CN103801325A - Co-precipitation preparation method of composite oxide denitration catalyst - Google Patents
Co-precipitation preparation method of composite oxide denitration catalyst Download PDFInfo
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- CN103801325A CN103801325A CN201410086510.5A CN201410086510A CN103801325A CN 103801325 A CN103801325 A CN 103801325A CN 201410086510 A CN201410086510 A CN 201410086510A CN 103801325 A CN103801325 A CN 103801325A
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Abstract
The invention discloses a co-precipitation preparation method of a composite oxide denitration catalyst and belongs to the technical field of preparation of nitric oxide reduction catalysts. The method comprises the following steps: in the presence of a solvent, mixing aluminum sulfate, titanium sulfate, ammonium vanadate and sodium metasilicate with at least one of ammonium tungstate, manganese chloride, nickel nitrate, cobalt nitrate and chromic nitrate; then placing an obtained precursor into a muffle furnace, and roasting the precursor to obtain the catalyst. According to the method, the use of TiO2 in a conventional V-W-Ti catalyst is reduced, and the cost is reduced; meanwhile, the specific surface area of the catalyst is increased. The formed catalyst contains two or more of components from Ti, Si, Al, V, W, Cr, Ni, Mn and Co; the denitration activity of the catalyst is favorably improved by the strong cooperative action of each active component and a carrier; the catalyst is applicable to SCR (selective catalytic reduction) denitration reaction at low temperature of 250-500 DEG C.
Description
Technical field
The invention belongs to catalyst for reduction of oxides of nitrogen preparing technical field, relate in particular to a kind of preparation method of SCR composite oxides denitrating catalyst.
Background technology
Protection of the environment is the fundamental state policy of China, and along with industrial expansion, problem of environmental pollution becomes increasingly conspicuous, especially the pollution problem of nitrogen oxide.NOx is one of pollutant causing acid rain, photochemical fog and depletion of the ozone layer.And more than 90% be to be produced by the combustion process of the fossil fuels such as coal, oil, natural gas, China is as maximum energy resource consumption state in the world now, and the emission problem of NOx has caused the extensive concern of government and national society.Country 12 explicitly points out in the works, realize nitrogen oxide emission in 2015 and reduce 10% compared with 2010, and this just requires the discharge standard of nitrogen oxide higher.Just current, the NOx of the enterprise discharge standards such as national most of coal-burning power plants, cement, glass, iron and steel are still low, and it is not good that its reason is rooted in the denitrating catalyst performance of use, causes denitration efficiency not high.And the external import of main dependence at present of the catalyst of better performances, cost is high, therefore, needs now research badly, prepares a kind of high efficiency, low cost SCR denitrating catalyst, to meet domestic industry Production requirement.
Gas denitrifying technology is mainly divided into SCR (SCR), SNCR (SNCR), absorption method etc.Wherein, SNCR is owing to not using catalyst, and its reaction temperature requires very high (800 ℃ of >), and ammonia is easily oxidized, produces NOx; Absorption method need to be used strong oxidizer (O because of it
3or H
2o
2or NO is oxidized to NO by effective catalyst
2) and hindered its industrial extensive use; And SCR from nineteen fifty-seven by after Engelhard company of U.S. invention, through the development of over half a century, realize industrialization in the developed country such as American-European, Japanese already, its denitration efficiency is high, selectively good.Commercialization SCR catalyst is mainly pure TiO
2carrier loaded V
2o
5and WO
3active component, its price is more expensive, and environmental pollution is larger.And suitably reduce TiO in carrier
2content, with the larger SiO of specific area
2and Al
2o
3replace, not only can save production cost, increase specific surface area of catalyst simultaneously.And being added with of other transition metal active components is beneficial to the performance of improving denitrating catalyst, augmenting response temperature window, suppresses the generation of side reaction, strengthens anti-poisoning capability simultaneously.Though the patent of preparing about denitrating catalyst domestic has tens of kinds more than, can be widely used in industrial little.Patent CN 101791549A discloses a kind of ultrasonic mixed precipitation legal system for moulding denitrating catalyst, take industrial sulphuric acid oxygen titanium as raw material, through homogeneous precipitation and Direct precipitation, and be aided with ultrasound-enhanced, make metatitanic acid carrier with this, then mix with active component and auxiliary agent, dry calcining and obtain catalyst.This method support material is extensively cheap, has reduced production cost, but still take pure titanium as carrier, heat endurance is poor, and carrier crystal formation easily changes, and in impregnation drying process, active component dispersion is inhomogeneous, affects denitration effect.Patent CN 1792431A discloses monoblock type denitrating catalyst of a kind of double oxide complex carrier and preparation method thereof, and it is take cordierite ceramic as framework material, Al
2o
3and TiO
2for complex carrier, wherein Al
2o
3for internal layer carrier, TiO
2for outer carrier, active component is V
2o
5, WO
3.This method is because cordierite ceramic specific area is less, and the load of its double oxide is more difficult, less stable, and also preparation process is comparatively complicated, needs multistep load.Patent CN 1919447A discloses a kind of cocurrent process co-precipitation by copper, magnesium, zinc, aluminium, iron, cobalt mixed liquor and NaOH, sodium carbonate liquor houghite processed, then adds auxiliary agent and makes preformed catalyst.Although this method adopts a step coprecipitation preparation, not SCR removes nitrogen oxide, but absorption method, this method is lower to NOx removal efficiency, and in the NOx flue gas of inapplicable and high-load.
Summary of the invention
For the higher defect of nitrogen oxides in effluent content, it is stable that object of the present invention is mainly to provide a kind of low cost, high conversion and active component, requirement is few, environmental pollution is little, and preparation technology is simply applicable to the co-precipitation preparation method of the composite oxides denitrating catalyst of low temperature composite oxides denitration.
Technical solution of the present invention is: under solvent existence condition, by at least one hybrid reaction in aluminum sulfate, titanium sulfate, ammonium vanadate, nine water sodium metasilicate and ammonium tungstate, manganese chloride, nickel nitrate, cobalt nitrate, chromic nitrate, obtain catalyst precursor, then precursor is placed in to Muffle furnace roasting and obtains catalyst.
The present invention adopts coprecipitation one step to prepare composite oxide catalysts, has not only reduced TiO in traditional V-W-Ti catalyst
2consumption, reduced cost, increased the specific area of catalyst simultaneously.In the catalyst forming, contain two or more components in Ti, Si, Al, V, W, Cr, Ni, Mn, Co, and stronger coordinative role between each active component and carrier, be conducive to the raising of catalyst denitration activity, be applicable to carry out SCR denitration reaction temperature at 250～500 ℃ of low temperature.
The present invention has following characteristics:
1) adopt a step coprecipitation to prepare composite oxides denitrating catalyst, not only reduced TiO
2consumption, reduces costs, and has increased the specific area of catalyst simultaneously, is beneficial to the dispersion optimization of active component.
2) TiO in obtained catalyst
2along with the different crystal forms of sintering temperature changes, and do not find the diffraction maximum of other components.
2) composite oxide carrier keeps good denitration activity in 250～500 ℃ of temperature ranges, all reaches more than 90%.
3) preparation method of the present invention is simple, easy operating.
Concrete precursor preparation method is: under 60～100 ℃ of constant temperatures, by any mixing in aluminum sulfate aqueous solution, titanium sulfate aqueous solution, ammonium vanadate hydrogen peroxide solution and ammonium tungstate aqueous solution, the manganese chloride aqueous solution, nickel nitrate aqueous solution, cobalt nitrate aqueous solution, chromium nitrate aqueous solution, under stirring condition, drip nine water sodium silicate aqueous solutions, occur after blackish green homogeneous precipitation, regulate pH to 8～9 of precipitation system, stratification under normal temperature after stirring, through suction filtration, get a layer hypostasis and wash extremely without Cl
-, then dry 0.5～24h under 80～130 ℃ of temperature conditions, obtains catalyst precursor, in the prepared presoma of this method each group precipitation complete, be evenly distributed.
With H
2sO
4the aqueous solution or NH
3h
2o regulates the pH value of precipitation system.
The temperature of roasting is 450～750 ℃, roasting time 4～6h.Within the scope of this sintering temperature, different sintering temperatures can obtain the catalyst of different crystal forms.
In order to make TiO in catalyst
2proportion is 10～50wt%, SiO
2be 20～80wt%, Al
2o
3be 5～40wt%, V
2o
5be 1～5wt%, WO
3be 0～5wt%, Cr
2o
3be 0～5wt%, NiO is 0～5wt%, MnO
2be 0～5wt%, Co
2o
3be 0～5wt%, in the time preparing precursor, described titanium sulfate, nine water sodium metasilicate, aluminum sulfate and the mass ratio that feeds intake by ammonium vanadate, ammonium tungstate, manganese chloride, nickel nitrate, cobalt nitrate, at least one mixture forming of chromic nitrate are 2.5～15 ︰ 8.5～38 ︰ 1.7～13 ︰ 1.
Accompanying drawing explanation
Fig. 1 is catalyst XRD figure under different sintering temperatures.
The specific embodiment
One, Kaolinite Preparation of Catalyst:
1, embodiment 1:
1) Kaolinite Preparation of Catalyst precursor preparation: under 60～100 ℃ of constant temperatures, take respectively 166.0g NaSiO
39H
2o, 112.0g TiCl
4, 83.0g AlCl
36H
2o and 3.0g ammonium metavanadate, 5.1g ammonium tungstate, 30.0g chromic nitrate, 13.6g nickel nitrate, 5.1g manganese chloride.
Add water respectively again or hydrogen peroxide, make NaSiO
39H
2o, titanium sulfate aqueous solution, AlCl
36H
2the O aqueous solution, ammonium vanadate hydrogen peroxide solution, ammonium tungstate aqueous solution, nickel nitrate aqueous solution, cobalt nitrate aqueous solution, chromium nitrate aqueous solution and the manganese chloride aqueous solution.
Above each solution is mixed, under stirring condition, drip nine water sodium silicate aqueous solutions, occur after blackish green homogeneous precipitation, with H
2sO
4the aqueous solution or NH
3h
2o regulates pH to 8～9 of precipitation system, and stratification under normal temperature after stirring, through suction filtration, is got a layer hypostasis and washed extremely without Cl
-, then dry 0.5～24h under 80～130 ℃ of temperature conditions, obtains catalyst precursor.
2) Kaolinite Preparation of Catalyst: it is the Muffle furnace roasting 4～6h of 450～750 ℃ that precursor is placed in to temperature, obtains catalyst.
3) analyze: make TiO in catalyst by co-precipitation
2content is 40%wt%, SiO
2for 30%wt%, Al
2o
3for 15%wt%, V
2o
5for 2%wt%, WO
3for 4%wt%, Cr
2o
3for 5%wt%, NiO is 3%wt%, MnO
2for 3%wt%.
2, embodiment 2:
With the method preparation identical with embodiment 1.Different: to take 249.0g NaSiO
39H
2o, 98.0g TiCl
4, 27.7g AlCl
36H
2o and 3.0g ammonium metavanadate, 5.1g ammonium tungstate, 30.0g chromic nitrate, 8.2g cobalt nitrate.
TiO in the catalyst that analysis is made
2content is 35%wt%, SiO
2for 45%wt%, Al
2o
3for 5%wt%, V
2o
5for 2%wt%, WO
3for 4%wt%, Cr
2o
3for 5%wt%, Co
2o
3for 4%wt%.
3, embodiment 3:
With the method preparation identical with embodiment 1.Different: to take 138.3g NaSiO
39H
2o, 140.0g TiCl
4, 55.4g AlCl
36H
2o and 3.8g ammonium metavanadate, 6.4g ammonium tungstate, 8.1g manganese chloride, make catalyst by co-precipitation.
TiO in the catalyst that analysis is made
2content is 50%wt%, SiO
2for 25%wt%, Al
2o
3for 10%wt%, V
2o
5for 2.5%wt%, WO
3for 5%wt%, MnO
2for 5%wt%.
4, embodiment 4:
With the method preparation identical with embodiment 1.Different: to take 111.0g NaSiO
39H
2o, 126.0g TiCl
4, 110.0g AlCl
36H
2o and 3.0g ammonium metavanadate, 6.4g ammonium tungstate, 12.0g chromic nitrate, 9.1g nickel nitrate, 4.9g manganese chloride, 6.2g cobalt nitrate, make catalyst by co-precipitation.
TiO in the catalyst that analysis is made
2content is 45%wt%, SiO
2for 20%wt%, Al
2o
3for 20%wt%, V
2o
5for 2%wt%, WO
3for 5%wt%, Cr
2o
3for 2%wt%, NiO is 2%wt%, MnO
2for 3%wt%, Co
2o
3for 3%wt%.
Two, catalyst activity test:
The catalyst that above each embodiment is obtained is under laboratory simulation flue gas condition, with NH
3as reducing agent, NH
3: NO=1:1, NO inlet concentration 2000ppm, O
2for 7%(V/V), N
2for carrier, air speed is 3600h
-1, experiment test NO conversion ratio result is as shown in following table (300 ℃ of reaction temperatures):
Three, will make TiO in catalyst
2along with the different crystal forms of sintering temperature changes, and do not find the diffraction maximum of other component, as shown in Figure 1.
As seen from Figure 1: the unfired amorphous forms that is mainly exists.And the catalyst obtaining occurs diffraction maximum at 25.3 °, be mainly Detitanium-ore-type TiO after 550 ℃ of roastings
2, its grain diameter is less.Along with the rising of sintering temperature, Detitanium-ore-type diffraction maximum is strengthened gradually, narrows, and sintering, reunion occur, and it is large that particle becomes, and reaches 750 ℃ to sintering temperature, occurs Rutile Type TiO
2characteristic diffraction peak.
Claims (5)
1. the co-precipitation preparation method of composite oxides denitrating catalyst, it is characterized in that: under solvent existence condition, by at least one hybrid reaction in aluminum sulfate, titanium sulfate, ammonium vanadate, nine water sodium metasilicate and ammonium tungstate, manganese chloride, nickel nitrate, cobalt nitrate, chromic nitrate, obtain catalyst precursor, then precursor is placed in to Muffle furnace roasting and obtains catalyst.
2. method according to claim 1, it is characterized in that: under 60～100 ℃ of constant temperatures, by any mixing in aluminum sulfate aqueous solution, titanium sulfate aqueous solution, ammonium vanadate hydrogen peroxide solution and ammonium tungstate aqueous solution, the manganese chloride aqueous solution, nickel nitrate aqueous solution, cobalt nitrate aqueous solution, chromium nitrate aqueous solution, under stirring condition, drip nine water sodium silicate aqueous solutions, occur after blackish green homogeneous precipitation, regulate pH to 8～9 of precipitation system, stratification under normal temperature after stirring, through suction filtration, get a layer hypostasis and wash extremely without Cl
-, then dry 0.5～24h under 80～130 ℃ of temperature conditions, obtains catalyst precursor.
3. method according to claim 2, is characterized in that: with H
2sO
4the aqueous solution or NH
3h
2o regulates the pH value of precipitation system.
4. method according to claim 1, is characterized in that: the temperature of roasting is 450～750 ℃, roasting time 4～6h.
5. according to method described in claim 1 or 2 or 3, it is characterized in that: described titanium sulfate, nine water sodium metasilicate, aluminum sulfate and the mass ratio that feeds intake by ammonium vanadate, ammonium tungstate, manganese chloride, nickel nitrate, cobalt nitrate, at least one mixture forming of chromic nitrate are 2.5～15 ︰ 8.5～38 ︰ 1.7～13 ︰ 1.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080566A (en) * | 2015-08-17 | 2015-11-25 | 中国石油大学(北京) | Flue gas denitrification powder catalyst as well as preparation method and application thereof |
| CN105214679A (en) * | 2015-08-17 | 2016-01-06 | 中国石油大学(北京) | A kind of water resistant sulfur resistive type denitrating flue gas powder catalyst, preparation method and its usage |
| CN108236947A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院宁波城市环境观测研究站 | A kind of low temperature manganese-base oxide catalyst and its application |
| CN108579409A (en) * | 2018-04-04 | 2018-09-28 | 江苏华本环境科技有限公司 | A kind of SCR denitration method for flue gas under hot conditions |
| CN108772072A (en) * | 2018-04-04 | 2018-11-09 | 江苏华本环境科技有限公司 | A kind of preparation method of composite catalyst for denitrating flue gas |
| CN108993530A (en) * | 2018-08-17 | 2018-12-14 | 太原理工大学 | A kind of preparation method and application of hydrotalcite NiMnTi catalyst |
| CN111686753A (en) * | 2019-03-14 | 2020-09-22 | 日本碍子株式会社 | Porous ceramic structure |
| CN114377683A (en) * | 2022-01-25 | 2022-04-22 | 大唐南京环保科技有限责任公司 | Anti-arsenic poisoning denitration catalyst and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080566A (en) * | 2015-08-17 | 2015-11-25 | 中国石油大学(北京) | Flue gas denitrification powder catalyst as well as preparation method and application thereof |
| CN105214679A (en) * | 2015-08-17 | 2016-01-06 | 中国石油大学(北京) | A kind of water resistant sulfur resistive type denitrating flue gas powder catalyst, preparation method and its usage |
| CN108236947A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院宁波城市环境观测研究站 | A kind of low temperature manganese-base oxide catalyst and its application |
| CN108579409A (en) * | 2018-04-04 | 2018-09-28 | 江苏华本环境科技有限公司 | A kind of SCR denitration method for flue gas under hot conditions |
| CN108772072A (en) * | 2018-04-04 | 2018-11-09 | 江苏华本环境科技有限公司 | A kind of preparation method of composite catalyst for denitrating flue gas |
| CN108993530A (en) * | 2018-08-17 | 2018-12-14 | 太原理工大学 | A kind of preparation method and application of hydrotalcite NiMnTi catalyst |
| CN108993530B (en) * | 2018-08-17 | 2021-05-18 | 太原理工大学 | Preparation method and application of hydrotalcite-based NiMnTi catalyst |
| CN111686753A (en) * | 2019-03-14 | 2020-09-22 | 日本碍子株式会社 | Porous ceramic structure |
| CN111686753B (en) * | 2019-03-14 | 2024-03-12 | 日本碍子株式会社 | Porous ceramic structure |
| CN114377683A (en) * | 2022-01-25 | 2022-04-22 | 大唐南京环保科技有限责任公司 | Anti-arsenic poisoning denitration catalyst and preparation method thereof |
| CN114377683B (en) * | 2022-01-25 | 2023-11-14 | 大唐南京环保科技有限责任公司 | Arsenic poisoning-resistant denitration catalyst and preparation method thereof |
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Application publication date: 20140521 |