CN107899568A - A kind of preparation method for loading O composite metallic oxide catalyst and its application in exhaust-gas treatment field - Google Patents
A kind of preparation method for loading O composite metallic oxide catalyst and its application in exhaust-gas treatment field Download PDFInfo
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- 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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- 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
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Abstract
A kind of preparation method for loading O composite metallic oxide catalyst and its application in exhaust-gas treatment field, belong to industrial waste gas processing technology field.The carrier of activated processing carries out ultrasound after incipient impregnation, drying in manganese, cobalt, cerium, iron, copper, nickel composite metal nitrate dipping solution, then by roasting, that is, obtains metal oxide-loaded catalyst.This preparation method is environmentally protective, easy to operate, is easy to industrialize.The catalyst prepared using the present invention, changes into NO by the NO in flue gas at low temperaturex, 500ppmNO, O3Molar ratio with NO is 0.6, and flue gas relative humidity is 10%, and reaction temperature is at 100 DEG C, with MnO after reaction 90mimx‐CeOx‑Al2O3As catalyst, NO conversion ratios are able to maintain that 40% or so, with MnOx‑Al2O3As catalyst, highest removal rate can have preferable O3 catalytic oxidation effect up to 80%.
Description
Technical field
The invention belongs to industrial waste gas processing technology field, is related specifically to a kind of load O composite metallic oxide catalyst
Preparation method and its application in exhaust-gas treatment field.
Background technology
The fixed nitrogen contained in mineral is oxidized to NO by fossil fuel in combustionx, after discharge to health with
And ecological environment can all cause greatly to endanger, including influence human respiratory and cardiovascular system, form acid rain and acid mist
And destroy ozone layer, additionally it is possible to form PM2.5 with other pollutant reactions in air.NOxIn have 90% above is with indissoluble
Exist in the NO forms of water, therefore handle the NO in flue gas to become the emphasis of denitrating flue gas.
At present, the most ripe technology of denitrating flue gas is high temperature ammonia process selective catalytic reduction (NH3- SCR), there is conversion ratio
The advantages that high, stable.But in order to reach the optimum activity temperature of catalyst, it is necessary to be heated to flue gas, add
Energy consumption.It is also possible to ammonia leakage occurs, secondary pollution is produced.
In addition, selective non-catalytic reduction (SNCR) is also at present using one of more technology.Its with small investment, account for
The advantages that ground area is small, easy to use.But this method high energy consumption, be also easy to produce secondary pollution, and removal efficiency is relatively low.
In recent years, NO oxidative absorptions Treatment process attracts wide attention, and NO is oxidized to the NO of more expensive statexAfter carry out
Liquid phase scrubbing.Ozone is extremely strong as a kind of oxidisability and the oxidant of secondary pollution will not be produced in oxidizing process, becomes
The hot spot of research.It has been reported that under room temperature, when the molar ratio of ozone and NO reaches 1, the conversion ratio of NO can reach 90~
95%, but the report at present on low-temperature catalyzed ozone oxidation NO is seldom.
The content of the invention
The purpose of the present invention is slightly solubility gas NO in processing flue gas, using the technical advantage of low-temperature catalyzed ozone oxidation,
A kind of Engineering of Supported Metal Oxide Catalysts at low temperature with good catalytic activity is made, by the NO catalysis ozones in flue gas
It is oxidized to ease of solubility gas NOx。
Technical scheme：
A kind of preparation method for loading O composite metallic oxide catalyst, at low temperature, the NO in flue gas is oxidized to
NOx, reaction principle may include following two aspects：
(1) and ozone reaction
NO+O3→NO2+O2
NO2+O3→NO3+O2
NO+NO2→N2O3
NO2+NO2→N2O4
NO2+NO3→N2O5
(2) and radical reaction
O3+M-OH→·OH+M-O3
NO+·OH→NO2+H·
NO2+·OH→HNO3
NO3+2·OH→HNO3+·HO2
N2O5+2·OH→HNO3+·HO2
Catalyst preparation step is as follows：
1. choose the γ-Al of a diameter of 1~2mm2O3Bead cleans 1~3 time, Ran Houyong as carrier with deionized water
The dilute hydrochloric acid soaked overnight of 0.10~0.25mol/L, finally with being dried after deionized water rinsing to water outlet neutrality, that is, obtain by
Catalyst carrier after activation process；
2. manganese, cobalt, cerium, iron, copper, the nitrate solution of nickel are prepared, under normal temperature condition, respectively to the load after activation process
Body carries out incipient impregnation, ultrasonic 2h, drying, then by 500 DEG C of roasting 4h, obtains the single component metal that load capacity is 1wt%
Oxide carried type catalyst；It is manganese nitrate to filter out best metal nitrate；
3. 2. manganese nitrate that step is filtered out is formulated as the solution of various concentrations, at normal temperatures, after activation process
Carrier carries out incipient impregnation, ultrasonic 2h, drying, then by 500 DEG C of roasting 4h, obtains the single group that load capacity is 0.5-4wt%
Part metal oxide catalyst；The optimum load amount for filtering out manganese is 3wt%；
4. 3. load capacity that step is filtered out is to mix cobalt, cerium, iron, copper, nickel in the manganese nitrate solution of 3wt% respectively
Nitrate is configured to composite metal salt maceration extract, at normal temperatures, the carrier after activation process is carried out incipient impregnation, ultrasound
2h, drying, then by 500 DEG C of roasting 4h, it is 1 to obtain load molar ratio:0.6 different two-component loaded catalysts；Screening
It is cerous nitrate to go out optimum doping metal nitrate；
5. 4. manganese nitrate and cerous nitrate that step is filtered out are configured to the composite metal salt maceration extract of various concentrations ratio,
At normal temperatures, incipient impregnation, ultrasonic 2h, drying are carried out to the carrier after activation process, then by 500 DEG C of roasting 4h, is obtained
Manganese cerium load capacity molar ratio is 1:0.2~1 two-component metal oxide catalyst；Filtering out optimal manganese cerium load molar ratio is
1：0.4；
6. the composition metal nitrate solution at normal temperatures, 5. step filtered out carries out the carrier after activation process etc.
Volume impregnation, ultrasonic 2h, drying, then roast 4h at 400~600 DEG C；The optimum calcinating temperature filtered out is 500 DEG C.
Catalyst screening application comprises the following steps that：
The catalyst of load metal oxide prepared by 10g is fitted into reaction unit, is passed through simulated flue gas, flue gas
Total flow is 1.0L/min, and keeps having certain relative humidity in flue gas.Simulated flue gas enters reaction by preheating apparatus
In device, reacted with the ozone being passed through, residue NO concentration in flue gas is detected by NOx meter.
As shown in Figure 1, NO concentration is 100~1000ppm, the O being passed through to the reaction unit in simulated flue gas3With NO
Molar ratio be 0.2~3.5, flue gas relative humidity be 2%~12%, reaction temperature be 20~120 DEG C, specific reaction condition regards
Depending on the composition of simulated flue gas.
Beneficial effects of the present invention：
(1) preparation method of metal oxide supported type catalyst proposed by the present invention is simple and practicable, environmentally protective
(2) the metal oxide supported type catalyst prepared using the present invention, can change into NO by NO at low temperaturex,
Avoid the energy consumption brought to flue gas heating.
(3) can be to avoid generation secondary pollution, process clean environment firendly using this ozone oxidation catalysis process.
Brief description of the drawings
Fig. 1 is low-temperature catalyzed ozone oxidation reaction installation drawing.
Fig. 2 is with MnOx-Al2O3And CuOx-Al2O3Odor at low temperature oxidation susceptibility comparison diagram as catalyst.
Fig. 3 is with MnOx-CeOx-Al2O3And MnOx-CoOx-Al2O3Odor at low temperature oxidation susceptibility as catalyst contrasts
Figure.
Fig. 4 is no catalyst, with MnOx-Al2O3As catalyst and with MnOx-CeOx-Al2O3Low temperature as catalyst
Ozone oxidation performance comparison figure.
Embodiment
Below in conjunction with attached drawing and technical solution, embodiment of the invention is further illustrated.
Embodiment 1：MnOx-Al2O3The preparation of catalyst and the application of O3 catalytic oxidation performance
Choose the γ-Al of 1~2mm2O3Bead is catalyst carrier, is cleaned 2 times with deionized water, then uses 0.10mol/L
Dilute hydrochloric acid soaked overnight, be finally washed with deionized water neutral to water outlet, 100 ± 2 DEG C of drying, that is, obtain after activation process
γ-Al2O3Bead；By the γ-Al after activation process2O3Suitable 50%Mn (the NO of bead3)2Solution is soaked in equal volume
Stain, in 105 DEG C of drying in oven 2.5h after ultrasonic 2h, then at 500 DEG C roasts 4h, you can obtain MnOx-Al2O3Catalyst.
By the MnO prepared by 10gx-Al2O3Catalyst is fitted into reaction unit, is passed through the simulated flue gas containing 500ppmNO,
Flue gas flow is set as 1L/min, and flue gas relative humidity is 10%, and reaction temperature is arranged to 100 DEG C, is passed through ozone gas, ozone
It is set as 0.6 with the molar ratio of NO, reacts 30min, records nitrogen oxides detector registration.
Embodiment 2：CuOx-Al2O3The preparation of catalyst and the application of O3 catalytic oxidation performance
Choose the γ-Al of 1~2mm2O3Bead is catalyst carrier, is cleaned 2 times with deionized water, then uses 0.10mol/L
Dilute hydrochloric acid soaked overnight, be finally washed with deionized water neutral to water outlet, 100 ± 2 DEG C of drying, that is, obtain after activation process
γ-Al2O3Bead；By the γ-Al after activation process2O3Suitable Cu (the NO of bead3)2Solution carries out incipient impregnation, surpasses
In 105 DEG C of drying in oven 2.5h after sound 2h, then in 500 DEG C of roasting 4h, you can obtain CuOx-Al2O3Catalyst.
By the CuO prepared by 10gx-Al2O3Catalyst is fitted into reaction unit, is passed through the simulated flue gas containing 500ppmNO,
Flue gas flow is set as 1L/min, and flue gas relative humidity is 10%, and reaction temperature is arranged to 100 DEG C, is passed through ozone gas, ozone
It is set as 0.6 with the molar ratio of NO, reacts 30min, records nitrogen oxides detector registration.
Embodiment 3：MnOx-CeOx-Al2O3The preparation of catalyst and the application of O3 catalytic oxidation performance
Choose the γ-Al of 1~2mm2O3Bead is catalyst carrier, is cleaned 2 times with deionized water, then uses 0.10mol/L
Dilute hydrochloric acid soaked overnight, be finally washed with deionized water neutral to water outlet, 100 ± 2 DEG C of drying, that is, obtain after activation process
γ-Al2O3Bead；By the γ-Al after activation process2O3Suitable Mn (the NO of bead3)2With Ce (NO3)2Mixed solution carries out
Incipient impregnation, in 105 DEG C of drying in oven 2.5h after ultrasonic 2h, then at 500 DEG C roasts 4h, you can obtain MnOx-CeOx-
Al2O3Catalyst.
By the MnO prepared by 10gx-CeOx-Al2O3Catalyst is fitted into reaction unit, is passed through the simulation containing 500ppmNO
Flue gas, flue gas flow are set as 1L/min, and flue gas relative humidity is 10%, and reaction temperature is arranged to 100 DEG C, is passed through ozone gas
The molar ratio of body, ozone and NO are set as 0.6, react 80min, record nitrogen oxides detector registration.
Embodiment 4：MnOx-CoOx-Al2O3The preparation of catalyst and the application of O3 catalytic oxidation performance
Choose the γ-Al of 1~2mm2O3Bead is catalyst carrier, is cleaned 2 times with deionized water, then uses 0.10mol/L
Dilute hydrochloric acid soaked overnight, be finally washed with deionized water neutral to water outlet, 100 ± 2 DEG C of drying, that is, obtain after activation process
γ-Al2O3Bead；By the γ-Al after activation process2O3Suitable Mn (the NO of bead3)2With Co (NO3)2Mixed solution carries out
Incipient impregnation, in 105 DEG C of drying in oven 2.5h after ultrasonic 2h, then at 500 DEG C roasts 4h, you can obtain MnOx–CoOx-
Al2O3Catalyst.
By the MnO prepared by 10gx–CoOx-Al2O3Catalyst is fitted into reaction unit, is passed through the simulation containing 500ppmNO
Flue gas, flue gas flow are set as 1L/min, and flue gas relative humidity is 10%, and reaction temperature is arranged to 100 DEG C, is passed through ozone gas
The molar ratio of body, ozone and NO are set as 0.6, react 80min, record nitrogen oxides detector registration.
Experimental result is as follows：
Fig. 2 shows, MnOx-Al2O3Catalytic effect compared with CuOx-Al2O3More preferably, react in 30min, with MnOx-Al2O3Make
For catalyst, the transformation efficiency of NO is 35%~45%.And with CuOx-Al2O3As catalyst, the transformation efficiency of NO only exists
25% or so.
Fig. 3 shows, MnOx-CeOx-Al2O3Catalytic effect compared with MnOx–CoOx-Al2O3More preferably, react in 80min, with
MnOx-CeOx-Al2O3As catalyst, the transformation efficiency of NO is 35%~65%.And with MnOx–CoOx-Al2O3As catalysis
Agent, the transformation efficiency of NO is only 25%~53%.
Shown in Fig. 4, with MnOx-CeOx-Al2O3And MnOx-Al2O3The conversion ratio of NO substantially compares O during as catalyst3Individually
It is high during oxidation.0-20min after reaction, MnOx-Al2O3Compare MnOx-CeOx-Al2O3Catalytic activity it is more preferable, NO conversion ratios are up to
80%.But 20-90minMnO after reactingx-Al2O3Catalytic activity decline obvious, MnOx-CeOx-Al2O3Catalytic activity it is excellent
In MnOx-Al2O3, NO conversion ratios remain to maintain 40% after reacting 90min.
Certainly, it is limitation of the present invention that described above, which is not, and the present invention is also not limited to above-mentioned case, the skill of this area
Art personnel make the change of reaction condition in the essential scope of the present invention, catalyst changes, also should be in the protection model of the present invention
In enclosing.
Claims (8)
1. a kind of preparation method for loading O composite metallic oxide catalyst, it is characterised in that step is as follows：
1. choose the γ-Al of a diameter of 1~2mm2O3Bead cleans 1~3 time as carrier, with deionized water, then with 0.10~
The dilute hydrochloric acid soaked overnight of 0.25mol/L, finally with being dried after deionized water rinsing to water outlet neutrality, that is, obtains by activation
Catalyst carrier after reason；
2. prepare manganese, cobalt, cerium, iron, copper, the nitrate solution of nickel, under normal temperature condition, respectively to the carrier after activation process into
Row incipient impregnation, ultrasonic 2h, drying, then by 500 DEG C of roasting 4h, obtain the single component metal that load capacity is 1wt% and aoxidize
Thing loaded catalyst；
3. 2. manganese nitrate that step is filtered out is formulated as the solution of various concentrations, at normal temperatures, to the carrier after activation process
Incipient impregnation, ultrasonic 2h, drying are carried out, then by 500 DEG C of roasting 4h, obtains the one-component gold that load capacity is 0.5-4wt%
Belong to oxide catalyst；
4. 3. load capacity that step is filtered out is to mix cobalt, cerium, iron, copper, nickel in the manganese nitrate solution of 0.5-4wt% respectively
Nitrate is configured to composite metal salt maceration extract, at normal temperatures, the carrier after activation process is carried out incipient impregnation, ultrasound
2h, drying, then by 500 DEG C of roasting 4h, it is 1 to obtain load molar ratio:0.6 different two-component loaded catalysts；Screening
It is cerous nitrate to go out optimum doping metal nitrate；
5. 4. manganese nitrate and cerous nitrate that step is filtered out are configured to the composite metal salt maceration extract of various concentrations ratio, normal
Under temperature, incipient impregnation, ultrasonic 2h, drying are carried out to the carrier after activation process, then by 500 DEG C of roasting 4h, obtain manganese cerium
Load capacity molar ratio is 1:0.2~1 two-component metal oxide catalyst；
6. at normal temperatures, 5. composition metal nitrate solution that step filters out carries out the carrier after activation process isometric
Dipping, ultrasonic 2h, drying, then 4h is roasted at 400~600 DEG C, obtain load O composite metallic oxide catalyst.
2. preparation method according to claim 1, it is characterised in that the load capacity of the manganese is 3wt%.
3. preparation method according to claim 1 or 2, it is characterised in that the manganese cerium load molar ratio is 1：0.4.
4. preparation method according to claim 1 or 2, it is characterised in that step 6. in, the calcining heat be 500
℃。
5. preparation method according to claim 3, it is characterised in that step 6. in, the calcining heat be 500 DEG C.
6. the catalyst that claim 1,2 or 5 is prepared is in the application in exhaust-gas treatment field, it is characterised in that step is as follows：
The load O composite metallic oxide catalyst being prepared is fitted into reaction unit, is passed through simulated flue gas, flue gas always flows
Measure and enter by preheating apparatus in reaction unit for 1.0L/min, simulated flue gas, reacted with the ozone being passed through, pass through nitrogen
Residue NO concentration in Determination of Oxide instrument detection flue gas；
NO concentration is 100~1000ppm, the O being passed through in simulated flue gas3Molar ratio with NO is 0.2~3.5, flue gas relative humidity
For 2%~12%, reaction temperature is 20~120 DEG C, and specific reaction condition is depending on the composition of simulated flue gas.
7. the catalyst that claim 3 is prepared is in the application in exhaust-gas treatment field, it is characterised in that step is as follows：
The load O composite metallic oxide catalyst being prepared is fitted into reaction unit, is passed through simulated flue gas, flue gas always flows
Measure and enter by preheating apparatus in reaction unit for 1.0L/min, simulated flue gas, reacted with the ozone being passed through, pass through nitrogen
Residue NO concentration in Determination of Oxide instrument detection flue gas；
NO concentration is 100~1000ppm, the O being passed through in simulated flue gas3Molar ratio with NO is 0.2~3.5, flue gas relative humidity
For 2%~12%, reaction temperature is 20~120 DEG C, and specific reaction condition is depending on the composition of simulated flue gas.
8. the catalyst that claim 4 is prepared is in the application in exhaust-gas treatment field, it is characterised in that step is as follows：
The load O composite metallic oxide catalyst being prepared is fitted into reaction unit, is passed through simulated flue gas, flue gas always flows
Measure and enter by preheating apparatus in reaction unit for 1.0L/min, simulated flue gas, reacted with the ozone being passed through, pass through nitrogen
Residue NO concentration in Determination of Oxide instrument detection flue gas；
NO concentration is 100~1000ppm, the O being passed through in simulated flue gas3Molar ratio with NO is 0.2~3.5, flue gas relative humidity
For 2%~12%, reaction temperature is 20~120 DEG C, and specific reaction condition is depending on the composition of simulated flue gas.
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