CN101972652B - Preparation method of composite SCR catalyst with zero-valent mercury conversion function - Google Patents
Preparation method of composite SCR catalyst with zero-valent mercury conversion function Download PDFInfo
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- CN101972652B CN101972652B CN2010105646144A CN201010564614A CN101972652B CN 101972652 B CN101972652 B CN 101972652B CN 2010105646144 A CN2010105646144 A CN 2010105646144A CN 201010564614 A CN201010564614 A CN 201010564614A CN 101972652 B CN101972652 B CN 101972652B
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Abstract
A preparation method of a composite SCR catalyst with zero-valent mercury conversion function belongs to the technical field of environmental protection, and comprises the steps of sequentially adding a ruthenium element precursor and a denitration basic catalytic component precursor into deionized water, uniformly stirring to obtain an impregnation solution, mixing a catalyst carrier with the impregnation solution, drying, and finally placing the dried catalyst carrier in a muffle furnace for roasting to obtain the composite SCR catalyst. The catalyst prepared by the invention can effectively convert zero-valent mercury in flue gas into easily-removed divalent mercury while reducing and converting nitrogen oxides, so that the divalent mercury convenient to capture is formed, and double effects of simultaneously denitrifying coal-fired flue gas and oxidizing the zero-valent mercury are realized.
Description
Technical field
What the present invention relates to is a kind of Preparation of catalysts method of environmental protection technical field, specifically is a kind of compound SCR Preparation of catalysts method with nonvalent mercury transformation.
Background technology
As everyone knows, mercury is a kind of toxic pollutant.It not only produces direct or indirect harm to health, and because it has characteristics such as bioaccumulation property and difficult degraded, also very big to the harm of environment.Coal-fired flue-gas is one of main human factor that causes by the atmosphere mercury pollution.China's big, coal-fired mercury content of coal-fired consumption is high, so the mercury pollution problem is more serious, and the international community's pressure that faces is also increasing, so it is extremely important to strengthen the emission control of flue gas mercury.
Mercury in coal-fired flue-gas mainly with particle mercury (Hg
P), gaseous state divalence mercury (Hg
2+) and gaseous state nonvalent mercury (Hg
0) three kinds of forms exist, Hg wherein
0Account for 20～80% of total mercury in the flue gas.Conventional smoke eliminator has collaborative demercuration: dust arrester can effectively be removed Hg
PHg
2+Soluble in water, can be removed by flue gas desulfur device.Yet, Hg
0Because volatile, be insoluble in water, be difficult to effectively removed by existing Air Pollution Control Board control equipment, so, Hg
0Efficiently remove difficult point and the emphasis that becomes current flue gas demercuration.
Take suitable ancillary method to realize Hg
0To Hg
2+Efficient conversion, to make full use of desulfurizer efficient absorption Hg
2+Be to control Hg at present
0Most economical feasible approach, and become the research focus gradually.But Hg
0To Hg
2+Efficient conversion be key and the difficult point place of high-efficiency mercury removal, the researcher does not obtain maturation method for transformation efficiently as yet at present.Confirmed that at present (Selective catalytic reduction, SCR) catalyst can promote that HCl is to Hg in the flue gas to SCR
0Oxidation; But oxidation efficiency is not high when the HCl concentration in the flue gas is low; And research show that also the ammonia that denitration added has certain inhibitory action to the oxidation of nonvalent mercury, sulfur in smoke also can influence the catalysed oxidn of SCR catalyst to nonvalent mercury.
Through the retrieval of prior art is found, some conventional scr catalyst to the catalyzed conversion effect of nonvalent mercury relatively poor (Kim, Appl.Catal.B.Environ.2010,99,272-278), the removal efficient of nonvalent mercury just can reach 90% under the 50ppmHCl effect.Yet the HCl concentration in common flue gas is difficult to reach so high requirement.The present invention then to current SCR modified catalyst under low HCl concentration to the not high problem of nonvalent mercury catalytic oxidation efficient, develop and under different temperatures, low concentration HCl, have higher nonvalent mercury and remove the SCR modified catalyst that efficient and nitrogen oxide are removed efficient.
Summary of the invention
The present invention is directed to the above-mentioned deficiency that prior art exists; A kind of compound SCR Preparation of catalysts method with nonvalent mercury transformation is provided; Utilize this catalyst can nitrogen oxide is reduced transform in; Nonvalent mercury in the flue gas effectively is converted into the divalence mercury that is easy to remove, thereby forms the divalence mercury of being convenient to capture.Ruthenium is as enhancement component, is used in combination with primary activity component (V, W or Mo etc.) in the SCR catalyst, and the content of its Ru element is in the 0.05-2.0% scope.The SCR catalyst that contains Mo helps further improving the reinforced effects and the anti-sulphur effect of ruthenium.In the preparation, ruthenium element can add in the SCR Preparation of catalysts raw material, or direct impregnation is processed said catalyst again behind drying and calcining to SCR catalyst finished product.Utilize this catalyst can realize double effects to coal-fired flue-gas denitration simultaneously and nonvalent mercury oxidation.
The present invention realizes through following technical scheme, the present invention includes following steps:
The first step, successively the basic catalyst component predecessor of ruthenium element predecessor and denitration is added deionized water and stir and obtain the metal ion total concentration and be: the dipping solution of 0.01g/mL-0.50g/mL, wherein: the mol ratio of the basic catalyst component ion of ruthenium ion and denitration is 0.01-0.2: 1.
Described ruthenium element predecessor is: a kind of or its combination in ruthenic chloride, nitric acid ruthenium, carbonic acid ruthenium, oxalic acid ruthenium or the ruthenium acetate.
The basic catalyst component predecessor of described denitration is: a kind of or its combination in vanadium oxalate, inclined to one side alum salts, tungstates or the molybdate.
Second step, directly dry after taking by weighing catalyst carrier and dipping solution mixing or add binding agent after dry;
Described catalyst carrier is a kind of or its combination in titanium dioxide, zirconia or the silica, perhaps directly with the carrier of commercial SCR catalyst as dipping solution.
Described oven dry is meant: impregnated catalyst carrier was dried 5-24 hour under 60 ℃～120 ℃ temperature;
The consumption of described binding agent is the 1-10% of catalyst carrier quality, and this binding agent is polyacrylamide or CMC sodium carboxymethylcellulose.
The 3rd step, the catalyst carrier after will drying place Muffle furnace to be 1～30 ℃/minute with heating rate and rise to 200 ℃ of roasting 0.5～2h; Rising to 400-500 ℃ of roasting 0.5～4h with 1～30 ℃/minute speed more fully decomposes predecessor; Mode with cooling naturally is cooled to normal temperature with catalyst at last, finally processes to be used for the composite SCR catalyst that nonvalent mercury transforms.
Through the compound SCR catalyst that method for preparing obtains, wherein active principle and mass percent are the Mo element of 0.2-10% and the ruthenium element of 0.05-2.0%, and this compound SCR catalyst is particle, honeycomb fashion or board-like.This catalyst to the catalytic oxidation ability of nonvalent mercury much larger than single component catalyst, and can be under the temperature (100～450 ℃) of broad and higher sulfur dioxide concentration the efficiently catalyzing and oxidizing nonvalent mercury, prevent the catalyst poisoning inactivation.
Description of drawings
Fig. 1 is the embodiment process chart.
The specific embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
As shown in Figure 1, following examples are at first carried out doping vario-property to the SCR catalyst and are prepared ruthenium metal oxide composite SCR catalyst, and modified catalyst is installed in the SCR catalysis system.In the SCR catalysis system, spray into oxidant gas then.Hg in flue gas
0Getting in the SCR catalysis system, is Hg by catalytic oxidation under the synergy of oxidant and catalyst
2+By the Hg of flying dust absorption in the flue gas
0And Hg
2+Can remove through dust pelletizing system, and the Hg in the gas phase
2+After getting into desulphurization system, absorbed by doctor solution.Through the SCR catalysis system, after dust pelletizing system and the desulphurization system, the mercury in the flue gas is effectively removed, and discharges through chimney at last.
Embodiment 1
With TiO
2For carrier S CR catalyst is a carrier, utilize immersion process for preparing SCR and Ru/SCR composite catalyst.
A, conventional scr Preparation of Catalyst dipping solution are formed: 0.3g ammonium metavanadate, 1.8g ammonium tungstate add deionized water and are diluted to 20ml, add the 0.5g polyacrylamide again as binding agent;
B, conventional scr Preparation of Catalyst dipping solution are formed: 0.3g ammonium metavanadate, 1.8g ammonium paramolybdate, and add deionized water and be diluted to 20ml, add the 0.5g polyacrylamide again as binding agent;
C, mix ruthenium SCR composite catalyst and prepare dipping solution and form: 0.2g ruthenic chloride, 0.3g ammonium metavanadate, 1.8g ammonium tungstate add deionized water and are diluted to 20ml, add the 0.5g polyacrylamide again as binding agent;
Utilize powdery TiO
2As catalyst carrier, take by weighing 3 parts, every part of 30g; Pour it in above-mentioned 3 kinds of solution dipping and stirring respectively; Soak and after 1 hour unnecessary maceration extract is poured out, and the powder behind the single-steeping is dried in 60-70 ℃ baking oven, again it is poured into respectively in the residual dipping solution afterwards; And fully stir, make maceration extract all by TiO
2Carrier blots.
SCR behind the dipping was dried 4-6 hour under 60-80 ℃ temperature again, rose to 300 ℃ of roasting 1h with 5 ℃/minute of heating rates in the transposition Muffle furnace; Rise to 400 ℃ of roasting 4h with 2 ℃/minute speed again predecessor nitrate is fully decomposed, with 2 ℃/minute cooldown rate catalyst is cooled to normal temperature again.Be called catalyst A-D successively through the prepared catalyst of said method.Utilize the prepared catalyst of said method following: A is common V/W/Ti type SCR catalyst, and B is for containing V/Mo/Ti type SCR catalyst; C is the V/W/Ti type composite SCR catalyst that Ru mixes; Through grinding, catalyst granules is the 40-60 order, and specific area is 44-46m
2/ g.
In temperature is 380 ℃, and air speed is 7.96 * 10
4h
-1, the HCl concentration of adding is 5ppm.When adding SO
2When making an experiment, its concentration is 500ppm.Under the situation that does not add sulfur dioxide, the nonvalent mercury catalytic oxidation efficient of catalyst A, B and modification Ru/SCR catalyst is respectively: 51%, 54% and 94%; When adding 500ppm SO
2Situation under, the nonvalent mercury catalytic oxidation efficient of each catalyst is followed successively by: 48%, 52% and 88%.The above results shows that SCR catalyst itself is lower to the oxidation efficiency of nonvalent mercury, but after mixing ruthenium, its efficient can significantly improve.
Have under the situation that sulfur dioxide exists above-mentioned, add 300ppm's and 250ppmNH again
3, the reduction efficiency of NO all in 90 (± 2) % scope, show that the adding ruthenium does not have obvious influence to the denitration efficiency of SCR catalyst, and under same condition, the conversion ratio of nonvalent mercury then is followed successively by 34%, 39% and 85%.Explain that the SCR catalyst that mixes behind the Ru does not receive obvious influence in the performance aspect the reduction denitration, and the ammonia in the system or nitrogen oxide are also little to the mercury transformation efficiency.
Embodiment 2
With TiO
2For carrier S CR catalyst is a carrier, utilizes immersion process for preparing to mix the ruthenium modification and contain molybdenum SCR composite catalyst.
Mix ruthenium SCR composite catalyst and prepare the dipping solution composition: the 0.2g ruthenic chloride, 0.3g ammonium metavanadate, 1.8g ammonium paramolybdate add deionized water and are diluted to 20ml, add the 0.5g polyacrylamide again as binding agent;
Take by weighing 30g powdery TiO
2As catalyst carrier; Pour it in the above-mentioned precursor solution dipping and stirring respectively; Soak and after 1 hour unnecessary maceration extract is poured out, and the powder behind the single-steeping is dried in 60-70 ℃ baking oven, again it is poured into respectively in the residual dipping solution afterwards; And fully stir, make maceration extract all by TiO
2Carrier blots.
SCR behind the dipping was dried 4-6 hour under 60-80 ℃ temperature again, rose to 300 ℃ of roasting 1h with 5 ℃/minute of heating rates in the transposition Muffle furnace; Rise to 400 ℃ of roasting 4h with 2 ℃/minute speed again predecessor nitrate is fully decomposed, with 2 ℃/minute cooldown rate catalyst is cooled to normal temperature again.Through the prepared catalyst of said method is the V/Mo/Ti type composite SCR catalyst that Ru mixes; Through grinding, catalyst granules is the 40-60 order, and specific area is 44-46m
2/ g.
In temperature is 380 ℃, and air speed is 7.96 * 10
4h
-1, the HCl concentration of adding is 5ppm.When adding SO
2When making an experiment, its concentration is 500ppm.Under the situation that does not add sulfur dioxide, the nonvalent mercury catalytic oxidation efficient of catalyst Ru-Mo/SCR is respectively 97%; When adding 500ppm SO
2Situation under, the nonvalent mercury catalytic oxidation efficient of catalyst Ru-Mo/SCR is 95%.The above results shows, the SCR catalyst that contains molybdenum mixes behind the ruthenium better to the changing effect of nonvalent mercury, and anti-sulfur dioxide interference performance is stronger.
Have under the situation that sulfur dioxide exists above-mentioned, add 300ppm's and 250ppmNH again
3, the reduction efficiency of NO show that the denitration efficiency of mixing after the ruthenium modification that contains molybdenum SCR catalyst does not have obvious influence, and under same condition, the conversion ratio of nonvalent mercury then is 92% all in 90 (± 2) % scope.
Embodiment 3
Directly be the basis, it is worn into 40-60 purpose particle, carry out the ruthenium doping vario-property again, utilize immersion process for preparing Ru/SCR catalyst with commercial V/W/Ti type SCR catalyst finished product.
The configuration dipping solution: the A:0.2g ruthenic chloride adds deionized water and is diluted to 20ml; B:0.2g ruthenic chloride, 0.5g ammonium paramolybdate add deionized water and are diluted to 20ml.
Utilize powdery SCR as catalyst carrier, take by weighing 2 parts, every part of 30g; Pour it in above-mentioned 2 kinds of solution dipping and stirring respectively; Soak and after 1 hour unnecessary maceration extract is poured out; And the SCR powder behind the single-steeping dried in 60-70 ℃ baking oven; Again it is poured into respectively in the residual dipping solution afterwards, and fully stir, maceration extract is all blotted by the SCR carrier.
SCR behind the dipping was dried 4-6 hour under 60-80 ℃ temperature again, rose to 300 ℃ of roasting 1h with 5 ℃/minute of heating rates in the transposition Muffle furnace; Rise to 400 ℃ of roasting 4h with 2 ℃/minute speed again predecessor nitrate is fully decomposed, with 2 ℃/minute cooldown rate catalyst is cooled to normal temperature again.Be called catalyst F and G successively through the prepared catalyst of said method, commercial V/W/Ti type SCR catalyst is called E.Its particle diameter is 20-100nm, and specific area is 44-47m
2/ g.
In temperature is 380 ℃, and air speed is 7.96 * 10
4h
-1, the HCl concentration of adding is 5ppm.When adding SO
2When making an experiment, its concentration is 500ppm.Under the situation that does not add sulfur dioxide, catalyst E, F, G are respectively the catalytic oxidation efficient of nonvalent mercury: 33%, 92% and 95%.When adding 500ppm SO
2Situation under, the nonvalent mercury catalytic oxidation efficient of each catalyst is followed successively by: 31%, 89% and 92%.Thus it is clear that, on the basis of commercial SCR catalyst, can obtain higher removal of mercury efficient behind the load ruthenium too.
Embodiment 4
Mix ruthenium SCR composite catalyst and prepare the dipping solution composition: 1g nitric acid ruthenium (anhydrous), 3g ammonium metavanadate, 2g ammonium molybdate, the 18g ammonium tungstate adds the maceration extract that deionized water is processed 150ml, adds 3gCMC again as binding agent; Take by weighing 200gTiO
2Powder, with its with process paste after maceration extract fully mixes.Utilize honeycomb die that the paste extruding is formed for ceramic honey comb, the profile of every ceramic honey comb is 50x50x100, and the size in hole is 3mmx3mm.Under 60-80 ℃ temperature, it was dried 4-6 hour again, rise to 300 ℃ of roasting 1h with 5 ℃/minute of heating rates in the transposition Muffle furnace; Rise to 500 ℃ of roasting 4h with 2 ℃/minute speed again predecessor salt is fully decomposed, with 2 ℃/minute cooldown rate catalyst is cooled to normal temperature again, process ceramic honey comb shape catalyst at last.
Getting 2 such composite catalysts, is 380 ℃ in temperature, and air speed is 15000h
-1Condition under, nonvalent mercury is handled (except that flow, other condition is with instance 1).Under the situation that does not add sulfur dioxide, utilize the HCl concentration of 5ppm, the nonvalent mercury catalytic oxidation efficient of catalyst Ru-Mo/SCR is respectively 95%; When adding 500ppm SO
2Situation under, the nonvalent mercury catalytic oxidation efficient of catalyst Ru-Mo/SCR is 93%.The above results shows, the SCR catalyst that contains molybdenum mixes behind the ruthenium better to the changing effect of nonvalent mercury, and anti-sulfur dioxide interference performance is stronger.And the SCR catalyst of use same specification under similarity condition, has only the clearance about 40% to nonvalent mercury.
Claims (5)
1. the compound SCR Preparation of catalysts method with nonvalent mercury transformation is characterized in that, may further comprise the steps:
The first step, successively the basic catalyst component predecessor of ruthenium element predecessor and denitration is added deionized water and stir and obtain the metal ion total concentration and be: the dipping solution of 0.01g/mL-0.50g/mL, wherein: the mol ratio of the basic catalyst component ion of ruthenium ion and denitration is 0.01-0.2: 1;
Second step, directly dry after taking by weighing catalyst carrier and dipping solution mixing or add binding agent after dry;
The 3rd step, the catalyst carrier after will drying place Muffle furnace to be 1～30 ℃/minute with heating rate and rise to 200 ℃ of roasting 0.5～2h; Rising to 400～500 ℃ of roasting 0.5-4h with 1～30 ℃/minute speed more fully decomposes predecessor; Mode with cooling naturally is cooled to normal temperature with catalyst at last; Finally process the composite SCR catalyst that is used for the nonvalent mercury conversion, the quality percentage composition of Ru element is at 0.05-2.0% in the prepared catalyst;
The basic catalyst component predecessor of described denitration is: a kind of or its combination in vanadium oxalate, metavanadate, tungstates or the molybdate.
2. according to claim 1 have a compound SCR Preparation of catalysts method that zeroth order is asked transformation, it is characterized in that described ruthenium element predecessor is: a kind of or its combination in ruthenic chloride, nitric acid ruthenium, carbonic acid ruthenium, oxalic acid ruthenium or the ruthenium acetate.
3. the compound SCR Preparation of catalysts method with nonvalent mercury transformation according to claim 1; It is characterized in that; Described catalyst carrier is a kind of or its combination in titanium dioxide, zirconia or the silica, perhaps directly with the carrier of commercial SCR catalyst as dipping solution.
4. the compound SCR Preparation of catalysts method with nonvalent mercury transformation according to claim 1 is characterized in that described oven dry is meant: impregnated catalyst carrier was dried 5-24 hour under 60 ℃-120 ℃ temperature.
5. the compound SCR Preparation of catalysts method with nonvalent mercury transformation according to claim 1; It is characterized in that; The consumption of described binding agent is the 1-10% of catalyst carrier quality, and this binding agent is polyacrylamide or CMC sodium carboxymethylcellulose.
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| GB2522547B (en) | 2012-06-01 | 2018-12-12 | Johnson Matthey Plc | Selective catalytic reduction wall flow filter incorporating a vanadate |
| CN103480371A (en) * | 2013-09-22 | 2014-01-01 | 中国神华能源股份有限公司 | Denitration and demercuration catalyst as well as preparing method and application thereof |
| CN103480271A (en) * | 2013-09-22 | 2014-01-01 | 中国神华能源股份有限公司 | Smoke treatment method |
| JP6257775B2 (en) * | 2013-12-11 | 2018-01-10 | ゼァージァン ユニバーシティ | Catalyst having NOx removal performance and mercury oxidation performance and its production method |
| CN106111135A (en) * | 2016-06-24 | 2016-11-16 | 北京工业大学 | A kind of low temperature resistant to sulfur vanadium titanium system's denitrating catalyst and preparation method |
| CN109173710A (en) * | 2018-09-30 | 2019-01-11 | 重庆大学 | Under a kind of low temperature in catalytic eliminating coal-fired flue-gas nonvalent mercury system and method |
| CN109529575B (en) * | 2018-12-26 | 2023-09-26 | 宁波大学 | Civil heating boiler desulfurization and denitrification system |
| CN110038564A (en) * | 2019-03-25 | 2019-07-23 | 宁波大学 | A kind of catalyst with core-casing structure and preparation method thereof of high-efficient purification burning waste gas |
| CN113426451A (en) * | 2021-06-18 | 2021-09-24 | 中建安装集团有限公司 | Preparation method and application of micron ozone catalyst |
| CN119425687A (en) * | 2025-01-09 | 2025-02-14 | 美斯顿(天津)催化剂有限公司 | Preparation method of a corrugated plate type flue gas comprehensive treatment catalyst |
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| JP4175465B2 (en) * | 2003-02-07 | 2008-11-05 | 三菱重工業株式会社 | Method and system for removing mercury from exhaust gas |
| WO2006025900A2 (en) * | 2004-08-27 | 2006-03-09 | Cichanowicz J Edward | Multi-stage heat absorbing reactor and process for scr of nox and for oxidation of elemental mercury |
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