CN103157480A - Vanadium oxide/iron oxide denitration catalyst, preparation method and application thereof - Google Patents
Vanadium oxide/iron oxide denitration catalyst, preparation method and application thereof Download PDFInfo
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- CN103157480A CN103157480A CN2013100429309A CN201310042930A CN103157480A CN 103157480 A CN103157480 A CN 103157480A CN 2013100429309 A CN2013100429309 A CN 2013100429309A CN 201310042930 A CN201310042930 A CN 201310042930A CN 103157480 A CN103157480 A CN 103157480A
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Abstract
The invention discloses a vanadium oxide/ iron oxide denitration catalyst, a preparation method of the vanadium oxide/ iron oxide denitration catalyst and application of the vanadium oxide/ iron oxide denitration catalyst. The catalyst is characterized in that the surface of iron oxide is immobilized with vanadium oxide nanometer particles, and the iron oxide cooperates with the nanometer vanadium oxide to catalyze ammonia to conduct reduction and denitration. The quality percentage of vanadium in the catalyst is 0.1-10%. The preparation method includes that after being measured with an oxalic acid solution of metavanadate, natural goethite particles or composite goethite powder which is prepared in a smashing mode is mixed with the oxalic acid solution of the metavanadate, and catalyst particle materials or powder is obtained through processes of stirring, aging, drying, and hot treating. The catalyst is used as a particle-shaped static bed or is used by being coated on other multi-hole structural materials. The vanadium oxide/ iron oxide denitration catalyst has high activity of reaction of catalyzing the ammonia to conduct the reduction and the denitration within the temperature range of 150-450 DEG C.
Description
One, technical field
The invention belongs to the Air Pollution Control Engineering field, especially for denitrifying catalyst with selective catalytic reduction and preparation method thereof.
Two, background technology
The all types of industries kiln such as thermal power plant, sintering plant, cement kiln and motor vehicles etc. produce a large amount of NOx in the high-temp combustion process.Discharged nitrous oxides not only causes acid rain, also can cause the Regional Environmental Pollution problems such as photochemical fog and depletion of the ozone layer.The technology that reduces now nitrogen oxides in effluent mainly contains two classes: the first kind is Combustion Process Control, namely improves combustion system, reduces the generation (comprising low oxygen combustion technology, multi-section-combustion technology etc.) of nitrogen oxide in combustion process; Equations of The Second Kind is end treatment, and namely denitrating flue gas, comprise absorption process, absorption method, non-selective catalytic reduction (SNCR) and SCR (SCR) etc.
The research of SCR denitrating catalyst receives great concern in recent years.Know that according to China online article offers data-searching, since two thousand deliver the Chinese Papers of relevant denitration up to 1930 pieces.Search for as descriptor with Selective Catalytic Reduction and NOx on Web of Science, since two thousand deliver relevant catalytic-reduction denitrified paper up to 1384 pieces.Up to now, 153 of Chinese invention patent applications are disclosed.Show that denitrating catalyst is the hot fields of studying always both at home and abroad.These denitrating catalysts are mainly TiO from carrier
2, Al
2O
3, active carbon, clay mineral etc., catalytic active component is mainly VO
x, MnO
x, CeO
2, SnO
2, also add the auxiliary catalysis component in some catalyst.
Based on V
2O
5/ TiO
2The SCR technology of catalyst has higher denitration efficiency with it and obtains using more widely on Flue Gas Denitrification Engineering abroad, and Some Domestic power plant has introduced this technology and carried out denitrating flue gas.The SCR method be with ammonia or urea as reducing agent under catalyst action with the NOx catalytic reduction, make ammonia can be selectively with flue gas in NOx reaction generation N
2And H
2O。
Catalyst V
2O
5/ TiO
2, have advantages of that denitration efficiency is high.V
2O
5/ TiO
2The denitrating catalyst weak point is: the one, and as the ultra-fine crystalline form TiO of the anatase titanium dioxide of carrier
2Domestic technology is immature, main dependence on import, and expensive, the catalysis preparation cost is higher; The 2nd, the catalyst preparation condition is comparatively strictly wayward; The 3rd, need to add auxiliary agent WO
3, MoO
3Deng to improve TiO
2Heat endurance.
The development of new catalyst is so that reaction (200 ℃ of left and right) at lower temperature is carried out, and this not only can reduce energy consumption of reaction, reduce costs; It is also conceivable that and take the SCR device is placed on the ESP(electric precipitation) afterwards, both can reduce or get rid of SO fully
2On the impact of catalyst,, do not need again original exhaust treatment system is carried out large-scale redevelopment.The low temperature SCR denitration catalyst of mentioning in domestic and foreign literature is mainly the MnO of infusion process preparation
X/ TiO
2, MnO
X/ AC, MnO
X/ Al
2O
3, MnO
X, MnO
x/ attapulgite has higher activity and steam less to the activity influence of catalyst, but SO in flue gas
2Can produce larger side effect to reactivity, although manganese-based catalyst has the high characteristics of low temperature active, easy inactivation, the life-span is short.Domestic publication (CN101352681) discloses take activated carbon as carrier impregnation load Mn, the preparation of V, Cu, Co, Fe oxide low-temperature SCR catalyst; Publication (CN101011659) discloses take activated carbon as carrier impregnation load MnO
X/ CeO
2The preparation of low-temperature SCR catalyst.The catalyst advantage of preparation is that the abundant specific area of absorbent charcoal carrier is conducive to the dispersion of active component take activated carbon as carrier, and has certain anti-SO
2Performance, but the active carbon high-temp ablation is too serious in the activating and regenerating process, causes catalyst attrition excessive.
Three, summary of the invention
The present invention overcomes weak point in prior art, a kind of convenient for production, with low cost, long service life, vanadium oxide that low-temperature catalytic activity is high/ferriferous oxide nano-composite catalyst are provided, be take ferriferous oxide as carrier, the composite of loaded with nano barium oxide.
Technical solution problem of the present invention adopts following technical scheme
The characteristics of vanadium oxide of the present invention/ferriferous oxide nano-composite catalyst are take goethite as raw material, by nano combined, are that the goethite crystals area load particle diameter of 80-150nm is less than the barium oxide particle of 10nm at diameter.
The characteristics of vanadium oxide of the present invention/ferriferous oxide nano-composite catalyst also are:
The content of described barium oxide in composite is not more than 10% by the vanadium mass percent.
In described goethite raw material, in the Hydrothermal Synthesis goethite, goethite content is not less than 98% by mass percentage; In natural goethite ore, goethite content is not less than 80% by mass percentage.
Vanadium oxide of the present invention/ferriferous oxide Nano-composite materials method is to operate as follows:
(1) selecting natural goethite ore is raw material, and wherein the content of goethite is greater than 80%, and all the other are quartzy, clay mineral impurity composition;
(2) goethite ore reduction is obtained the particle of 0.2-1mm, perhaps grinding becomes 200 purpose powders;
Perhaps selecting the Hydrothermal Synthesis goethite is raw material, and in raw material, the content of goethite is greater than 98%;
(3) ammonium metavanadate is dissolved in the oxalic acid aqueous solution that mass concentration is 3-10%, in solution, vanadium concentration is calculated according to the load capacity of vanadium in prepared catalyst;
(4) the goethite particle is flooded with isopyknic vanadate solution, spend the night aging, then dry;
Perhaps goethite powder and isopyknic vanadate solution mixing 0.5h, spend the night aging, then dry;
(5) dried material at 250-700 ℃, Static Calcination 0.5-2h;
Perhaps at 250-700 ℃, fluosolids roasting;
(6) be the barium oxide after calcining/ferriferous oxide nano composite material pulverizing the powder below 200 orders, water is deployed into the suspension that mass concentration is 10-50%, mode by spraying or dipping is coated in voidage to the barium oxide/silicon/iron oxide composite material of preparation on the surface of the porous structure material more than 80%, as Extruded Monolithic Celluar Ceramics, foam nickel material, honeycomb aluminum plate material, honeycomb iron plate material, obtain catalyst article and be used for catalytic unit;
Perhaps being different grades with 0.1-1mm graininess goethite dipping, material screening dry, the calcining acquisition, as 0.1-0.3mm, 0.3-0.6mm, 0.6-1.0mm, be used for particles filled fixed bed catalytic reactor.
Good effect of the present invention is embodied in:
1, with synthetic TiO
2Compare, the goethite source is abundanter, price is cheaper, and environmental pollution is light, prepares as carrier cost and the environmental pollution that denitrating catalyst is conducive to reduce catalyst.
2, in 250-400 ℃ of calcining, due to thermal decomposition dehydration, the bloodstone of product nano-pore structure, specific area improves 7-10 doubly to goethite under air atmosphere.
3, with synthetic TiO
2Compare, the bloodstone of goethite phase-change product nano-pore structure has stronger compatibility to micromolecular polar gases such as ammonia, nitrogen oxide, thereby ammonia, nitrogen oxide are shown higher adsorption activity, larger adsorption capacity.
4, ferriferous oxide has facilitation as denitration catalyst carrier to improving denitration activity and efficient.
5, the bloodstone of goethite phase-change product nano-pore structure has higher acid and alkali-resistance, heat endurance, and the catalyst of preparation has the little characteristics of loss in application process.
Four, description of drawings
Fig. 1: the field emission scanning electron microscope image of Hydrothermal Synthesis goethite, goethite presents needle-like, diameter 80-150nm.
Fig. 2: the specific area of heat treatment goethite shows that with the variation of heat treatment temperature heat treated goethite has higher specific area between 250-400 ℃..
Fig. 3: 300 ℃ of heat treatment goethite images of transmissive electron microscope show because Dehydration is the bloodstone with nano-pore structure.
Fig. 4: embodiment 1 Kaolinite Preparation of Catalyst images of transmissive electron microscope.
Fig. 5: 300 ℃ of different vanadium load capacity catalyst denitration efficiencies of calcining preparation are with the reaction temperature change curve.
Fig. 6: 500 ℃ of different vanadium load capacity catalyst denitration efficiencies of calcining preparation are with the reaction temperature change curve.
Five, the specific embodiment
Embodiment 1:
It is in 6% oxalic acid aqueous solution that the 0.1g ammonium vanadate is dissolved into respectively the 10ml mass concentration;
Natural goethite ore reduction screening, obtain the particle of 0.3-0.6mm;
Taking above-mentioned goethite particle 10g joins in above-mentioned vanadate solution and floods 1-10h, then 105 ℃ of oven dry;
Dried material is calcined 0.5h at 300 ℃;
The catalyst material of preparation is seated in little reaction fixed bed catalytic reactor, with air speed 9000 h
-1Gas speed, carry out catalysis ammonia selective reducing NO denitration experiment at different temperature, in 250-400 ℃ of interval, the NO conversion ratio is greater than 95%.
Embodiment 2:
It is in 6% oxalic acid aqueous solution that the 0.3g ammonium vanadate is dissolved into respectively the 10ml mass concentration;
Natural goethite ore reduction screening, obtain the particle of 0.3-0.6mm;
Taking above-mentioned goethite particle 10g joins in above-mentioned vanadate solution and floods 1-10h, then 105 ℃ of oven dry;
Dried material is calcined 0.5h at 300 ℃;
The catalyst material of preparation is seated in little reaction fixed bed catalytic reactor, with air speed 9000 h
-1Gas speed, carry out catalysis ammonia selective reducing NO denitration experiment at different temperature, in 250-400 ℃ of interval, the NO conversion ratio is greater than 95%.
Embodiment 3:
It is in 6% oxalic acid aqueous solution that the 0.7g ammonium vanadate is dissolved into respectively the 10ml mass concentration;
Natural goethite ore reduction screening, obtain the particle of 0.3-0.6mm;
Taking above-mentioned goethite particle 10g joins in above-mentioned vanadate solution and floods 1-10h, then 105 ℃ of oven dry;
Dried material is calcined 0.5h at 300 ℃;
The catalyst material of preparation is seated in little reaction fixed bed catalytic reactor, with air speed 9000 h
-1Gas speed, carry out catalysis ammonia selective reducing NO denitration experiment at different temperature, in 250-400 ℃ of interval, the NO conversion ratio is greater than 95%.
Embodiment 4:
It is in 6% oxalic acid aqueous solution that the 0.3g ammonium vanadate is dissolved into respectively the 10ml mass concentration;
Natural goethite ore reduction screening, obtain the particle of 0.3-0.6mm;
Taking above-mentioned goethite particle 10g joins in above-mentioned vanadate solution and floods 1-10h, then 105 ℃ of oven dry;
Dried material is calcined 0.5h at 500 ℃;
The catalyst material of preparation is seated in little reaction fixed bed catalytic reactor, with air speed 9000 h
-1Gas speed, carry out catalysis ammonia selective reducing NO denitration experiment at different temperature, in 250-400 ℃ of interval, the NO conversion ratio is greater than 95%.
Embodiment 5:
It is in 6% oxalic acid aqueous solution that the 0.7g ammonium vanadate is dissolved into respectively the 10ml mass concentration;
Natural goethite ore reduction screening, obtain the particle of 0.3-0.6mm;
Taking above-mentioned goethite particle 10g joins in above-mentioned vanadate solution and floods 1-10h, then 105 ℃ of oven dry;
Dried material is calcined 0.5h at 500 ℃;
The catalyst material of preparation is seated in little reaction fixed bed catalytic reactor, at air speed 12000 h
-1Condition under, carry out catalysis ammonia selective reducing NO denitration experiment at different temperature, in 250-400 ℃ of interval, the NO conversion ratio is greater than 95%.
Embodiment 6:
It is in 6% oxalic acid aqueous solution that the 0.3g ammonium vanadate is dissolved into respectively the 20ml mass concentration;
Claim synthetic goethite powder 10g to join in above-mentioned vanadate solution and stir, become suspension;
Above-mentioned suspension is coated in the foam nickel material surface, obtains catalyst article;
The catalyst material of preparation is seated in little reaction fixed bed catalytic reactor, at air speed 12000 h
-1Condition under, carry out catalysis ammonia selective reducing NO denitration experiment at different temperature, in 250-400 ℃ of interval, the NO conversion ratio is greater than 95%.
Embodiment 7:
It is in 6% oxalic acid aqueous solution that the 0.3g ammonium vanadate is dissolved into respectively the 20ml mass concentration;
200 purpose powders were worn in natural goethite ore reduction;
Taking above-mentioned goethite powder 10g joins in above-mentioned vanadate solution and is made into suspension;
Above-mentioned suspension is coated in the Extruded Monolithic Celluar Ceramics surface, obtains catalyst article;
The catalyst material of preparation is seated in catalytic reactor, at air speed 12000 h
-1Condition under, carry out catalysis ammonia selective reducing NO denitration experiment at different temperature, in 250-400 ℃ of interval, the NO conversion ratio is greater than 95%.
Claims (2)
1. vanadium oxide/ferriferous oxide denitrifying catalyst with selective catalytic reduction, it is characterized in that nano-iron oxide area load nano vanadium oxide, in catalyst, the vanadium load capacity counts 0.1 ~ 10% by the vanadium mass percent, nano-iron oxide diameter 80-200nm, barium oxide diameter 2-10nm.
2. according to claim 1, a kind of vanadium oxide/ferriferous oxide catalytic-reduction denitrified catalyst preparation method, its concrete steps are:
(1) selecting natural goethite ore is raw material, and wherein the content of goethite is greater than 80%, and all the other are quartzy, clay mineral impurity composition;
(2) goethite ore reduction is obtained the particle of 0.2-1mm, perhaps grinding becomes 200 purpose powders;
Perhaps selecting the Hydrothermal Synthesis goethite is raw material, and in raw material, the content of goethite is greater than 98%;
(3) ammonium metavanadate is dissolved in the oxalic acid aqueous solution that mass concentration is 3-10%, in solution, vanadium concentration is calculated according to the load capacity of vanadium in prepared catalyst;
(4) the goethite particle with isopyknic metavanadate solution impregnation, spend the night aging, then dry;
Perhaps goethite powder and isopyknic metavanadate solution mixing 0.5h, spend the night aging, then dry;
(5) dried material at 250-700 ℃, Static Calcination 0.5-2h;
Perhaps at 250-700 ℃, fluosolids roasting;
(6) be the barium oxide after calcining/ferriferous oxide nano composite material pulverizing the powder below 200 orders, water is deployed into the suspension that mass concentration is 10-50%, mode by spraying or dipping is coated in voidage to the barium oxide/silicon/iron oxide composite material of preparation on the surface of the porous structure material more than 80%, as Extruded Monolithic Celluar Ceramics, foam nickel material, honeycomb aluminum plate material, honeycomb iron plate material, obtain catalyst article and be used for catalytic unit;
Perhaps be 0.1-0.3mm, 0.3-0.6mm, 0.6-1.0mm using 0.1-1mm graininess goethite dipping, drying, calcine the material that obtains, sieving, for fixed bed catalytic reactor.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107282066A (en) * | 2016-04-13 | 2017-10-24 | 安徽工业大学 | A kind of SCR denitration and its methods for making and using same based on Natural Manganese iron ore |
| WO2018121676A1 (en) * | 2016-12-30 | 2018-07-05 | Basf Se | An extruded honeycomb catalyst |
| CN108349745A (en) * | 2015-11-20 | 2018-07-31 | 柯尼卡美能达株式会社 | The manufacturing method of particle containing vanadium dioxide |
| US20180272318A1 (en) * | 2016-09-12 | 2018-09-27 | The Chugoku Electric Power Co., Inc. | Denitration catalyst and method for producing the same |
| CN114054039A (en) * | 2021-12-01 | 2022-02-18 | 合肥工业大学 | Preparation of MnOx/alpha-Fe by utilizing artificially synthesized goethite2O3Method for preparing composite denitration catalyst and application thereof |
| CN114588914A (en) * | 2022-03-21 | 2022-06-07 | 冯垚 | Method for preparing catalyst by using tailings |
| CN115254094A (en) * | 2022-08-04 | 2022-11-01 | 安徽元琛环保科技股份有限公司 | Preparation method of metal-based anti-knock denitration catalyst and prepared catalyst |
| CN115945198A (en) * | 2023-01-31 | 2023-04-11 | 太原理工大学 | Preparation method and application of low-temperature ammonium bisulfate-resistant layered iron-vanadium composite oxide denitration catalyst |
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| CN108349745B (en) * | 2015-11-20 | 2021-02-02 | 柯尼卡美能达株式会社 | Method for producing vanadium dioxide-containing particles |
| CN108349745A (en) * | 2015-11-20 | 2018-07-31 | 柯尼卡美能达株式会社 | The manufacturing method of particle containing vanadium dioxide |
| CN107282066A (en) * | 2016-04-13 | 2017-10-24 | 安徽工业大学 | A kind of SCR denitration and its methods for making and using same based on Natural Manganese iron ore |
| US10767535B2 (en) | 2016-09-12 | 2020-09-08 | The Chugoku Electric Power Co., Inc. | Method for recycling denitration catalyst |
| US10746074B2 (en) | 2016-09-12 | 2020-08-18 | The Chugoku Electric Power Co., Inc. | Method for recycling denitration catalyst |
| US10746073B2 (en) | 2016-09-12 | 2020-08-18 | The Chugoku Electric Power Co., Inc. | Denitration catalyst and method for producing the same |
| US20180272318A1 (en) * | 2016-09-12 | 2018-09-27 | The Chugoku Electric Power Co., Inc. | Denitration catalyst and method for producing the same |
| US10865684B2 (en) | 2016-09-12 | 2020-12-15 | The Chugoku Electric Power Co., Inc. | Combustion system |
| WO2018121676A1 (en) * | 2016-12-30 | 2018-07-05 | Basf Se | An extruded honeycomb catalyst |
| CN114054039A (en) * | 2021-12-01 | 2022-02-18 | 合肥工业大学 | Preparation of MnOx/alpha-Fe by utilizing artificially synthesized goethite2O3Method for preparing composite denitration catalyst and application thereof |
| CN114588914A (en) * | 2022-03-21 | 2022-06-07 | 冯垚 | Method for preparing catalyst by using tailings |
| CN115254094A (en) * | 2022-08-04 | 2022-11-01 | 安徽元琛环保科技股份有限公司 | Preparation method of metal-based anti-knock denitration catalyst and prepared catalyst |
| CN115254094B (en) * | 2022-08-04 | 2024-07-26 | 安徽元琛环保科技股份有限公司 | Preparation method of metal-based anti-knock denitration catalyst and prepared catalyst |
| CN115945198A (en) * | 2023-01-31 | 2023-04-11 | 太原理工大学 | Preparation method and application of low-temperature ammonium bisulfate-resistant layered iron-vanadium composite oxide denitration catalyst |
| CN115945198B (en) * | 2023-01-31 | 2023-10-24 | 太原理工大学 | Preparation method and application of low-temperature ammonium bisulfate-resistant layered iron-vanadium composite oxide denitration catalyst |
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