CN101767012B - Low-temperature combustion catalyst for eliminating diesel engine carbon black - Google Patents
Low-temperature combustion catalyst for eliminating diesel engine carbon black Download PDFInfo
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- CN101767012B CN101767012B CN200910163233A CN200910163233A CN101767012B CN 101767012 B CN101767012 B CN 101767012B CN 200910163233 A CN200910163233 A CN 200910163233A CN 200910163233 A CN200910163233 A CN 200910163233A CN 101767012 B CN101767012 B CN 101767012B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 39
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 17
- 239000006229 carbon black Substances 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 6
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000975 co-precipitation Methods 0.000 claims abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000013049 sediment Substances 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910002651 NO3 Inorganic materials 0.000 claims description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910001268 Ferrocerium Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 229910000510 noble metal Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 238000009938 salting Methods 0.000 claims description 4
- 238000000875 high-speed ball milling Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 9
- 239000002244 precipitate Substances 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical group O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract 1
- 238000011049 filling Methods 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 150000002823 nitrates Chemical class 0.000 abstract 1
- 239000010970 precious metal Substances 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 229910002092 carbon dioxide Inorganic materials 0.000 description 9
- 239000001569 carbon dioxide Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- 239000000779 smoke Substances 0.000 description 6
- 239000004071 soot Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- 230000000977 initiatory effect Effects 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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Abstract
The invention discloses a low-temperature combustion catalyst for eliminating diesel engine carbon black, the low-temperature combustion catalyst does not contain alkali metal and precious metal and is ferro-cerium-zirconium composite oxide; wherein the mole percentage composition of CeO2 is 50 percent, the mole percentage composition of Fe2O3 is 5-50 percent, and the mole percentage composition of ZrO2 is 45-0 percent; two preparation methods are included, the method I is coprecipitation hydrothermal synthesis method, the method II is mechanical mixing method; the method I comprises the following steps: Ce, Fe and Zr nitrates are prepared into saline solution with 0.1-0.5mol/L of total concentration according to stoichiometric ratio, and then H2O2 with proper amount is added, the mixture is fully stirred and mixed uniformly; under the strong stirring condition, the mixing solution is dropped in 3-8mol/L of ammonia water at 2-10mL/mim speed, so as to obtain precipitate; after the precipitating is completely carried out, the solution is continuously stirred for 30-120min. after aging is carried out for 30-180min, partial supernatant liquid is removed, the precipitate is transferred to a high pressure reactor (50-70 percent of filling degree) with 160-240 DEG C for 24-72 hours. The obtained product is washed respectively by deionized water and ethanol, and is dried 6-24h at 80-120 DEG C, so as to obtain the target catalyst. The material has high catalytic activity and heat stability, and has no pollution to environment.
Description
Technical field
The present invention relates to a kind of catalysis material that is used to eliminate diesel engine carbon black, belong to the environmental catalysis field.
Background technology
Compare with gasoline car, diesel vehicle has advantages such as good dynamic property, economy, durability and low carbon dioxide emission amount, makes it obtain fast development and extensive use in recent years.But a large amount of soots (soot) that contain in the diesel engine vent gas are very harmful to environment and human body, are to cause environmental pollution and one of the major pollutants that are detrimental to health.Therefore, in environmental regulation strict day by day today, the discharging of effectively controlling soot particulate is that the development diesel engine is badly in need of the key issue that solves.Under the prerequisite that does not change available engine system and fuel structure; The mode that filter combines with the soot low-temperature combustion catalyst is considered to the most promising diesel engine vent gas treatment technology, and the development of carbon-smoke combustion low temperature high activity catalyst also has more and more important position.
In numerous diesel emission soot combustion catalysts, the catalyst of transition metal oxide of loaded noble metal catalyst and alkali metal modified has advantages of high catalytic activity.But the noble metal scarcity of resources costs an arm and a leg, and is prone to poisoning and deactivation, and reduction is difficulty, and contaminated environment.The perovskite oxide is as the existing report of soot combustion catalyst, but its activity can't satisfy actual requirement.Alkali metal oxide is owing to have lower fusing point, and the Chang Zuowei additive improves catalyst performance, but the alkali metal vapour pressure is higher, is easy to run off, and is unfavorable for the stability of catalyst.Therefore, develop the processing that a kind of cost is low, activity is good, the life-span long, the little catalyst of pollution is used for the carbon smoke pollution thing, significant to solving the diesel engine pollution problem.
Summary of the invention
The purpose of this invention is to provide a kind of combination Fe
2O
3And ZrO
2Cerium based composite catalysis material, be used to handle the diesel engine carbon black pollutant.Fe
2O
3The Fe cheap, that valence state is lower
3+Introduce CeO
2In the lattice, what can not only significantly improve cerium oxide stores the oxygen performance, and the existence of iron species can also improve CeO
2Surface state, promote the formation of oxygen adsorption potential; And the Zr that radius is less
4+Mix CeO
2In the lattice, then can improve CeO effectively
2Stability and anti-caking power.Therefore, the cerium sill that adopts Fe and Zr to modify is handled soot, can when significantly reducing cost, improve the treatment effeciency of pollutant.
For realizing foregoing invention, technical scheme of the present invention is following:
The present invention mainly is the cerium sill that preparation Fe and Zr mix.The preparation process is following:
Method 1: co-precipitation hydrothermal synthesis method
The nitrate of getting Ce, Fe, Zr is by predetermined molar ratio (CeO wherein
2Molar content be 50%, Fe
2O
3Molar content be 5%-50%, ZrO
2Molar content be 45%-0%, it is 100% that these three kinds of oxides add up to molar contents) be mixed with the salting liquid that total concentration is 0.1-1mol/L, add an amount of H again
2O
2, fully stir, evenly mix.Under vigorous stirring, the speed of above-mentioned mixed solution with 2-10mL/min is splashed in the ammoniacal liquor of 3-8mol/L, obtain sediment.Precipitate complete continued and stir 30-120min.Remove the part supernatant liquor behind the aging 30-180min, the gained sediment is moved in the autoclave (compactedness is 50-70%), insulation 24-72h in the time of 160-240 ℃.After products therefrom washed respectively with deionized water and ethanol, 80-120 ℃ of dry 6-24h obtained the target catalyst.
Method 2: mechanical mixing
Employing method one is prepared pure CeO
2, Fe
2O
3And ZrO
2Behind the powder, by predetermined molar ratio (CeO wherein
2Molar content be 50%, Fe
2O
3Molar content be 5%-50%, ZrO
2Molar content be 45%-0%, it is 100% that these three kinds of oxides add up to molar contents) with the CeO that obtains
2, Fe
2O
3And ZrO
2Powder mixes is even, behind the high speed ball milling 30-120min, obtains the target catalyst.
Utilize the cheaper raw material of price, adopt simple free of contamination preparation method, the material that makes is used to handle the diesel engine carbon black pollutant, and this material has the following advantages:
(1) do not use noble metal and alkali metal, and utilize the cheaper CeO of price
2, Fe
2O
3And ZrO
2, not only there is not secondary pollution, also given full play to the advantage of China rare earth resources big country, significantly reduced the cost of catalyst;
(2) Fe
2O
3Play unique catalytic action, itself and ZrO
2And CeO
2In conjunction with the material that obtains, catalytic activity is high, good stability;
(3) method for preparing catalyst is simple, is easy to industrialization;
(4) dependence of catalyst contrast table area is low, the material sintering that especially causes at high heat release environment, and then still can keep higher activity under the situation that causes specific surface to reduce;
(5) catalyst is the inorganic material with high stability, and moulding is simple, can process the integral catalyst of all size, high mechanical properties separately, is used for dissimilar diesel engines, and adaptive capacity is strong.
Description of drawings
Fig. 1 prepares the catalysis material process flow diagram for the co-precipitation hydrothermal synthesis method;
Fig. 2 prepares the catalysis material process flow diagram for mechanical mixing.
The specific embodiment
Further specify flesh and blood of the present invention with instance below, but content of the present invention is not limited to this.
Embodiment 1: mol ratio is that 5: 5 Ce, Fe nitrate is mixed with the solution that total concentration is 0.2mol/L, adds an amount of H again
2O
2, evenly mix.Speed with 3ml/min splashes into mixed solution in the ammoniacal liquor of 5mol/L, obtains sediment.Precipitate complete continued and stir 30min.Behind the aging 60min, the gained slurry is moved in the autoclave (compactedness is 65%) 200 ℃ of insulation 48h.Products therefrom washing, alcohol are washed, obtain the ferrocerium composite oxide catalysts after the drying.Initiation temperature (the T of the catalyst carbon-smoke combustion of preparation
i) be 257 ℃, summit temperature (T
p) be 324 ℃, the average selectivity of carbon dioxide is 98.6%.600 ℃ and 800 ℃ respectively behind the roasting 10h, T
iAnd T
pBe respectively 293 ℃ and 380 ℃, the average selectivity of carbon dioxide is 97.8%.
The nitrate of embodiment 2:Ce, Fe is mixed with the salting liquid that concentration is 0.25mol/L respectively, adds an amount of H again
2O
2, evenly mix.Speed with 5ml/min splashes into mixed solution in the ammoniacal liquor of 6M, obtains sediment.Precipitate complete continued and stir 60min.Behind the aging 60min, the gained slurry is moved in the autoclave (compactedness is 65%) 220 ℃ of insulation 48h.Products therefrom washing, alcohol are washed, obtain pure CeO after the drying
2And Fe
2O
3Powder.According to the mol ratio of Ce, Fe be 5: 5 with CeO
2And Fe
2O
3Mix, behind the high speed ball milling 30min, obtain the ferrocerium composite oxide catalysts.Initiation temperature (the T of the catalyst carbon-smoke combustion of preparation
i) be 273 ℃, summit temperature (T
p) be 323 ℃, the average selectivity of carbon dioxide is 98.9%.Behind 800 ℃ of roasting 20h, T
iAnd T
pBe respectively 277 ℃ and 369 ℃, the average selectivity of carbon dioxide is 98.8%.
Embodiment 3: mol ratio is that 0.5: 0.35: 0.15 Ce, Fe, Zr nitrate is mixed with the solution that total concentration is 0.25mol/L, adds an amount of H again
2O
2, evenly mix.Speed with 5ml/min splashes into mixed solution in the ammoniacal liquor of 5M, obtains sediment.Precipitate complete continued and stir 60min.Behind the aging 90min, the gained slurry is moved in the autoclave (compactedness is 60%) 220 ℃ of insulation 48h.Products therefrom washing, alcohol are washed, obtain ferrocerium zirconium mixed oxide catalyst after the drying.Initiation temperature (the T of the catalyst carbon-smoke combustion of preparation
i) be 257 ℃, summit temperature (T
p) be 318 ℃, the average selectivity of carbon dioxide is 99.8%.Behind 800 ℃ of roasting 20h, activity of such catalysts is still higher, T
iAnd T
pBe respectively 276 ℃ and 373 ℃, the average selectivity of carbon dioxide is 99.1%.
Embodiment 4: mol ratio is that 0.5: 0.10: 0.40 Ce, Fe, Zr nitrate is mixed with the solution that total concentration is 0.3mol/L, adds an amount of H again
2O
2, evenly mix.Speed with 4ml/min splashes into mixed solution in the ammoniacal liquor of 6mol/L, obtains sediment.Precipitate complete continued and stir 80min.Behind the aging 100min, the gained slurry is moved in the autoclave (compactedness is 65%) 220 ℃ of insulation 48h.Products therefrom washing, alcohol are washed, obtain ferrocerium zirconium mixed oxide catalyst after the drying.Initiation temperature (the T of the catalyst carbon-smoke combustion of preparation
i) be 267 ℃, summit temperature (T
p) be 321 ℃, the average selectivity of carbon dioxide is 98.9%.Behind 800 ℃ of roasting 20h, activity of such catalysts is still higher, T
iAnd T
pBe respectively 270 ℃ and 343 ℃, the average selectivity of carbon dioxide is 98.1%.
Claims (5)
1. low-temperature combustion catalyst that is used to eliminate diesel engine carbon black, it is characterized in that: composition is the composite oxides of ferrocerium zirconium, wherein CeO
2Molar content be 50%, Fe
2O
3Molar content be 5%-50%, ZrO
2Molar content be greater than 0 and smaller or equal to 45%, it is 100% that these three kinds of oxides add up to molar contents;
Said low-temperature combustion catalyst does not contain alkali metal and noble metal.
2. the preparation method who is used to eliminate the low-temperature combustion catalyst of diesel engine carbon black according to claim 1 is characterized in that: adopt the preparation of co-precipitation hydrothermal synthesis method, concrete steps are following:
(1) nitrate of getting Ce, Fe, Zr is example in molar ratio: CeO
2Molar content be 50%, Fe
2O
3Molar content be 5%-50%, ZrO
2Molar content be greater than 0 and smaller or equal to 45%, be mixed with the salting liquid that total concentration is 0.1-1mol/L, add an amount of H again
2O
2, fully stir, evenly mix;
(2) under vigorous stirring, the speed of above-mentioned mixed solution with 2-10mL/min is splashed in the ammoniacal liquor, obtain sediment;
(3) the complete continued of deposition stirs 30-120min;
(4) remove the part supernatant liquor behind the aging 30-180min, the gained sediment is moved in the autoclave, insulation 24-72h in the time of 160-240 ℃;
(5) after products therefrom washed respectively with deionized water and ethanol, 80-120 ℃ of dry 6-24h obtained the target catalyst.
3. Preparation of catalysts method according to claim 2 is characterized in that: the concentration of described ammoniacal liquor is 3-8mol/L, and the compactedness in the described autoclave is 50-70%.
4. low-temperature combustion catalyst that is used to eliminate diesel engine carbon black, it is characterized in that: do not contain alkali metal and noble metal, composition is the composite oxides of ferrocerium zirconium, wherein CeO
2Molar content be 50%, Fe
2O
3Molar content be 5%-50%, ZrO
2Molar content be greater than 0 and smaller or equal to 45%, it is 100% that these three kinds of oxides add up to molar contents, and adopts the mechanical mixing preparation, concrete steps are following:
(1) nitrate with Ce, Fe, Zr is mixed with the salting liquid that concentration is 0.1-1mol/L respectively, adds an amount of H again
2O
2, evenly mix;
(2) under vigorous stirring, the speed of above-mentioned mixed solution with 2-10mL/min is splashed in the ammoniacal liquor, obtain sediment; (3) the complete continued of deposition stirs 30-120min;
(4) remove the part supernatant liquor behind the aging 30-180min, the gained sediment is moved in the autoclave, insulation 24-72h in the time of 160-240 ℃; Products therefrom washing, alcohol are washed, obtain pure CeO after the drying
2, Fe
2O
3And ZrO
2Powder,
(5) by predetermined molar ratio (CeO wherein
2Molar content be 50%, Fe
2O
3Molar content be 5%-50%, ZrO
2Molar content be 45%-0%, it is 100% that these three kinds of oxides add up to molar contents) with the above-mentioned CeO that obtains
2, Fe
2O
3And ZrO
2Powder mixes is even, behind the high speed ball milling 30-120min, obtains the target catalyst.
5. a kind of low-temperature combustion catalyst that is used to eliminate diesel engine carbon black according to claim 4 is characterized in that: the concentration of described ammoniacal liquor is 3-8mol/L, and the compactedness in the described autoclave is 50-70%.
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|---|---|---|---|
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910163233A CN101767012B (en) | 2009-12-25 | 2009-12-25 | Low-temperature combustion catalyst for eliminating diesel engine carbon black |
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| CN101767012B true CN101767012B (en) | 2012-10-17 |
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| CN104549301B (en) * | 2013-10-13 | 2017-07-25 | 西北大学 | One kind has core shell structure Fe2O3@MFe2O4Synthetic method |
| CN104707623A (en) * | 2013-12-16 | 2015-06-17 | 裴振昭 | Method for preparing catalyst for catalytic combustion of methane |
| CN103977805A (en) * | 2014-05-20 | 2014-08-13 | 天津大学 | Catalyst for removing soot particles in tail gas of diesel vehicle, and preparation method thereof |
| CN106807385B (en) * | 2016-12-27 | 2019-05-14 | 中国科学院上海硅酸盐研究所 | A kind of soot combustion catalyst of nest like and its preparation method and application |
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|---|---|---|---|---|
| CN101479037A (en) * | 2006-07-12 | 2009-07-08 | 丰田自动车株式会社 | Exhaust gas purifying catalyst and its manufacturing method |
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