CN105797706A - Cerium-lanthanum solid solution catalyst for purifying diesel vehicle exhaust particles and preparation method thereof - Google Patents
Cerium-lanthanum solid solution catalyst for purifying diesel vehicle exhaust particles and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a cerium-lanthanum solid solution catalyst for purifying diesel vehicle exhaust particles and a preparation method thereof, and belongs to the field of environmental protection. The cerium-lanthanum solid solution catalyst comprises cerium and lanthanum elements, wherein cerium and lanthanum exist in a cerium-lanthanum solid solution form with a cerium oxide fluorite cubic structure, and difference between mole percentage between cerium-lanthanum and lanthanum on the surface of the catalyst as well as mole percentage between cerium-lanthanum and lanthanum on the bulk of the catalyst is higher than 5%. Lanthanum can be enriched on the surface of a sample according to specific preparation methods and conditions due to different hydrolysis rates of cerium and lanthanum ions, so that oxygen fluidity of a carrier is increased, oxidation-reduction ability of the catalyst is improved, and catalytic oxidation and decomposition of carbonaceous particles are promoted. The cerium-lanthanum solid solution catalyst can be used as a carrier for carrying precious metals in order to form a load type metal catalyst, so that activity is further improved; the catalyst can be individually coated on porous ceramics or the catalyst can be coated on porous ceramics with precious metals in order to be used as an integral catalyst.
Description
Technical field
The present invention relates to diesel car tail gas refining technology, be specifically related to a kind of catalyst purified for Diesel exhaust particles extracts, particularly to a kind of diesel vehicle particle purifying catalyst based on cerium lanthanum solid solution and preparation method thereof, belong to field of environment protection.
Background technology
Diesel vehicle adopts Lean Burning Technique, has higher power, fuel economy and durability than gasoline car.And oxygen-enriched combusting inhibits the formation of CO and Hydrocarbon, decrease the content of pollutant in tail gas.It is worth pointing out that play the three-way catalyst of good result in tail-gas from gasoline automobiles purifies, nitrogen oxides in exhaust gas from diesel vehicle and particulate matter in cannot removing, restricting its wide variety of key factor, the purification techniques being therefore developed for exhaust gas from diesel vehicle is extremely urgent.
At present, people's complexion changed to PM2.5 what is said or talked about, the particulate matter of vehicular emission is one of its main precursor, wherein in exhaust gas from diesel vehicle, the content of particulate matter has exceeded 30～80 times than gasoline car, and therefore " trouble of cardiopulmonary " for solving urbanite are played important facilitation by development Diesel exhaust particles extracts purification techniques.
Particulate matter in exhaust gas from diesel vehicle is generally made up of three parts, i.e. soot, dissolved organic matter and sulfate, and wherein the ratio shared by various compositions is with the difference of engine type, technical merit, operating mode and oil property and difference to some extent.Diesel vehicle purification techniques specifically includes that oxidation catalyst and particulate filter, improve the catalyst catalytic oxidation activity to soot and dissolved organic matter, reduce the ignition temperature of combustible in particulate matter, so that particulate filter can continuous operation for a long time, to improve particulate matter purification efficiency will play a key effect.
Due to particulate matter catalytic purification reaction be one gas-solid (particulate matter) solid-(catalyst) three-phase complexity deep oxidation process, therefore the raising of catalyst activity is not only closely related with the redox property of oxide catalyst itself, also relevant to the exposure level of solid catalyst Yu particulate matter.The catalyst of same active component, more strong with particulate matter engagement capacity, activity is more good.Although correlational study achieves good effect, but catalyst is adopted close contact and the loose way of contact all different from the way of contact of particulate matter with when generally evaluating oxidation catalyst in actual application, and the pattern being accurately controlled catalyst will improve the preparation cost of catalyst, and due to limited mechanical strength, in use procedure, pattern is also more easily damaged.It is to say, by the composition improving catalyst, remain one of important channel of raising oxidation catalyst particles thing clean-up effect.
Currently used Diesel exhaust particles extracts cleaning catalyst can be generally divided into three types, it may be assumed that perovskite type catalyst, noble metal catalyst and oxide catalyst, and wherein perovskite and oxide also can as the carriers of noble metal catalyst.Particle purifying catalyst belongs to oxidation catalyst, therefore has the cerio material, particularly cerium zirconium sosoloid that well store oxygen function and obtains good research.Cerium oxide lattice introduces zirconium and can improve the specific surface area of cerio material and anti-caking power, and more oxygen vacancies can be introduced, improve the oxidation activity of catalyst.But cerium and zirconium generally all exist with the form of 4 valencys in cerium zirconium sosoloid, and the amount of the oxygen vacancies of introducing is limited.If addition lanthanum, owing to it shows 3 valencys, it is possible to introduce more oxygen vacancies, cerio material is made to obtain better redox property.And much study and all point out, lanthanum is introduced cerium oxide lattice and can improve the noble metal dispersion ability of cerio material, make cerium lanthanum solid solution supported precious metal catalyst obtain better redox property.And, China is the country that rare earth resources is very abundant, and lanthanum, cerium are the compositions that in Rare Earth Mine, content is the abundantest, and cerium lanthanum solid solution directly can be prepared by not separated cerium lanthanum rare earth salt-mixture, also more environmental protection more economical compared to other cerio materials.Therefore, preparing a kind of catalyst based on cerium lanthanum solid solution, the performance improving current Diesel exhaust particles extracts cleaning catalyst further has feasibility and necessity.
Summary of the invention
Present invention is primarily targeted at offer a kind of for Diesel exhaust particles extracts cleaning catalyst, its redox property improves, and the particle purifying performance of catalyst is also improved.
A kind of Diesel exhaust particles extracts purifies with cerium lanthanum solid solution catalyst, including at least cerium (Ce) and two kinds of elements of lanthanum (La), wherein cerium and lanthanum exist with the cerium lanthanum solid solution thereof in cerium oxide fluorite cubic structure, and the molar percentage [La/ (Ce+La) of catalyst surface lanthanum and cerium and lanthanum, mol.%] with the difference of caltalyst phase lanthanum and cerium and the molar percentage [La/ (Ce+La), mol%] of lanthanum more than 5%.
The lattice structure of catalyst can be measured by x-ray powder diffraction instrument (XRD).The surface-element content of catalyst can be measured by X-ray photoelectron spectroscopic analysis (XPS), and the body phase constituent content of catalyst can be measured by inductively coupled plasma emission spectrography (ICP-AES).And in order to make testing result more accurate, it is possible to by the sample of Known Elements cellulose content as reference.
In the present invention based in the catalyst of cerium lanthanum solid solution, precious metal element can also be comprised, the introducing of noble metal can improve the activity of particle purifying catalyst significantly, and cerio material is the good carrier of noble metal, the noble metal carrier catalyst that therefore it is carrier with above-mentioned cerium lanthanum solid solution that the present invention also provides for.
One or more combination in described precious metal element selected from rhodium (Rh), platinum (Pt), palladium (Pd), iridium (Ir), ruthenium (Ru), gold (Au).Although under normal circumstances, the particle purifying effect of catalyst strengthens with the increase of bullion content, it is contemplated that noble metal is expensive, addition is unsuitable too high, therefore in described catalyst, the mass content of noble metal is 0～5wt.%, it is preferably 0.01～5wt.%, more preferably 0.5～1.5wt.%.
The doping of lanthanum is too low will not have the effect improving cerium lanthanum solid solution redox property, and La doped amount is too high by disruptive oxidation cerium fluorite cubic structure, solid solution can not be formed, therefore, molar percentage [the La/ (Ce+La) of described caltalyst middle lanthanum and cerium and lanthanum mutually, mol.%] it is 10～80%, it is preferred to 20～50%, more preferably 25～35%.
The preparation method that present invention also offers cerium lanthanum solid solution, wherein it is crucial that make lanthanum produce surface enrichment.In process prepared by cerium lanthanum solid solution, due to La3+And Ce3+Hydrolysis rate different, by controlling the addition of precipitant, it is possible to make La3+At cerium lanthanum solid solution surface enrichment.Find by studying, although the overall composition of catalyst and lattice structure will not be caused obvious change by this enrichment, but be able to improve significantly the redox property of catalyst, and then improve the particle purifying performance of catalyst.
The preparation method of a kind of Diesel exhaust particles extracts purification cerium lanthanum solid solution, including coprecipitation and homogeneous co-precipitation.
Described coprecipitation comprises the steps:
(1) the precursor salt of cerium and lanthanum being made into mixed solution, wherein lanthanum is 10～80% with the molar percentage [La/ (Ce+La), mol.%] of cerium and lanthanum；
(2) appropriate precipitant is added；
(3) precipitation separates after terminating, washing is precipitated thing；
(4) after precipitate being dried, roasting under certain sintering temperature, obtain cerium lanthanum solid solution.
In step (1), the presoma salt of described cerium and lanthanum, it is preferred to cerium and more than at least one or two combination in the carbonate after the chloride of lanthanum, nitrate, acidolysis, mixed rare earth chlorides；It is preferred that, the mixed rare earth chlorides of cerium and lanthanum, the i.e. mixture of not separated cerium chloride and lanthanum chloride in rare-earth smelting separation process.Molar percentage [the La/ (Ce+La) of lanthanum and cerium and lanthanum in Ce-La mixed rare earth chloride, mol.%] about 30%, it is exactly in preferred ratio range, and this material is cheap, a lot of Rare Earth Production producers can provide, wide material sources.Directly prepared cerium lanthanum solid solution catalyst by this thing, by than a lot of steps of reproduction after being mixed by cerium salt and lanthanum salt.
In step (2), described precipitant, it is preferably in sodium carbonate, potassium carbonate, sodium hydroxide, potassium hydroxide, ammonia combination more than at least one or two, wherein mol ratio [precipitant/(Ce+La) of precipitant and cerium and lanthanum, mol.%] it is 1.5～20, it is preferred to 5～20.
In step (4), owing to particulate matter catalytic oxidation typically requires higher temperature, described sintering temperature is preferably 400～800 DEG C；More preferably 650～750 DEG C.
Described homogeneous co-precipitation comprises the steps:
(1) the precursor salt of cerium and lanthanum being made into mixed solution, wherein lanthanum is 10～80% with the molar percentage [La/ (Ce+La), mol.%] of cerium and lanthanum；
(2) using appropriate carbamide as precipitant, under 80～95 DEG C of temperature conditions, reaction is to precipitation completely；
(3) precipitation separates after terminating, washing is precipitated thing；
(4) after precipitate being dried, roasting under certain sintering temperature, obtain cerium lanthanum solid solution.
In step (1), the presoma salt of described cerium and lanthanum, it is preferably in the carbonate after cerium and the chloride of lanthanum, nitrate, acidolysis, mixed rare earth chlorides combination more than at least one or two, it is preferred that the mixed rare earth chlorides of cerium and lanthanum, the i.e. mixture of not separated cerium chloride and lanthanum chloride in rare-earth smelting separation process.
In step (2), the mol ratio [Urea/ (Ce+La), mol.%] of carbamide and cerium and lanthanum is 4～25, it is preferred to 8～15, and the mode of heating in course of reaction can adopt microwave.
In step (4), described sintering temperature is preferably 400～800 DEG C；More preferably 650～750 DEG C.
Heretofore described cerium lanthanum solid solution is mainly characterized by lanthanum at surface enrichment, and this enrichment phenomenon when cerium lanthanum solid solution be used alone as catalyst, as carrier-supported precious metal after use, or be coated on various honeycomb ceramic carrier after slurrying and prepare when integral catalyst uses all exist and all can play a role.
When adopting cerium lanthanum solid solution as carrier, the carrying method of noble metal is infusion process, the sedimentation method, ion exchange.
Described infusion process needs to comprise the steps of
(1) by appropriate noble metal salt wiring solution-forming；
(2) appropriate cerium lanthanum solid solution be impregnated in appropriate precious metal salt solution；
(3) impregnate post-drying, roasting, obtain the cerium lanthanum solid solution of carried noble metal.
In step (1), described precious metal salt is preferably rhodium salt, palladium salt, platinum salt, ruthenium salt, iridium salt.Rhodium salt is preferably radium chloride；Palladium salt is preferably Palladous chloride., Palladous nitrate.；Platinum salt is preferably platinum chloride, platinum nitrate；Ruthenium salt is preferably ruthenic chloride；Iridium salt is preferably iridium chloride, chloro-iridic acid.
In step (3), described roasting is preferably roasting in 300～900 DEG C of air in Muffle furnace；Described roasting time is 1～24h, it is preferred to 2～12h, more preferably 4～6h；Sintering temperature is preferably 300～600 DEG C, more preferably 450～550 DEG C.
In the cerium lanthanum solid solution catalyst of the carried noble metal that said method obtains, the mass content of noble metal is 0～5wt.%, it is preferred to 0.01～5wt.%, more preferably 0.5～1.5wt.%.
Present invention have the advantage that
1) described cerium lanthanum solid solution catalyst has redox property more better than usual cerium lanthanum solid-solution material due to the lanthanum enrichment on surface, therefore also has higher diesel vehicle particulate matter tail gas clean-up activity.
2) method by reducing precipitant dosage, the cerium lanthanum solid solution preparing surface enrichment lanthanum that just can be very easy.
3) Ce-La mixed rare earth salt is adopted to be that precursor power cerium lanthanum solid solution economical and effective, method be simple and energy-conserving and environment-protective.
The catalyst that the present invention purifies for Diesel exhaust particles extracts, it includes at least cerium and two kinds of elements of lanthanum, and cerium and lanthanum are to exist with the solid solution thereof in cerium oxide fluorite cubic structure.Due to the difference of cerium and the hydrolysis rate of lanthanum ion, under specific preparation method and condition, lanthanum can be enriched with at sample surfaces, and increases the oxygen mobility of carrier, improves the redox property of catalyst, promotes that the catalytic oxidation of carbonaceous particle thing decomposes.This cerium lanthanum solid solution catalyst also as carrier, can support noble metal composition loaded noble metal catalyst, thus improving activity further, it is possible to individually or be together coated on porous ceramics with noble metal, uses as integer catalyzer.No matter how catalyst uses, and may benefit from the surface lanthanum enrichment relative to body phase lanthanum.
Detailed description of the invention
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art understand the present invention it will be clearly understood that described embodiment is only adapted to assist in, and are not construed as the concrete restriction to the present invention.
Embodiment 1
Ce-La mixed rare earth salt is dissolved in water, it is made into the solution of [La+Ce]=0.5mol/L, Ce-La mixed rare earth salt is the mixture of not separated cerium chloride and lanthanum chloride in rare-earth smelting separation process, wherein lanthanum is 36.2% with the molar percentage [La/ (Ce+La), mol.%] of cerium and lanthanum；Appropriate carbamide is added in this solution, making urea concentration in mixed liquor is 2.5mol/L, continuous stirring 12h under 90 DEG C of temperature conditions, then sucking filtration and washing, filter cake is put in baking oven and dry overnight in 110 DEG C, prepare powder through Muffle furnace roasting 5h in 700 DEG C of air after, be called catalyst A.
Embodiment 2
Other condition such as embodiment 1 is constant, and change urea concentration is 5mol/L, prepares catalyst B.
Embodiment 3
Other condition such as embodiment 1 is constant, and change urea concentration is 10mol/L, prepares catalyst C.
Embodiment 4
Take the catalyst C prepared in appropriate embodiment 1, add appropriate rhodium chloride solution, adopt infusion process to make the load type rhodium catalyst that load capacity is 1wt.%.Product after load is put in baking oven and dry overnight in 110 DEG C, after, prepare powder catalyst D through Muffle furnace roasting 3h in 700 DEG C of air.
Embodiment 5
0.07mol cerous nitrate and 0.03mol Lanthanum (III) nitrate are dissolved in 200mL water, it is made into the solution of [La+Ce]=0.5mol/L, 30g carbamide is added in this solution, continuous stirring 24h under 90 DEG C of temperature conditions, then sucking filtration and washing, filter cake is put in baking oven and dry overnight in 110 DEG C, prepare powder through Muffle furnace roasting 5h in 700 DEG C of air after, be called catalyst E.
Embodiment 6
Other condition such as embodiment 1 is constant, and changing carbamide dosage is 60g, prepares catalyst F.
Embodiment 7
0.07mol cerous nitrate and 0.03mol Lanthanum (III) nitrate are dissolved in 200mL water, it is made into the solution of [La+Ce]=0.5mol/L, 60g carbamide is added in this solution, adopt the mode of microwave heating, make reaction mixture keep 12h continuous stirring under 90 DEG C of temperature conditions, then sucking filtration and washing, filter cake is put in baking oven and dry overnight in 110 DEG C, prepare powder through Muffle furnace roasting 5h in 700 DEG C of air after, be called catalyst G.
Embodiment 8
Embodiment 1-7 is prepared catalyst and carries out XPS and ICP test, and calculate surface and body phase lanthanum content [La/ (La+Ce) respectively, mol%] content, and adopt thermogravimetric analyzer that the particle purifying activity of catalyst is evaluated, particulate matter model carbon Degussa (Printex-U) is simulated, and the mass ratio of catalyst and particulate matter is 1:4, and heating rate is 2 DEG C/min, close contact, result is as shown in table 1.Wherein T50The temperature of 50wt.% is reached for Removal efficiency of particulate matter.
Table 1 catalyst activity evaluation result
| Catalyst | T50 | Surface [La/ (Ce+La), mol.%] | Body phase [La/Ce+La, mol.%] |
| A | 438 | 36.8% | 34.3% |
| B | 416 | 42.2% | 35.1% |
| C | 408 | 50.3% | 35.8% |
| D | 352 | 50.1% | 36.1% |
| E | 424 | 34.3% | 28.8% |
| F | 398 | 45.3% | 29.6% |
| G | 404 | 42.7% | 29.5% |
As shown in Table 1, the T of catalyst C, F, G that lanthanum enrichment degree in surface is high50A, E catalyst low significantly lower than surface lanthanum enrichment degree, illustrates that the effect of its particle purifying is better.By the activity contrast of catalyst A, D it will be seen that after catalyst surface carried noble metal, the activity of catalyst significantly improves.
Applicant states, the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment, but the invention is not limited in above-mentioned detailed process equipment and technological process, namely do not mean that the present invention has to rely on above-mentioned detailed process equipment and technological process could be implemented.The equivalence of each raw material of product of the present invention, it will be clearly understood that any improvement in the present invention, is replaced and the interpolation of auxiliary element, concrete way choice etc. by person of ordinary skill in the field, all falls within protection scope of the present invention and open scope.
Claims (10)
1. a Diesel exhaust particles extracts purifies with cerium lanthanum solid solution catalyst, it is characterized in that: comprise cerium and two kinds of elements of lanthanum, wherein cerium and lanthanum exist with the cerium lanthanum solid solution thereof in cerium oxide fluorite cubic structure, and the difference of the molar percentage of catalyst surface lanthanum and cerium and lanthanum and caltalyst phase lanthanum and cerium and the molar percentage of lanthanum is more than 5%.
2. Diesel exhaust particles extracts purification cerium lanthanum solid solution catalyst according to claim 1, it is characterised in that: in described catalyst, also comprise precious metal element.
3. Diesel exhaust particles extracts purification cerium lanthanum solid solution catalyst according to claim 2, it is characterised in that: one or more the combination in described precious metal element selected from rhodium, platinum, palladium, iridium, ruthenium and gold；In described catalyst, the mass content of noble metal is 0～5wt.%.
4. Diesel exhaust particles extracts purification cerium lanthanum solid solution catalyst according to claim 1, it is characterised in that: described caltalyst mutually in, the molar percentage of lanthanum and cerium and lanthanum is 10～80%.
5. a Diesel exhaust particles extracts purifies by the preparation method of cerium lanthanum solid solution catalyst, it is characterised in that adopts coprecipitation to prepare, comprises the steps:
(1) the precursor salt of cerium and lanthanum being made into mixed solution, wherein lanthanum is 10～80% with the molar percentage of cerium and lanthanum；The presoma salt of described cerium and lanthanum is the carbonate after cerium and the chloride of lanthanum, nitrate, acidolysis and one or more the combination in mixed rare earth chlorides；
(2) adding precipitant, described precipitant is one or more the combination in sodium carbonate, potassium carbonate, sodium hydroxide, potassium hydroxide and ammonia；Wherein precipitant is 1.5～20 with the mol ratio [precipitant/(Ce+La), mol.%] of cerium and lanthanum；
(3) precipitation separates after terminating, washing is precipitated thing；
(4), after being dried by precipitate, roasting, sintering temperature is 400～800 DEG C, obtains cerium lanthanum solid solution.
6. a Diesel exhaust particles extracts purifies by the preparation method of cerium lanthanum solid solution catalyst, it is characterised in that adopts homogeneous co-precipitation to prepare, comprises the steps:
(1) the precursor salt of cerium and lanthanum being made into mixed solution, wherein lanthanum is 10～80% with the molar percentage of cerium and lanthanum；The presoma salt of described cerium and lanthanum is the carbonate after cerium and the chloride of lanthanum, nitrate, acidolysis and one or more the combination in mixed rare earth chlorides；
(2) using carbamide as precipitant, the mol ratio [Urea/ (Ce+La), mol.%] of carbamide and cerium and lanthanum is 4～25；Under 80～95 DEG C of temperature conditions, reaction is to precipitation completely；Mode of heating can be selected for conduction of heat or microwave；
(3) precipitation separates after terminating, washing is precipitated thing；
(4), after being dried by precipitate, roasting, sintering temperature is 400～800 DEG C, obtains cerium lanthanum solid solution.
7. the preparation method of cerium lanthanum solid solution catalyst of the Diesel exhaust particles extracts purification according to claim 5 or 6, it is characterized in that: the cerium lanthanum solid solution obtained is as carrier-supported precious metal, or is coated on honeycomb ceramic carrier after slurrying and prepares integral catalyst.
8. the preparation method of Diesel exhaust particles extracts purification cerium lanthanum solid solution catalyst according to claim 7, it is characterised in that: cerium lanthanum solid solution is infusion process, the sedimentation method or ion exchange as the method for carrier-supported precious metal.
9. the preparation method of Diesel exhaust particles extracts purification cerium lanthanum solid solution catalyst according to claim 8, it is characterised in that described infusion process comprises the steps of
(1) by noble metal salt wiring solution-forming, described precious metal salt is rhodium salt, palladium salt, platinum salt, ruthenium salt and/or iridium salt；
(2) cerium lanthanum solid solution be impregnated in precious metal salt solution；
(3) impregnate post-drying, roasting, obtain the cerium lanthanum solid solution of carried noble metal.
10. the preparation method of Diesel exhaust particles extracts purification cerium lanthanum solid solution catalyst according to claim 9, it is characterised in that: in the cerium lanthanum solid solution of described carried noble metal, the mass content of noble metal is 0～5wt.%.
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| CN110721682A (en) * | 2019-10-23 | 2020-01-24 | 华北电力大学（保定） | Novel anti-aging automobile exhaust catalyst |
| CN112121784A (en) * | 2020-09-29 | 2020-12-25 | 广东石油化工学院 | Potassium cerium lanthanum composite oxide catalyst, preparation method and application thereof |
| WO2021241841A1 (en) * | 2020-05-28 | 2021-12-02 | 한국화학연구원 | Ammonia cracking catalyst, and method of cracking ammonia and generating hydrogen by using same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110721682A (en) * | 2019-10-23 | 2020-01-24 | 华北电力大学（保定） | Novel anti-aging automobile exhaust catalyst |
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| CN113996293A (en) * | 2021-11-23 | 2022-02-01 | 有研工程技术研究院有限公司 | Cerium-lanthanum solid solution supported iridium catalyst, and preparation method and application thereof |
| CN113996293B (en) * | 2021-11-23 | 2024-04-16 | 有研工程技术研究院有限公司 | Cerium lanthanum solid solution supported iridium catalyst, preparation method and application thereof |
| CN115069242A (en) * | 2022-05-05 | 2022-09-20 | 有研工程技术研究院有限公司 | Catalyst for hydrogen production by oxidation and reforming of ethanol and preparation and activation methods thereof |
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