CN105597732A - Composite carrier type SCR denitration catalyst capable of simultaneously removing nitrate and mercury, and preparation method thereof - Google Patents
Composite carrier type SCR denitration catalyst capable of simultaneously removing nitrate and mercury, and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite carrier type SCR denitration catalyst capable of simultaneously removing nitrate and mercury, and a preparation method thereof. The catalyst comprises, by mass, 0.2 to 1.2% of V2O5 and 1.0 to 10% of WO3, with the balance being a TiO2-Ce2 composite oxide carrier. The nanometer TiO2-Ce2 composite oxide carrier has a higher specific surface area, enables active components to be better dispersed and has good water resistance and sulfur resistance; through interaction between the active components and the carrier, activity of the catalyst is further improved, and the catalyst has strong HgO oxidation activity in absence of HCl or under the condition of low HCl; and the catalyst simultaneously completes catalytic reduction of NOx and catalytic oxidation of HgO without additional installation of flue gas purifying facilities of a coal-fired power plant, thereby realizeing simultaneous controlling of NOx and HgO.
Description
Technical field
The invention belongs to field of environment protection, be adapted to the gas cleaning of coal-burning power plant, comprise the control of nitrogen oxide and mercury. Be specifically related to one and there is Selective Catalytic Reduction of NO simultaneouslyxAnd to Hg0SCR denitrating catalyst and the preparation method of catalysed oxidn.
Background technology
NOxNatural environment and health are had to destruction, can cause great environmental problem such as photochemical fog, acid rain, greenhouse effects and ozone hole effect, seriously polluted; Mercury, because having the bioconcentration of extremely strong volatility, persistence, easy animal migration and height, also produces great threat to population health and ecological environment, becomes one of pollutant of global extensive concern. Therefore, to NOxBecome the emphasis in world environments protection field with the improvement of mercury. Countries in the world are to NOxFormulated more and more stricter standard with the discharge of mercury, China's " fossil-fuel power plant atmospheric pollutant emission standard " (GB13223-2011) specifies, NO in all coal-fired plant boiler flue gasesxDischarge capacity must not exceed 100mg/m3; Mercury and mercuric compounds discharge capacity must not exceed 0.03mg/m3. This has had stricter requirement to denitrating flue gas demercuration technology undoubtedly, will certainly improve the cost of thermal power generation. Therefore,, in order to reduce costs, coal-burning power plant need to utilize existing pollutant control appliance to remove the mercury in flue gas conventionally, in dedusting, desulphurization and denitration, can realize removing of mercury.
The existence form of mercury in flue gas mainly comprises particle mercury (Hgp), oxidation state mercury (Hg2+) and simple substance state mercury (Hg0). When flue gas passes through conventional fume treatment auxiliary, Hg2+Because it is water-soluble better, major part can be removed by wet scrubbing system acquisition; Most HgpCan be caught and remove by deduster; But Hg0Because the special physico-chemical character of its low melting point, high equilibrium vapour pressure and low aqueous solubility is difficult to be removed by conventional fume treatment auxiliary. Therefore, flue gas is by after conventional fume treatment auxiliary, and mercury is mainly with Hg0Form be discharged. So, Hg0Being the main existence form of mercury in atmospheric environment, is the mercury shape to the mankind and environmental hazard maximum. Control the Hg in flue gas0It is the Focal point and difficult point of controlling Mercury Emissions from Coal-Fired Boilers.
All Ran back zones, coal-burning power plant at least can some pollutant control appliance, such as electrostatic precipitation (ESP), bag-type dust (FF), wet method or dry flue gas desulphurization (FGD) and SCR (SCR) etc. In order to reduce costs, coal-burning power plant need to utilize existing pollutant control appliance to remove the mercury in flue gas conventionally. At present, coal-fired flue gas mercury removal mainly concentrates on the research of adsorbent, catalyst and how to utilize the research of the aspects such as existing pollutant purification device demercuration. The cooperation-removal that utilizes existing desulphurization and denitration equipment to realize mercury can reduce extra cost. SCR denitration technology is current most study, most widely used, is also the most effective flue gas NOxRemove technology. SCR denitrating catalyst not only can Reduction of NOxAnd can be by the Hg in flue gas0Catalytic Oxygen changes into Hg2+. By utilizing SCR denitrating catalyst by Hg0Efficient oxidation becomes Hg soluble in water2+, the Hg of generation2+Removed by follow-up desulfurizer, can reach and remove NO simultaneouslyxWith Hg0Object. Therefore, SCR equipment collaboration wet FGD system removes Hg in coal-fired flue-gas0Be considered to a kind of Mercury Emissions from Coal-Fired Boilers control technology that has application potential. The method removal efficiency is high, without additional investment and operating cost, can be widely used in the purification of coal-fired flue-gas.
But, SCR denitrating catalyst catalytic oxidation Hg0Still Shortcomings: SCR denitrating catalyst is to Hg0Oxidation limited, depend on greatly existence and the concentration of HCl, exist without HCl or the condition of low HCl under Hg0Oxidation is extremely low. And China's coal is mostly low chlorine coal (in flue gas, HCl content is 30-50PPm). Therefore, those can or promote under without HCl condition that at low HCl the SCR denitrating catalyst of mercury efficient oxidation will have boundless application prospect. In addition, conventional commercial SCR specific surface area of catalyst is less, and catalytic performance has much room for improvement. Therefore, to existing V2O5-WO3/TiO2SCR denitrating catalyst carries out modification to improve it at low HCl or without the Hg under HCl condition0Catalytic oxidation performance and specific surface area become problem in the urgent need to address.
Summary of the invention
In order to reduce costs, overcome the deficiency that above-mentioned catalyst exists, the present invention proposes SCR denitrating catalyst having while denitration demercuration and preparation method thereof.
In order to achieve the above object, technical scheme provided by the invention is:
The described complex carrier type SCR denitrating catalyst with while denitration demercuration is made up of the component of following mass percent: V2O5：0.2%～1.2%，WO3: 1.0%～10%, all the other are TiO2-CeO2Composite oxide carrier, each constituent mass percentage sum is 100%.
Described TiO2-CeO2The specific area of composite oxide carrier is 80～120m2/ g, total pore volume is 0.1～0.4cm2/ g, average pore size is 8～12nm, TiO2-CeO2CeO in composite oxide carrier2With TiO2Mol ratio be 0.02～0.2.
Prepare described TiO2-CeO2The method of composite oxide carrier comprises the steps:
(1), by butyl titanate and absolute ethyl alcohol mix and blend 25～35min, preferably 30min, obtains solution A; By deionized water, absolute ethyl alcohol, red fuming nitric acid (RFNA) and cerous nitrate mix and blend 25～35min, preferably 30min, obtains solution B again; Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, deionized water, absolute ethyl alcohol, red fuming nitric acid (RFNA) and cerous nitrate is: (0.08～0.12): (2.1～2.5): (1.6～2.4): (0.5～0.8): (0.08～0.12): (0.005～0.05), control CeO2With TiO2Mol ratio be 0.02～0.2;
(2) A solution is added in B solution, stirs 3～6h, form the colloidal sol of even yellow transparent, by colloidal sol at 35～45 DEG C, preferably ageing 1.5～2.5h under 40 DEG C of conditions, preferably, after 2h, in 75～85 DEG C, preferably 80 DEG C, dry 20～28h, obtains TiO2-CeO2Xerogel, then by TiO2-CeO2Xerogel, in 400～600 DEG C of calcining 3～6h, obtains TiO2-CeO2Composite oxide carrier.
The method of preparing above-mentioned catalyst is by the TiO stating2-CeO2Composite oxide carrier is placed in compound maceration extract, at 75～85 DEG C, preferably under 80 DEG C of conditions, stirs 1～3h, dipping 3～15h, in 100～110 DEG C, preferably 105 DEG C dry after again in 400 DEG C～600 DEG C calcining 2～6h, to obtain final product; Described compound maceration extract is made up of the component of following mass percent: ammonium metavanadate: 0.02%～0.16%, and ammonium tungstate: 0.1%～1.2%, oxalic acid: 0.02%～0.2%, all the other are water.
The invention will be further described below:
The present invention uses sol-gal process to prepare nanoscale TiO2-CeO2Composite oxide carrier, adopts infusion process to prepare V2O5-WO3/TiO2-CeO2Catalyst, active component is evenly distributed on TiO2-CeO2Carrier surface. CeO2There is powerful oxygen storage capacity and special Ce thereof3+/Ce4+Redox couple, CeO2With V2O5There is collaborative facilitation; Add CeO2Can further improve denitration demercuration activity and the water resistant sulfur resistance of catalyst.
By CeO2Be doped in TiO with certain proportioning2On carrier, can effectively promote the denitration demercuration activity of catalyst and the stability of catalyst activity. Preparation CeO2/TiO2Mol ratio is 0.02～0.2 TiO2-CeO2Complex carrier; Mass percent is the compound dipping solution of 0.02%～0.16% ammonium metavanadate, 0.1%～1.2% ammonium tungstate, 0.2%～0.2% oxalic acid; By infusion process by TiO2-CeO2Complex carrier is placed in compound maceration extract, makes ammonium metavanadate and ammonium tungstate at TiO2-CeO2Upper fully dispersion and load, after being dried, under 400～600 DEG C of conditions, sample is calcined to 2～6h, thereby prepare with TiO2-CeO2For carrier, load has 0.2%～1.2%V2O5、1.0%～10%WO3Catalyst, wherein V2O5、WO3For catalyst activity component; CeO2Doping vario-property TiO2Carrier, has improved the specific area of catalyst, and active component is better disperseed; CeO2With V2O5Synergy improved denitration demercuration performance and the anti-sulphur of water resistant of catalyst.
Compared with existing SCR catalyst, advantage of the present invention is:
1, the present invention is with nanoscale TiO2-CeO2Composite oxides are carrier, CeO2There is higher specific area, CeO2To TiO2Doping vario-property can increase the effect of specific surface area of catalyst, and then can make active component better be disperseed, by the interaction between active component and carrier, further improve the activity of catalyst simultaneously, under the condition without HCl existence or low HCl, there is stronger Hg0Oxidation activity. ;
2, this catalyst, without separately establishing special demercuration equipment, completes NO in original flue gas denitration catalyst reactor simultaneouslyxCatalytic reduction and Hg0Catalytic oxidation, the Hg of generation2+In smoke-gas wet desulfurization process subsequently, be removed, do not increasing under the prerequisite of coal-fired plant flue gas purification facility, realize NOxAnd Hg0When discharge, control;
3、CeO2Doping vario-property improve catalytic activity at a lower temperature of catalyst, meanwhile, improve the water resistant sulfur resistance of catalyst.
In a word, the present invention is with CeO2Doping vario-property TiO2Carrier, makes nanoscale TiO2-CeO2Composite oxides are as the carrier of SCR denitrating catalyst. This catalyst not only has higher specific area, the anti-sulphur of water resistant preferably, and at low HCl or under without HCl condition, also there is very strong Hg0Oxidation susceptibility, can be by NOxSCR becomes N2Time by Hg0Be oxidized to Hg2+, can complete demercuration reaction at original denitrating flue gas SCR reactor.
Detailed description of the invention
Embodiment 1
The described complex carrier type SCR denitrating catalyst with while denitration demercuration is made up of the component of following mass percent: V2O5：0.8%，WO3: 8%, all the other are TiO2-CeO2Composite oxide carrier. Described TiO2-CeO2The specific area of composite oxide carrier is 80～120m2/ g, total pore volume is 0.1～0.4cm2/ g, average pore size is 8～12nm, TiO2-CeO2CeO in composite oxide carrier2With TiO2Mol ratio be 0.02.
Prepare described TiO2-CeO2The method of composite oxide carrier comprises the steps:
By 0.1mol butyl titanate and 2.3mol absolute ethyl alcohol mix and blend 30min, obtain solution A; By 1.9mol deionized water, 0.6mol absolute ethyl alcohol, 0.1mol red fuming nitric acid (RFNA) and 0.005mol cerous nitrate mix and blend 30min, obtain solution B again; A solution is slowly added in B solution, and vigorous stirring 3～6h, forms the colloidal sol of even yellow transparent, under 40 DEG C of conditions after ageing 2h, in 80 DEG C dry 24 hours, obtain TiO2-CeO2Xerogel, then by TiO2-CeO2Xerogel, in 400～600 DEG C of calcining 3～6h, obtains TiO2-CeO2Composite oxide carrier.
The method of preparing described catalyst is by the TiO stating2-CeO2Composite oxide carrier is placed in compound maceration extract, under 80 DEG C of conditions, stir after 1-3h, dipping 3h～15h, in 105 DEG C dry, then in 400 DEG C～600 DEG C calcining 2～6h, to obtain final product; Described compound maceration extract is made up of the component of following mass percent: ammonium metavanadate: 0.1%, and ammonium tungstate: 1.0%, oxalic acid: 0.08%, all the other are water.
Described catalyst can represent by following formula, VW/TiCe0.02, wherein CeO2With TiO2Mol ratio is 0.02.
Embodiment 2
The preparation condition of described catalyst and preparation method are with embodiment 1, different, CeO2With TiO2Mol ratio is 0.05; Described catalyst can represent by following formula, VW/TiCe0.05
Embodiment 3
The preparation condition of described catalyst and preparation method are with embodiment 1, different, CeO2With TiO2Mol ratio is 0.08; Described catalyst can represent by following formula, VW/TiCe0.08
Embodiment 4
The preparation condition of described catalyst and preparation method are with embodiment 1, different, CeO2With TiO2Mol ratio is 0.11; Described catalyst can represent by following formula, VW/TiCe0.11
Embodiment 5
The preparation condition of described catalyst and preparation method are with embodiment 1, different, CeO2With TiO2Mol ratio is 0.15; Described catalyst can represent by following formula, VW/TiCe0.15
Embodiment 6
Catalyst of the present invention is desulphurization denitration performance test simultaneously
Use respectively five kinds of different catalysts (VWTiCe of the present inventionx) and conventional flue gas SCR denitration catalyst (code name is VWTi), in fixed bed reactors, carry out while denitration demercuration activity test. Catalyst is packed in catalytic reactor, and catalyst loading amount is 0.5g; The composition that passes into simulated flue gas is: 5%vol.O2，700ppmNO，700ppmNH3，400ppmSO2，70.00μg/m3Hg0, balanced gas N2; Be 50000h in air speed-1, under the condition of reaction temperature 100-400 DEG C, detecting catalyst is denitration demercuration performance simultaneously.
Result shows, CeO2Increase, improved the catalyst catalytic performance of denitration demercuration simultaneously, in the 100-400 DEG C of temperature range, SO2Under the condition existing, NOxConversion ratio can reach 88.78%. Hg0Oxidation efficiency reach 87.87%. In addition, along with CeO2/TiO2Mol ratio increases, and also improves at the catalytic performance of low temperature.
Embodiment 7
The anti-sulphur test of catalyst water resistant of the present invention
1, the anti-sulphur test of catalyst of the present invention
0.50g catalyst (the VWTiCe preparing with example 3 of the present invention0.08) be experimental subjects; Air speed is: 50000h-1; Simulated flue gas composition is: 5%vol.O2，700ppmNO，700ppmNH3，400ppmSO2(need to use time), 70.00 μ g/m3Hg0, balanced gas N2; In 250 DEG C of detecting catalysts denitration demercuration activity simultaneously. VWTiCe0.08Denitration activity passing into SO2Front and back change very little, and Hg0Oxidation efficiency increases. Illustrate that thus catalyst of the present invention has stronger sulfur resistance, SO2Promote Hg0Effect.
2, catalyst of the present invention water-resistance test
Catalyst (the VWTiCe preparing with example 3 of the present invention0.08), in fixed bed reactors, carry out water-resistance test. Catalyst is packed in catalytic reactor, and catalyst loading amount is 0.5g; Passing into simulated flue gas component is: 5%vol.O2，700ppmNO，700ppmNH3，400ppmSO2，8%vol.H2When O(need to use), all the other are balanced gas N2; Be 50000h in air speed-1, under the condition that reaction temperature is 250 DEG C, detecting catalyst water-resistance performance. Add H2After O, denitration demercuration efficiency slightly declines, and denitration efficiency is 84.66%, and demercuration efficiency is 82.90%. Result shows, with TiO2-CeO2Composite oxides are that the catalyst of carrier has stronger water repelling property. Can reduce SO in flue gas2，H2O is to remove NO simultaneouslyxNegative effect with mercury;
Embodiment 8
The BET of catalyst of the present invention and SEM test
In the present invention, all to adopt Micromeritics Instrument Corp. U.S.A (MicromeriticsInstrumentCrop, USA) model be that the specific area of MicromeriticsTristar 3020 and pore size distribution determining instrument are measured for the specific area of all catalyst and pore structure analysis. Test condition: analytical gas and saturation pressure mensurated gas composition are N2, backfill gas and mensuration free space gas are He, and temperature is 77K, and testing sample is in 180 DEG C of degassed 5h. Specific area is that to have pore volume and the aperture that BET (Brunauer-Emmett-Teller) formula calculates under the condition of 0.05-0.35 partial pressure be by desorption curve negotiating BJH(Barrett-Joyner-Halenda) calculate; In addition the scanningelectronmicroscope(SEM of catalyst of the present invention) analyze all adopt the S-4800FESEM of Hitachi, Ltd type SEM instrument to measure. The surface texture of sample is exaggerated respectively 10000 and 100000 times.
Result shows, CeO2Interpolation increased the specific area of catalyst, the active component making is better disperseed, catalytic efficiency is higher. Meanwhile, from SEM image, can see the TiO of this catalyst invention2-CeO2Composite oxide carrier belongs to Nano grade, has improved the interaction between active component and carrier, has further improved the catalytic activity of catalyst.
Claims (4)
1. have a complex carrier type SCR denitrating catalyst for denitration demercuration simultaneously, it is characterized in that, described catalyst is made up of the component of following mass percent:
V2O5：0.2%～1.2%，WO3: 1.0%～10%, all the other are TiO2-CeO2Composite oxide carrier, each constituent mass percentage sum is 100%.
2. catalyst as claimed in claim 1, is characterized in that, described TiO2-CeO2The specific area of composite oxide carrier is 80～120m2/ g, total pore volume is 0.1～0.4cm2/ g, average pore size is 8～12nm, TiO2-CeO2CeO in composite oxide carrier2With TiO2Mol ratio be 0.02～0.2.
3. prepare TiO as claimed in claim 1 or 2 for one kind2-CeO2The method of composite oxide carrier, is characterized in that, described method comprises the steps:
By butyl titanate and absolute ethyl alcohol mix and blend 25～35min, obtain solution A; By deionized water, absolute ethyl alcohol, red fuming nitric acid (RFNA) and cerous nitrate mix and blend 25～35min, obtain solution B again; Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, deionized water, absolute ethyl alcohol, red fuming nitric acid (RFNA) and cerous nitrate is: (0.08～0.12): (2.1～2.5): (1.6～2.4): (0.5～0.8): (0.08～0.12): (0.005～0.05), control CeO2With TiO2Mol ratio be 0.02～0.2;
A solution is added in B solution, stir 3～6h, form the colloidal sol of even yellow transparent, colloidal sol after ageing 1.5～2.5h, in 75～85 DEG C of dry 20～28h, is obtained to TiO under 35～45 DEG C of conditions2-CeO2Xerogel, then by TiO2-CeO2Xerogel, in 400～600 DEG C of calcining 3～6h, obtains TiO2-CeO2Composite oxide carrier.
4. prepare a method for catalyst as claimed in claim 1 or 2, it is characterized in that, described method is by the TiO described in claim 1 or 22-CeO2Composite oxide carrier is placed in compound maceration extract, under 75～85 DEG C of conditions, stirs 1～3h, dipping 3～15h, in 100～110 DEG C dry after again in 400 DEG C～600 DEG C calcining 2～6h, to obtain final product; Described compound maceration extract is made up of the component of following mass percent: ammonium metavanadate: 0.02%～0.16%, and ammonium tungstate: 0.1%～1.2%, oxalic acid: 0.02%～0.2%, all the other are water.
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| CN108126707A (en) * | 2017-12-28 | 2018-06-08 | 东北大学 | A kind of low temperature, SCR denitration, the preparation method and application that nontoxic, composite oxides are carrier |
| CN108144598A (en) * | 2018-01-31 | 2018-06-12 | 东北大学 | A kind of mechanism compound type oxide low-temperature denitration catalyst and preparation method thereof |
| CN108993477A (en) * | 2018-06-27 | 2018-12-14 | 江苏大学 | A kind of preparation method and application of the modified SCR denitration of novel neodymium |
| CN110180261A (en) * | 2019-05-13 | 2019-08-30 | 西安热工研究院有限公司 | A kind of preparation method of denitration filtrate |
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| CN106311291A (en) * | 2016-09-07 | 2017-01-11 | 武汉大学 | Composite catalyst based on denitration and demercuration reinforcing function of prepositive SCO smoke of coal-fired power plant and preparation method thereof |
| CN108126707A (en) * | 2017-12-28 | 2018-06-08 | 东北大学 | A kind of low temperature, SCR denitration, the preparation method and application that nontoxic, composite oxides are carrier |
| CN108144598A (en) * | 2018-01-31 | 2018-06-12 | 东北大学 | A kind of mechanism compound type oxide low-temperature denitration catalyst and preparation method thereof |
| CN108993477A (en) * | 2018-06-27 | 2018-12-14 | 江苏大学 | A kind of preparation method and application of the modified SCR denitration of novel neodymium |
| CN110180261A (en) * | 2019-05-13 | 2019-08-30 | 西安热工研究院有限公司 | A kind of preparation method of denitration filtrate |
| CN110180261B (en) * | 2019-05-13 | 2021-12-28 | 西安热工研究院有限公司 | Preparation method of denitration filter material |
| CN110721670A (en) * | 2019-10-30 | 2020-01-24 | 中国科学院过程工程研究所 | Low-vanadium denitration, demercuration and dioxin removal catalyst and preparation method and application thereof |
| CN110721670B (en) * | 2019-10-30 | 2020-12-04 | 中国科学院过程工程研究所 | Low-vanadium denitration, demercuration and dioxin removal catalyst and preparation method and application thereof |
| CN113559852A (en) * | 2021-07-23 | 2021-10-29 | 华侨大学 | Hg removal suitable for medium and low temperature conditions0Catalyst and preparation method thereof |
| CN113559852B (en) * | 2021-07-23 | 2023-10-31 | 华侨大学 | Hg removing device suitable for medium and low temperature conditions 0 Catalyst and preparation method thereof |
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Application publication date: 20160525 |