heat for 20-30 minutes;
s3, catalyst synthesis: adding titanyl sulfate aqueous solution into the material prepared in the step S2, stirring uniformly, adding sodium tungstate aqueous solution, adjusting the pH =7-8 after adding, heating to 70-80 ℃, and keeping the temperature for 1-2 hours to obtain the catalyst, wherein the mass ratio of titanium dioxide to tungsten trioxide to silicon dioxide is 1: 4-5;
s4, washing: washing the material prepared in the step S3 with water until the conductivity of the washing water is below 300 mu S/cm;
s5, drying: drying and granulating the material prepared in the step S4;
s6, calcining: and calcining the dried material obtained in the step S5 at the temperature of 400-450 ℃ for 1-2 hours to obtain the denitration catalyst.
2. The method for preparing a fluidized bed denitration catalyst according to claim 1, characterized in that: in step S2, after the sodium silicate solution is added into the reaction tank, the sodium silicate solution is stirred at the speed of 100-200 rpm at the temperature of 20-30 ℃, and the sulfuric acid solution is added at the speed of 50-100 mL/min.
3. The method for preparing a fluidized bed denitration catalyst according to claim 1, characterized in that: in step S3, the rate of adding the aqueous solution of sodium tungstate containing tungsten trioxide is 50-100 mL/min.
4. The method for preparing a fluidized bed denitration catalyst according to claim 1, characterized in that: in the step S5, the operation temperature of drying and granulation is 200-250 ℃ at the inlet, 90-100 ℃ at the outlet, and the average particle size is 150-200 mu m.
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