CN107790117A - A kind of preparation method of denitrating catalyst - Google Patents
A kind of preparation method of denitrating catalyst Download PDFInfo
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- CN107790117A CN107790117A CN201610790293.7A CN201610790293A CN107790117A CN 107790117 A CN107790117 A CN 107790117A CN 201610790293 A CN201610790293 A CN 201610790293A CN 107790117 A CN107790117 A CN 107790117A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
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- 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
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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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
- B01D53/86—Catalytic processes
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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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0213—Preparation of the impregnating solution
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- B01D2258/0283—Flue gases
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Abstract
The invention discloses a kind of preparation method of denitrating catalyst, including following content:(1)Carbon powder is added in the ethanol solution containing silicon source, is well mixed under the conditions of ultrasonic disperse, processing is dried in separation of solid and liquid, solid phase, obtains the carbon powder of silicon source modification;(2)By step(1)Obtained carbon powder is well mixed with Alumina gel, obtains coating slurry;(3)The cordierite honeycomb ceramic matrix of pretreatment is immersed in coating slurry processing, takes out, blows away raffinate, dry, then high-temperature process in an oxygen-free atmosphere, obtains loading the cordierite honeycomb ceramic matrix of coating;(4)With the maceration extract impregnation steps containing active component(3)Obtained carrier, dry, roasting, obtain final product.Certain mechanical strength is also ensured simultaneously containing more macropore in denitrating catalyst coating prepared by the inventive method, there is good denitration activity, stability and antitoxinization performance, preparation technology is simple, suitable for commercial Application.
Description
Technical field
The present invention relates to a kind of preparation method of denitrating catalyst.
Background technology
NOxIt is the major pollutants to form acid rain, photochemical fog and Atmospheric Ozone Layer Depletion.It is bright during " 12 "
True requirement need to be to NOxRealize overall control.Implement within 2012《Fossil-fuel power plant atmospheric pollutant emission standard》, it is desirable to NOxDischarge limit
It is worth for 100mg/m3.Therefore, the nitrogen oxides how effectively removed in flue gas turns into the problem of in the urgent need to address.Current
In denitration technology, selective catalytic reduction(SCR)It is selective to give up by the effect of catalyst using reducing agents such as ammonia
NO in gasxReduction is converted into the N harmless to air2And H2O, there is selective good and efficiency high, turn into application at present most
Extensive gas denitrifying technology.
Denitrating catalyst is the core of SCR technology, and because the exhaust gas volumns such as power plant, Industrial Boiler are big, denitrating catalyst is general
Using monolithic construction.CN101380543A discloses a kind of flue gas denitration composite catalyst, and the catalyst is with aluminium base or silicon substrate
Ceramics are first vector, and sial composite oxides are Second support, and cerium zirconium metal composite oxide is active component.
CN101961656A discloses a kind of denitrating catalyst, and the catalyst is to be loaded with TiO2-SiO2The cordierite honeycomb ceramic of coating
For carrier, active component V2O5、WO3、MoO3、SO4 2-In two or more mixing.CN102008952A discloses one kind
Denitration composite oxide catalysts, the catalyst is using ceramic honey comb as carrier, using Ti-Zr composite oxides as carrier coating, with
Tin cerium tungsten composite oxides are active component.CN101357328A discloses a kind of denitrating catalyst, and the catalyst is made pottery with silicon substrate
Porcelain is carrier, active SiO2For Second support, it is active component that cerium oxide, which adds appropriate transition metal,.CN1593752A is disclosed
A kind of catalyst for generating plant flue gas SCR denitration.The catalyst loads Al on cordierite honeycomb2O3For carrier coating, load
V2O5And WO3For active component.CN101234345A discloses a kind of denitrating catalyst, the catalyst using Al-base ceramic as carrier,
Active Al2O3For Second support, CeO2It is active component to add appropriate metal oxide.CN101053838A discloses a kind of de-
Denox catalyst, the catalyst load Al using cordierite as carrier2O3After coating, then Supported CuO is active component.
In above-mentioned patent in prepares coating colloidal sol or slurry processes, 2% ~ 5% chemical pore creating material is typically all added, is such as urinated
Element, polyethylene glycol etc., the duct quantity of face coat is improved, increase specific surface area, be advantageous to the progress of denitration reaction, due to
Ammonium hydrogen sulfate generated in flying dust and reaction among flue gas etc. is constantly deposited on inside duct, is blocked duct, is finally made to urge
Agent inactivates.So further improve the quantity of macropore in coating, it is possible to increase the space of catalyst reaction and anti-flying dust and
The ability of salt poisoning, and increasing for the quantity of macropore, certainly will influence whether the mechanical strength of catalyst coat, it is seen that the number of macropore
There is insoluble contradiction between amount and the mechanical strength of coating, conventional technology of preparing is difficult to take into account the two problems.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of preparation method of denitrating catalyst, prepared by the inventive method
Denitrating catalyst coating in containing more macropore also ensure certain mechanical strength simultaneously, there is good denitration to live
Property, stability and antitoxinization performance, preparation technology are simple, suitable for commercial Application.
The preparation method of the denitrating catalyst of the present invention, including following content:
(1)Carbon powder is added in the ethanol solution containing silicon source, is well mixed under the conditions of ultrasonic disperse, separation of solid and liquid,
Processing is dried in solid phase, obtains the carbon powder of silicon source modification;
(2)By step(1)Obtained carbon powder is well mixed with Alumina gel, obtains coating slurry;
(3)The cordierite honeycomb ceramic matrix of pretreatment is immersed in coating slurry processing, takes out, blows away raffinate, dry, then
High-temperature process in an oxygen-free atmosphere, obtain loading the cordierite honeycomb ceramic matrix of coating;
(4)With the maceration extract impregnation steps containing active component(3)Obtained carrier, dry, roasting, obtain final product.
In the inventive method, step(1)Described carbon powder can be selected from commercial goods, as acetylene carbon black, N330 carbon blacks,
FW200 carbon blacks etc..
In the inventive method, step(1)Described silicon source is methyl silicate, tetraethyl orthosilicate, positive silicic acid propyl ester or just
One or more in butyl silicate.
In the inventive method, step(1)The solid-liquid mass ratio of described carbon powder and the ethanol solution containing silicon source is 1:5~
1:30.
In the inventive method, step(1)Described silicon source is counted with the mass ratio of carbon powder as 5 using silica:1~1:1.
In the inventive method, step(1)Described ultrasonic disperse condition is:The energy density of ultrasonic disperse is 0.2 ~ 4kW/
L, ultrasonic disperse temperature are 15 ~ 80 DEG C, and the ultrasonic disperse time is 0.5 ~ 10 hour.
In the inventive method, step(1)Described separation of solid and liquid can use the usual manners such as filtering, centrifugation.
In the inventive method, step(1)Described drying condition is:30 ~ 100 DEG C of drying temperature, drying time be 0.1 ~
10 hours.
In the inventive method, step(2)The cordierite honeycomb ceramic matrix of described pretreatment is to be activated through peracid treatment
Cordierite honeycomb ceramic matrix.
In the inventive method, step(2)The carbon powder and the mass ratio of Alumina gel that described silicon source is modified are 1:1~1:10,
Preferably 1:3~1:7.
In the inventive method, step(2)Described Alumina gel counts concentration as 5wt% ~ 30wt% using aluminum oxide;Described aluminium is molten
Glue can use commercial goods, can also be prepared by method well known to those skilled in the art;Can also basis in Alumina gel
Need to add the chemical enlargement agent such as urea, ammonium hydrogen carbonate, addition is the 2% ~ 5% of Alumina gel weight.
In the inventive method, step(3)Described immersion processing time be 1 ~ 120 minute, preferably 3 ~ 60 minutes, after taking-up
Surplus liquid in matrix space is blown off with compressed air.
In the inventive method, step(4)The described impregnation time be 1 ~ 120 minute, preferably 3 ~ 60 minutes, after taking-up
Surplus liquid in matrix space is blown off with compressed air.
In the inventive method, step(4)Described maceration extract is the aqueous solution of the soluble compound containing manganese and iron, excellent
Select the aqueous solution of manganese nitrate, ferric nitrate, impregnation concentration 10wt% ~ 20wt%.
In the inventive method, step(4)Using volume impregnation, dip time be 1 ~ 120 minute, preferably 5 ~ 60 minutes.
In the inventive method, step(4)Described sintering temperature be 400 ~ 600 DEG C, preferably 500 ~ 600 DEG C, roasting time
For 2 ~ 10 hours, it is calcined and is carried out in oxygen-containing atmosphere, generally air atmosphere.
In the inventive method, step(3)And step(4)Described drying temperature is 60 ~ 150 DEG C, preferably 80 ~ 120 DEG C, is done
The dry time be 3 ~ 12 hours, preferably 6 ~ 10 hours,
In the inventive method, described mixed process is using modes such as stirring, ultrasound or high shears.
Application of the denitrating catalyst in denitrating flue gas in the present invention, general preferable process conditions are:Temperature is 180
~ 500 DEG C, reaction velocity is 4000 ~ 10000h-1, NOxConcentration is 500 ~ 1500ppm, SO2Concentration is 0 ~ 500ppm, O2Volume contains
Measure as 2% ~ 3%, H2O volume contents are 0 ~ 10%.
Compared with prior art, denitrating catalyst of the present invention has following features:
In the prior art by the property of silicon source denitrating catalyst coating, the specific duct to coating that can not typically have target changes
Property, in modifying process, Ludox micelle is easily penetrated into coating(Such as aluminum oxide)Most of duct(It is macropore, mesoporous)In, cause
The pore volume of carrier is greatly lowered.The present invention is mixed with the coating of modified carbon black powder, passed through by wrapping up silicon source on carbon black powder surface
Anaerobic is heat-treated so that silicon source fully contacts with aluminum oxide, and is converted into silica, further by calcination process, removes
Carbon powder particle, while reaming, SiO2The big hole surface of carbon powder particle formation is remained stuck to, plays a supporting role, enhances
The intensity of aluminum oxide coating layer, while SiO2Modifying function, reduce the interaction of active component and alumina carrier surface
And the acidity on macroporous aluminium oxide surface is improved, the activity of catalyst is improved, additionally, due to SiO2Supporting role ensure
The mechanical strength of aluminum oxide macropore so that alumina support is not easy to cave in, in preparation process, can add compared with prior art
More carbon powders, so as to form more macropores, so as to improve the mass-transfer efficiency of denitrating flue gas, catalyst duct be not easy by
Flying dust and sulfate block, and extend the life-span of catalyst.
Embodiment
Technical scheme is illustrated in more detail below by specific embodiment, and the embodiment is not
It is interpreted as the limitation of the scope of the invention.The size of cordierite honeycomb ceramic used is that section length is in embodiment
50mm rectangular carrier.
Embodiment 1
Cordierite pre-processes:Cordierite honeycomb ceramic is totally submerged in 5wt% salpeter solution, soak time is 1 hour,
Deionized water rinsing is used after taking-up 3 times, be put into baking oven under the conditions of 120 DEG C, dry 10 hours, obtain the cordierite of surface active
Honeycomb ceramic carrier.
Alumina gel preparation process is as follows:20 grams of boehmites are added in 150mL deionized waters, while stirring
7 grams of concentrated nitric acids are added dropwise.After stirring certain time, be heated to 80 DEG C, nitric acid be added dropwise to complete peptization, control solution ph 2 ~ 5,
Ageing 24 hours, obtains transparent Alumina gel, content is counted as 8wt% using aluminum oxide.
It is prepared by activearm liquid separation:40 grams of manganese nitrates and 10 grams of ferric nitrates are added into 200ml deionized waters, are stirred to complete
Dissolving, obtains activearm liquid separation.
(1)Carbon powder is added in the ethanol solution containing tetraethyl orthosilicate(Wherein solid-liquid mass ratio is 1:8, positive silicon
Acetoacetic ester is with SiO2The mass ratio of meter and carbon powder is 2:1), under the conditions of ultrasonic disperse(The energy density of ultrasonic disperse is
0.6kW/L, ultrasonic disperse temperature are 40 DEG C, and the ultrasonic disperse time is 1 hour)It is well mixed, filter, 2 are dried at 50 DEG C of solid phase
Hour, drying process, obtain the carbon powder of silicon source modification;
(2)By step(1)Obtained carbon powder is with Alumina gel according to mass ratio 1:8 is well mixed, obtains coating slurry;
(3)The cordierite honeycomb ceramic matrix of pretreatment is immersed in coating slurry 10 minutes, takes out, raffinate is blown away, at 110 DEG C
Dry 10 hours, then in nitrogen 400 DEG C handle 3 hours, obtain load coating cordierite honeycomb ceramic matrix;
(4)With the maceration extract impregnation steps containing active component(3)Obtained carrier, dried 8 hours at 110 DEG C, after drying
Material be calcined 5 hours at 550 DEG C in air atmosphere, obtain catalyst CT1, in the catalyst, Mn load capacity is
8wt%, Fe load capacity are 2wt%.
Embodiment 2
Cordierite pre-processes:With embodiment 1.
Alumina gel is commercial goods(Solid content is 15%).
It is prepared by activearm liquid separation:50 grams of manganese nitrates are added into 200ml deionized waters and 10 grams of ferric nitrates are stirred to complete
Dissolving, obtains activearm liquid separation.
(1)Carbon powder is added in the ethanol solution containing tetraethyl orthosilicate(Wherein solid-liquid mass ratio is 1:8, positive silicon
Acetoacetic ester is with SiO2The mass ratio of meter and carbon powder is 3:1), under the conditions of ultrasonic disperse(The energy density of ultrasonic disperse is
0.8kW/L, ultrasonic disperse temperature are 45 DEG C, and the ultrasonic disperse time is 1 hour)It is well mixed, filter, 2 are dried at 50 DEG C of solid phase
Hour, drying process, obtain the carbon powder of silicon source modification;
(2)By step(1)Obtained carbon powder is with Alumina gel according to mass ratio 1:6 is well mixed, obtains coating slurry;
(3)The cordierite honeycomb ceramic matrix of pretreatment is immersed in coating slurry 10 minutes, takes out, raffinate is blown away, at 120 DEG C
Dry 9 hours, then in nitrogen 450 DEG C handle 3.5 hours, obtain load coating cordierite honeycomb ceramic matrix;
(4)With the maceration extract impregnation steps containing active component(3)Obtained carrier, dried 8 hours at 110 DEG C, after drying
Material be calcined 5 hours at 550 DEG C in air atmosphere, obtain catalyst CT2, in the catalyst, Mn load capacity is
6.67wt%, Fe load capacity are 1.33wt%.
Embodiment 3
Cordierite pre-processes:With embodiment 1.
It is prepared by Alumina gel:With embodiment 1.
It is prepared by activearm liquid separation:60 grams of manganese nitrates and 10 grams of ferric nitrates are added into 200ml deionized waters, are stirred to complete
Dissolving, obtains activearm liquid separation.
(1)Carbon powder is added in the ethanol solution containing tetraethyl orthosilicate(Wherein solid-liquid mass ratio is 1:20, positive silicon
Acetoacetic ester is with SiO2The mass ratio of meter and carbon powder is 4:1), under the conditions of ultrasonic disperse(The energy density of ultrasonic disperse is
2kW/L, ultrasonic disperse temperature are 30 DEG C, and the ultrasonic disperse time is 1 hour)It is well mixed, filter, it is small that 2 are dried at 60 DEG C of solid phase
When, drying process, obtain the carbon powder of silicon source modification;
(2)By step(1)Obtained carbon powder is with Alumina gel according to mass ratio 1:3 is well mixed, obtains coating slurry;
(3)The cordierite honeycomb ceramic matrix of pretreatment is immersed in coating slurry 20 minutes, takes out, raffinate is blown away, at 110 DEG C
Dry 10 hours, then in nitrogen 400 DEG C handle 3 hours, obtain load coating cordierite honeycomb ceramic matrix;
(4)With the maceration extract impregnation steps containing active component(3)Obtained carrier, dried 8 hours at 110 DEG C, after drying
Material be calcined 5 hours at 550 DEG C in air atmosphere, obtain catalyst CT3, in the catalyst, Mn load capacity is
4.29wt%, Fe load capacity are 0.71wt%.
Comparative example 1
In addition to carbon black powder is modified by silicon source, other are the same as embodiment 1.
Comparative example 2
Except step(3)Middle nitrogen atmosphere is changed to outside air atmosphere, and other are the same as embodiment 1.
The porous compressive strength test instrument SDY of digital display manufactured using Xiang Tan Xiang Yi Instrument Ltd. has carried out catalyst
Strength test, it the results are shown in Table 1.
The strength test results of the catalyst of table 1.
In order to evaluate the denitration effect of catalyst, activity rating is carried out to denitrating catalyst prepared by the present invention, evaluates bar
Part is:NOxConcentration is 500 ~ 1000ppm, O2Volume content be 2%, SO2Concentration is 300ppm, H2O volume contents are 5%, NH3/
NOx=1:1 (mol ratio), air speed are 4000 ~ 10000h-1, reaction temperature is respectively 400 DEG C, NOxRemoval effect is shown in Table 2;380℃
Under reaction temperature, long-term operation the results are shown in Table 3.
2 400 DEG C of Activity evaluations of table.
3 380 DEG C of long-term operation result of the tests of table.
Found by Experimental Comparison, catalyst of the invention has very for the removal of nitrogen oxide efficiency high in flue gas
Good denitration activity.Contain water and SO in flue gas2Under conditions of, after continuously running 500 hours, still remain high denitration effect
Rate, illustrate that the catalyst is not easily blocked, there is good stability, service life length.
Claims (14)
1. a kind of preparation method of denitrating catalyst, including following content:(1)It is molten that carbon powder is added to the ethanol containing silicon source
In liquid, it is well mixed under the conditions of ultrasonic disperse, processing is dried in separation of solid and liquid, solid phase, obtains the carbon powder of silicon source modification;
(2)By step(1)Obtained carbon powder is well mixed with Alumina gel, obtains coating slurry;(3)By the cordierite honeycomb of pretreatment
Ceramic matrix is immersed in coating slurry processing, takes out, blows away raffinate, dries, then high-temperature process in an oxygen-free atmosphere, is born
Carry the cordierite honeycomb ceramic matrix of coating;(4)With the maceration extract impregnation steps containing active component(3)Obtained carrier, do
It is dry, roasting, obtain final product.
2. in accordance with the method for claim 1, it is characterised in that:Step(1)Described silicon source is methyl silicate, positive silicic acid
One or more in ethyl ester, positive silicic acid propyl ester or butyl silicate.
3. in accordance with the method for claim 1, it is characterised in that:Step(1)Described carbon powder and the ethanol containing silicon source are molten
The solid-liquid mass ratio of liquid is 1:5~1:30.
4. in accordance with the method for claim 1, it is characterised in that:Step(1)Described silicon source is in terms of silica and carbon black
The mass ratio of powder is 5:1~1:1.
5. in accordance with the method for claim 1, it is characterised in that:Step(1)Described ultrasonic disperse condition is:Ultrasonic disperse
Energy density be 0.2 ~ 4kW/L, ultrasonic disperse temperature is 15 ~ 80 DEG C, and the ultrasonic disperse time is 0.5 ~ 10 hour.
6. in accordance with the method for claim 1, it is characterised in that:Step(1)Described drying condition is:Drying temperature 30 ~
100 DEG C, drying time is 0.1 ~ 10 hour.
7. in accordance with the method for claim 1, it is characterised in that:Step(2)The carbon powder and aluminium that described silicon source is modified are molten
The mass ratio of glue is 1:1~1:10.
8. in accordance with the method for claim 1, it is characterised in that:Step(2)Described Alumina gel concentration in terms of aluminum oxide is
5wt%~30wt%。
9. in accordance with the method for claim 1, it is characterised in that:Step(3)Described immersion processing time is 1 ~ 120 point
Clock, surplus liquid in matrix space is blown off with compressed air after taking-up.
10. in accordance with the method for claim 1, it is characterised in that:Step(4)The described impregnation time is 1 ~ 120 point
Clock, surplus liquid in matrix space is blown off with compressed air after taking-up.
11. in accordance with the method for claim 1, it is characterised in that:Step(4)Described maceration extract be containing manganese and iron can
The aqueous solution of soluble compound, impregnation concentration 10wt% ~ 20wt%;Using volume impregnation, dip time be 1 ~ 120 minute.
12. in accordance with the method for claim 1, it is characterised in that:Step(4)Described sintering temperature is 400 ~ 600 DEG C, roasting
It is 2 ~ 10 hours to burn the time.
13. in accordance with the method for claim 1, it is characterised in that:Step(3)With(4)Described drying temperature is 60 ~ 150
DEG C, drying time is 3 ~ 12 hours.
14. the denitrating catalyst prepared according to the method described in claim 1 ~ 13 any claim answering in denitrating flue gas
With process conditions are:Temperature is 180 ~ 500 DEG C, and reaction velocity is 4000 ~ 10000h-1, NOxConcentration is 500 ~ 1500ppm, SO2
Concentration is 0 ~ 500ppm, O2Volume content is 2% ~ 3%, H2O volume contents are 0 ~ 10%.
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Cited By (4)
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CN111068706A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Preparation method of denitration catalyst |
CN111151259A (en) * | 2018-11-08 | 2020-05-15 | 中国石油化工股份有限公司 | Preparation method of denitration catalyst |
CN111298802A (en) * | 2018-12-12 | 2020-06-19 | 中国石油化工股份有限公司 | Preparation method of flue gas denitration catalyst |
CN113499768A (en) * | 2021-07-09 | 2021-10-15 | 安徽元琛环保科技股份有限公司 | Preparation method of coating type high-strength denitration catalyst and prepared denitration catalyst |
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CN104415780A (en) * | 2013-08-22 | 2015-03-18 | 中国石油化工股份有限公司 | Denitration catalyst and preparation method thereof |
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