CN103920488A - Denitrification catalyst adopting tungsten acidified zirconia as carrier as well as preparation method and application thereof - Google Patents
Denitrification catalyst adopting tungsten acidified zirconia as carrier as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a denitrification catalyst adopting tungsten acidified zirconia as a carrier as well as a preparation method and application thereof. The tungsten acidified zirconia is used as the carrier, and cerium oxide and vanadium pentoxide are used as active components; the molar ratio of tungsten to zirconium in the carrier is 0.6 to 5; the molar ratio of Ce to V in the active components is 0.05 to 20. The denitrification catalyst is excellent in denitrification activity, selectivity and alkali metal/alkaline-earth metal toxicity resistance. A simulated smoke test result proves that when the reaction temperature is 200 to 420 DEG C, the NOx purification efficiency is higher than 95 percent, the N2 selectivity in products is higher than 98 percent, and after the catalyst is soaked and loaded with the alkali metal/alkaline-earth metal substances with the mass fraction of 5 percent, the NOX purification efficiency still can be higher than 90 percent.
Description
Technical field
The invention belongs to air pollution control technique field, be specifically related to a kind of denitrating catalyst and preparation and application thereof that wolframic acid zirconia is carrier of take.
Background technology
Biomass combustion is considered to one of replacer of fossil fuel, can reduce CO2 emission.In world wide, there are a plurality of countries to propose the hard objectives of Developing Biomass fuel, as: according to European Union, be planned in one's early years 2010, in living beings heat supply and fuel used to generate electricity, living beings account for 10%.Biomass boiler also develops rapidly in China in recent years, according to China < < regenerative resource Long-and Medium-term Development planning > >, to the year two thousand twenty, biomass power generation total installation of generating capacity will reach 3,000 ten thousand kilowatts, biomass solid formed fuel year utilization will reach 5,000 ten thousand tons.Biomass combustion will inevitably produce nitrogen oxide (NOx), cause environmental pollution.
Cement industry is the important basic activity of China, but be also the key industry that nitrogen oxide is controlled simultaneously, the NOx discharge capacity of national cement industry in 2010 accounts for 10% of China NOx industrial source total emission volumn, has become the third-largest fixed discharge source occupying after station boiler and Industrial Boiler.The emission problem of NOx has become the restraining factors of cement industry sustainable development.
SCR (SCR) technology is the one preferred technique that stationary source NOx controls, V
2o
5(WO
3)/TiO
2it is the maximum commercial denitrating catalyst of application.In the industry always denitration efficiency, selective, stability, mechanical strength, SO
2oxygenation efficiency is as the most important Performance Evaluating Indexes of denitrating catalyst, yet along with the application of SCR technology at biomass electric power plant and cement industry, catalyst also becomes important Performance Evaluating Indexes to the resistance of alkali and alkaline earth metal ions.In biomass boiler and cement kiln flue gas, alkali and alkaline earth metal ions content is far above coal-burning power plant, and denitrating catalyst is rapid inactivation under the effect of alkali and alkaline earth metal ions.In recent years, Chinese scholars had been reported alkali metal, the alkaline-earth metal intoxicating phenomenon of the catalyst such as vanadium class, cerium class, manganese class, iron class successively, attracted wide attention.As: in the U.S., certain uses on the boiler of scoot and PRB coal (close with the ature of coal of China shenfu coal), and the vanadium class catalyst deactivation rate of every thousand hours is up to 18%, and its main cause is deposition, the growth of alkali and alkaline earth metal ions sulfate.About deactivation mechanism, early stage research is mostly owing to catalyst surface
the destruction of acidic site and duct are stopped up, and research afterwards finds that active material is combined the decline of rear oxidation reducing power with poisonous substance be also major reason.
For the technical need of adapted biomass boiler and cement kiln denitration, the catalyst that exploitation has excellent alkali metal/alkaline-earth metal resistance is significant.Chinese patent CN102658172A discloses a kind of denitrating catalyst that Sulfated zirconia is co-catalyst as carrier, the rare-earth oxide of take as active component, the transition metal oxide of take of take, and this catalyst has good anti-alkali and alkaline earth metal ions poisoning performance.Chinese patent CN102500358B discloses a kind of denitrating catalyst that protonated titanium nanotube is active material and co-catalyst as carrier, metal oxide of take, and this catalyst has a good especially resistance to alkali and alkaline earth metal ions is poisoning.The disclosed catalyst of above-mentioned patent all has excellent alkali metal/alkaline-earth metal resistance, is successful case, yet in order to strengthen stability, mechanical strength, SO
2the performances such as oxygenation efficiency, often need to add co-catalyst, cause the preparation technology of catalyst comparatively complicated.
Summary of the invention
For solving the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is to provide a kind of denitrating catalyst that wolframic acid zirconia is carrier of take.
Another object of the present invention is to provide above-mentioned preparation method of take the denitrating catalyst that wolframic acid zirconia is carrier.
A further object of the present invention is to provide above-mentioned application of take the denitrating catalyst that wolframic acid zirconia is carrier.
For achieving the above object, the present invention adopts following technical scheme:
The denitrating catalyst that the wolframic acid zirconia of take is carrier, it is carrier that described denitrating catalyst be take the zirconia of wolframic acid, take cerium oxide and vanadic anhydride as active component; In described carrier, the mol ratio of tungsten and zirconium is 0.6～5; The mol ratio of described active component cerium and vanadium is 0.05～20.
Preferably, the mass fraction of described active component in denitrating catalyst is 0.1～15%.
Above-mentioned preparation method of take the denitrating catalyst that wolframic acid zirconia is carrier, comprises the following steps:
(1) presoma of the presoma of zirconium and tungsten is soluble in water, make precursor solution; Then in precursor solution, add ammoniacal liquor, pH is adjusted to 8～9, after stirring 2～6h, standing 2～48h is standby;
(2) reacting liquid filtering after step (1) is standing, taking precipitate, then by it 60～120 ℃ of oven dry, then in 400～800 ℃ of roasting 2～12h, make wolframic acid zirconia, be finally ground into powder;
(3) presoma of vanadium is dissolved with saturated oxalic acid solution, the presoma water of cerium is dissolved, then two kinds of solution are mixed, obtain precursor mixed solution; The wolframic acid Zirconium oxide powder again step (2) being made adds in precursor mixed solution, stirs dipping 2～48h, after 60～120 ℃ of oven dry, and in 400～800 ℃ of roasting 2～12h, the denitrating catalyst that the wolframic acid zirconia of take described in obtaining is carrier.
Preferably, the presoma of described zirconium is a kind of in zirconyl nitrate, zirconyl chloride and zirconium carbonate.
Preferably, the presoma of described tungsten is ammonium paratungstate or wolframic acid.
Preferably, the presoma of described vanadium is ammonium metavanadate.
Preferably, the presoma of described cerium is cerous nitrate or ammonium ceric nitrate.
Above-mentionedly take the application in the flue gas of processing high-load alkali and alkaline earth metal ions of denitrating catalyst that wolframic acid zirconia is carrier.
Principle of the present invention is: zirconia has good heat endurance and mechanical performance, but acidity a little less than.Wolframic acid zirconia has strong acid characteristic, can slow down the destruction of alkali and alkaline earth metal ions to acidity of catalyst position, and meanwhile, highly acid position can interact with alkali and alkaline earth metal ions, they is fixed, thereby stop their contact active components.The present invention has introduced W elements in tungsten acidization, and this will further improve the heat endurance of catalyst, and suppresses to a certain extent SO
2oxygenation efficiency.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) denitrating catalyst of the present invention has excellent denitration activity, selective and alkali resistant metal/alkaline-earth metal poisoning performance, and simulated flue gas test result shows, between 200～420 ℃ of reaction temperatures, NOx purification efficiency is higher than 95%, N in product
2selectively higher than 98%, catalyst soakage load after mass fraction alkali metal/alkaline-earth metal material that is 5%, NOx purification efficiency still can be higher than 90%.
(2) denitrating catalyst preparation method of the present invention is simple, and without load tungsten is as co-catalyst separately, the catalyst making is compared traditional commercial catalyst and had the longer life-span.
(3) denitrating catalyst of the present invention is specially adapted to the flue gas that alkali and alkaline earth metal ions content is high, such as biomass electric power plant and cement kiln flue gas.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
A preparation method for the denitrating catalyst that the wolframic acid zirconia of take is carrier, comprises the following steps:
(1) take respectively 20g zirconyl nitrate and 14.7g ammonium paratungstate, the two is dissolved in 50mL deionized water and is mixed with solution; Toward dripping ammoniacal liquor to pH value in solution, be 8, stir 2h, standing 2h;
(2) reactant liquor after step (1) is standing leaches sediment, and by sediment 60 ℃ of oven dry in baking oven, in Muffle furnace, 400 ℃ of roasting 12h, make wolframic acid zirconia, are ground into powder;
(3) take 0.027g ammonium metavanadate, be dissolved in 25mL saturated oxalic acid solution, take 0.005g cerous nitrate, be dissolved in 25mL deionized water, two kinds of solution are mixed; Then add the ground wolframic acid zirconia of step (2), stir dipping 2h, 60 ℃ of oven dry in baking oven, in Muffle furnace, 400 ℃ of roasting 12h, make catalyst finished product.
The W/Zr mol ratio of catalyst finished product is that 0.6, Ce/V mol ratio is 0.05, and active component mass fraction is 0.1%.Catalyst finished product is ground, get the wherein catalyst fines 0.5g of 40～60 order sizes, put into quartz tube reactor and test its denitration activity, result shows, between 200～420 ℃ of reaction temperatures, NOx purification efficiency is higher than 95%, N in product
2selectively higher than 98%; Toward the potassium compound of dip loading 5% in catalyst finished product, and then by above-mentioned steps and method test denitration activity, result shows, NOx purification efficiency still can be higher than 90%.
Embodiment 2
A preparation method for the denitrating catalyst that the wolframic acid zirconia of take is carrier, comprises the following steps:
(1) take respectively 1g zirconyl chloride and 3.88g wolframic acid, the two is dissolved in 50mL deionized water and is mixed with solution; Toward dripping ammoniacal liquor to pH value in solution, be 9, stir 6h, standing 6h;
(2) reactant liquor after step (1) is standing leaches sediment, and by sediment 70 ℃ of oven dry in baking oven, in Muffle furnace, 450 ℃ of roasting 10h, make wolframic acid zirconia, are ground into powder;
(3) take 0.01g ammonium metavanadate, be dissolved in 25mL saturated oxalic acid solution, take 0.937g ammonium ceric nitrate, be dissolved in 25mL deionized water, two kinds of solution are mixed; Then add the ground wolframic acid zirconia of step (2), stir dipping 6h, 70 ℃ of oven dry in baking oven, in Muffle furnace, 450 ℃ of roasting 10h, make catalyst finished product.
The W/Zr mol ratio of catalyst finished product is that 5, Ce/V mol ratio is 20, and active component mass fraction is 7%.Catalyst finished product is ground, get the wherein catalyst fines 0.5g of 40～60 order sizes, put into quartz tube reactor and test its denitration activity, result shows, between 200～420 ℃ of reaction temperatures, NOx purification efficiency is higher than 95%, N in product
2selectively higher than 98%; Toward the calcium compound of dip loading 5% in catalyst finished product, and then by above-mentioned steps and method test denitration activity, result shows, NOx purification efficiency still can be higher than 90%.
Embodiment 3
A preparation method for the denitrating catalyst that the wolframic acid zirconia of take is carrier, comprises the following steps:
(1) take respectively 1.5g zirconium carbonate and 1.03g ammonium paratungstate, the two is dissolved in 50mL deionized water and is mixed with solution; Toward dripping ammoniacal liquor to pH value in solution, be 8.5, stir 3h, standing 12h;
(2) reactant liquor after step (1) is standing leaches sediment, and by sediment 80 ℃ of oven dry in baking oven, in Muffle furnace, 550 ℃ of roasting 8h, make wolframic acid zirconia, are ground into powder;
(3) take 0.1g ammonium metavanadate, be dissolved in 25mL saturated oxalic acid solution, take 0.47g ammonium ceric nitrate, be dissolved in 25mL deionized water, two kinds of solution are mixed; Then add the ground wolframic acid zirconia of step (2), stir dipping 12h, 80 ℃ of oven dry in baking oven, in Muffle furnace, 550 ℃ of roasting 8h, make catalyst finished product.
The W/Zr mol ratio of catalyst finished product is that 1, Ce/V mol ratio is 1, and active component mass fraction is 15%.Catalyst finished product is ground, get the wherein catalyst fines 0.5g of 40～60 order sizes, put into quartz tube reactor and test its denitration activity, result shows, between 200～420 ℃ of reaction temperatures, NOx purification efficiency is higher than 95%, N in product
2selectively higher than 98%; Toward the sodium compound of dip loading 5% in catalyst finished product, and then by above-mentioned steps and method test denitration activity, result shows, NOx purification efficiency still can be higher than 90%.
Embodiment 4
A preparation method for the denitrating catalyst that the wolframic acid zirconia of take is carrier, comprises the following steps:
(1) take respectively 1.5g zirconyl chloride and 3.24g wolframic acid, the two is dissolved in 50mL deionized water and is mixed with solution; Toward dripping ammoniacal liquor to pH value in solution, be 8.2, stir 4h, standing 24h;
(2) reactant liquor after step (1) is standing leaches sediment, and by sediment 90 ℃ of oven dry in baking oven, in Muffle furnace, 650 ℃ of roasting 6h, make wolframic acid zirconia, are ground into powder;
(3) take 0.1g ammonium metavanadate, be dissolved in 25mL saturated oxalic acid solution, take 0.1g cerous nitrate, be dissolved in 25mL deionized water, two kinds of solution are mixed; Then add the ground wolframic acid zirconia of step (2), stir dipping 24h, 90 ℃ of oven dry in baking oven, in Muffle furnace, 650 ℃ of roasting 6h, make catalyst finished product.
The W/Zr mol ratio of catalyst finished product is that 2.79, Ce/V mol ratio is 0.27, and active component mass fraction is 3.2%.Catalyst finished product is ground, get the wherein catalyst fines 0.5g of 40～60 order sizes, put into quartz tube reactor and test its denitration activity, result shows, between 200～420 ℃ of reaction temperatures, NOx purification efficiency is higher than 95%, N in product
2selectively higher than 98%; Toward the potassium compound of dip loading 5% in catalyst finished product, and then by above-mentioned steps and method test denitration activity, result shows, NOx purification efficiency still can be higher than 90%.
Embodiment 5
A preparation method for the denitrating catalyst that the wolframic acid zirconia of take is carrier, comprises the following steps:
(1) take respectively 1.5g zirconyl nitrate and 3.96g ammonium paratungstate, the two is dissolved in 50mL deionized water and is mixed with solution; Toward dripping ammoniacal liquor to pH value in solution, be 8.7, stir 5h, standing 36h;
(2) reactant liquor after step (1) is standing leaches sediment, and by sediment 100 ℃ of oven dry in baking oven, in Muffle furnace, 750 ℃ of roasting 4h, make wolframic acid zirconia, are ground into powder;
(3) take 0.01g ammonium metavanadate, be dissolved in 25mL saturated oxalic acid solution, take 0.937g ammonium ceric nitrate, be dissolved in 25mL deionized water, two kinds of solution are mixed; Then add the ground wolframic acid zirconia of step (2), stir dipping 36h, 100 ℃ of oven dry in baking oven, in Muffle furnace, 750 ℃ of roasting 4h, make catalyst finished product.
The W/Zr mol ratio of catalyst finished product is that 2.15, Ce/V mol ratio is 20, and active component mass fraction is 7%.Catalyst finished product is ground, get the wherein catalyst fines 0.5g of 40～60 order sizes, put into quartz tube reactor and test its denitration activity, result shows, between 200～420 ℃ of reaction temperatures, NOx purification efficiency is higher than 95%, N in product
2selectively higher than 98%; Toward the calcium compound of dip loading 5% in catalyst finished product, and then by above-mentioned steps and method test denitration activity, result shows, NOx purification efficiency still can be higher than 90%.
Embodiment 6
A preparation method for the denitrating catalyst that the wolframic acid zirconia of take is carrier, comprises the following steps:
(1) take respectively 1.5g zirconium carbonate and 3.62g wolframic acid, the two is dissolved in 50mL deionized water and is mixed with solution; Toward dripping ammoniacal liquor to pH value in solution, be 8.8, stir 3.5h, standing 48h;
(2) reactant liquor after step (1) is standing leaches sediment, and by sediment 120 ℃ of oven dry in baking oven, in Muffle furnace, 800 ℃ of roasting 2h, make wolframic acid zirconia, are ground into powder;
(3) take 0.1g ammonium metavanadate, be dissolved in 25mL saturated oxalic acid solution, take 0.47g ammonium ceric nitrate, be dissolved in 25mL deionized water, two kinds of solution are mixed; Then add the ground wolframic acid zirconia of step (2), stir dipping 48h, 120 ℃ of oven dry in baking oven, in Muffle furnace, 800 ℃ of roasting 2h, make catalyst finished product.
The W/Zr mol ratio of catalyst finished product is that 4, Ce/V mol ratio is 1, and active component mass fraction is 5.6%.Catalyst finished product is ground, get the wherein catalyst fines 0.5g of 40～60 order sizes, put into quartz tube reactor and test its denitration activity, result shows, between 200～420 ℃ of reaction temperatures, NOx purification efficiency is higher than 95%, N in product
2selectively higher than 98%; Toward the sodium compound of dip loading 5% in catalyst finished product, and then by above-mentioned steps and method test denitration activity, result shows, NOx purification efficiency still can be higher than 90%.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (8)
1. the denitrating catalyst that the wolframic acid zirconia of take is carrier, is characterized in that, it is carrier that described denitrating catalyst be take the zirconia of wolframic acid, take cerium oxide and vanadic anhydride as active component; In described carrier, the mol ratio of tungsten and zirconium is 0.6～5; The mol ratio of described active component cerium and vanadium is 0.05～20.
2. denitrating catalyst according to claim 1, is characterized in that, the mass fraction of described active component in denitrating catalyst is 0.1～15%.
3. the preparation method of take the denitrating catalyst that wolframic acid zirconia is carrier described in claim 1 or 2, is characterized in that, comprises the following steps:
(1) presoma of the presoma of zirconium and tungsten is soluble in water, make precursor solution; Then in precursor solution, add ammoniacal liquor, pH is adjusted to 8～9, after stirring 2～6h, standing 2～48h is standby;
(2) reacting liquid filtering after step (1) is standing, taking precipitate, then by it 60～120 ℃ of oven dry, then in 400～800 ℃ of roasting 2～12h, make wolframic acid zirconia, be finally ground into powder;
(3) presoma of vanadium is dissolved with saturated oxalic acid solution, the presoma water of cerium is dissolved, then two kinds of solution are mixed, obtain precursor mixed solution; The wolframic acid Zirconium oxide powder again step (2) being made adds in precursor mixed solution, stirs dipping 2～48h, after 60～120 ℃ of oven dry, and in 400～800 ℃ of roasting 2～12h, the denitrating catalyst that the wolframic acid zirconia of take described in obtaining is carrier.
4. preparation method according to claim 3, is characterized in that, the presoma of described zirconium is a kind of in zirconyl nitrate, zirconyl chloride and zirconium carbonate.
5. preparation method according to claim 3, is characterized in that, the presoma of described tungsten is ammonium paratungstate or wolframic acid.
6. preparation method according to claim 3, is characterized in that, the presoma of described vanadium is ammonium metavanadate.
7. preparation method according to claim 3, is characterized in that, the presoma of described cerium is cerous nitrate or ammonium ceric nitrate.
8. described in claim 1 or 2, take the application in the flue gas of processing high-load alkali and alkaline earth metal ions of denitrating catalyst that wolframic acid zirconia is carrier.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104148052A (en) * | 2014-08-14 | 2014-11-19 | 浙江大学 | Cerium-vanadium-silicon-titanium composite oxide catalyst and preparation method thereof |
| CN112403485A (en) * | 2020-11-19 | 2021-02-26 | 高化学（江苏）化工新材料有限责任公司 | V/Cu/B/W-TiO2-ZrO2Production method of composite low-temperature denitration catalyst |
| CN116099528A (en) * | 2023-02-28 | 2023-05-12 | 上海电气电站环保工程有限公司 | SCR denitration catalyst, preparation method and application thereof in marine diesel engine tail gas |
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| CN102000589A (en) * | 2010-11-09 | 2011-04-06 | 中国海洋石油总公司 | Method for preparing low-temperature ammonia selective catalytic reduction denitration catalyst |
| CN102658172A (en) * | 2012-04-20 | 2012-09-12 | 浙江大学 | SCR denitration catalyst as well as preparation method and application thereof |
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2014
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20040074811A1 (en) * | 2002-10-21 | 2004-04-22 | George Yaluris | NOx reduction compositions for use in FCC processes |
| CN102000589A (en) * | 2010-11-09 | 2011-04-06 | 中国海洋石油总公司 | Method for preparing low-temperature ammonia selective catalytic reduction denitration catalyst |
| CN102658172A (en) * | 2012-04-20 | 2012-09-12 | 浙江大学 | SCR denitration catalyst as well as preparation method and application thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104148052A (en) * | 2014-08-14 | 2014-11-19 | 浙江大学 | Cerium-vanadium-silicon-titanium composite oxide catalyst and preparation method thereof |
| CN112403485A (en) * | 2020-11-19 | 2021-02-26 | 高化学（江苏）化工新材料有限责任公司 | V/Cu/B/W-TiO2-ZrO2Production method of composite low-temperature denitration catalyst |
| CN116099528A (en) * | 2023-02-28 | 2023-05-12 | 上海电气电站环保工程有限公司 | SCR denitration catalyst, preparation method and application thereof in marine diesel engine tail gas |
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Application publication date: 20140716 |