CN104437080A - Denitration method for microwave catalytic decomposition of NO and method of preparing Cu-ZSM-11 - Google Patents
Denitration method for microwave catalytic decomposition of NO and method of preparing Cu-ZSM-11 Download PDFInfo
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Abstract
The invention provides a denitration method for microwave catalytic decomposition of NO; the method comprises the step: metal oxide/CU-ZSM-11 catalyst is filled in a reaction tube of a microwave catalytic reactor to form a microwave catalytic reaction bed; when passing through the microwave catalytic reaction bed, to-be-processed waste gas are reacted in a gas-solid catalytic reaction under the common actions of the microwaves and the catalyst; and NO is directly catalytically decomposed to N2 and O2; the metal oxide is Ni2O3 or MnO-2. Preferably, the catalyst is Ni2O3 / Cu-ZSM-11. The invention further provides a method of preparing the Cu-ZSM-11; the method comprises a pre-treatment step and an ion exchange step under microwave irradiation. According to the method of preparing the Cu-ZSM-11, copper-based molecular sieve catalyst containing higher content of copper can be prepared by exchanging ions within a short time, and the prepared catalyst has good catalytic activity of directly catalytically decomposing NO.
Description
Technical field
The present invention relates to microwave catalysis and microwave catalyst field, be specifically related to the method for a kind of microwave catalysis decomposing N O denitration and the preparation method of a kind of Cu-ZSM-11.
Background technology
Along with the fast development of modern industry, nitrogen oxide (NO
x) discharge capacity increase year by year, if China is not controlled, estimate that the discharge capacity of the year two thousand twenty nitrogen oxide reaches 30,000,000 tons.The nitrogen oxide of high concentration can cause very large harm to atmospheric environment and health, and NO_x Reduction by Effective has become the important topic in environmental protection.New " thermal power plant's atmosphere pollution discharging standards " specifies NO
xconcentration of emission be less than 100mg/m
3(123ppm), far super US and European, becomes the tightest standard." New emission standard " performs as strict as possible and faces immense pressure and difficulty.Therefore study new efficient removal NO technology, there is realistic meaning.
At present, out of stock main method has two large classes: wet method is out of stock and dry method is out of stock.The out of stock main employing liquid absorption of wet method, NO
xremoval efficiency only have 70%, and there is the problems such as energy consumption is large, so there is no industrialization.It is SCR (SCR) that Dry denitration is applied to industrialized, with ammonia as reducing agent and NO
xreaction generates NH
3and water, be denitration technology the most ripe at present, but it is easily poisoning to there is catalyst, consumption NH
3amount is large, the defects such as reactor is corroded, catalyst operating temperature narrow range (623K-673K).The most promising in current Dry denitration, the most attracting a kind of denitration mode is direct catalytic decomposition.Direct catalytic decomposition NO does not need reducing agent, and product is N
2and O
2, environmentally safe.NO Direct Resolution is N
2and O
2be possible (during 298K, △ G=-86KJ/mol) from thermodynamics, but be then difficult to carry out this reaction (Ea=364KJ/mol) at low temperatures from dynamics.This just needs to find a kind of catalyst makes this reaction carry out at a lower temperature.Cu-ZSM-5 catalyst is the best catalyst of current low-temperature catalyzed decomposing N O, is also now active research object.Iwamoto etc. find when reaction temperature 550 DEG C, and the conversion ratio of NO reaches 55% ~ 60%.Zhou Jicheng (CN:201110451237.8) etc. quotes Microwave New Techniques, utilizes microwave irradiation Catalysts Cu O-Cu-ZSM-5 catalysis Direct Resolution NO to be N
2and O
2efficiency especially up to 99%.But, in the method Cu-ZSM-5 preparation need at PH=7, stir and water-bath 50 DEG C at ion-exchange 10h and exchange twice, the preparation process of this catalyst is consuming time very long.
Therefore, this area also needs to develop new catalyst for catalyzing N O denitration, or also needs the preparation method developing new microwave catalyst to solve the problem.
Summary of the invention
Therefore, first the present invention provides a kind of new microwave catalyst for catalyzing N O denitration, and described catalyst is Ni
2o
3/ Cu-ZSM-11 or MnO
2/ Cu-ZSM-11; The present invention also provides a kind of method preparing described Cu-ZSM-11 molecular sieve catalyst.
The invention provides the method for a kind of microwave catalysis decomposing N O denitration, be included in the reaction tube of microwave catalysis reactor and fill metal oxide/Cu-ZSM-11 catalyst formation microwave catalysis reaction bed, pending waste gas by microwave catalysis reaction bed time, issue raw gas-solid catalytic reaction in the acting in conjunction of microwave and described catalyst, the direct catalytic decomposition of NO wherein becomes N
2and O
2; Described metal oxide is Ni
2o
3or MnO
2.Described catalyst is more preferably Ni
2o
3/ Cu-ZSM-11.
In a kind of concrete embodiment, in described catalyst, the mass ratio of metal oxide and Cu-ZSM-11 is 0.5 ~ 2:1.Particularly, in the present invention, catalytic reaction temperature is 100 ~ 450 DEG C, preferably 150 ~ 350 DEG C, more preferably 200 ~ 300 DEG C.
In a kind of concrete embodiment, the content of the copper in Cu-ZSM-11 of the present invention is 1 ~ 15wt%, is preferably 2 ~ 8wt%.
In the embodiment that another kind is concrete, Cu-ZSM-11 described in catalysis process of the present invention is through that following method prepares: first by Na-ZSM-11 molecular sieve at NaNO
3supersound washing in solution, then obtain pretreated Na-ZSM-11 molecular sieve through Separation of Solid and Liquid, washing, drying and roasting; Again described pretreated Na-ZSM-11 molecular sieve is stirred and evenly mixed at Cu (NO
3)
2in solution, and react under this solution is inserted microwave field, then obtain described Cu-ZSM-11 molecular sieve after Separation of Solid and Liquid, drying and roasting.
In the reaction that catalyzing N O of the present invention decomposes, the Cu-ZSM-11 used can be the Cu-ZSM-11 using the method in the present invention to prepare, also can be use the Cu-ZSM-11 that in prior art, other method (as by the method in patent application CN103127950A) prepares, commercially available Cu-ZSM-11 can also be used.
The present invention is the corresponding preparation method providing a kind of Cu-ZSM-11 molecular sieve also, comprises ion-exchange step under pre-treatment step and microwave irradiation, pretreatment: Na-ZSM-11 molecular sieve is at NaNO
3supersound washing in solution, then obtain pretreated Na-ZSM-11 molecular sieve through Separation of Solid and Liquid, washing, drying and roasting; Ion-exchange under microwave irradiation: above-mentioned pretreated Na-ZSM-11 molecular sieve stirs and evenly mixs at Cu (NO
3)
2in solution, react under this solution is inserted microwave field, then obtain described Cu-ZSM-11 molecular sieve after Separation of Solid and Liquid, drying and roasting.
In a kind of concrete embodiment, the microwave treatment time under described microwave irradiation in ion-exchange step is 1min ~ 3h, preferred 2min ~ 2h.Described Cu (NO
3)
2in solution, the concentration of copper nitrate is 0.005 ~ 1mol/L, preferably 0.01 ~ 0.2mol/L.Under microwave irradiation, the power of microwave described in ion-exchange step is 500 ~ 800W, preferably 200 ~ 400W.In the present invention, described Na-ZSM-11 molecular sieve and Cu (NO
3)
2the solid-to-liquid ratio of solution is such as 10 ~ 20g/L.
In a kind of concrete embodiment, the exchange times of ion-exchange under described microwave irradiation is 1 ~ 3 time, preferably 2 times.
The wash temperature of supersound washing in pre-treatment step of the present invention is room temperature, and the time of supersound washing is such as 1h.
Copper based molecular sieve Cu-ZSM-11 prepared by the present invention and metal oxide Ni
2o
3or MnO
2the performance of catalyst direct catalytic decomposition NO in microwave field of common formation is good.Cu-ZSM-11 preparation method of the present invention is compared with traditional ion-exchange, and in the present invention, swap time shortens greatly.
That is, preparation method provided by the invention not only can prepare containing the higher copper based molecular sieve catalyst of Cu amount in short time ion-exchange, and obtained catalyst has the catalytic activity of well directly catalytic decomposition NO.
Detailed description of the invention
Following examples are for illustration of the present invention, but protection scope of the present invention is not limited to the scope disclosed in embodiment.
Major experimental instrument and raw material in following examples: microwave catalysis reactor is the HAMILab-T1 type that ChangSha SYNO-THERM Co., Ltd. produces, and NOx analyzer is the Model 42i-HL type of Thermo Scientific.Testing NO used for Dalian great Te gas Co., Ltd provides, and oxygen provides for Xiangtan City special gas Co., Ltd.Other unlisted laboratory apparatus and raw material are commercially available laboratory apparatus and raw material.
Described waste gas for investigating NO rates of decomposing and transforming in waste gas is N in the lab
2with the gaseous mixture of NO composition, wherein NO concentration is 1000ppm, and also optionally containing certain density oxygen in described waste gas.The microwave power of microwave reactor is at 0-1000w continuously adjustabe, and frequency is 2400-2500MHz.Quartz tube reactor is WG1/2.45-Φ 5.4 × 54.This tests wave transparent type quartz pipe range 540mm used, internal diameter 10mm.Packed catalyst forms beds in quartz tube reactor, and the waste gas of above-mentioned test carries out the reaction of microwave catalysis Direct Resolution NO through beds.
Embodiment 1
Get the NaNO of 10g Na-ZSM-11 500ml 0.01mol/L
3solution washs one hour in ultrasonic cleaner, filters, with milli-Q water four times, then with ethanol wash once, at 80 DEG C of drying box inner drying 6h, then roasting 5h at 600 DEG C in Muffle furnace.Under the Na-ZSM-11 getting above-mentioned process re-uses microwave irradiation, ion-exchange prepares Cu-ZSM-11.Particularly, the Na-ZSM-11 getting 4.5g process adds the Cu (NO of 0.01mol/L
3)
2in solution, mix, solution is placed in Microwave synthesize instrument.Then stir respectively under microwave power P=200W irradiation and exchange 2min, 4min, 6min, 10min, 30min, 60min and 120min.To be cooled, filter, dry, roasting prepares Cu-ZSM-11.As shown in table 1 by the content results of Cu in atomic absorption instrument test Cu-ZSM-11.
Table 1
| Swap time (min) | 2 | 4 | 6 | 10 | 30 | 60 | 120 |
| Cu content (wt%) | 2.9182 | 3.2105 | 3.4767 | 3.6352 | 3.688 | 3.7762 | 4.02 |
From table 1, under same copper nitrate solution concentration and microwave power, along with the increase of ion-exchange time under microwave, the content of Cu progressively rises.In 2min ~ 120min, the content of Cu rises to about 4wt% from about 3wt%.The data result of table 1 illustrates that ion-exchange time is on the content impact of Cu obviously under microwave within the specific limits.
Embodiment 2
Get the NaNO of 10g Na-ZSM-11 500ml 0.01mol/L
3solution washs one hour in ultrasonic cleaner, filters, with milli-Q water four times, then with ethanol wash once, at 80 DEG C of drying box inner drying 6h, then roasting 5h at 600 DEG C in Muffle furnace.Under the Na-ZSM-11 getting above-mentioned process re-uses microwave irradiation, ion-exchange prepares Cu-ZSM-11.Particularly, the Na-ZSM-11 getting the above-mentioned process of 4.5g adds Cu (NO
3)
2in solution, mix, solution is placed in Microwave synthesize instrument.Cu (NO
3)
2the concentration of solution is respectively 0.005mol/L, 0.01mol/L, 0.015mol/L, 0.05mol/L, 0.1mol/L.Then stir under the mixed solution configured being placed in microwave P=200W power and exchange 2min, to be cooled, filter, dry, roasting prepares Cu-ZSM-11.Cu ion concentration result in Cu-ZSM-11 is surveyed as shown in table 2 with atomic absorption instrument.
Table 2
| Exchange liquid concentration (mol/L) | 0.005 | 0.01 | 0.015 | 0.05 | 0.1 |
| Cu content (wt%) | 2.5182 | 2.9182 | 3.1094 | 3.6137 | 3.7536 |
From table 2, under same microwave irradiation under ion-exchange time and microwave power, along with the increase of copper nitrate solution concentration, the content of Cu progressively rises.Data in table 2 illustrate that copper nitrate solution concentration within the specific limits on the content impact of Cu obviously.
Embodiment 3
Get the NaNO of 10g Na-ZSM-11 500ml 0.01mol/L
3solution washs one hour in ultrasonic cleaner, filters, with milli-Q water four times, then with ethanol wash once, at 80 DEG C of drying box inner drying 6h, then roasting 5h at 600 DEG C in Muffle furnace.Under the Na-ZSM-11 getting above-mentioned process re-uses microwave irradiation, ion-exchange prepares Cu-ZSM-11.Particularly, the Na-ZSM-11 getting the above-mentioned process of 4.5g adds the Cu (NO of 0.01mol/L
3)
2in solution, mix, solution is placed in Microwave synthesize instrument.Then stir under microwave power is 0W, 200W, 400W, 600W, 800W irradiation respectively and exchange 2min.To be cooled, filter, dry, roasting prepares Cu-ZSM-11.As shown in table 3 by the content results of Cu in atomic absorption instrument test Cu-ZSM-11.
Table 3
| Microwave action power (W) | 0 | 200 | 400 | 600 | 800 |
| Cu content (wt%) | 0.4472 | 2.9182 | 3.0283 | 3.0824 | 3.1375 |
From table 3, under same microwave irradiation under ion-exchange time and copper nitrate solution concentration, along with the increase of microwave power, the content of Cu progressively rises.But the data in table 3 illustrate that the content impact of microwave power within the specific limits on Cu is very micro-.When this also illustrates that ion-exchange prepares Cu-ZSM-11 under use microwave irradiation of the present invention, namely microwave power used can provide enough microwave heat energy at about 200W.
Embodiment 4
Get the NaNO of 10g Na-ZSM-11 500ml 0.01mol/L
3solution washs one hour in ultrasonic cleaner, filters, with milli-Q water four times, then with ethanol wash once, at 80 DEG C of drying box inner drying 6h, then roasting 5h at 600 DEG C in Muffle furnace.Under the Na-ZSM-11 getting above-mentioned process re-uses microwave irradiation, ion-exchange prepares Cu-ZSM-11.Particularly, the Na-ZSM-11 getting the above-mentioned process of 4.5g adds the Cu (NO of 0.01mol/L
3)
2in solution, mix, solution is placed in Microwave synthesize instrument.Then under microwave power P=200W irradiation, exchange 2min, to be cooled, filter, dry, roasting prepares Cu-ZSM-11.Make to use the same method (with same copper nitrate solution and same microwave irradiation power and time) exchange once, twice and three times respectively.Cu content results is recorded as shown in table 4 with atomic absorption instrument.
Table 4
| Exchange times | 1 | 2 | 3 |
| Cu content (wt%) | 2.9182 | 5.4514 | 5.401 |
From table 4, generally, the exchange times using ion-exchange under microwave irradiation to prepare Cu-ZSM-11 is good with about 2 times.Exchange times changes 2 times into by 1 time affects highly significant to the content of copper, but has little significance to the content of copper when exchange times is too much and even have the content that can make copper on the contrary to reduce.
Embodiment 5
Get the NaNO of 10g Na-ZSM-11 500ml 0.01mol/L
3solution washs one hour in ultrasonic cleaner, filters, with milli-Q water four times, then with ethanol wash once, at 80 DEG C of drying box inner drying 6h, then roasting 5h at 600 DEG C in Muffle furnace.The Na-ZSM-11 getting the above-mentioned process of 4.5g adds the Cu (NO of 0.01mol/L
3)
2in solution, mix, solution is placed in Microwave synthesize instrument.Then stir under microwave power P=200W irradiation and exchange 120min, to be cooled, filter, dry, roasting prepares Cu-ZSM-11, and in gained Cu-ZSM-11, the content of Cu is 4.02wt%.Make to use the same method after exchange twice and prepare Cu-ZSM-11 used in following denitration reaction, wherein the content of Cu is 7.85wt%.
Cu-ZSM-11 and Ni prepared by said method is got Deng mass ratio
2o
3mechanical mixture is even, and pressure forming, sieves and obtain Ni
2o
3/ Cu-ZSM-11 catalyst, its particle is 40-60 order.
Get 2g Ni
2o
3/ Cu-ZSM-11 catalyst is inserted in microwave catalysis reaction unit for direct catalytic decomposition NO.NO concentration initial concentration is 1000ppm, is designated as C
0(NO).NO and N
2the volume flow of (wherein NO concentration is 1000ppm) is 114ml/min, and in waste gas, oxygen volume flow is 6ml/min.Catalytic reaction temperature being set to 200 DEG C respectively, 250 DEG C, 300 DEG C, 350 DEG C, 400 DEG C by controlling microwave power, using and surveying blood urea/nitrogen analyzer (NOx analyzer) analytical reactions product, measuring reacted NO
xconcentration, is designated as C1 (NO
x), then NO resolution ratio computing formula is:
Under obtaining different catalytic reaction temperature, NO Direct Resolution conversion results is as shown in table 5.
Table 5
| Reaction bed temperature | 200℃ | 250℃ | 300℃ | 350℃ | 400℃ |
| NO conversion ratio (%) | 89.83％ | 93.87％ | 95.84％ | 99.27％ | 80％ |
From table 5, use Ni
2o
3during/Cu-ZSM-11 catalyst microwave catalysis NO Direct Resolution, the conversion ratio impact of reaction temperature on NO is remarkable, and reaction temperature is good with 250 ~ 350 DEG C.When reaction temperature is 350 DEG C, the rates of decomposing and transforming of the NO in the present embodiment is more than 99%.
Embodiment 6
Identical with case study on implementation 5, just change the intake of oxygen in waste gas.Such as, when oxygen concentration is 0%, do not pass into oxygen; When oxygen content is 8vol%, NO and oxygen intake are respectively 110.4ml/min, 9.6ml/min.The NO conversion results of catalyzing N O Direct Resolution reaction gained is as shown in table 6.
Table 6
From table 6, use Ni
2o
3during/Cu-ZSM-11 catalyst microwave catalysis NO Direct Resolution, the conversion ratio impact of the oxygen content in raw material waste gas on NO is little.It can thus be appreciated that, the Ni used in the present invention
2o
3/ Cu-ZSM-11 catalyst is high to the oxygen tolerance level in pending waste gas.
Embodiment 7
Identical with case study on implementation 5, just by metal oxide Ni
2o
3change MnO into
2.Gained catalyst MnO
2the NO conversion results that/Cu-ZSM-11 is used for catalyzing N O Direct Resolution reaction gained is as shown in table 7.
Table 7
| Reaction bed temperature | 150℃ | 200℃ | 250℃ | 300℃ | 350℃ | 400℃ |
| NO conversion ratio (%) | 81.72％ | 90.93％ | 86.24％ | 80.17％ | 74.70％ | 70.09％ |
From table 7, use MnO
2during/Cu-ZSM-11 catalyst microwave catalysis NO Direct Resolution, the conversion ratio impact of reaction temperature on NO is remarkable, and reaction temperature is good with 150 ~ 300 DEG C.In addition, from the contrast of data result in table 5 and table 7, Ni
2o
3/ Cu-ZSM-11 molecular sieve catalyst compares MnO
2/ Cu-ZSM-11 molecular sieve catalyst is more suitable for the catalyst for the direct catalytic decomposition of NO.
Claims (10)
1. the method for microwave catalysis decomposing N O denitration, be included in the reaction tube of microwave catalysis reactor and fill metal oxide/Cu-ZSM-11 catalyst formation microwave catalysis reaction bed, pending waste gas by microwave catalysis reaction bed time, issue raw gas-solid catalytic reaction in the acting in conjunction of microwave and described catalyst, the direct catalytic decomposition of NO wherein becomes N2 and O
2; Described metal oxide is Ni
2o
3or MnO
2.
2. method according to claim 1, is characterized in that, the mass ratio of metal oxide and Cu-ZSM-11 is 0.5 ~ 2:1 in the catalyst.
3. method according to claim 1, is characterized in that, catalytic reaction temperature is 100 ~ 450 DEG C, preferably 150 ~ 350 DEG C, more preferably 200 ~ 300 DEG C.
4. method according to claim 1, is characterized in that, the content of the copper in described Cu-ZSM-11 is 1 ~ 15wt%, is preferably 2 ~ 8wt%.
5. according to the preparation method in Claims 1 to 4 described in any one, it is characterized in that, described Cu-ZSM-11 is through that following method prepares: first by Na-ZSM-11 molecular sieve at NaNO
3supersound washing in solution, then obtain pretreated Na-ZSM-11 molecular sieve through Separation of Solid and Liquid, washing, drying and roasting; Again described pretreated Na-ZSM-11 molecular sieve is stirred and evenly mixed at Cu (NO
3)
2in solution, and react under this solution is inserted microwave field, then obtain described Cu-ZSM-11 molecular sieve after Separation of Solid and Liquid, drying and roasting.
6. a preparation method for Cu-ZSM-11 molecular sieve, comprises ion-exchange step under pre-treatment step and microwave irradiation,
Pretreatment: Na-ZSM-11 molecular sieve is at NaNO
3supersound washing in solution, then obtain pretreated Na-ZSM-11 molecular sieve through Separation of Solid and Liquid, washing, drying and roasting;
Ion-exchange under microwave irradiation: above-mentioned pretreated Na-ZSM-11 molecular sieve stirs and evenly mixs at Cu (NO
3)
2in solution, react under this solution is inserted microwave field, obtained described Cu-ZSM-11 molecular sieve after Separation of Solid and Liquid, drying and roasting.
7. method according to claim 6, is characterized in that, the microwave treatment time under described microwave irradiation in ion-exchange step is 1min ~ 3h, preferred 2min ~ 2h.
8. method according to claim 6, is characterized in that, described Cu (NO
3)
2in solution, the concentration of copper nitrate is 0.005 ~ 1mol/L, preferably 0.01 ~ 0.2mol/L.
9. according to the method in claim 6 ~ 8 described in any one, it is characterized in that, the power of described microwave is 500 ~ 800W, preferably 200 ~ 400W.
10. according to the method in claim 6 ~ 8 described in any one, it is characterized in that, the exchange times of ion-exchange under described microwave irradiation is 1 ~ 3 time, preferably 2 times.
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| CN111921555A (en) * | 2020-08-06 | 2020-11-13 | 大连海事大学 | Catalyst for NO decomposition and denitration and preparation method and application thereof |
| CN111921556A (en) * | 2020-08-06 | 2020-11-13 | 大连海事大学 | Composite molecular sieve catalyst for NO decomposition and denitration, and preparation method and application thereof |
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| CN111921556A (en) * | 2020-08-06 | 2020-11-13 | 大连海事大学 | Composite molecular sieve catalyst for NO decomposition and denitration, and preparation method and application thereof |
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