CN102489152B - Denitration method by microwave catalytic reaction for direct decomposition of NO - Google Patents
Denitration method by microwave catalytic reaction for direct decomposition of NO Download PDFInfo
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- CN102489152B CN102489152B CN201110451237.8A CN201110451237A CN102489152B CN 102489152 B CN102489152 B CN 102489152B CN 201110451237 A CN201110451237 A CN 201110451237A CN 102489152 B CN102489152 B CN 102489152B
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Abstract
The invention provides a denitration method by microwave catalytic reaction for direct decomposition of NO. The method comprises the steps of: installing a reaction tube filled with a catalyst in a microwave field so as to form a reaction bed, with the reaction tube made of quartz glass or other wave-transmitting materials; while an NO-containing flue gas/ exhaust gas passes the reaction bed, under a set reaction temperature and the combined action of the microwave field and the catalyst, carrying out a gas-solid catalytic reaction. The method is characterized in that: the catalyst in the reaction bed is a copper molecular sieve catalyst Cu-ZSM-5; the temperature of the catalyst bed in the reaction is 100DEG C-450DEG C, preferably 280DEG C-380 DEG C. When the treated gas passes the microwave catalyzed reaction bed, the copper molecular sieve Cu-ZSM-5 is employed as the catalyst for direct catalytic decomposition of NO in the gas into nitrogen and oxygen, thus realizing nitrogen oxide removal. The method of the invention has the advantages of high direct decomposition conversion rate, small energy consumption, energy saving and environmental protection, no reducing agent consumption, and low operating cost, etc.
Description
Technical field
The present invention relates to a kind of method that removes nitrogen oxides of exhaust gas, particularly nitric oxide production method in the direct waste gas decomposition of a kind of microwave catalysis.
Background technology
Nitrogen oxide is one of major pollutants of serious harm human health, and its 95% above composition is NO.According to estimates, within 2015, the NOx of coal-burning power plant of China discharge capacity will reach 1,310 ten thousand tons, and the discharge of controlling as seen NO is very important.Along with improving constantly of human living standard, research, the promotion and application of administering containing nitrogen oxides emissions are all paid much attention in countries in the world.
The direct breakdown method of NO is because having economy, not consuming NH
3, CO, CH
4deng reducing agent, do not produce the feature of secondary pollution, be considered to the most attractive method.The reaction that NO decomposes is
nO is directly decomposed into N
2and O
2it is feasible within the scope of thermodynamics, reaching 99%, but reaction activity is up to 364kl/mol, therefore the decomposition essence of studying NO is to inquire into its dynamic (dynamical) problem, finds a kind of suitable catalyst and a kind of efficient energy to carry out acting in conjunction and reduces the key that the activation energy reacting is the direct decomposition of NO.
If Cu-ZSM-5 molecular sieve catalyst is the active best catalyst of NO low-temperature decomposition of finding up to now, it is also current most active research object.The optimum activity temperature of Cu-ZSM-5 molecular sieve catalyst is within the scope of 450 ℃～550 ℃, and optimal conversion is in 70% left and right, and the existence of oxygen has suppressed the activity of catalyst.The Cu-ZSM-5 catalyst of modification is subject to O as Ce-Cu-ZSM-5 is less
2prevent, but its NO conversion ratio also can only remain on 75%.
Microwave energy gains universal acceptance as one is high-effect.The people such as Huang Kama have done long-time a series of research, think that microwave can change the interaction between molecule, significantly improve the speed of some chemical reaction and change the mechanism of reacting, and have " special effects ".The people such as Zhang Tao utilize microwave discharge to process NO, have obtained good effect.Tang Junwang carries out denitration research with Fe/ZSM-5 catalyst under heating using microwave pattern and conventional heating pattern, result show heating using microwave can allow originally can not catalytic decomposition reaction really occurred, and NO reaches 70% conversion ratio.
Although above-mentioned research is all a lot, but from disclosed data, it is that the optimum activity temperature of 75%, Cu-ZSM-5 molecular sieve catalyst is within the scope of 450 ℃～550 ℃ that best decomposing N O leads, optimal conversion is in 70% left and right, and the existence of oxygen has suppressed the activity of catalyst.The Cu-ZSM-5 catalyst of modification is subject to O as Ce-Cu-ZSM-5 is less
2prevent, but its NO conversion ratio also can only remain on 75%.Removal efficiency is not high, is subject in waste gas influence of oxygen content large, and the method does not reach and removes requirement.
Summary of the invention
Not high in order to solve the nitric oxide removal efficiency existing in prior art, the problem of technique more complicated, the invention provides a kind of high, the economical and practical method that removes nitrogen oxides of exhaust gas of removal efficiency simple for process, nitrogen oxide.
The object of the invention is to realize in the following way:
A kind of nitric oxide production method in microwave catalysis waste gas decomposition, comprises the steps:
(1) reaction tube of having filled catalyst is arranged on and in microwave field, forms reaction bed, described reaction tube can wave transparent, and described catalyst is copper zeolite catalyst;
(2) by passing through above-mentioned reaction bed containing nitric oxide production waste gas with certain speed, at the temperature of 100 ℃～450 ℃ of microwave catalysis reaction beds, under the acting in conjunction of microwave field and catalyst, carry out the reaction of gas-solid microwave catalysis.
Nitric oxide production method in above-mentioned microwave catalysis waste gas decomposition, wherein said copper zeolite catalyst is that Cu-ZSM-5 molecular sieve catalyst or CuO add Cu-ZSM-5 molecular sieve catalyst.
Nitric oxide production method in above-mentioned microwave catalysis waste gas decomposition, the weight ratio of wherein said Cu-ZSM-5 molecular sieve catalyst copper content is 0.1%～15%, preferably 5%～10%, molecular screen base is ZSM-5, and the silica alumina ratio in ZSM-5 molecular sieve is 30～60.
Nitric oxide production method in above-mentioned microwave catalysis waste gas decomposition, the addition that wherein said CuO adds cupric oxide in Cu-ZSM-5 molecular sieve catalyst is 10%～70% of molecular sieve catalyst weight, preferably 25%～50%; The weight ratio of Cu-ZSM-5 molecular sieve catalyst copper content is 0.1%～10%, and the silica alumina ratio in molecular screen base ZSM-5 molecular sieve is 30～60.
Nitric oxide production method in above-mentioned microwave catalysis waste gas decomposition, wherein said reaction tube is quartz ampoule.
Nitric oxide production method in above-mentioned microwave catalysis waste gas decomposition, the loading of wherein said catalyst in reaction tube is the 50%-100% of reaction tube volume.
Nitric oxide production method in above-mentioned microwave catalysis waste gas decomposition, the microwave frequency of wherein said microwave field is 500-3000MHz.
Nitric oxide production method in above-mentioned microwave catalysis waste gas decomposition, the microwave frequency of wherein said microwave field is 500-2350MHz.
Nitric oxide production method in above-mentioned microwave catalysis waste gas decomposition, the microwave frequency of wherein said microwave field is 856-965MHz.
Nitric oxide production method in above-mentioned microwave catalysis waste gas decomposition, wherein said gas space velocity is 1000～8000h
-1.
Compared with prior art, the present invention has the following advantages: the direct decomposing N O reaction of microwave catalysis does not have secondary pollution, and technique is simple, and easy to operate being easy to controlled, and efficient (NO conversion ratio reaches 99%), antioxidant is strong, energy-conservation, and operating cost is low.
The specific embodiment
Be described in further detail below in conjunction with examples of implementation:
Method of the present invention comprises the process that waste gas is processed by the beds in microwave field; Described reaction unit is that number of patent application is 201010517324.4, and the date of application is 2010.10.25, and application people is University Of Xiangtan, and publication number is " the novel microwave catalytic reactor device system " of CN 102133516 A; Described beds is microwave catalyst bed, described microwave catalyst is a class copper zeolite Catalysts Cu-ZSM-5, can be Cu-ZSM-5 or CuO-Cu-ZSM-5, utilize the acting in conjunction of microwave field and microwave catalyst to carry out the direct decomposing N O reaction of microwave catalysis.
The microwave frequency of described microwave field is 500-3000MHz, 500-2350MHz or 856-965MHz.Preferably 915MHz, 2450MHz.
Described microwave catalyst bed operating temperature is 100 ℃～450 ℃.Preferably 280 ℃～380 ℃.
The air speed of described waste gas is 1000～8000h
-1.
Described copper Cu-ZSM-5 molecular sieve catalyst can be Cu-ZSM-5 or CuO-Cu-ZSM-5; The copper content of Cu-ZSM-5 is 0.1wt%～15wt%, preferably 5%～10%; In CuO-Cu-ZSM-5, the addition of CuO is 10wt%～70wt%, preferably 25%～50%; Cu-ZSM-5 molecular sieve catalyst matrix ZSM-5 molecular sieve silica alumina ratio (mol ratio) is 30～60.
Embodiment 1:
In laboratory, adopt the specific practice of this method, that described waste gas provides for Dalian great Te gas Co., Ltd is N
2with the gaseous mixture of NO composition, wherein NO concentration is 1000ppm.
Gas analyzer is Americanized 42C NO-NO
2-NO
xanalyzer.
The power 0-1000w of microwave field is adjustable continuously, and frequency is 2400-2500MHz.Quartz tube reactor is WG1/2.45-Φ 5.4 × 54.This tests quartzy pipe range 535mm used, internal diameter 10mm.
Catalyst is filled in composition microwave catalyst bed in quartz tube reactor, and the waste gas of above-mentioned test use carries out the direct decomposing N O reaction of microwave catalysis through microwave catalyst bed.
The amount of fill of catalyst is 4g, and the mass fraction of Cu is 5%.Air inlet NO concentration is 1000ppm, and flow-control is at 160ml/min, and oxygen content is 5.88%, to the control of microwave power automatic catch, makes reaction bed temperature maintain respectively 120 ℃, 150 ℃, 180 ℃, and reaction pressure is normal pressure.Carry out the experiment that microwave catalysis removes NO, change the reaction result of different temperatures as table 1:
The reaction result of table 1. different catalysts bed temperature
In the time that reaction bed temperature is 180 ℃, the conversion ratio of NO has reached 82.4%, and in the situation of visible low temperature, microwave catalysis Cu-ZSM-5 molecular sieve catalyst decomposing N O has good effect.
Embodiment 2:
In laboratory, adopt the specific practice of this method, that described waste gas provides for Dalian great Te gas Co., Ltd is N
2with the gaseous mixture of NO composition, wherein NO concentration is 1000ppm.
Gas analyzer is Americanized 42C NO-NO
2-NO
xanalyzer.
The power 0-1000w of microwave field is adjustable continuously, and frequency is 2400-2500MHz.Quartz tube reactor is WG1/2.45-Φ 5.4 × 54.This tests quartzy pipe range 535mm used, internal diameter 10mm.
Catalyst is filled in composition microwave catalyst bed in quartz tube reactor, and the waste gas of above-mentioned test use carries out the reaction of the direct decomposing N O of microwave catalysis through microwave catalyst bed.
The catalyst of loading is 5g CuO-Cu-ZSM-5, and in Cu-ZSM-5, the mass fraction of Cu is that the mass fraction of CuO in 5%, CuO-Cu-ZSM-5 is 40%.Air inlet NO concentration is 1000ppm, and flow-control is at 160ml/min, and oxygen content is 5.88%, to the control of microwave power automatic catch, makes reaction bed temperature maintain respectively 180 ℃, 300 ℃, 380 ℃, and reaction pressure is normal pressure.Carry out the experiment that microwave catalysis removes NO, change the reaction result of different temperatures as table 2:
The reaction result of table 2. different catalysts bed temperature
In the time of 380 ℃ of reaction bed temperatures, CuO-Cu-ZSM-5 has the effect of magical decomposing N O in microwave catalysis reactor, and NO conversion ratio reaches 98.93%.
Embodiment 3:
Substantially with embodiment 2, wherein reaction temperature is set in 300 ℃, and reaction bed temperature maintains 300 ℃, changes the content of oxygen, investigates the antioxidant of this catalyst in the time of microwave catalysis decomposing N O.Result is as table 3.
The impact of table 3. oxygen content on microwave catalysis decomposing N O
Wherein, import NO content is 1000ppm, and when oxygen exists, NO is almost all converted into safe N
2, reaction bed temperature is controlled at 300 ℃, and NO conversion ratio is all more than 98%; Oxygen content is on microwave catalysis decomposing N O conversion ratio without impact, and when microwave catalysis, catalyst has good antioxidant.
Embodiment 4:
Substantially with embodiment 2, the mass fraction that changes CuO in CuO-Cu-ZSM-5 catalyst is 50%, changes microwave power, on microwave reactor, selects " manually controlling ", and it is 400w, 600w that microwave power is set, and reaction result is listed in table 4.
The impact of table 4 microwave power
Microwave power is 600 watt-hours, and NO removal efficiency reaches 88.1%, and now the equilibrium temperature of beds is 365 ℃.
Comparative example 1
In laboratory, adopt the specific practice of this method, that described waste gas provides for Dalian great Te gas Co., Ltd is N
2with the gaseous mixture of NO composition, wherein NO concentration is 1000ppm.
Gas analyzer is Americanized 42C NO-NO
2-NO
xanalyzer.
The amount of fill of Cu-ZSM-5 catalyst is 4g, and the mass fraction of Cu is 5%.Air inlet NO concentration is 1000ppm, flow-control is at 160ml/min, oxygen content is 5.88%, select conventional Electric heating to prepare the experiment of carrying out catalytic decomposition NO on MRT-6123 minisize reaction experimental provision in Beijing Xin Hangdun company, conventional heating and microwave catalysis are contrasted in the experiment of decomposing N O, and reaction result is as table 5:
Table 5Cu-ZSM-5 catalyst catalytic decomposition NO experimental result on minisize reaction experimental provision
Electric heating, optimal reaction temperature is 550 ℃, the highest NO conversion ratio is 53.6%.Removal efficiency can not reach the requirement of practical application.Even if reaction temperature is during up to 550 ℃, NO conversion ratio also only has 53.6%, and the direct decomposing N O of microwave catalysis Cu-ZSM-5 catalyst is in the time that reaction bed temperature is 180 ℃, and NO conversion ratio just can reach 82.4% (referring to table 1).
Comparative example 2:
The disclosed data of background technology, it is 75% that its best decomposing N O leads.
The optimum activity temperature of Cu-ZSM-5 molecular sieve catalyst is within the scope of 450 ℃～550 ℃, and optimal conversion is in 70% left and right, and the existence of oxygen has suppressed the activity of catalyst.The Cu-ZSM-5 catalyst of modification is subject to O as Ce-Cu-ZSM-5 is less
2prevent, but its NO conversion ratio also can only reach 75% in the time of 550 ℃ of higher reaction temperatures.
From 2 comparative examples above, the removal efficiency of method of the present invention can reach 98.93%.Removal efficiency than existing technology is high.Thereby use method of the present invention can be efficiently directly catalytic decomposition NO remove the nitrogen oxide of waste gas/flue gas.
Claims (4)
1. a nitric oxide production method in microwave catalysis waste gas decomposition, is characterized in that, comprises the steps:
(1) reaction tube of having filled catalyst is arranged on and in microwave field, forms reaction bed, described reaction tube can wave transparent, and described catalyst is that CuO adds Cu-ZSM-5 molecular sieve catalyst;
(2) by passing through above-mentioned reaction bed containing nitric oxide production waste gas with certain speed, at the temperature of 100 ℃～450 ℃ of microwave catalysis reaction beds, under the acting in conjunction of microwave occasion catalyst, carry out the reaction of gas-solid microwave catalysis;
The addition that described CuO adds cupric oxide in Cu-ZSM-5 molecular sieve catalyst is 10%～70% of molecular sieve catalyst weight; In Cu-ZSM-5 molecular sieve catalyst, the weight ratio of the addition of copper is 0.1%～10%, and the silica alumina ratio in molecular screen base ZSM-5 molecular sieve is 30～60;
The microwave frequency of described microwave field is 856-965MHz.
2. nitric oxide production method in microwave catalysis waste gas decomposition as claimed in claim 1, is characterized in that, described reaction tube is quartz ampoule.
3. the nitric oxide production method in microwave catalysis waste gas decomposition as claimed in claim 1, is characterized in that, the loading of described catalyst in reaction tube is 50%～100% of reaction tube volume.
4. the nitric oxide production method in microwave catalysis waste gas decomposition as claimed in claim 1, is characterized in that 1000～8000h of described gas space velocity
-1.
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| CN201110451237.8A CN102489152B (en) | 2011-12-30 | 2011-12-30 | Denitration method by microwave catalytic reaction for direct decomposition of NO |
| PCT/CN2012/087342 WO2013097676A1 (en) | 2011-12-30 | 2012-12-24 | Process for removing nitrogen oxides by microwave catalysis |
| US14/318,740 US9199196B2 (en) | 2011-12-30 | 2014-06-30 | Process for removing nitrogen oxides from gas using microwave catalytic reaction by microwave catalysis |
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| WO2013097676A1 (en) * | 2011-12-30 | 2013-07-04 | 湘潭大学 | Process for removing nitrogen oxides by microwave catalysis |
| CN102764586A (en) * | 2012-07-26 | 2012-11-07 | 复旦大学 | Application of CuZSM-11 catalyst in efficient decomposition of N2O |
| CN102974387A (en) * | 2012-12-11 | 2013-03-20 | 北京石油化工学院 | Catalyst for simultaneously carrying out desulfurization and denitrification on smoke, preparation method and application of catalyst |
| CN104437079A (en) * | 2014-12-05 | 2015-03-25 | 湘潭大学 | Method for denitration by catalytic direct decomposition of NO with perovskite type catalyst |
| CN104524934B (en) * | 2014-12-29 | 2017-06-16 | 湘潭大学 | A kind of method of microwave catalysis decomposing hydrogen sulfide hydrogen and sulphur |
| CN106345292A (en) * | 2016-10-10 | 2017-01-25 | 湘潭大学 | Method for directly decomposing NO by microwave catalysis and catalyst |
| CN109647156B (en) * | 2018-12-28 | 2021-01-26 | 武汉理工大学 | Microwave high-temperature selective non-catalytic denitration device |
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| JPH05212248A (en) * | 1991-08-26 | 1993-08-24 | Osaka Gas Co Ltd | Method for purifying nox in waste combustion gas of natural gas |
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