CN1824372A - Method of desulfurizing and denitrate simultaneously of exhaust gas by micro wave catalysis - Google Patents
Method of desulfurizing and denitrate simultaneously of exhaust gas by micro wave catalysis Download PDFInfo
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- CN1824372A CN1824372A CN 200610023550 CN200610023550A CN1824372A CN 1824372 A CN1824372 A CN 1824372A CN 200610023550 CN200610023550 CN 200610023550 CN 200610023550 A CN200610023550 A CN 200610023550A CN 1824372 A CN1824372 A CN 1824372A
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- flue gas
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Abstract
The present invention discloses a flue gas purifying method capable of catalyzing flue gas by using microwave and simultaneously making desulfurization and denitration. Said method is characterized by that firstly, the catalyst is placed in a special-designed fixed bed reactor, then the normal-pressure simulated flue gas is introduced to make microwave catalytic desulfurization and denitration reaction. Its desulfurization and denitration efficiency is high, when the space velocity is 8000h-1 and the temperature is 150deg.C, its desulfurization rate can be up to 95% and its denitration rate can be up to 87%, and its catalyst can be regenerated and reused.
Description
Technical field
The invention belongs to the industrial waste gas process field, be specifically related to a kind of method of desulfurizing and denitrate simultaneously of exhaust gas by micro wave catalysis.
Background technology
Coal is the main energy sources of China.In following considerable time, the utilization of coal in China will be based on burning.The a large amount of SO that discharge in the coal-fired process
2And NOx, ecological environments such as severe contamination atmosphere.Therefore, how to control SO in the coal-fired flue-gas cost-effectively
2And NO
xDischarging become the significant problem that presses for solution in China's strategy of sustainable development, also be the developing direction of world's pollution that caused by coal burning control technology.SO in to coal-fired flue-gas both at home and abroad
2And NO
xDeveloped a lot of technology Deng the control aspect of pollutant, as the coal washing desulfurization, in-furnace desulfurization, denitration and flue gas desulfurization and denitrification etc.
The electron beam desulphurization denitration technology that development in recent years is got up, be the electronics in the vacuum chamber to be accelerated by applying high voltage, electronics obtains 100eV～800eV energy, behind the thick titanium window of 20～40 μ m by having the vacuum seal effect, electronics also has the energy about 30eV, and the gas in its excitation normal pressure lower flue is ionized into the oxygen in the flue gas, water etc. free radicals such as hydroxyl, after adding ammonia under 65～80 ℃ of conditions, generate ammonium sulfate and ammonium salt, reclaimed with electric cleaner again.This method is successful Application on the 200MW of Chengdu steam power plant unit.The subject matter that this method exists is: need to inject NH
3, in transportation and storage process, easily leak; The denitration rate is low and only be adapted at sulphur coal area and use; Electron accelerator and vacuum system equipment are huge, a cost height; X-radiation harm need be provided with the thick radiation proof cement layer of 1～2m; Titanium target window is fragile etc.
For overcoming some shortcomings of electronic beam method desulfurization, some scholars intend adopting high voltage pulse corona (time) discharge electric field to replace electron accelerator and vacuum sealing system.But because pulsed discharge electric-field intensity only is about 20kV/cm, the average energy that electronics obtains only is 2eV, electron energy is to distribute by Maxwell's rule in the discharge electric field, can reach electronics and only account for a few percent, that is to say the SO that has only a few percent with ionization oxygen molecular energy (12.6eV)
2Become H by free-radical oxidations such as OH
2SO
4, and then and NH
3Effect generates (NH
4)
2SO
4, all the other products are gaseous state (greater than 54 ℃) (NH
4)
2SO
3, can't reclaim (the NH in the atmosphere under the hot conditions
4)
2SO
3Be decomposed into NH
3And SO
2Deng pernicious gas, can't reclaim the ammonia of injection and cause secondary pollution.
Microwave is that frequency is the high energy electromagnetic wave of 300MHz～300GHz.Heating using microwave is the body heating of from-inner-to-outer, have the homogeneous heating that is different from conventional heating, rapidly, selectivity is strong, be convenient to advantages such as control, non-secondary pollution, thereby in chemical reaction especially catalytic reaction, be widely used.
Heating using microwave catalysis flue gas desulfurization and denitrification is compared with routine heating desulphurization denitration, can effectively improve the denitration rate, reduces reaction temperature, improves reaction speed; Compare with electronic beam method, then have equipment investment few, the capacity usage ratio height, advantage such as system is stable, maintenance cost is low is in the filed of flue gas purification potentiality that grow a lot.
The artificial power consumptions of saving in the electronic beam method such as Romania scholar Marilena T.Radoiu are introduced microwave discharge in the electron beam desulphurization denitration method, and its desulfurization degree is greater than 95%, and the denitration rate can reach about 80%.But the electron gun costliness in this method; Reaction temperature is 70 ℃, and flue gas needs cooling earlier to handle, and needs heat temperature raising again during discharging; Use NH
3Reclaim SO
2And NO, NH
3Transportation and store all may to exist to reveal and cause secondary pollution.
Heating using microwave is used for smoke catalytic denitration at the existing report of Chinese patent (application number 200510027964.6), and not only denitration rate of heating using microwave can also reduce reaction temperature, improve reaction speed up to more than 90%; But how not regenerate and SO after relating to catalysqt deactivation in this patent
3, NO
2Problems such as recovery.
Summary of the invention
The object of the present invention is to provide a kind of microwave flue gas and desulfurizing and denitrifying purification method.
A kind of microwave flue gas and desulfurizing and denitrifying purification method, it is the microwave fixed bed reactors that earlier catalyst placed particular design, feed the normal pressure simulated flue gas again and carry out the microwave catalysis desulfurization and denitrification reaction, gaseous product absorbs with diluted acid can obtain certain density sulfuric acid, nitric acid mixed solution, and the beds after its absorption is saturated can be recycled behind washing, micro-wave drying; Washing lotion is concentrated through heating, crystallisation by cooling obtains manganese sulfate salt, and manganese sulfate salt reduces with reducing agent again, and resulting manganese oxide turns back to beds and reuses.
Though dust in flue gas can not influence desulphurization denitration rate of the present invention, before handling, should carry out conventional dust removal process to flue gas earlier, in order to avoid a large amount of dust sneak into and accumulate the removal effect that the catalyst that recycles is made in influence.
Catalyst activity component of the present invention can be in manganese oxide, manganese dioxide, iron oxide, the cupric oxide a kind of, two or more; Catalyst carrier can be in activated carbon, aluminium oxide, diatomite, the flyash a kind of, two or more.
Manganese dioxide is mainly derived from pyrolusite, under resources supplIes allows, former pyrolusite stone can be pulverized the offspring directly uses for manganese dioxide, experimental result shows, be present in major impurity compositions such as iron in the ore, aluminium, silicon and can desulfurization off sulfide effect do not had a negative impact, desulfurization off sulfide effect is satisfied.Iron oxide, cupric oxide also can be replaced by iron content, the copper-bearing waste material from various factories.
Catalyst immersion process for preparing, active component are MnO
2, carrier is γ-Al
2O
3
It is H that the present invention is used to reduce the reducing agent of manganese sulfate salt
2, NH
3, CH
4In a kind of.
Concrete desulphurization denitration process of the present invention is simple, under the heating using microwave flue gas is fully contacted and can finish with catalyst.According to the conventional method of gas, solid catalytic reaction, it is the most favourable to make flue gas and beds do counter current contacting.Because the inventive method time of staying is short, so except that making the two fully contacts, all do not have too much requirement in the use of catalyst and practical operation, therefore common absorption column of gas under the microwave radiation just can be finished in the packed tower as the band dividing plate.Desulfurization off sulfide effect can be according to flue gas flow rate and contained SO
2The ratio of/NO is regulated by the use amount of suitable adjusting microwave output power or catalyst.Under the normal condition, the present invention can make the desulfurization degree of flue gas be stabilized in 95～99%, and the denitration rate is stabilized in 80～90%.
Concrete operations condition of the present invention is that microwave output power is 230～400W, and reaction temperature is controlled at 80～180 ℃, and the flue gas air speed is 800～8000h
-1, SO in the flue gas
2The ratio of/NO molar concentration is 2～6, O in the flue gas
2Volume content be 4～10%, the volume content of steam is 4～6% in the flue gas, washing temperature is normal temperature～90 ℃, the spray irrigation number of times is 2～3 times.
The principle of microwave flue gas and desulfurizing and denitrifying purification method of the present invention is that high loss Wave absorbing catalyst surface produces hot localised points in microwave field, temperature is higher than the bulk temperature of catalyst and carrier, at hot localised points energy efficiently catalyzing and oxidizing sulfur dioxide and nitric oxide, reacted gas can get certain density sulfuric acid and nitric acid mixed solution after absorbing with diluted acid (molar concentration be about 10% dilute sulfuric acid or the mixed acid of rare nitric acid or sulfuric acid and nitric acid low concentration), thereby significantly improves the efficient of flue gas desulfurization and denitrification.Active component manganese dioxide and alumina catalyst support in the catalyst of the present invention are all water insoluble, and reacted small amount of solid product manganese sulfate salt is water-soluble, beds is through repeatedly washing, behind the micro-wave drying, activity is constant substantially, washing lotion through add thermal release, crystallisation by cooling obtains manganese sulfate salt, manganese sulfate salt is through H
2Deng can turning back to the beds recycling after the reducing agent reduction.
The present invention compared with prior art has following advantage:
(1) the catalyst raw material is cheap and easy to get, simple, the easily regeneration of preparation, cost performance height, easily large-scale mass production;
(2) reaction time is short, has saved reaction institute energy requirement greatly;
(3) while desulphurization denitration in same reactor is fit to the coal-fired plant flue gas exhaust temperature and uses down for 120～150 ℃, can mate with existing boiler;
(4) especially denitration rate of desulphurization denitration rate height has adaptability and Steam Generator in Load Follow preferably to the variation of exhaust gas volumn;
(5) byproduct is all recycled, aneroid, solid-state secondary pollution;
(6) small investment is applicable to that China is new, the flue gas desulfurization and denitrification of especially old power plant of old power plant.
The specific embodiment
Below by EXPERIMENTAL EXAMPLE the present invention is specifically described, it is important to point out that present embodiment only is used for that the present invention will be further described, can not be interpreted as the restriction of the present invention being protected the expansion scope, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
Granularity is the Powdered γ-Al of 200～300 purposes
2O
3In a certain amount of concentration 50% Mn (NO
3)
2Flood in the solution, mixing, under the normal temperature and pressure air-dry 4 hours, the 50MPa lower sheeting, then in 180 ℃ dry down, in air atmosphere, calcine again, being ground into granularity after the cooling is 10～40 purpose graininess MnO
2/ γ-Al
2O
3(being designated hereinafter simply as catalyst A).
Embodiment 2
A certain amount of catalyst A is placed the fixed bed reactors of particular design, and normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 385W) heating simultaneously, and wherein simulated flue gas consists of SO
2560ppm, NO 280ppm, O
2Shared volume is 10%, N
2Be balance gas, air speed is 800h
-1, SO in the time of 180 ℃
2Removal efficiency reaches 95%, and the NO removal efficiency reaches 82%.
Embodiment 3
A certain amount of catalyst A is placed the fixed bed reactors of particular design, and normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 385W) heating simultaneously, and wherein simulated flue gas consists of SO
2560ppm, NO280ppm, O
2Shared volume is 10%, N
2Be balance gas, air speed is 5600h
-1, in the time of 180 ℃, SO
2Removal efficiency reaches 98%, and the NO removal efficiency reaches 89%.
Embodiment 4
A certain amount of catalyst A is placed the fixed bed reactors of particular design, and normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 385W) heating simultaneously, and wherein simulated flue gas consists of SO
2560ppm, NO 280ppm, O
2Shared volume is 10%, N
2Be balance gas, air speed is 8000h
-1, in the time of 150 ℃, SO
2Removal efficiency reaches 95%, and the NO removal efficiency reaches 87%.
Embodiment 5
A certain amount of catalyst A is placed the fixed bed reactors of particular design, and normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 230W) heating simultaneously, and wherein simulated flue gas consists of SO
2560ppm, NO 280ppm, O
2Shared volume is 10%, N
2Be balance gas, air speed is 5600h
-1, SO in the time of 180 ℃
2Removal efficiency reaches 98%, and the NO removal efficiency reaches 91%.
Embodiment 6
A certain amount of catalyst A is placed the fixed bed reactors of particular design, and normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 385W) heating simultaneously, and wherein simulated flue gas consists of SO
2560ppm, NO 280ppm, O
2Shared volume is 6%, N
2Be balance gas, air speed is 5600h
-1, SO in the time of 180 ℃
2Removal efficiency reaches 97%, and the NO removal efficiency reaches 89%.
Embodiment 7
A certain amount of catalyst A is placed the fixed bed reactors of particular design, and normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 385W) heating simultaneously, and wherein simulated flue gas consists of SO
2540ppm, NO 180ppm, O
2Shared volume is 10%, N
2Be balance gas, air speed is 5600h
-1, SO in the time of 180 ℃
2Removal efficiency reaches 96%, and the NO removal efficiency reaches 85%.
Embodiment 8
A certain amount of catalyst A is placed the fixed bed reactors of particular design, and normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 385W) heating simultaneously, and wherein simulated flue gas consists of SO
2640ppm, NO 160ppm, O
2Shared volume is 10%, N
2Be balance gas, air speed is 5600h
-1, SO in the time of 150 ℃
2Removal efficiency reaches 100%, and the NO removal efficiency reaches 83%.
Embodiment 9
A certain amount of catalyst A is placed the fixed bed reactors of particular design, and normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 385W) heating simultaneously, and wherein simulated flue gas consists of SO
2560ppm, NO 280ppm, O
2Shared volume is 10%, and the shared volume of steam is 6%, N
2Be balance gas, air speed is 5600h
-1, SO in the time of 120 ℃
2Removal efficiency reaches 93%, and the NO removal efficiency reaches 82%.
Embodiment 10
A certain amount of catalyst A is placed the fixed bed reactors of particular design, and normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 385W) heating simultaneously, and wherein simulated flue gas consists of SO
2560ppm, NO 280ppm, O
2Shared volume is 10%, and the shared volume of steam is 4%, N
2Be balance gas, air speed is 5600h
-1, SO in the time of 120 ℃
2Removal efficiency reaches 95%, and the NO removal efficiency reaches 83%.
Embodiment 11
With the flushing of the water under the room temperature 3 times, after the precipitate and separate, the catalyst heated by microwave continues to use the manganese sulfate salt that washing lotion is concentrated through heating, crystallisation by cooling can obtain minute quantity after removing moisture behind the catalysqt deactivation.Get the fixed bed reactors that catalyst behind a certain amount of washing and drying places particular design, normal temperature and pressure feeds simulated flue gas down and carries out microwave (power output is 385W) heating simultaneously, and wherein simulated flue gas consists of SO
2560ppm, NO 280ppm, O
2Shared volume is 10%, and the shared volume of steam is 4%, N
2Be balance gas, air speed is 5600h
-1, SO in the time of 180 ℃
2Removal efficiency reaches 100%, and the NO removal efficiency reaches 82%.
Claims (9)
1. microwave flue gas and desulfurizing and denitrifying purification method, it is characterized in that: the microwave fixed bed reactors that earlier catalyst placed particular design, feed the normal pressure simulated flue gas again and carry out the microwave catalysis desulfurization and denitrification reaction, gaseous product absorbs with diluted acid can obtain certain density sulfuric acid, nitric acid mixed solution, and the beds after its absorption is saturated can be recycled behind washing, micro-wave drying; Washing lotion is concentrated through heating, crystallisation by cooling obtains manganese sulfate salt, and manganese sulfate salt reduces with reducing agent again, and resulting manganese oxide turns back to beds and reuses.
2. the method for claim 1, it is characterized in that: flue gas should carry out the microwave catalysis desulphurization denitration earlier again after dust removal process.
3. the method for claim 1, it is characterized in that: microwave output power is 230～400W, and reaction temperature is controlled at 80～180 ℃, and the flue gas air speed is 800～8000h
-1, SO in the flue gas
2The ratio of/NO molar concentration is 2～6, O in the flue gas
2Volume content be 4～10%, the volume content of steam is in the flue gas: 4～6%.
4. the method for claim 1 is characterized in that: the catalyst activity component be in manganese oxide, manganese dioxide, iron oxide, the cupric oxide a kind of, two or more; Catalyst carrier be in activated carbon, aluminium oxide, diatomite, the flyash a kind of, two or more.
5. as claim 1 and the described method of claim 4, it is characterized in that: the active component manganese dioxide in the catalyst can be replaced by the pyrolusite that is crushed to certain particle size, and iron oxide, cupric oxide can be replaced by iron content, the copper-bearing waste material from various factories.
6. the method for claim 1, it is characterized in that: reducing agent is H
2, NH
3, CH
4In a kind of.
7. as claim 1,4,5 described methods, it is characterized in that: catalyst immersion process for preparing, active component are MnO
2, carrier is γ-Al
2O
3
8. the method for claim 1 is characterized in that: the water temperature of washing is normal temperature～90 ℃, and the spray irrigation number of times is 2～3 times.
9. the method for claim 1 is characterized in that: the diluted acid that is used to absorb gaseous product is the dilute sulfuric acid of molar concentration about 10% or the mixed acid of rare nitric acid or sulfuric acid and nitric acid low concentration.
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| WO2011041956A1 (en) | 2009-10-10 | 2011-04-14 | 贵州红星发展股份有限公司 | Method for preparing manganese sulfate monohydrate by desulfurizing fume with middle-low grade manganese dioxide ore |
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| CN101972603A (en) * | 2010-10-25 | 2011-02-16 | 湘潭大学 | Method for removing nitrogen oxides from waste gas |
| CN102698680A (en) * | 2011-05-27 | 2012-10-03 | 欧阳秉利 | Large industrial microwave desulphurization denitrification terminal equipment for harmful gas environmental pollution treatment |
| WO2013097676A1 (en) * | 2011-12-30 | 2013-07-04 | 湘潭大学 | Process for removing nitrogen oxides by microwave catalysis |
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| CN102407113A (en) * | 2011-12-30 | 2012-04-11 | 湘潭大学 | Microwave catalyst and application method thereof |
| CN102489152A (en) * | 2011-12-30 | 2012-06-13 | 湘潭大学 | Denitration method by microwave catalytic reaction for direct decomposition of NO |
| CN102407072A (en) * | 2011-12-30 | 2012-04-11 | 湘潭大学 | Method for denitrating by utilizing microwave catalytic reaction |
| CN102407073A (en) * | 2011-12-30 | 2012-04-11 | 湘潭大学 | Denitration method for two-section microwave catalytic reaction bed |
| CN102489152B (en) * | 2011-12-30 | 2014-05-21 | 湘潭大学 | Denitration method by microwave catalytic reaction for direct decomposition of NO |
| CN104874288A (en) * | 2015-07-01 | 2015-09-02 | 杜小卫 | Kiln tail gas treatment method |
| CN105964130A (en) * | 2016-07-25 | 2016-09-28 | 合肥天翔环境工程有限公司 | Environment-friendly flue gas denitrifying agent and preparation method thereof |
| CN106178863A (en) * | 2016-08-16 | 2016-12-07 | 胡安平 | A kind of desulfurization denitration method of boiler smoke |
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