CN110237837A - A kind of preparation method of fluidized bed denitration catalyst - Google Patents
A kind of preparation method of fluidized bed denitration catalyst Download PDFInfo
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- CN110237837A CN110237837A CN201810536035.5A CN201810536035A CN110237837A CN 110237837 A CN110237837 A CN 110237837A CN 201810536035 A CN201810536035 A CN 201810536035A CN 110237837 A CN110237837 A CN 110237837A
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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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- 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
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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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
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- 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
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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
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Abstract
The invention discloses a kind of preparation methods of fluidized bed denitration catalyst, including raw material preparation, precursor synthesis, catalyst synthesis, washing, dry, calcining process.The catalyst produced is able to maintain the high throughput and low pressure drop of the out of stock device of flue gas SCR, and catalyst desulfurizing is high-efficient, at low cost.
Description
Technical field
The present invention relates to Inorganic synthese denitrfying agent field, espespecially a kind of preparation method of fluidized bed denitration catalyst.
Background technique
With the industrialized development in China, the pollution of air environment is increasingly severe, and environmental protection problem gradually causes society
Concern, environmental regulation has constantly obtained perfect.Have determined that fuel combustion is the master for causing atmosphere NOx content to rise at present
Want reason.
Denitration technology is one of most efficient NOx control measure in recent years, at present the method for denitration packet of comparative maturity
Absorption process and catalysis method are included, and SCR (Urea-based Selective CatalyticReduction) technology is because of its tool
Have the advantages that efficient, highly selective, economy and it is easy to operate and be widely adopted processing steam power plant, the chimneys tail gas such as incineration plant with
And exhaust gas from diesel vehicle.The catalyst used in the chimney tail gas of steam power plant and incineration plant generally uses honeycombed catalyst, by
In chimney tail gas, there are a large amount of dust, as the cellular duct blocking of the extension of time declines catalyst efficiency.At present
Study more compared with fine catalyst, but that there are pressure drops is big, easily purging, the disadvantages of mechanical strength is small for fine catalyst, Bu Nengzhi
Connect industrial applications.
Summary of the invention
To solve the above problems, the present invention provides a kind of preparation method of fluidized bed denitration catalyst, the catalyst energy produced
The high throughput and low pressure drop of the out of stock device of flue gas SCR are kept, catalyst desulfurizing is high-efficient, at low cost.
To achieve the above object, the technical solution adopted by the present invention is that providing a kind of preparation side of fluidized bed denitration catalyst
Method, comprising the following steps:
S1. raw material is prepared: sodium metasilicate is configured to the aqueous solution of the 0-15%wt containing silica 1；Sulfuric acid is configured to 30-40%wt
Aqueous solution；Sodium tungstate is configured to the aqueous solution of the 10-15%wt containing tungstic acid；Titanyl sulfate is configured to 5- containing titanium dioxide
10%wt aqueous solution is spare；
S2. precursor synthesis: reactor tank stirring is added in silica containing sodium silicate aqueous solution, while aqueous sulfuric acid is added
Stop to PH4-5, is subsequently agitated for；Slurry after reaction is warming up to 50-60 DEG C, heat preservation；Solution PH is adjusted to 4-5, and is heated up
To 50-60 DEG C, the stability of presoma can be kept to the maximum extent；
S3. catalyst synthesizes: the aqueous solution of titanyle sulfate containing titanium dioxide being added to the material of step S2 preparation, is stirred evenly
Afterwards, the wolframic acid sodium water solution containing tungstic acid is added, PH7-8 is adjusted after the completion of being added, then heats to 70-80 DEG C, keep the temperature,
Wherein the mass ratio between titanium dioxide, tungstic acid, silica is 1:1:4-5, and the activity of catalysis is made to reach best；
S4. it washes: the step S3 material prepared is washed, being washed till wash water conductivity is 300 μ S/cm or less；
S5. it dries: granulation is dried in the step S4 material prepared;
S6. it calcines: material of the step S5 after dry being calcined 1-2 hours at 400-450 DEG C, denitrating catalyst is made.
Specifically, in step S2, after reactor tank is added in sodium silicate aqueous solution, at 20-30 DEG C, with 100-200 revs/min of speed
Aqueous sulfuric acid is added with the speed of 50-100ml/min in the lower stirring of degree, and soaking time is 20-30 minutes.In lower temperature
Under degree, higher speed of agitator, slower charging rate, it can control, gel state does not occur in presoma.
Specifically, in step S3, the speed that the wolframic acid sodium water solution containing tungstic acid is added is 50-100ml/min, so that
Wolframic acid sodium water solution mixing containing tungstic acid is more uniform, and soaking time is 1-2 hours, so that the hydrolysis of sodium tungstate is more thorough
Bottom.
Specifically, in step S5, the operation temperature of drying-granulating is 200-250 DEG C of import, exports 90-100 DEG C, Ke Yiti
High drying efficiency；Average grain diameter is 150-200 μm, so that the fluidizing performance as fluidized bed is preferable.
The beneficial effects of the present invention are: the carrier due to forming catalyst is substantially a kind of with space three-dimensional structure
Silica-gel carrier, and there is porosity.The spatial distribution of the active component of catalyst is more uniform.Therefore denitration prepared by the present invention
Catalyst, have it is high-efficient, it is at low cost, be easy to the advantages that industrializing, be able to maintain the high throughput and low pressure of the out of stock device of flue gas SCR
Drop.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
S1. raw material is prepared: preparing the sodium silicate aqueous solution 1000g of the 0%wt containing silica 1, sodium tungstate is configured to containing three oxidations
Titanyl sulfate is configured to the aqueous solution 500g of 5%wt containing titanium dioxide, with 30% wt's of Sulphuric acid by the aqueous solution 250g of tungsten 10%wt
Aqueous solution is spare；
S2. precursor synthesis: being added reactor tank for the sodium silicate aqueous solution of preparation, at 30 DEG C, open 100 turns of mixing speed/
Point, stopped with the speed addition aqueous sulfuric acid of 100ml/min to PH4.2, and stir 30 minutes, is warming up to 50 DEG C and keeps the temperature 30 points
Clock；
S3. catalyst synthesizes: aqueous solution of titanyle sulfate 500g is added to the material of step S2 preparation, after mixing evenly, then with
Wolframic acid sodium water solution 250g is added in the speed of 100ml/min, adjusts PH7.5 with ammonium hydroxide after the completion of addition, then heats to 80 DEG C,
Heat preservation 2 hours.
S4. it washes: the step S3 material prepared is washed, being washed till wash water conductivity is that the following are conjunctions by 300 μ S/cm
Lattice；For washing, other washing equipments are can also be used as being centrifuged for sheet frame press machine in the washing equipment that the present embodiment uses certainly
Machine, this is not limiting the scope of the present invention certainly, as long as realizing that being washed to conductivity to material is 300 μ S/cm；
S5. it dries: granulation is dried in the step S4 material prepared, operation temperature is 225 DEG C of import, exports 100 DEG C, averagely
Partial size is 200 μm；Granulation is dried by the way of spray drying in the present embodiment, and other modes can also be used certainly.
S6. it calcines: by the material after step S5 drying at 400 DEG C, calcining 2 hours, fluidized bed denitration catalyst is made.
Embodiment 2
S1. raw material is prepared: preparing the aqueous solution 1000g of the 2%wt containing silica 1, sodium tungstate is configured to containing tungstic acid 12%
Titanyl sulfate is configured to the aqueous solution 375g of 8%wt containing titanium dioxide, with the water-soluble of 33% wt of Sulphuric acid by the aqueous solution 250g of wt
Liquid is spare；
S2. precursor synthesis: being added reactor tank for the sodium silicate aqueous solution of preparation, at 25 DEG C, open 75 turns of mixing speed/
Point, stopped with the speed addition aqueous sulfuric acid of 100ml/min to PH4.5, and stir 35 minutes, is warming up to 55 DEG C and keeps the temperature 30 points
Clock；
S3. catalyst synthesizes: aqueous solution of titanyle sulfate 375g is added to the material of step S2 preparation, after mixing evenly, then with
Wolframic acid sodium water solution 250g is added in the speed of 80ml/min, is adjusted to PH7.8 after the completion of being added, and then heats to 75 DEG C, heat preservation
1.5 hour.
S4. it washes: the step S3 material prepared is washed, being washed till wash water conductivity is that the following are conjunctions by 300 μ S/cm
Lattice；For washing, other washing equipments are can also be used as being centrifuged for sheet frame press machine in the washing equipment that the present embodiment uses certainly
Machine, this is not limiting the scope of the present invention certainly, as long as realizing that being washed to conductivity to material is 300 μ S/cm；
S5. it dries: granulation is dried using spray drying in material prepared by step S4, operation temperature is 250 DEG C of import, out
100 DEG C of mouth, average grain diameter are 180 μm；Granulation is dried by the way of spray drying in the present embodiment, it can also be used certainly
His mode；
S6. it calcines: by the material after step S5 drying at 425 DEG C, calcining 1.5 hours, fluidized bed denitration catalyst is made.
Embodiment 3
S1. raw material is prepared: preparing the aqueous solution 1000g of the 5%wt containing silica 1, sodium tungstate is configured to containing tungstic acid 15%
Titanyl sulfate is configured to the aqueous solution 300g of 10%wt containing titanium dioxide, with the water-soluble of 40% wt of Sulphuric acid by the aqueous solution 200g of wt
Liquid is spare；
S2. precursor synthesis: being added reactor tank for the sodium silicate aqueous solution of preparation, at 25 DEG C, open 75 turns of mixing speed/
Point, stopped with the speed addition aqueous sulfuric acid of 100ml/min to PH4.5, and stir 35 minutes, is warming up to 55 DEG C and keeps the temperature 30 points
Clock；
S3. catalyst synthesizes: aqueous solution of titanyle sulfate 375g is added to the material of step S2 preparation, after mixing evenly, then with
Wolframic acid sodium water solution 250g is added in the speed of 80ml/min, is adjusted to PH7.8 after the completion of being added, and then heats to 70 DEG C, heat preservation
1.5 hour.
S4. it washes: the step S3 material prepared is washed, being washed till wash water conductivity is that the following are conjunctions by 300 μ S/cm
Lattice；For washing, other washing equipments are can also be used as being centrifuged for sheet frame press machine in the washing equipment that the present embodiment uses certainly
Machine, this is not limiting the scope of the present invention certainly, as long as realizing that being washed to conductivity to material is 300 μ S/cm；
S5. it dries: granulation is dried using spray drying in material prepared by step S4, operation temperature is 250 DEG C of import, out
100 DEG C of mouth, average grain diameter are 150 μm；Granulation is dried by the way of spray drying in the present embodiment, it can also be used certainly
His mode；
S6. it calcines: by the material after step S5 drying at 400 DEG C, calcining 2 hours, fluidized bed denitration catalyst is made.
Table 1 is the performance test that catalyst is made in embodiment 1-3.
| Embodiment | Bulk density g/ml | Average grain diameter μm | Denitration efficiency % |
| 1 | 0.67 | 200 | 65.0 |
| 2 | 0.61 | 180 | 66.2 |
| 3 | 0.59 | 150 | 64.5 |
Table 1
Embodiment of above is only that preferred embodiments of the present invention will be described, is not limited the scope of the present invention
Fixed, without departing from the spirit of the design of the present invention, this field ordinary engineering and technical personnel makees technical solution of the present invention
Various changes and improvements out, should fall within the scope of protection determined by the claims of the present invention.
Claims (6)
1. a kind of preparation method of fluidized bed denitration catalyst, which comprises the following steps:
S1. raw material is prepared: sodium metasilicate is configured to the aqueous solution of the 0-15%wt containing silica 1；Sulfuric acid is configured to 30-40%wt
Aqueous solution；Sodium tungstate is configured to the aqueous solution of the 10-15%wt containing tungstic acid；Titanyl sulfate is configured to 5- containing titanium dioxide
10%wt aqueous solution is spare；
S2. precursor synthesis: reactor tank stirring is added in silica containing sodium silicate aqueous solution, while aqueous sulfuric acid is added
Stop to PH4-5, and stirs；Slurry after reaction is warming up to 50-60 DEG C, heat preservation；
S3. catalyst synthesizes: the aqueous solution of titanyle sulfate containing titanium dioxide being added to the material of step S2 preparation, is stirred evenly
Afterwards, the wolframic acid sodium water solution containing tungstic acid is added, PH7-8 is adjusted after the completion of being added, then heats to 70-80 DEG C, keep the temperature,
Wherein the mass ratio between titanium dioxide, tungstic acid, silica is 1:1:4-5；
S4. it washes: the step S3 material prepared is washed, being washed till wash water conductivity is 300 μ S/cm or less；
S5. it dries: granulation is dried in the step S4 material prepared;
S6. it calcines: material of the step S5 after dry being calcined 1-2 hours at 400-450 DEG C, denitrating catalyst is made.
2. a kind of preparation method of fluidized bed denitration catalyst according to claim 1, it is characterised in that: in step S2,
After reactor tank is added in sodium silicate aqueous solution, at 20-30 DEG C, to be stirred under 100-200 revs/min of speed, with 50-100ml/min
Speed be added aqueous sulfuric acid.
3. a kind of preparation method of fluidized bed denitration catalyst according to claim 2, it is characterised in that: protected in step S2
The warm time is 20-30 minutes.
4. a kind of preparation method of fluidized bed denitration catalyst according to claim 1, it is characterised in that: in step S3,
The speed that the wolframic acid sodium water solution containing tungstic acid is added is 50-100ml/min.
5. a kind of preparation method of fluidized bed denitration catalyst according to claim 4, it is characterised in that: in step S3,
Soaking time is 1-2 hours.
6. a kind of preparation method of fluidized bed denitration catalyst according to claim 1, it is characterised in that: in step S5,
The operation temperature of drying-granulating is 200-250 DEG C of import, exports 90-100 DEG C, average grain diameter is 150-200 μm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112108153A (en) * | 2020-09-25 | 2020-12-22 | 北京信息科技大学 | High-throughput preparation micro system and method for iron-carbon catalyst |
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