CN101767003A - Low-temperature SCR catalyst with V-doped TiO2 as carrier and preparation method thereof - Google Patents
Low-temperature SCR catalyst with V-doped TiO2 as carrier and preparation method thereof Download PDFInfo
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- CN101767003A CN101767003A CN200910219515A CN200910219515A CN101767003A CN 101767003 A CN101767003 A CN 101767003A CN 200910219515 A CN200910219515 A CN 200910219515A CN 200910219515 A CN200910219515 A CN 200910219515A CN 101767003 A CN101767003 A CN 101767003A
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Abstract
The invention relates to a low-temperature SCR catalyst with V-doped TiO2 as a carrier and a preparation method thereof. The low-temperature SCR catalyst is characterized in that: the catalyst adopts the V-doped TiO2 as the carrier and adopts load MnOX as an active component, wherein the mole ratio of the doped element V is 1 to 10% of that of the element Ti in the TiO2, and the loading capacity of the MnOX is within 10 to 60%. The preparation method for the catalyst includes the following steps: V-doped TiO2 gel is prepared by a sol-gel method, the active component of the load MnOX is ball-milled by a wet method, and finally the low-temperature SCR denitration catalyst is obtained through drying, calcining and grinding. As the TiO2 carrier is V-doped and preparation conditions are optimized, the denitration efficiency of the catalyst is increased and a catalytic activity temperature window is widened.
Description
Technical field
The invention belongs to air contaminant treatment technology and environment protection catalytic material field, be specifically related to a kind of TiO that mixes with V
2Be low-temperature SCR catalyst of carrier and preparation method thereof.
Background technology
The scope and the degree of China NOx pollution in recent years are quite serious.People such as German scholar Richter reported on Nature in 2005: NO in the troposphere, area, Eastern China
2Content, having increased nearly 50%, 1997 year growth rate from 1996 to 2004 is 4%, and 2002 annual growths have reached 12%.People such as American scholar Streets report that China's nineteen ninety-five NOx total emission volumn is 1,200 ten thousand tons, and prediction is not if take control measure, will reach 26,600,000 tons to the total emission volumn of the year two thousand twenty NOx.Therefore, the NOx that eliminates as one of atmosphere pollution main source just becomes particularly important.From on July 1st, 2004, China announces and implements " thermal power plant's atmosphere pollutants emission standards ", thermal power plant's discharged nitrous oxides is required to have increased significantly, in order to satisfy the NOx emission request that government formulates, the elimination of NOx (DeNOx) technology is one of object of paying close attention to of researcher always, in numerous denitration technologies, SCR (selective catalytic reduction) technology denitration efficiency is the highest, is the research focus that removes in the NOx field.
The carrier of most of SCR catalyst adopts TiO
2Or loose structure such as zeolite, also there is the research report to use Al
2O
3, activated carbon and activated coke be as the carrier of SCR catalyst.Though it is active to prove that through actual project quality inspection these carriers have a good adaptation, owing to form simply, to sulphur and steam sensitivity, and catalyst can wear and tear by dust in flue gas, influences service life.Therefore existing SCR denitrating catalyst is improved to improve and become the problem that presses for solution in its denitration efficiency and service life.
Summary of the invention
The purpose of this invention is to provide a kind of TiO that mixes with V
2Be low-temperature SCR catalyst of carrier and preparation method thereof, the out of stock efficient of catalyst that exists with effective solution prior art is lower, the problem that service life is short.
For addressing the above problem, the technical solution adopted in the present invention is: a kind of TiO that mixes with V
2Low-temperature SCR catalyst for carrier is characterized in that: described catalyst is the TiO that mixes with V
2Be carrier, load MnO
XAs the activity of such catalysts component.
In the above-mentioned catalyst, the molal quantity of doped chemical V is TiO
21～10% of middle Ti element molal quantity, MnO
XLoad capacity be 10～60%.
Above-mentioned Preparation of catalysts method comprises the steps: successively
Step 1: absolute ethyl alcohol and butyl titanate 1: 0.4 by volume～1.2 are mixed, obtain solution A; Be 1: 0.3～0.8: 3～5 to mix again by volume with C solution, glacial acetic acid and absolute ethyl alcohol, obtain solution B, wherein the composition of C solution is that the concentration of a certain amount of ammonium metavanadate of dissolving is 50% oxalic acid solution, and the molal quantity of control V is 1～10% of a Ti element molal quantity.
Step 2: 1: 0.3 by volume～3 slowly are added drop-wise to B solution in the A solution, constantly stir, and form the colloidal sol of homogeneous transparent, and ageing is after 24～72 hours, place baking oven in 100 ℃ of dryings 24 hours, obtain V doped Ti O
2Xerogel.
Step 3: with active component MnO
XForm with manganese acetate is introduced, wherein the TiO of manganese acetate and V doping
2Xerogel is poured ball grinder in the ratio of load capacity 10～60%, wet ball grinding mixes, mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 300～600 ℃ of calcinings 1～3 hour again it after drying is finished, and obtains load MnO after the grinding
XV doped Ti O
2Low-temperature SCR catalyst.
Compared with prior art, advantage of the present invention is:
1, processing step is simple to operate, and production cost reduces greatly.
2, Zhi Bei low-temperature SCR catalyst denitration efficiency height, wide, the long service life of active temperature windows have bigger specific area and higher heat endurance.
The specific embodiment
The present invention is described in detail below in conjunction with the specific embodiment.
Embodiment 1
30mL absolute ethyl alcohol and 12mL butyl titanate are obtained solution A through mixing; The concentration that to dissolve ammonium metavanadate 0.17g again is that 50% oxalic acid solution 10mL, glacial acetic acid 3mL, absolute ethyl alcohol 30mL obtain solution B through mixing; B solution slowly is added drop-wise in the A solution, constantly stirs, form the colloidal sol of homogeneous transparent, ageing is after 24～24 hours, places baking oven in 100 ℃ of dryings 24 hours, obtains V doped Ti O
2Xerogel; 2.68g manganese acetate and above-mentioned xerogel are poured in the ball grinder, and wet ball grinding mixes, and mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 300 ℃ of calcinings 1 hour again it after drying is finished, and obtains load MO after the grinding
XV doped Ti O
2The low-temperature SCR catalyst sample.
Catalyst is packed in the catalytic reactor, feed simulated flue gas, gas composition: the NO about 0.05% (intrinsic standoff ratio) (wherein contains about NO of about 5%
2), the NH of 0.05% (intrinsic standoff ratio)
3, O
2Intrinsic standoff ratio 5%, all the other are balanced gas N
2, be 12000h in air speed
-1, under the condition that reaction temperature is 150～300 ℃, NO removal efficiency 85～98%.
Embodiment 2
30mL absolute ethyl alcohol and 12mL butyl titanate are obtained solution A through mixing; The concentration that to dissolve ammonium metavanadate 0.17g again is that 50% oxalic acid solution 10mL, glacial acetic acid 3mL, absolute ethyl alcohol 30mL obtain solution B through mixing; B solution slowly is added drop-wise in the A solution, constantly stirs, form the colloidal sol of homogeneous transparent, ageing is after 24～24 hours, places baking oven in 100 ℃ of dryings 24 hours, obtains V doped Ti O
2Xerogel; 16.08g manganese acetate and above-mentioned xerogel are poured in the ball grinder, and wet ball grinding mixes, and mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 300 ℃ of calcinings 3 hours again it after drying is finished, and obtains load MO after the grinding
XV doped Ti O
2The low-temperature SCR catalyst sample.
Catalyst is packed in the catalytic reactor, feed simulated flue gas, gas composition: the NO about 0.05% (intrinsic standoff ratio) (wherein contains about NO of about 5%
2), the NH of 0.05% (intrinsic standoff ratio)
3, O
2Intrinsic standoff ratio 5%, all the other are balanced gas N
2, be 12000h in air speed
-1, under the condition that reaction temperature is 150～300 ℃, NO removal efficiency 85～98%.
Embodiment 3
30mL absolute ethyl alcohol and 12mL butyl titanate are obtained solution A through mixing; The concentration that to dissolve ammonium metavanadate 0.17g again is that 50% oxalic acid solution 10mL, glacial acetic acid 3mL, absolute ethyl alcohol 30mL obtain solution B through mixing; B solution slowly is added drop-wise in the A solution, constantly stirs, form the colloidal sol of homogeneous transparent, ageing is after 24～24 hours, places baking oven in 100 ℃ of dryings 24 hours, obtains V doped Ti O
2Xerogel; 2.68g manganese acetate and above-mentioned xerogel are poured in the ball grinder, and wet ball grinding mixes, and mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 500 ℃ of calcinings 1 hour again it after drying is finished, and obtains load MO after the grinding
XV doped Ti O
2The low-temperature SCR catalyst sample.
Catalyst is packed in the catalytic reactor, feed simulated flue gas, gas composition: the NO about 0.05% (intrinsic standoff ratio) (wherein contains about NO of about 5%
2), the NH of 0.05% (intrinsic standoff ratio)
3, O
2Intrinsic standoff ratio 5%, all the other are balanced gas N
2, be 12000h in air speed
-1, under the condition that reaction temperature is 150～300 ℃, NO removal efficiency 85～98%.
Embodiment 4
30mL absolute ethyl alcohol and 12mL butyl titanate are obtained solution A through mixing; The concentration that to dissolve ammonium metavanadate 0.17g again is that 50% oxalic acid solution 10mL, glacial acetic acid 3mL, absolute ethyl alcohol 30mL obtain solution B through mixing; B solution slowly is added drop-wise in the A solution, constantly stirs, form the colloidal sol of homogeneous transparent, ageing is after 24～24 hours, places baking oven in 100 ℃ of dryings 24 hours, obtains the xerogel of V doped Ti O2; 16.08g manganese acetate and above-mentioned xerogel are poured in the ball grinder, and wet ball grinding mixes, and mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 500 ℃ of calcinings 3 hours again it after drying is finished, and obtains load MO after the grinding
XV doped Ti O
2The low-temperature SCR catalyst sample.
Catalyst is packed in the catalytic reactor, feed simulated flue gas, gas composition: the NO about 0.05% (intrinsic standoff ratio) (wherein contains about NO of about 5%
2), the NH of 0.05% (intrinsic standoff ratio)
3, O
2Intrinsic standoff ratio 5%, all the other are balanced gas N
2, be 12000h in air speed
-1, under the condition that reaction temperature is 150～300 ℃, NO removal efficiency 85～98%.
Embodiment 5
30mL absolute ethyl alcohol and 36mL butyl titanate are obtained solution A through mixing; The concentration that to dissolve ammonium metavanadate 5.1g again is that 50% oxalic acid solution 30mL, glacial acetic acid 24mL, absolute ethyl alcohol 90mL obtain solution B through mixing; B solution slowly is added drop-wise in the A solution, constantly stirs, form the colloidal sol of homogeneous transparent, ageing is after 24～24 hours, places baking oven in 100 ℃ of dryings 24 hours, obtains V doped Ti O
2Xerogel; 2.68g manganese acetate and above-mentioned xerogel are poured in the ball grinder, and wet ball grinding mixes, and mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 300 ℃ of calcinings 1 hour again it after drying is finished, and obtains load MO after the grinding
XV doped Ti O
2The low-temperature SCR catalyst sample.
Catalyst is packed in the catalytic reactor, feed simulated flue gas, gas composition: the NO about 0.05% (intrinsic standoff ratio) (wherein contains about NO of about 5%
2), the NH of 0.05% (intrinsic standoff ratio)
3, O
2Intrinsic standoff ratio 5%, all the other are balanced gas N
2, be 12000h in air speed
-1, under the condition that reaction temperature is 150～300 ℃, NO removal efficiency 85～98%.
Embodiment 6
30mL absolute ethyl alcohol and 36mL butyl titanate are obtained solution A through mixing; The concentration that to dissolve ammonium metavanadate 5.1g again is that 50% oxalic acid solution 30mL, glacial acetic acid 24mL, absolute ethyl alcohol 90mL obtain solution B through mixing; B solution slowly is added drop-wise in the A solution, constantly stirs, form the colloidal sol of homogeneous transparent, ageing is after 24～24 hours, places baking oven in 100 ℃ of dryings 24 hours, obtains V doped Ti O
2Xerogel; 16.08g manganese acetate and above-mentioned xerogel are poured in the ball grinder, and wet ball grinding mixes, and mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 300 ℃ of calcinings 3 hours again it after drying is finished, and obtains load MO after the grinding
XV doped Ti O
2The low-temperature SCR catalyst sample.
Catalyst is packed in the catalytic reactor, feed simulated flue gas, gas composition: the NO about 0.05% (intrinsic standoff ratio) (wherein contains about NO of about 5%
2), the NH of 0.05% (intrinsic standoff ratio)
3, O
2Intrinsic standoff ratio 5%, all the other are balanced gas N
2, be 12000h in air speed
-1, under the condition that reaction temperature is 150～300 ℃, NO removal efficiency 85～98%.
Embodiment 7
30mL absolute ethyl alcohol and 36mL butyl titanate are obtained solution A through mixing; The concentration that to dissolve ammonium metavanadate 5.1g again is that 50% oxalic acid solution 30mL, glacial acetic acid 24mL, absolute ethyl alcohol 90mL obtain solution B through mixing; B solution slowly is added drop-wise in the A solution, constantly stirs, form the colloidal sol of homogeneous transparent, ageing is after 24～24 hours, places baking oven in 100 ℃ of dryings 24 hours, obtains V doped Ti O
2Xerogel; 2.68g manganese acetate and above-mentioned xerogel are poured in the ball grinder, and wet ball grinding mixes, and mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 500 ℃ of calcinings 1 hour again it after drying is finished, and obtains load MO after the grinding
XV doped Ti O
2The low-temperature SCR catalyst sample.
Catalyst is packed in the catalytic reactor, feed simulated flue gas, gas composition: the NO about 0.05% (intrinsic standoff ratio) (wherein contains about NO of about 5%
2), the NH of 0.05% (intrinsic standoff ratio)
3, O
2Intrinsic standoff ratio 5%, all the other are balanced gas N
2, be 12000h in air speed
-1, under the condition that reaction temperature is 150～300 ℃, NO removal efficiency 85～98%.
Embodiment 8
30mL absolute ethyl alcohol and 36mL butyl titanate are obtained solution A through mixing; The concentration that to dissolve ammonium metavanadate 5.1g again is that 50% oxalic acid solution 30mL, glacial acetic acid 24mL, absolute ethyl alcohol 90mL obtain solution B through mixing; B solution slowly is added drop-wise in the A solution, constantly stirs, form the colloidal sol of homogeneous transparent, ageing is after 24～24 hours, places baking oven in 100 ℃ of dryings 24 hours, obtains V doped Ti O
2Xerogel; 16.08g manganese acetate and above-mentioned xerogel are poured in the ball grinder, and wet ball grinding mixes, and mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 500 ℃ of calcinings 3 hours again it after drying is finished, and obtains load MO after the grinding
XV doped Ti O
2The low-temperature SCR catalyst sample.
Catalyst is packed in the catalytic reactor, feed simulated flue gas, gas composition: the NO about 0.05% (intrinsic standoff ratio) (wherein contains about NO of about 5%
2), the NH of 0.05% (intrinsic standoff ratio)
3, O
2Intrinsic standoff ratio 5%, all the other are balanced gas N
2, be 12000h in air speed
-1, under the condition that reaction temperature is 150～300 ℃, NO removal efficiency 85～98%.
Claims (3)
1. TiO who mixes with V
2Low-temperature SCR catalyst for carrier is characterized in that: described catalyst is the TiO that mixes with V
2Be carrier, load MnO
XAs the activity of such catalysts component.
2. a kind of TiO that mixes with V according to claim 1
2Low-temperature SCR catalyst for carrier is characterized in that: the molal quantity of doped chemical V is TiO
21～10% of middle Ti element molal quantity, MnO
XLoad capacity be 10～60%.
3. a kind of TiO that mixes with V according to claim 1 and 2
2Low-temperature SCR catalyst for carrier is characterized in that: above-mentioned Preparation of catalysts method comprises the steps: successively
Step 1: absolute ethyl alcohol and butyl titanate 1: 0.4 by volume～1.2 are mixed, obtain solution A; Be 1: 0.3～0.8: 3～5 to mix again by volume with C solution, glacial acetic acid and absolute ethyl alcohol, obtain solution B, wherein the composition of C solution is that the concentration of a certain amount of ammonium metavanadate of dissolving is 50% oxalic acid solution, and the molal quantity of control V is 1～10% of a Ti element molal quantity;
Step 2: 1: 0.3 by volume～3 slowly are added drop-wise to B solution in the A solution, constantly stir, and form the colloidal sol of homogeneous transparent, and ageing is after 24～72 hours, place baking oven in 100 ℃ of dryings 24 hours, obtain V doped Ti O
2Xerogel;
Step is with active component MnO
XForm with manganese acetate is introduced, wherein the TiO of manganese acetate and V doping
2Xerogel is poured ball grinder in the ratio of load capacity 10～60%, wet ball grinding mixes, mixture places baking oven in 100 ℃ of dryings 24 hours, places Muffle furnace in 300～600 ℃ of calcinings 1～3 hour again it after drying is finished, and obtains load MnO after the grinding
XV doped Ti O
2Low-temperature SCR catalyst.
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| CN102125834A (en) * | 2011-01-14 | 2011-07-20 | 上海交通大学 | Titanium-based nano-composite metal oxide catalyst and preparation method thereof |
| CN105964244A (en) * | 2016-05-09 | 2016-09-28 | 大唐南京环保科技有限责任公司 | Vanadium-titanium powder suitable for denitration catalyst with multitime regeneration as well as preparation method and application thereof |
| CN108380225A (en) * | 2018-02-07 | 2018-08-10 | 齐齐哈尔大学 | A kind of synthetic method of the anti-inactivation denitrating catalyst of efficient cryogenic |
| CN109675549A (en) * | 2019-01-08 | 2019-04-26 | 中盐金坛盐化有限责任公司 | A kind of stratiform MXene doping prepares the method for catalyst and the application in gas purification |
| CN111790401A (en) * | 2020-06-22 | 2020-10-20 | 山东东岳高分子材料有限公司 | Catalyst for synthesizing hexafluoroisopropanol, preparation method and application |
| CN112121788A (en) * | 2020-09-22 | 2020-12-25 | 江苏大学 | Preparation method and application of B-modified vanadium-titanium low-temperature SCR catalyst |
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| CN101480611B (en) * | 2009-02-04 | 2010-12-08 | 北京科技大学 | Vanadium-doped titanium-base flue gas denitration catalyst material and preparation method thereof |
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2009
- 2009-12-16 CN CN200910219515XA patent/CN101767003B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102125834A (en) * | 2011-01-14 | 2011-07-20 | 上海交通大学 | Titanium-based nano-composite metal oxide catalyst and preparation method thereof |
| CN105964244A (en) * | 2016-05-09 | 2016-09-28 | 大唐南京环保科技有限责任公司 | Vanadium-titanium powder suitable for denitration catalyst with multitime regeneration as well as preparation method and application thereof |
| CN105964244B (en) * | 2016-05-09 | 2018-11-09 | 大唐南京环保科技有限责任公司 | A kind of vanadium titanium valve and the preparation method and application thereof being suitable for repeatedly regeneration denitrating catalyst |
| CN108380225A (en) * | 2018-02-07 | 2018-08-10 | 齐齐哈尔大学 | A kind of synthetic method of the anti-inactivation denitrating catalyst of efficient cryogenic |
| CN108380225B (en) * | 2018-02-07 | 2022-11-29 | 齐齐哈尔大学 | Synthetic method of low-temperature efficient deactivation-resistant denitration catalyst |
| CN109675549A (en) * | 2019-01-08 | 2019-04-26 | 中盐金坛盐化有限责任公司 | A kind of stratiform MXene doping prepares the method for catalyst and the application in gas purification |
| CN111790401A (en) * | 2020-06-22 | 2020-10-20 | 山东东岳高分子材料有限公司 | Catalyst for synthesizing hexafluoroisopropanol, preparation method and application |
| CN112121788A (en) * | 2020-09-22 | 2020-12-25 | 江苏大学 | Preparation method and application of B-modified vanadium-titanium low-temperature SCR catalyst |
| CN112121788B (en) * | 2020-09-22 | 2023-07-18 | 江苏大学 | Preparation method and application of B-modified vanadium-titanium low-temperature SCR catalyst |
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