CN105396609A - Preparation of high-efficient denitration catalyst - Google Patents
Preparation of high-efficient denitration catalyst Download PDFInfo
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- CN105396609A CN105396609A CN201410454921.5A CN201410454921A CN105396609A CN 105396609 A CN105396609 A CN 105396609A CN 201410454921 A CN201410454921 A CN 201410454921A CN 105396609 A CN105396609 A CN 105396609A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002808 molecular sieve Substances 0.000 claims abstract description 30
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 26
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010457 zeolite Substances 0.000 claims abstract description 26
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 13
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 13
- 229920006184 cellulose methylcellulose Polymers 0.000 claims description 13
- 239000011153 ceramic matrix composite Substances 0.000 claims description 13
- 238000012710 chemistry, manufacturing and control Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 230000001413 cellular effect Effects 0.000 claims description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 34
- 238000000034 method Methods 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 230000000274 adsorptive effect Effects 0.000 abstract 1
- 230000003100 immobilizing effect Effects 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 239000000779 smoke Substances 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 abstract 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 7
- 239000003546 flue gas Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000003421 catalytic decomposition reaction Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000004155 Chlorine dioxide Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000001147 anti-toxic effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000019398 chlorine dioxide Nutrition 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical class [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Exhaust Gas Treatment By Means Of Catalyst (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a high-efficient denitration catalyst, and belongs to the technical field of preparation of a denitration catalyst. The method comprises: taking cheap easily-available titanium tetrachloride as a titanium precursor; adopting a zeolite molecular sieve with excellent adsorptive property as a catalyst carrier; and immobilizing a component of a catalyst onto the zeolite molecular sieve to obtain the catalyst with the denitration efficiency more than 90%. The catalyst has characteristics of low cost, simple process, good low-temperature activity, and high denitration efficiency, has excellent pressure resistance and wear resistance, and can satisfy the requirement, of removing a nitrogen oxide from smoke for a long time in the real environment, of a denitration device.
Description
Technical field
The present invention relates to a kind of preparation method of high-efficiency denitration catalyst, particularly belong to SCR(selective catalytic reduction, SelectiveCatalyticReduction) denitrating catalyst preparing technical field.
Technical background
Nitrogen oxide is the general name of the many oxide of nitrogen, causes mainly nitric oxide (NO) and the nitrogen dioxide (NO of atmosphere pollution in nitrogen oxide
2).Nitrogen oxide is except entering human body by respiratory system and stimulate human body skin and causing primary pollution to people, larger harm is also that it forms acid rain by the change of multiple physics or chemistry, simultaneously can with the visible ray of hydrocarbon in daylight or UV-irradiation under there is a series of photochemical reaction and form photochemical fog.
At present, nitrogen oxide more than 90% in air is discharged into from fuel combustion process by various mode.During high temp. combustion of fuel in various industrial furnace, Civil energy-saving cooking stove, motor vehicle and other internal combustion engines, the nitrogen substance oxidation in fuel generates nitrogen oxide.From the energy resource structure that China is current, during our primary energy and power generation energy resource are formed, coal and the material relevant to coal occupy absolute leading position, and the coal of China's overwhelming majority is all directly burning, especially in power station, Industrial Boiler and civil boiler.In one quite long period, concerning us, the NO in flue gas
xdischarge is the principal element causing China's Pollution Index in Air Nitric Oxides.Therefore, the discharged nitrous oxides how reducing stationary source is the important research direction that atmospheric environment is administered.
The main way reducing fume emission is that scale adopts gas denitrifying technology, is mainly divided into Dry denitration and the large class of wet denitration two at present.Wet flue gas denitration refers to utilize liquid phase chemical reagent by the nox adsorption in flue gas and be converted into more stable material and realizes removing, method comprises Chlorine Dioxide Oxidation absorption process, ozone oxidation absorption process and potassium permanganate oxidation absorption process etc., its advantage easily realizes simultaneous SO_2 and NO removal, but it is more to have problems: (1) NO is insoluble in water, before absorption, need NO to be oxidized to NO
2, this process cost is higher; (2) nitrous acid generated or nitrate need process further; (3) a large amount of waste water can be produced; (4) can discharge, so wet denitration technology is still in laboratory stage rank at present after the flue gas after purification needs reheating; Dry denitration mainly comprises SCR SCR, SNCR SNCR (SNCR), the multiple methods such as electron beam denitration and direct catalytic decomposition, wherein directly catalytic decomposition and electron beam denitration two kinds of methods are only in the experimental study stage at present, still have gap from commercial Application, what real business was applied only has SCR and SNCR method.
The principle of SCR denitration technology sprays into NH in boiler emission flue gas
3deng reducing agent, these reducing agents react with the nitrogen oxide in flue gas and generate harmless nitrogen and water under the effect of catalyst.The core of SCR denitration technology is SCR catalyst, and typical SCR catalyst is carrier with titanium dioxide, with V
2o
5-WO
3be active component Deng metal oxide containing precious metals.The mode of appearance of SCR denitration has honeycomb fashion, flat and corrugated plate dst, and arrangement is vertically be covered with in, the casing of high 2 meters about long 2 meters, wide 1 meter at, forms denitrification catalyst module.The primary raw material of current SCR catalyst carrier is TiO
2powder, but shaping after catalyst major part material be sintered in inside, can not be fully used, the cost of titanium dioxide powder is far above shaping carriers such as conventional zeolite molecular sieves.
Therefore, prepare a kind of technique simple, with low cost and denitrating catalyst that is energy efficient removal nitrogen oxides in effluent has great application prospect and Research Significance.
Summary of the invention
The invention discloses a kind of preparation method of high-efficiency denitration catalyst, belong to denitrating catalyst preparing technical field.The object of the present invention is to provide a kind of preparation method of high-efficiency denitration catalyst, this catalyst has the advantages that cost is low, technique is simple, good, the out of stock efficiency of low temperature active is high, there is good resistance to compression and anti-wear performance simultaneously, long-time (>10000h) under denitration device true environment can be met and remove the nitrogen oxide requirement in flue gas.
For achieving the above object, the technical scheme taked of the present invention is as follows:
A kind of high-efficiency denitration catalyst, by weight, it is prepared from by following raw material: 15 ~ 25 parts of TiCl
4, 60 ~ 70 parts of zeolite molecular sieve, 3 ~ 5 parts of WO
3, 1 ~ 3 part of V
2o
5, 5 ~ 10 parts of ammoniacal liquor, 8 parts of CMCs (CMC) and 50 parts of deionized waters.
The present invention also provides the preparation method of described high-efficiency denitration catalyst, comprises the following steps:
1) by other all the mixing according to described ratio uniform except zeolite molecular sieve of above-described raw material, and under normal temperature, normal pressure, more than 24 hours are left standstill after fully stirring;
2) zeolite molecular sieve of described deal is immersed completely in the Homogeneous phase mixing system that step 1 obtains, flood more than 24 hours under normal temperature and pressure;
3) molecular sieve after step 3 being flooded through super-dry until moisture content lower than 3% after, at entirety is placed in 600 ~ 700 DEG C calcine 10 ~ 12 hours, namely obtain high-efficiency denitration catalyst of the present invention.
Zeolite molecular sieve of the present invention is common type ZSM 5 molecular sieve, and described zeolite molecular sieve is cellular.
High-efficiency denitration catalyst of the present invention belongs to the vanadium Titanium series catalyst (V of improvement
2o
5/ TiO
2catalyst), in its raw material, TiCl
4tiO
2presoma, V
2o
5as activated centre, WO
3as auxiliary element.Described raw material components is prepared into low cost SCR catalyst according to special ratios by the present invention, through experimental verification, obtains excellent low temperature active and antitoxin, resistance to compression and anti-wear performance, for obtaining the out of stock efficiency of more than 90% in traditional denitrating technique.
Compared with prior art, the effective effect of catalyst of the present invention is as follows:
1, there is excellent low-temperature catalytic activity, scuff resistance, compression strength, denitration efficiency;
2, low cost TiCl is adopted
4-as presoma, effectively reduce the cost of catalyst;
3, adopt zeolite molecular sieve as catalyst matrix, there is better adsorption capacity.
Detailed description of the invention
Further illustrate the present invention by the following examples:
embodiment 1
A kind of high-efficiency denitration catalyst, by weight, it is prepared from by following raw material: 25 parts of TiCl
4, 70 parts of zeolite molecular sieve, 5 parts of WO
3, 1 part of V
2o
5, 5 parts of ammoniacal liquor, 8 parts of CMCs (CMC) and 50 parts of deionized waters.
Wherein the length of zeolite molecular sieve is 800mm, inner wall thickness 1mm, outer wall thickness 3mm, and aperture is 5mm.
Preparation process is as follows:
1) 25 parts of TiCl
4, 5 parts of WO
3, 1 part of V
2o
5, 5 parts of ammoniacal liquor, 8 parts of CMC and 50 part deionized waters fully mix and leave standstill 48 hours after stirring;
2) get 70 parts of zeolite molecular sieves, in the mixed system that immersion above-mentioned steps 1 obtains completely, flood after 36 hours dry;
3) take out the zeolite molecular sieve after the dipping that obtains of step 2, dryly then enter calcining furnace until moisture content reaches 3%, calcine 12 hours at being placed in 650 DEG C, described low cost SCR catalyst can be obtained.
The catalyst getting the present embodiment carries out marking the denitration test under condition, and denitration rate reaches 91%.
embodiment 2
A kind of high-efficiency denitration catalyst, by weight, it is prepared from by following raw material: 35 parts of TiCl
4, 65 parts of zeolite molecular sieve, 4 parts of WO
3, 3 parts of V
2o
5, 5 parts of ammoniacal liquor, 8 parts of CMCs (CMC) and 50 parts of deionized waters.
Wherein the length of zeolite molecular sieve is 900mm, inner wall thickness 2mm, outer wall thickness 2mm, and aperture is 6mm.
Preparation process is as follows:
1) 35 parts of TiCl
4, 4 parts of WO
3, 3 parts of V
2o
5, 5 parts of ammoniacal liquor, 8 parts of CMC and 50 part deionized waters fully mix and leave standstill 48 hours after stirring;
2) get 65 parts of zeolite molecular sieves, in the mixed system that immersion above-mentioned steps 1 obtains completely, flood after 32 hours dry;
3) take out the zeolite molecular sieve after the dipping that obtains of step 2, dryly then enter calcining furnace until moisture content reaches 3%, calcine 11 hours at being placed in 650 DEG C, described low cost SCR catalyst can be obtained.
The catalyst getting the present embodiment carries out marking the denitration test under condition, and denitration rate reaches 92%.
embodiment 3
A kind of high-efficiency denitration catalyst, by weight, it is prepared from by following raw material: 35 parts of TiCl
4, 60 parts of zeolite molecular sieve, 3 parts of WO
3, 2 parts of V
2o
5, 5 parts of ammoniacal liquor, 8 parts of CMCs (CMC) and 50 parts of deionized waters.
Wherein the length of zeolite molecular sieve is 900mm, inner wall thickness 2mm, outer wall thickness 2mm, and aperture is 4mm.
Preparation process is as follows:
1) 35 parts of TiCl
4, 3 parts of WO
3, 2 parts of V
2o
5, 5 parts of ammoniacal liquor, 8 parts of CMC and 50 part deionized waters fully mix and leave standstill 48 hours after stirring;
2) get 60 parts of zeolite molecular sieves, in the mixed system that immersion above-mentioned steps 1 obtains completely, flood after 48 hours dry;
3) take out the zeolite molecular sieve after the dipping that obtains of step 2, dryly then enter calcining furnace until moisture content reaches 3%, calcine 12 hours at being placed in 700 DEG C, described low cost SCR catalyst can be obtained.
The catalyst getting the present embodiment carries out marking the denitration test under condition, and denitration rate reaches 95%.
Claims (3)
1. a high-efficiency denitration catalyst, is characterized in that by weight, and it is prepared from by following raw material: 15 ~ 25 parts of TiCl
4, 60 ~ 70 parts of zeolite molecular sieve, 3 ~ 5 parts of WO
3, 1 ~ 3 part of V
2o
5, 5 ~ 10 parts of ammoniacal liquor, 8 parts of CMCs (CMC) and 50 parts of deionized waters.
2. high-efficiency denitration catalyst according to claim 1, is characterized in that preparation method comprises the following steps:
1) by other all the mixing according to described ratio uniform except zeolite molecular sieve of above-described raw material, and under normal temperature, normal pressure, more than 24 hours are left standstill after fully stirring;
2) zeolite molecular sieve of described deal is immersed completely in the Homogeneous phase mixing system that step 1 obtains, flood more than 24 hours under normal temperature and pressure;
3) molecular sieve after step 3 being flooded through super-dry until moisture content lower than 3% after, at entirety is placed in 600 ~ 700 DEG C calcine 10 ~ 12 hours, namely obtain high-efficiency denitration catalyst of the present invention.
3. high-efficiency denitration catalyst according to claim 1, it is characterized in that described zeolite molecular sieve is common type ZSM 5 molecular sieve, described zeolite molecular sieve is cellular.
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|---|---|---|---|
| CN201410454921.5A CN105396609A (en) | 2014-09-09 | 2014-09-09 | Preparation of high-efficient denitration catalyst |
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|---|---|---|---|
| CN201410454921.5A CN105396609A (en) | 2014-09-09 | 2014-09-09 | Preparation of high-efficient denitration catalyst |
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| Publication Number | Publication Date |
|---|---|
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Family
ID=55462560
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107694553A (en) * | 2016-08-09 | 2018-02-16 | 丰田自动车株式会社 | NOxThe manufacture method of occlusion reducing catalyst |
| CN109675619A (en) * | 2019-03-06 | 2019-04-26 | 中自环保科技股份有限公司 | The method of molecular screen base SCR catalyst activity temperature window is controlled in a kind of preparation process |
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| US20090104096A1 (en) * | 2004-08-23 | 2009-04-23 | Basf Catalysts Llc | Zone Coated Catalyst to Simultaneously Reduce NOx and Unreacted Ammonia |
| CN102921405A (en) * | 2012-09-29 | 2013-02-13 | 重庆大学 | A kind of SiO2 added denitrification catalyst and preparation method thereof |
| CN103769137A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Preparation method of high-strength flue gas denitration catalyst |
-
2014
- 2014-09-09 CN CN201410454921.5A patent/CN105396609A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090104096A1 (en) * | 2004-08-23 | 2009-04-23 | Basf Catalysts Llc | Zone Coated Catalyst to Simultaneously Reduce NOx and Unreacted Ammonia |
| CN102921405A (en) * | 2012-09-29 | 2013-02-13 | 重庆大学 | A kind of SiO2 added denitrification catalyst and preparation method thereof |
| CN103769137A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Preparation method of high-strength flue gas denitration catalyst |
Non-Patent Citations (3)
| Title |
|---|
| LUCA LIETTI ET AL.: "Selective catalytic reduction (SCR) of NO by NH3 over TiO2-supported V2O5–WO3 and V2O5–MoO3 catalysts", 《TOPICS IN CATALYSIS》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107694553A (en) * | 2016-08-09 | 2018-02-16 | 丰田自动车株式会社 | NOxThe manufacture method of occlusion reducing catalyst |
| CN107694553B (en) * | 2016-08-09 | 2020-07-03 | 丰田自动车株式会社 | NOxMethod for producing occluding and reducing catalyst |
| CN109675619A (en) * | 2019-03-06 | 2019-04-26 | 中自环保科技股份有限公司 | The method of molecular screen base SCR catalyst activity temperature window is controlled in a kind of preparation process |
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Application publication date: 20160316 |