CN101695656B - Method for preparing powdery selective catalytic reduction denitration catalyst by sol impregnation method - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000005470 impregnation Methods 0.000 title abstract description 10
- 238000010531 catalytic reduction reaction Methods 0.000 title abstract description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N oxalic acid Substances OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 67
- 230000008569 process Effects 0.000 claims abstract description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 230000003197 catalytic effect Effects 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 235000006408 oxalic acid Nutrition 0.000 claims description 16
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- NIFHFRBCEUSGEE-UHFFFAOYSA-N oxalic acid Chemical compound OC(=O)C(O)=O.OC(=O)C(O)=O NIFHFRBCEUSGEE-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000000227 grinding Methods 0.000 abstract description 5
- 238000011068 loading method Methods 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000004408 titanium dioxide Substances 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000012216 screening Methods 0.000 abstract 2
- 239000000779 smoke Substances 0.000 abstract 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 30
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 16
- 239000003426 co-catalyst Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000003546 flue gas Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- -1 metavanadic acid ammonium salt Chemical class 0.000 description 2
- XEEVLJKYYUVTRC-UHFFFAOYSA-N oxomalonic acid Chemical compound OC(=O)C(=O)C(O)=O XEEVLJKYYUVTRC-UHFFFAOYSA-N 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002803 maceration Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
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- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The method for preparing the powdery selective catalytic reduction denitration catalyst by using the sol impregnation method is a method for preparing the powdery SCR denitration catalyst by using sol metatitanic acid as an impregnation carrier. The method comprises the steps of carrying out primary impregnation loading on sol metatitanic acid serving as a carrier and an ammonium tungstate-oxalic acid solution, carrying out secondary impregnation loading on the prepared composite powder and an ammonium metavanadate-oxalic acid solution after a calcination, grinding and screening process, and finally carrying out secondary calcination, grinding and screening treatment to complete the preparation process of the powdery SCR denitration catalyst. Compared with the traditional SCR denitration catalyst preparation process, the method has the advantages of simple process and low economic cost, and is suitable for an integrated production mode of a titanium dioxide preparation process and an SCR denitration catalyst production process. The catalyst prepared by the method has the characteristics of large specific surface area, uniform and reasonable micropore structure, good thermal stability, ideal catalytic conversion efficiency on NOx components in smoke and the like.
Description
Technical field
The present invention relates to its preparation method of a kind of powdery selective catalytic reduction (SCR) denitrating catalyst, belong to environmental pollution prevention and control and clean coal combustion technology field.
Background technology
Coal is the main primary energy of China, the annual NOx that discharges in a large amount of coal-burning power plants that exist huge destruction to the environment band, nitrogen oxide (NOx) is that acid rain causes into gas with photochemical pollution.It is serious day by day that China NOx pollutes, and the air nitrous oxides concentration of some megapolis exceeds standard, and the environmental carrying capacity of nitrogen oxide is in saturation state basically, and some are local even photochemical fog occurs.
China carries out new " thermal power plant's atmosphere pollutants emission standards " (GB13223-2003) on January 1st, 2004, and NOx is discharged further strict regulations; Regulation in " collection of drainage dues use and management regulations " was imposed and SO NOx from July, 2005
2Identical charges for disposing pollutants.In China's power industry environmental protection Tenth Five-year plan, also the NOx improvement to power-plant flue gas has proposed concrete target and requirement.Based on these requirements, China all must take measures the discharging of NOx is controlled in most coal-burning power plants.
The selective catalytic reduction gas denitrifying technology has the efficient height as a kind of effective NOx improvement technology, and advantages such as selectivity is strong, good reliability through years of development, have obtained using widely in developed country, and just at the early-stage in China.The catalyst change cost of SCR method denitration accounts for very big proportion in operating cost, at present used catalyst all is external development and production, costs an arm and a leg.And, the existing TiO of China
2Raw material Deng producing denitrating catalyst does not also reach specification requirement, and the denitrating catalyst production technology does not also possess.These have become China's extensive use SCR method to carry out the main restricting factor that the power-plant flue gas denitration is handled.For this reason; Develop the SCR catalyst of low-cost production domesticization; Form technology with proprietary intellectual property rights and form investment and the operating cost that suitability for industrialized production will reduce China's denitrating flue gas greatly, to the development that China's flue gas NOx is handled, the improvement of China's environment plays huge impetus.
Among traditional SCR denitrating catalyst preparation technology, be employed in the powder catalytic agent carrier usually (like TiO
2) go up the method that dipping loads co-catalyst and catalytic active component, be about to material to be impregnated (like co-catalyst WO
3, catalyst body material V
2O
5) be dissolved as maceration extract, make TiO
2Powder immerses wherein, and the control temperature makes water evaporates, and then effective ingredient can be separated out and be added on TiO
2Matrix surface is accomplished loading procedure.After grind calcining, promptly obtained the SCR denitrating catalyst.This method operating process is easy, but there is following problem through analyzing: in the dipping process, such as WO
3Can only be carried in TiO Deng the co-catalyst composition
2Powder surface, matrix and dip composition structurally can not be combined closely, and can impact catalyst activity and heat endurance etc.
And utilize colloidal sol shape metatitanic acid to load active principle as the catalyst carrier step impregnation, then can effectively address the above problem.
Summary of the invention
Technical problem: the object of the present invention is to provide a kind of legal system of sol impregnation efficiently to be equipped with the method for powdery selective catalytic reduction denitration catalyst.
Technical scheme: proposed by the invention a kind of utilize colloidal sol shape metatitanic acid as impregnated carrier to prepare the method for Powdered SCR denitrating catalyst.Can be summarized as and utilize colloidal sol shape metatitanic acid earlier, carry out single-steeping with ammonium tungstate-oxalic acid solution and load, after calcining and grinding, make titanium dioxide-tungstic acid composite powder as carrier.Again this composite powder and ammonium metavanadate-oxalic acid solution are carried out the double-steeping loading, after process the powder catalyst finished product after the calcining and grinding.
Concrete grammar is:
Step 1. is with titanyl sulfate TiOSO
4Add in the entry, constantly stirring is dissolved it fully; Add a small amount of concentrated sulfuric acid simultaneously, regulator solution pH value is to 1-1.5;
Step 2. adds ammoniacal liquor rapidly in the solution that step 1 makes, make its pH value rise to 6.5-7.5, under 70 ℃～85 ℃ heating conditions, stirs 1～2 hour fast simultaneously, then obtains white metatitanic acid colloidal sol H
2TiO
3With this colloidal sol filtration washing repeatedly, remove wherein behind the heteroion subsequent use;
Step 3. is with oxalic acid C
2H
2O
4The oxalic acid solution of processing soluble in water is again with wolframic acid ammonium salt (NH
4)
5H
6[H
2(WO
4)
6] H
2O is dissolved in the oxalic acid solution, processes colourless ammonium tungstate-oxalic acid solution;
Step 4. is mixed ammonium tungstate-oxalic acid solution that step 3 makes with the metatitanic acid colloidal sol that step 2 makes, stirred 3～5 hours down in 50 ℃～65 ℃ heating conditions, makes first kind of mixed solution;
The mixed solution that step 5. makes step 4 was calcined 5～6 hours in 430 ℃～450 ℃ air atmospheres in the oven dry down of 100 ℃～105 ℃ environment again, ground to form behind the pressed powder of particle diameter less than 0.1mm subsequent use after the resultant solid cooled;
Step 6. is with the oxalic acid oxalic acid solution of processing soluble in water, again with metavanadic acid ammonium salt NH
4VO
3Be dissolved in the oxalic acid solution, process yellow ammonium metavanadate-oxalic acid solution;
After step 7. made step 6 ammonium metavanadate-oxalic acid solution and leaves standstill 1～1.5 hour, solution changed blueness gradually into;
The pressed powder that step 8. makes step 5 adds step 7 and goes on foot in the ammonium metavanadate-oxalic acid solution that makes, and stirs 3～5 hours down in 50 ℃～65 ℃ heating conditions, makes second kind of mixed solution;
Step 9. is dried second kind of mixed solution that step 8 makes down in 100 ℃～105 ℃ environment, in 430 ℃～450 ℃ air atmospheres, calcines 5～6 hours again, is ground to particle diameter after the resultant solid cooled less than 0.1mm, then makes required catalyst.
In step 1, with titanyl sulfate TiOSO
4Add in the entry, the amount ratio of titanyl sulfate and water is controlled in 8g～12g:100ml scope.
Amount ratio at step 3 mesoxalic acid and water is controlled at 8g～10g: in the 800ml scope.
The amount ratio of ammonium tungstate and titanyl sulfate is controlled at 5.2～8.0g in step 3: in the 100g scope.
Amount ratio at step 6 mesoxalic acid and water is controlled at 8g～10g: in the 600ml scope.
The amount ratio of ammonium metavanadate and titanyl sulfate is controlled at 0.4～0.8g in step 6: in the 100g scope.
Beneficial effect: prepared catalyst has following characteristics: the catalyst external form is graininess aspect microstructure, and the granule interior composition is mainly titanium dioxide (carrier) and tungstic acid (co-catalyst), and the two combines closely.And the particle skin is coated with vanadic anhydride composition (major catalyst) formation thin layer.This structure helps carrier and gives full play to its support and peptizaiton to co-catalyst, and helps bringing into play the raising catalyst overall thermal stability of co-catalyst, improves V
2O
5And TiO
2Between electronic action, the effect that improves catalyst activity, selectivity and stability.In addition, major catalyst forms outside thin layer, be of value to its with flue gas in fully the contacting of NOx composition, effectively bring into play the effect of catalyst reducing NOx.Apparent-microcosmic phenetic analysis to catalyst shows that the catalyst that makes than this method of conventional method has bigger reaction specific area; And the result of performance test test shows that too this catalyst has desirable NOx catalyzed conversion usefulness.
Be applicable to aspect the suitability for industrialized production in addition; Compare the method that the conventional powder dipping prepares catalyst; Adopt the sol impregnation method can omit titania-based system and be equipped with in the process drying steps middle product metatitanic acid colloidal sol; Load, reduced the complexity and the cost of catalyst manufacturing process and directly utilize colloidal sol to carry out active ingredient.Can effectively promote being connected between titanium dioxide production industry and the industry of SCR Preparation of Catalyst, for the integrated mode of production of the two, this invention has good applicability.
The specific embodiment
The preparation method of a kind of Powdered efficiently SCR denitrating catalyst of the present invention, catalytic component and content proportioning are controlled to be 1%V
2O
5-10%WO
3/ TiO
2(mass fraction), it is following that it produces step:
1) with (amount ratio of titanyl sulfate and water is controlled at 10g: 100ml) in a certain amount of titanyl sulfate adding suitable quantity of water; Constantly stirring dissolves it fully; Add a small amount of concentrated sulfuric acid simultaneously, (amount ratio of the concentrated sulfuric acid and water is controlled at 0.5ml to regulator solution pH value: 100ml) about 1;
2) 1) add a certain amount of ammoniacal liquor rapidly in the solution that makes of step; Make its pH value rise to that (amount ratio of industrial 30% concentration ammoniacal liquor and water is about 50ml: 300ml) about 7; Under 80 ℃ of heating conditions, stirred 1 hour fast simultaneously, then obtain white metatitanic acid colloidal sol (H
2TiO
3).With this colloidal sol filtration washing repeatedly, remove wherein behind the heteroion subsequent use;
3) process oxalic acid solution (amount ratio of oxalic acid and water is controlled at 10g: 800ml) oxalic acid is soluble in water; Again quantitative wolframic acid ammonium salt is dissolved in that (amount ratio of ammonium tungstate and titanyl sulfate is 6.6g: 100g), process colourless ammonium tungstate-oxalic acid solution in the oxalic acid solution;
4) with 3) ammonium tungstate-oxalic acid solution and 2 of making of step) the metatitanic acid colloidal sol that makes of step mixes, descends stirring 3 hours in 60 ℃ of heating conditions;
5) with 4) step makes mixed solution in the down oven dry of 105 ℃ of environment, calcining 5 hours in 450 ℃ of air atmospheres again, it is subsequent use after less than 0.1mm to be ground to particle diameter after the resultant solid cooled, has then accomplished the single-steeping process;
6) process oxalic acid solution (amount ratio of oxalic acid and water is controlled at 10g: 600ml) a certain amount of oxalic acid is soluble in water; Again quantitative metavanadic acid ammonium salt is dissolved in that (amount ratio of ammonium metavanadate and titanyl sulfate is 0.8g: 100g), process yellow ammonium metavanadate-oxalic acid solution in the oxalic acid solution;
7) with 6) after the step made ammonium metavanadate-oxalic acid solution and leave standstill 1 hour, solution changed blueness gradually into;
8) with 5) pressed powder that makes of step adds 7) in ammonium metavanadate-oxalic acid solution of making of step, and stirred 3 hours down in 60 ℃ of heating conditions;
9) with 8) step makes mixed solution in the down oven dry of 105 ℃ of environment, calcining 5 hours in 450 ℃ of air atmospheres again is ground to particle diameter less than 0.1mm after the resultant solid cooled, accomplish the double-steeping process after, then make required Powdered SCR denitrating catalyst.
Directly utilize colloidal sol shape metatitanic acid material in the preparation process; Than the method for preparing catalyst of the Powdered titanium dioxide of Traditional use as carrier; Omitted titania-based system and be equipped with in the process, reduced the complexity and the cost of catalyst manufacturing process steps such as the drying of middle product metatitanic acid colloidal sol and grindings.With the carrier of colloidal sol shape metatitanic acid as the single-steeping process, help the uniform load of co-catalyst composition at carrier surface, prepared catalyst has bigger specific area and uniform surface micropore gap structure, and has good heat endurance.
Adopt the powder impregnation method to carry out the double-steeping loading procedure, help of the stratification load of major catalyst composition on carrier and co-catalyst surface.And, help itself and fully the contacting of flue gas, so prepared catalyst has good catalytic conversion usefulness to the NOx component in the flue gas because the covering that the major catalyst composition can not receive other material is sheltered.
Claims (1)
1. the preparation method of a Powdered efficiently SCR denitrating catalyst is characterized in that catalytic component and mass fraction content proportioning are controlled to be 1%V
2O
5-10%WO
3/ TiO
2, it is following that it produces step:
1). a certain amount of titanyl sulfate is added in the suitable quantity of water; The amount ratio of titanyl sulfate and water is controlled at 10g: 100ml, and constantly stirring is dissolved it fully, adds a small amount of concentrated sulfuric acid simultaneously; Regulator solution pH value is 1, and the amount ratio of the concentrated sulfuric acid and water is controlled at 0.5ml: 100ml;
2). 1) add ammoniacal liquor rapidly in the solution that makes of step, make its pH value rise to 7, quick stirring 1 hour under 80 ℃ of heating conditions simultaneously then obtains white metatitanic acid colloidal sol H
2TiO
3,, remove wherein behind the heteroion subsequent use with this colloidal sol filtration washing repeatedly;
3). with the oxalic acid oxalic acid solution of processing soluble in water, the amount ratio of oxalic acid and water is controlled at 10g: 800ml, more quantitative ammonium tungstate is dissolved in the oxalic acid solution, the amount ratio of ammonium tungstate and titanyl sulfate is 6.6g: 100g, processes colourless ammonium tungstate-oxalic acid solution;
4). with 3) ammonium tungstate-oxalic acid solution and 2 of making of step) the metatitanic acid colloidal sol that makes of step mixes, descends stirring 3 hours in 60 ℃ of heating conditions;
5). with 4) step makes mixed solution in the down oven dry of 105 ℃ of environment, calcining 5 hours in 450 ℃ of air atmospheres again, it is subsequent use after less than 0.1mm to be ground to particle diameter after the resultant solid cooled, has then accomplished the single-steeping process;
6). with a certain amount of oxalic acid oxalic acid solution of processing soluble in water; The amount ratio of oxalic acid and water is controlled at 10g: 600ml; Quantitative ammonium metavanadate is dissolved in the oxalic acid solution, the amount ratio of ammonium metavanadate and titanyl sulfate is 0.8g: 100g again, processes yellow ammonium metavanadate-oxalic acid solution;
7). with 6) after the step made ammonium metavanadate-oxalic acid solution and leave standstill 1 hour, solution changed blueness gradually into;
8). with 5) pressed powder that makes of step adds 7) in ammonium metavanadate-oxalic acid solution of making of step, and stirred 3 hours down in 60 ℃ of heating conditions;
9). with 8) step makes mixed solution in the down oven dry of 105 ℃ of environment, calcining 5 hours in 450 ℃ of air atmospheres again is ground to particle diameter less than 0.1mm after the resultant solid cooled, accomplish the double-steeping process after, then make required Powdered SCR denitrating catalyst.
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| CN102000562B (en) * | 2010-12-29 | 2012-05-23 | 中国科学院广州能源研究所 | Efficient denitration catalyst and preparation method thereof |
| CN102091613A (en) * | 2011-01-26 | 2011-06-15 | 东南大学 | Dual-flocculation forming preparation method of selective catalytic reduction denitration catalyst |
| CN102350339A (en) * | 2011-08-23 | 2012-02-15 | 无锡迅德环保科技有限公司 | Catalyst used for power plant coal-fired flue gas SCR (selective catalyctic reduction) denitration and a preparation method |
| CN103028394A (en) * | 2011-10-10 | 2013-04-10 | 河南佰利联化学股份有限公司 | Preparation method of titanium dioxide for denitration through use of metatitanic acid |
| CN103028392A (en) * | 2011-10-10 | 2013-04-10 | 河南佰利联化学股份有限公司 | Preparation method of titanium dioxide for denitration through use of titanium tetrachloride |
| DE102016110374A1 (en) * | 2016-06-06 | 2017-12-07 | Huntsman P&A Germany Gmbh | Titanium dioxide sol, process for its preparation and products derived therefrom |
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