CN110237837B - Preparation method of fluidized bed denitration catalyst - Google Patents
Preparation method of fluidized bed denitration catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 17
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 12
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims description 46
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 23
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 14
- 239000004115 Sodium Silicate Substances 0.000 claims description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003546 flue gas Substances 0.000 abstract description 3
- 230000004907 flux Effects 0.000 abstract description 3
- 238000006477 desulfuration reaction Methods 0.000 abstract description 2
- 230000023556 desulfurization Effects 0.000 abstract description 2
- 238000001694 spray drying Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
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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
-
- 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
-
- 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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- 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
- 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
-
- 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
-
- 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
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- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
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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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