CN105688800A - MnO2/flyash-attapulgite catalyst/adsorbent and method thereof for removing elemental mercury in smoke - Google Patents
MnO2/flyash-attapulgite catalyst/adsorbent and method thereof for removing elemental mercury in smoke Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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Abstract
The invention discloses an MnO2/flyash-attapulgite catalyst/adsorbent and a method thereof for removing elemental mercury in smoke. According to the catalyst, flyash-attapulgite is taken as a carrier, and MnO2 is taken as an active component. The catalyst is prepared from the following components in percentage by weight: 90-99% of flyash-attapulgite carrier and 1.0-10% of MnO2. The method for removing elemental mercury in smoke comprises the following steps: filling the MnO2/flyash-attapulgite catalyst/adsorbent in a fixed-bed reactor, controlling the reaction temperature to be 120-200 DEG C, and filling normal-pressure mercury-containing smoke in at an air speed of 5000-30000/h. The catalyst/adsorbent has high capability of catalyzing, oxidizing, adsorbing and removing the mercury in a smoke-discharging temperature range, is capable of catalyzing and oxidizing HgO to be Hg<2+> compounds as well as adsorbing the Hg<2+> compounds on the catalyst/adsorbent; the catalyst/adsorbent takes solid waste flyash of coal-fired power plants and low-cost and easily available attapulgite as the carriers; the preparation cost and the operation cost of the catalyst are reduced; the catalyst/adsorbent has a good actual application prospect in the field of mercury removal from the smoke.
Description
Technical field
The invention belongs to technical field of air pollution control, the elimination relating to elemental mercury from coal-fired flue gas purifies, specifically a kind of MnO2/ flyash-attapulgite catalysis/adsorbent and for removing the method for Elemental Mercury in flue gas。
Background technology
Coal is the main energy sources of China, and in primary energy structure, proportion is very big, and the utilization of coal is directly to burn。Hydrargyrum is one of harmful heavy metal pollutant of coal combustion release, it is possible to long-distance migration in atmosphere of floating, and can enter human body by food chain, ecological environment and health can be caused serious, lasting harm。Coal-fired mercury pollution has caused the most attention of developed country, and countries in the world government has promulgated that laws and regulations are to limit the mercury emissions of coal-burning power plant in succession。China has issued " fossil-fuel power plant atmospheric pollutant emission standard " of new revision on January 1st, 2012, the discharge of thermal power plant's hydrargyrum is made that clear stipulaties, the discharge value of mercury in flue gas is limited to 0.03mg/m3。Control to carry out correlational study to coal-fired mercury pollution although national governments have put into huge fund, but not yet form cost-effective control technology at present。
In coal-fired flue-gas, the form of Hg mainly has the Hg of gaseous state0And Hg2+And it is adsorbed in the Hg on flying dustp。Major part HgpAnd Hg2+Can be removed by the existing dust arrester of power plant, wet desulphurization device (WFGD)。Hg0Account in coal-fired flue-gas the 20%～50% of gaseous state Hg, owing to its volatility is high, be insoluble in the characteristic of water, it is difficult to is controlled device by existing power plant pollution thing and remove, thus become the emphasis that coal-fired flue-gas Hg elimination is researched and developed。
Currently for Hg in coal-fired flue-gas0Emission control, main method is to spray into the adsorptive gaseous hydrargyrum of active carbon powder in flue, then removing dust device elimination。The method need to spray activated carbon before dedusting, and flue-gas temperature is higher, causes that activated carbon adsorptive capacity is relatively low, utilization rate is low, straying quatity is big, will consume substantial amounts of activated carbon, costly。Another kind of method is by Hg0Catalytic oxidation is Hg2+, then then through the existing pollutant catabolic gene device elimination of power plant。Studying more catalyst at present is V2O5Base business SCR catalyst, this catalyst series is many with TiO2For carrier, to Hg0Having higher oxidation activity, but its operation temperature is higher, absorbability is very low, it is necessary to be combined with the wet desulphurization device in downstream, could by Hg0The Hg that oxidation generates2+Elimination。Therefore, the effective new catalyst of exploiting economy and carrier thereof so that it is have catalysis activity and absorbability concurrently, become Hg in coal-fired flue-gas0One of study hotspot of elimination。
Summary of the invention
It is an object of the invention to the deficiency for existing coal-fired flue-gas mercury pollution control technology, it is provided that a kind of MnO2/ flyash-attapulgite catalysis/adsorbent, can Hg in efficiently catalyzing and oxidizing flue gas0Generate Hg2+Compound, and it is adsorbed on MnO2On/flyash-attapulgite, it is not necessary to remove then through downstream WFGD, this catalysis/adsorbent, with coal-burning power plant's solid waste flyash and attapulgite cheap and easy to get for carrier, reduces preparation cost and the operating cost of catalysis/adsorbent。
For achieving the above object, in technical scheme, based on the catalyst for denitrating flue gas (publication number CN102000564A, flyash-attapulgite compound SCR denitration catalyst and preparation method thereof) of our early development, preparation has the MnO of catalysis activity and absorbability2/ flyash-attapulgite catalysis/adsorbent, and for removing the Hg in coal-fired flue-gas0。
MnO2/ flyash-attapulgite catalysis/sorbent preparation method is to be mixed homogeneously according to the ratio of 1: 1 with attapulgite by flyash, add water post-drying, calcining, the pulverizing of stirring, sieve and obtain the particulate catalyst support of particle diameter 30-60 order, by this carrier incipient impregnation in certain density Mn (NO3)2In solution, stir, stand through room temperature, dry, in 250-600 DEG C of nitrogen and air atmosphere, then calcine 2-5h successively, obtain MnO2/ flyash-attapulgite catalysis/adsorbent。
The MnO of the present invention2/ flyash-attapulgite catalysis/adsorbent application process is by MnO2/ flyash-attapulgite catalysis/adsorbent is loaded in fixed bed reactors, controls reaction temperature 120-200 DEG C, passes into normal pressure mercury fume, and wherein the concentration of hydrargyrum is 10-201 μ g/m3, air speed 5000-30000h-1。
The present invention compared with prior art, has following remarkable advantage:
1, load MnO2To MnO prepared by flyash-Attapulgite carrier2/ flyash-attapulgite catalysis/adsorbent, to Hg within the scope of exhaust gas temperature0There is higher catalytic oxidation activity and absorbability, can by Hg0Catalytic oxidation generates Hg2+Compound is also adsorbed on MnO2On/flyash-attapulgite, it is not necessary to remove then through WFGD, be placed in the last of coal-fired plant flue gas cleaning system, it is not necessary to flue gas is heated again。
2, SO in flue gas2Not only to MnO2/ flyash-attapulgite catalysis/adsorbent Non-toxic effect, on the contrary to its elimination Hg0There is certain facilitation。
3、MnO2/ flyash-attapulgite catalysis/adsorbent adopts coal-burning power plant's solid waste flyash and attapulgite cheap and easy to get to be carrier, preparation is simple, and renewable recycling, reduces preparation cost and operating cost, solve secondary pollution problem simultaneously, have a good application prospect。
Detailed description of the invention
Embodiment 1
Flyash is mixed homogeneously according to mass ratio 1: 1 with attapulgite, adds water and after stirring, stand 2h, 50 DEG C of dry 5h, 110 DEG C of dry 5h, in air atmosphere, 300 DEG C of calcining 3h, pulverize, sieve and obtain granular powder coal ash-Attapulgite carrier that particle diameter is 30-60 order。By this carrier incipient impregnation of 10g in the Mn (NO of 8mL0.026g/mL3)2In solution, stirring, place 12h in atmosphere, 50 DEG C of dry 5h, 110 DEG C of dry 5h, then 350 DEG C of calcining 3h in nitrogen atmosphere, in air atmosphere, 300 DEG C of calcining 2h, obtain MnO2The MnO of load capacity 1wt%2/ flyash-attapulgite catalysis/adsorbent。
Being filled in fixing bed quartz tube reactor by this catalysis/adsorbent, two ends are fixed with silica wool。The temperature programming in the reactor of catalysis/adsorbent keeps constant temperature after 150 DEG C, starts to pass into containing Hg0Simulated flue gas, air speed 5000h-1。Simulated flue gas consists of: 6%O2, 5%H2O, 1500ppmSO2, N2For Balance Air, Hg0Concentration is 80 μ g/m3。Thermostatic absorption reaction 4h, Hg0Removal efficiency be 67%。
Embodiment 2
Flyash is mixed homogeneously according to mass ratio 1: 1 with attapulgite, adds water and after stirring, stand 2h, 50 DEG C of dry 5h, 110 DEG C of dry 5h, in air atmosphere, 300 DEG C of calcining 3h, pulverize, sieve and obtain granular powder coal ash-Attapulgite carrier that particle diameter is 30-60 order。By this carrier incipient impregnation of 10g in the Mn (NO of 8mL0.26g/mL3)2In solution, stirring, place 10h in atmosphere, 50 DEG C of dry 10h, 110 DEG C of dry 10h, then 400 DEG C of calcining 4h in nitrogen atmosphere, in air atmosphere, 350 DEG C of calcining 3h, obtain MnO2The MnO of load capacity 10wt%2/ flyash-attapulgite catalysis/adsorbent。
Being filled in fixing bed quartz tube reactor by this catalysis/adsorbent, two ends are fixed with silica wool。The temperature programming in the reactor of catalysis/adsorbent keeps constant temperature after 180 DEG C, starts to pass into containing Hg0Simulated flue gas, air speed 10000h-1。Simulated flue gas consists of: 6%O2, 5%H2O, 1500ppmSO2, N2For Balance Air, Hg0Concentration is 80 μ g/m3。Thermostatic absorption reaction 4h, Hg0Removal efficiency be 91%。
Embodiment 3
Flyash is mixed homogeneously according to mass ratio 1: 1 with attapulgite, adds water and after stirring, stand 2h, 50 DEG C of dry 5h, 110 DEG C of dry 5h, in air atmosphere, 300 DEG C of calcining 3h, pulverize, sieve and obtain granular powder coal ash-Attapulgite carrier that particle diameter is 30-60 order。By this carrier incipient impregnation of 10g in the Mn (NO of 8mL0.208g/mL3)2In solution, stirring, place 5h in atmosphere, 50 DEG C of dry 5h, 110 DEG C of dry 5h, then 500 DEG C of calcining 3h in nitrogen atmosphere, in air atmosphere, 300 DEG C of calcining 2h, obtain MnO2The MnO of load capacity 8wt%2/ flyash-attapulgite catalysis/adsorbent。
Being filled in fixing bed quartz tube reactor by this catalysis/adsorbent, two ends are fixed with silica wool。The temperature programming in the reactor of catalysis/adsorbent keeps constant temperature after 200 DEG C, starts to pass into containing Hg0Simulated flue gas, air speed 5000h-1。Simulated flue gas consists of: 6%O2, 5%H2O, 1500ppmSO2, N2For Balance Air, Hg0Concentration is 80 μ g/m3。Thermostatic absorption reaction 4h, Hg0Removal efficiency be 84%。
Embodiment 4
Flyash is mixed homogeneously according to mass ratio 1: 1 with attapulgite, adds water and after stirring, stand 2h, 50 DEG C of dry 5h, 110 DEG C of dry 5h, in air atmosphere, 300 DEG C of calcining 3h, pulverize, sieve and obtain granular powder coal ash-Attapulgite carrier that particle diameter is 30-60 order。By this carrier incipient impregnation of 10g in the Mn (NO of 8mL0.13g/mL3)2In solution, stirring, place 5h in atmosphere, 50 DEG C of dry 5h, 110 DEG C of dry 5h, then 600 DEG C of calcining 3h in nitrogen atmosphere, in air atmosphere, 350 DEG C of calcining 2h, obtain MnO2The MnO of load capacity 5wt%2/ flyash-attapulgite catalysis/adsorbent。
Being filled in fixing bed quartz tube reactor by this catalysis/adsorbent, two ends are fixed with silica wool。The temperature programming in the reactor of catalysis/adsorbent keeps constant temperature after 180 DEG C, starts to pass into containing Hg0Simulated flue gas, air speed 14000h-1。Simulated flue gas consists of: 6%O2, 5%H2O, 1500ppmSO2, N2For Balance Air, Hg0Concentration is 40 μ g/m3。Thermostatic absorption reaction 4h, Hg0Removal efficiency be 86%。
Embodiment 5
Flyash is mixed homogeneously according to mass ratio 1: 1 with attapulgite, adds water and after stirring, stand 2h, 50 DEG C of dry 5h, 110 DEG C of dry 5h, in air atmosphere, 300 DEG C of calcining 3h, pulverize, sieve and obtain granular powder coal ash-Attapulgite carrier that particle diameter is 30-60 order。By this carrier incipient impregnation of 10g in the Mn (NO of 8mL0.26g/mL3)2In solution, stirring, place 8h in atmosphere, 50 DEG C of dry 8h, 110 DEG C of dry 8h, then 350 DEG C of calcining 4h in nitrogen atmosphere, in air atmosphere, 300 DEG C of calcining 2h, obtain MnO2The MnO of load capacity 10wt%2/ flyash-attapulgite catalysis/adsorbent。
Being filled in fixing bed quartz tube reactor by this catalysis/adsorbent, two ends are fixed with silica wool。The temperature programming in the reactor of catalysis/adsorbent keeps constant temperature after 200 DEG C, starts to pass into containing Hg0Simulated flue gas, air speed 5000h-1。Simulated flue gas consists of: 6%O2, 5%H2O, 1500ppmSO2, N2For Balance Air, Hg0Concentration is 40 μ g/m3。Thermostatic absorption reaction 4h, Hg0Removal efficiency be 95%。
Embodiment 6
Flyash is mixed homogeneously according to mass ratio 1: 1 with attapulgite, adds water and after stirring, stand 2h, 50 DEG C of dry 5h, 110 DEG C of dry 5h, in air atmosphere, 300 DEG C of calcining 3h, pulverize, sieve and obtain granular powder coal ash-Attapulgite carrier that particle diameter is 30-60 order。By this carrier incipient impregnation of 10g in the Mn (NO of 8mL0.26g/mL3)2In solution, stirring, place 5h in atmosphere, 50 DEG C of dry 5h, 110 DEG C of dry 5h, then 500 DEG C of calcining 3h in nitrogen atmosphere, in air atmosphere, 300 DEG C of calcining 3h, obtain MnO2The MnO of load capacity 10wt%2/ flyash-attapulgite catalysis/adsorbent。
Being filled in fixing bed quartz tube reactor by this catalysis/adsorbent, two ends are fixed with silica wool。The temperature programming in the reactor of catalysis/adsorbent keeps constant temperature after 180 DEG C, starts to pass into containing Hg0Simulated flue gas, air speed 30000h-1。Simulated flue gas consists of: 6%O2, 5%H2O, 1500ppmSO2, N2For Balance Air, Hg0Concentration is 40 μ g/m3。Thermostatic absorption reaction 4h, Hg0Removal efficiency be 82%。
Embodiment 7
Flyash is mixed homogeneously according to mass ratio 1: 1 with attapulgite, adds water and after stirring, stand 2h, 50 DEG C of dry 5h, 110 DEG C of dry 5h, in air atmosphere, 300 DEG C of calcining 3h, pulverize, sieve and obtain granular powder coal ash-Attapulgite carrier that particle diameter is 30-60 order。By this carrier incipient impregnation of 10g in the Mn (NO of 8mL0.26g/mL3)2In solution, stirring, place 10h in atmosphere, 50 DEG C of dry 5h, 110 DEG C of dry 5h, then 350 DEG C of calcining 5h in nitrogen atmosphere, in air atmosphere, 300 DEG C of calcining 3h, obtain MnO2The MnO of load capacity 10wt%2/ flyash-attapulgite catalysis/adsorbent。
Being filled in fixing bed quartz tube reactor by this catalysis/adsorbent, two ends are fixed with silica wool。The temperature programming in the reactor of catalysis/adsorbent keeps constant temperature after 180 DEG C, starts to pass into containing Hg0Simulated flue gas, air speed 5000h-1。Simulated flue gas consists of: 6%O2, 5%H2O, 1500ppmSO2, N2For Balance Air, Hg0Concentration is 201 μ g/m3。Thermostatic absorption reaction 4h, Hg0Removal efficiency be 88%。
Embodiment 8
Flyash is mixed homogeneously according to mass ratio 1: 1 with attapulgite, adds water and after stirring, stand 2h, 50 DEG C of dry 5h, 110 DEG C of dry 5h, in air atmosphere, 300 DEG C of calcining 3h, pulverize, sieve and obtain granular powder coal ash-Attapulgite carrier that particle diameter is 30-60 order。By this carrier incipient impregnation of 10g in the Mn (NO of 8mL0.26g/mL3)2In solution, stirring, place 5h in atmosphere, 50 DEG C of dry 5h, 110 DEG C of dry 5h, then 400 DEG C of calcining 4h in nitrogen atmosphere, in air atmosphere, 300 DEG C of calcining 3h, obtain MnO2The MnO of load capacity 10wt%2/ flyash-attapulgite catalysis/adsorbent。
Being filled in fixing bed quartz tube reactor by this catalysis/adsorbent, two ends are fixed with silica wool。The temperature programming in the reactor of catalysis/adsorbent keeps constant temperature after 180 DEG C, starts to pass into containing Hg0Simulated flue gas, air speed 5000h-1。Simulated flue gas consists of: 6%O2, 5%H2O, 1500ppmSO2, N2For Balance Air, Hg0Concentration is 10 μ g/m3。Thermostatic absorption reaction 4h, Hg0Removal efficiency be 96%。
Claims (3)
1. a MnO2/ flyash-attapulgite catalysis/adsorbent and for removing the method for Elemental Mercury in flue gas, it is characterised in that this catalysis/adsorbent is with flyash-attapulgite for complex carrier, MnO2For active component, its percentage by weight composition is: flyash-attapulgite complex carrier 90-99%, with MnO2For measurement unit Mn oxide 1.0-10%；By MnO2/ flyash-attapulgite catalysis/adsorbent is loaded in fixed bed reactors, controls reaction temperature at smoke evacuation warm area 120-200 DEG C, passes into normal pressure mercury fume, and wherein the concentration of hydrargyrum is 10-201 μ g/m3, air speed 5000-30000h-1。
2. MnO according to claim 12The preparation method of/flyash-attapulgite catalysis/adsorbent, it is characterized in that, by flyash-attapulgite complex carrier incipient impregnation in certain density manganese salt precursor liquid solution, stir, through room temperature stand, 50 DEG C and 110 DEG C dry, then successively in 250-600 DEG C of nitrogen and air atmosphere calcine 2-5h prepare MnO2/ flyash-attapulgite catalysis/adsorbent；Described manganese salt precursor body is Mn (NO3)2Or Mn (CH3COO)2。
3. MnO according to claim 22The preparation method of/flyash-attapulgite catalysis/adsorbent, it is characterised in that described manganese salt precursor body is Mn (NO3)2。
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| CN106237982A (en) * | 2016-10-25 | 2016-12-21 | 安庆师范大学 | CuO/ attapulgite catalyst-sorbent and for removing the method for Elemental Mercury in flue gas |
| CN106492805A (en) * | 2016-10-25 | 2017-03-15 | 安庆师范大学 | Fe2O3/ flyash attapulgite catalyst and its for removing Hg in coal gas0Method |
| CN109847689A (en) * | 2019-01-09 | 2019-06-07 | 西安热工研究院有限公司 | It is a kind of for removing the adsorbent and preparation method thereof of sulfur trioxide in flue gas, heavy metal simultaneously |
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Application publication date: 20160622 |