CN102125845A - Nano-quantum-dot-level fuel borne catalyst for diesel vehicle as well as preparation method and application thereof - Google Patents
Nano-quantum-dot-level fuel borne catalyst for diesel vehicle as well as preparation method and application thereof Download PDFInfo
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- CN102125845A CN102125845A CN 201010611602 CN201010611602A CN102125845A CN 102125845 A CN102125845 A CN 102125845A CN 201010611602 CN201010611602 CN 201010611602 CN 201010611602 A CN201010611602 A CN 201010611602A CN 102125845 A CN102125845 A CN 102125845A
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Abstract
The invention discloses a nano-quantum-dot-level fuel borne catalyst for a diesel vehicle as well as a preparation method and an application thereof, and the preparation method comprises the following steps: adding a trivalent cerium metal salt or a mixture of trivalent cerium and a trivalent iron metal salt into alcohol ether, and preparing a solution enabling the total concentration of cations to be 0.001-0.04mol/L; and adopting the two-section heating method to perform a heating reaction on the solution, firstly heating to 100 DEG C, condensing, refluxing till the solution is uniformly mixed, then heating to 160-200 DEG C, performing the reaction till the color of the solution changes, and finally getting a cerium oxide catalyst or a cerium-iron composite oxide catalyst. In the preparation method, pH does not need to be regulated, the reaction is performed at normal temperature and normal pressure, the reaction is simple and can be controlled through the temperature, the operation is convenient, the appearance of the catalyst can achieve 100%, the yield is high, and the catalyst can be applied in diesel engineering machinery, diesel trucks, diesel passenger vehicles, diesel urban buses and other tools in a large-scale manner.
Description
Technical field
The present invention relates to a kind of diesel vehicle Catalysts and its preparation method and application, be specifically related to a kind of diesel vehicle fuel addition type Catalysts and its preparation method and application that is used for the particle trap regeneration and the part nitrogen oxide is reduced, belong to diesel vehicle particle trap regeneration and catalyst technical field.
Background technology
Diesel engine is used widely with good dynamic property, economy and reliability.PM and NO
xBe two big pollutants of diesel emission.Present stage realizes that the main means of PM emission control are assembly wall streaming DPF(diesel particulate filters in blast pipe).DPF reaches the purpose of removal by the particulate in diffusion, deposition and the bump collection waste gas.But, must in time remove and impel its regeneration because the continuous deposition of PM on DPF constantly raises its back pressure.Utilize the regenerability that can improve DPF with the catalyst that PM closely contacts preferably.Directly adding FBC in fuel oil, periodically add FBC to cylinder or blast pipe spray, is a kind of PM of generation and the effective means that catalyst closely contacts, and can solve coated catalysts contacts defective tightness with PM problem.In the DPF catalytic regeneration, FBC can also impel NO
xBe reduced to nitrogen, reduce NO
xDischarging.
The most frequently used composition of FBC is metal (compound) oxides such as cerium and iron, but relevant relevant rarely seen report (the T. Campenon of synthetic method, P. Wouters, G. Blanchard, P. Macaudiere, T. Seguelong, SAE Tech. Paper, p. 2004-01-0071).Cerium oxide (CeO
2) be composition indispensable in the three-way catalyst, it mainly acts on and is: (1) is by oxidation state CeO
2With go back ortho states Ce
2O
3Between conversion, realized the storage and the release of oxygen; (2) disperse noble metal; (3) alumina support is played stabilization.As far back as late nineteen nineties, CeO
2Just be applied to the DPF catalytic regeneration.Facts have proved CeO
2Base FBC can limit the peak value of dpf regeneration heat release, can be from preventing that in essence DPF from because of the long-term too high mechanical breakdown that causes of temperature, prolonging the life-span of DPF.At CeO
2Middle doped F e can improve the dynamics of carbon-smoke combustion as promoter, has particularly reduced addition.Catalyst is blended into the contact performance that the quantum dot level can significantly improve catalyst and soot.Though done many work in the document, exist synthetic particle bigger, or the method complexity, or presoma price height, or can not suitability for industrialized production etc. shortcoming.
Synthetic method related to the present invention utilizes diglycol and slaine (acetate, alkoxide and halide) to prepare CeO
2And Fe
2O
3Nano particle (13:101), particle diameter does not prepare the ferrocerium composite oxides more than 30 nm for C. Peldmann, Adv. Funct. Mater. 2003.Synthetic method related to the present invention is utilized triethylene-glycol and ferric acetyl acetonade (Fe (acac)
3) prepared pure Fe
3O
4Nano particle (J. Colloid Interface Sci. 2007 305:366), does not prepare cerium oxide and ferrocerium composite oxides nano particle for W. Cai, J. Wan.Synthetic method related to the present invention utilizes polyethylene glycol and cerous nitrate to prepare pure CeO
2Nano particle (N. Uekawa, M. Ueta, Y. Wu, K. Kakegawa, Chem. Lett. 2002:854), particle diameter does not prepare ferrocerium composite oxides nano particle at 7 ~ 9 nm.
Summary of the invention
The present invention is directed to above deficiency, a kind of nano-quantum point level diesel vehicle fuel addition type Catalysts and its preparation method is provided, this method is not only applicable to the preparation of pure Ce oxide FBC, also is applicable to the preparation of Ce-Fe composite oxides FBC.This method is simple to operate, and raw material is easy to get, the catalyst particle size of gained below 5 nm, the yield height, stability is strong, under airtight condition, room temperature is placed the several months and precipitation can not occurred.
The present invention also provides the application of this nano-quantum point level fuel catalyst, catalyst is used for fuel tank, engine or blast pipe, can eliminate exhaust gas from diesel vehicle pollutes, promote particle PM(particulate matter) burning, make particle trap (diesel particulate filter, DPF) regeneration reduces the discharging of particle, and can be with part nitrogen oxide (NO
x) be reduced to nitrogen (about 10%).
The present invention is achieved by the following measures:
A kind of preparation method of nano-quantum point level fuel catalyst is characterized in that may further comprise the steps:
(1) with in trivalent cerium slaine or trivalent cerium and the ferric iron metal salt mixture adding alcohol ether, is made into the solution that the cation total concentration is 0.001 ~ 0.04 mol/L;
(2) adopt two sections temperature-raising methods that above-mentioned solution is added thermal response, at first be warming up to 100 ℃, condensing reflux to solution mixes, and is warming up to 160 ~ 200 ℃ then, reacts to solution changes color promptly to get cerium oxide catalyst or ferrocerium composite oxide catalysts.
Among the above-mentioned preparation method, described trivalent cerium slaine is cerous nitrate, cerous acetate or cerium chloride; Described ferric iron slaine is ferric nitrate, ferric acetate, iron chloride or ferric acetyl acetonade.
Further, the preferred following situation of used slaine: in the step (1), during trivalent cerium slaine wiring solution-forming, have the crystallization water in the used trivalent cerium slaine, during the common wiring solution-forming of trivalent cerium slaine and ferric iron slaine, at least a crystallization water that has in trivalent cerium slaine and the ferric iron slaine.
Among the above-mentioned preparation method, described alcohol ether is diglycol or triethylene-glycol.
Among the above-mentioned preparation method, in the gained ferrocerium composite oxide catalysts, the atomic ratio of Fe/ (Ce+Fe) is between 1 ~ 30 %.
Among the above-mentioned preparation method, in the step (2), when only containing cerium ion in the solution, reactant liquor gets the cerium oxide catalyst when faint yellow by colourless becoming, when containing cerium ion and iron ion simultaneously in the solution, reactant liquor is by the faint yellow ferrocerium composite oxide catalysts that gets when becoming yellowish-brown.
Among the above-mentioned preparation method, the particle diameter of gained catalyst is below 5 nm.
Among the above-mentioned preparation method, during two sections temperature-raising methods, the 30 min times of insulation reaction in the time of 100 ℃ are then at 160 ~ 200 ℃ of following condensing reflux 30 ~ 90 min.
This nano-quantum point level fuel catalyst can be added in fuel tank, engine or the blast pipe, is used to eliminate exhaust gas from diesel vehicle and pollutes, promotes particle PM burning and dpf regeneration, and the part nitrogen oxide is reduced to nitrogen.
Preparation method of the present invention has utilized the intersolubility of slaine and alcohol ether, and precipitation and thermal decomposition by slaine obtain nano particle.Because nano particle is wrapped up by organic solvent and protects, be difficult for behind their forming cores assembling and growing up, therefore can obtain stabilized nano particle,colloid solution.Alcohol ether is simultaneously as solvent, stabilizing agent, reducing agent and protective agent in the course of reaction; the stabilizing agent, reducing agent and the protective agent that do not add other; and also may bring water in the raw material that adds in the course of reaction; water also can dissolve each other with slaine, alcohol ether; the growing amount and the particle diameter of all right conditioned reaction product increase the productive rate of product.The present invention adopts two sections temperature-raising methods to add thermal response, beginning is fully to dissolve evenly for the water that allows inorganic metal salt, alcohol ether solvents and may exist at 100 ℃ of insulation certain hours, thereby the particle diameter that makes follow-up generation is unlikely to excessive, and continuing to be heated to 160 ~ 200 ℃ is in order to allow metal salt precipitate, decomposition and reduction.In this process, can observe solution and become faint yellow by colourless (Ce) or become yellowish-brown by faint yellow (Ce-Fe), illustrate that product generates.
The present invention has following advantage:
(1) as precursor, the raw material selectivity is more, and raw material is easy to get with slaine in reaction.
(2) utilize alcohol ether simultaneously as stabilizing agent, reducing agent and protective agent, use common vessel and conventional synthesis device, need not to regulate pH, reaction is carried out at normal temperatures and pressures, and reaction is simple, can control by temperature, and is easy to operate.
(3) the metal oxide nano quantum dot catalyst pattern of gained can reach 100 %, the productive rate height.
(4) catalyst particle size of gained is less than 5 nm, and available bases (as ammoniacal liquor), alcohol (as ethanol) and water sedimentation are got off, and specific area is up to 303 m
2/ g, and can be distributed to once more in organic solvent and the water, therefore catalyst precipitation can be got off to transport preservation, disperse again in use to get final product, easy to use.
(5) this quantum dot level catalyst can be applied to diesel oil engineering machinery, diesel trucks, diesel oil passenger vehicle, diesel oil Light-duty Vehicle, diesel-powered car, diesel oil city bus etc. on a large scale, has promotion and application widely and is worth.
Description of drawings
Fig. 1 is the XRD spectra of the embodiment of the invention 1 gained catalyst.
Fig. 2 is the HR-TEM photo of the embodiment of the invention 1 gained catalyst.
Fig. 3 is the XRD spectra of the embodiment of the invention 2 gained catalyst.
Fig. 4 is the TEM photo of the embodiment of the invention 2 gained catalyst.
Fig. 5 is the O of the embodiment of the invention 3
2The temperature programmed oxidation spectrum.
Fig. 6 is the NO/O of the embodiment of the invention 3
2The temperature programmed oxidation spectrum.
Fig. 7 is the O of the embodiment of the invention 12
2The temperature programmed oxidation spectrum.
The specific embodiment
The present invention will be further elaborated below in conjunction with specific embodiment, should be understood that, following explanation only is in order to explain the present invention, its content not to be limited.
Embodiment 1
Take by weighing 0.868 g Ce (NO
3)
36H
2The O adding fills in the three-neck flask of 50 mL triethylene-glycols, is 100 ℃ of following condensing reflux 30 min in temperature, continues to be warming up to 160 ℃ and condensing reflux 30 min, obtains the following quantum stage CeO of 5 nm
2Colloid.
Embodiment 2
Take by weighing 0.7812 g Ce (NO
3)
36H
2O and 0.0808 g Fe (NO
3)
39H
2The O adding fills in the three-neck flask of 50 mL triethylene-glycols, in temperature is 100 ℃ of following condensing reflux 30 min, continue to be warming up to 200 ℃ and remain on condensing reflux 90 min under this temperature, obtain the following ferrocerium composite oxides colloid of 5 nm, wherein the atomic ratio of Fe/ (Ce+Fe) is 10%.
Embodiment 3
Adopt deposition-precipitation method, with CeO
2Deposit on the soot, to reach the effect that soot and catalyst closely contact, wherein the ratio of soot and catalyst is 1:9.Specific practice is that 0.0396 g soot is joined 50 mLCeO
2In the colloid, ultrasonic dispersion 30 min mix, and the ratio according to 1:1:1.5 adds absolute ethyl alcohol and ammoniacal liquor in this mixture then, and with centrifugal 60 min of 9000 r/min, gained is deposited in 80 ℃ of vacuum drying 24 h in the vacuum drying chamber, obtains CeO
2The sample that closely contacts with soot.
O
2The temperature programmed oxidation test is carried out on fixed bed reactors.With silica wool with 50 mg CeO
2Be encapsulated in the crystal reaction tube with the soot sample, in the He of 50 mL/min gas, be warming up to 200 ℃, preliminary treatment 30 min.After reducing to room temperature, switch to the reaction gas of 200 mL/min, wherein O
2Concentration is 5 vol.%, and balance gas is He gas.Speed with 2 ℃/min is warming up to 550 ℃, product C O and CO in the gas-chromatography monitoring tail gas
2
NO/O
2The temperature programmed oxidation test is carried out on fixed bed reactors.With silica wool with 50 mg CeO
2Be encapsulated in the crystal reaction tube with the soot sample, in the He of 50 mL/min gas, be warming up to 200 ℃, preliminary treatment 30 min.After reducing to room temperature, switch to the reaction gas of 200 mL/min, wherein O
2Concentration is 5 vol.%, and NO concentration is 500 ppm, and balance gas is He gas.Speed with 2 ℃/min is warming up to 550 ℃, with product C O and the CO in the gas-chromatography monitoring tail gas
2, use NO
xAnalyzer monitoring NO and NO
2, the result as illustrated in Figures 5 and 6.As can be seen from the figure, use the temperature of catalyst reaction to shift to an earlier date, the peak temperature drop is low.
Embodiment 4
Take by weighing 0.1243 g Ce (Ac)
35H
2The O adding fills in the three-neck flask of 50 mL triethylene-glycols, is 100 ℃ of following condensing reflux 30 min in temperature, continues to be warming up to 180 ℃ and condensing reflux 60 min, obtains the following quantum stage CeO of 5 nm
2Colloid.
Embodiment 5
Take by weighing 0.0217 g Ce (NO
3)
36H
2O adds and to fill 50 mL one and contract in the Mitsui flask of two hexylene glycols, is 100 ℃ of following condensing reflux 30 min in temperature, continues to be warming up to 170 ℃ and 30 min that reflux, and obtains the following quantum dot level CeO of 5 nm
2Colloid.
Embodiment 6
Take by weighing 0.1304 g CeCl
37H
2O and 0.0530 g Fe (acac)
3Add and fill in the three-neck flask of 50 mL triethylene-glycols, in temperature is 100 ℃ of following condensing reflux 30 min, continue to be warming up to 180 ℃ and remain on condensing reflux 70 min under this temperature, obtain the following ferrocerium composite oxides colloid of 5 nm, wherein the atomic ratio of Fe/ (Ce+Fe) is 30%.
Embodiment 7
Take by weighing 0.4471 g CeCl
37H
2O and 0.0811 g FeCl
36H
2The O adding fills in the three-neck flask of 50 mL diglycols, in temperature is 100 ℃ of following condensing reflux 30 min, continue to be warming up to 170 ℃ and remain on condensing reflux 80 min under this temperature, obtain the following ferrocerium composite oxides colloid of 5 nm, wherein the atomic ratio of Fe/ (Ce+Fe) is 20%.
Embodiment 8
Take by weighing 0.4923 g Ce (Ac)
35H
2O and 0.0040 g Fe (NO
3)
39H
2The O adding fills in the three-neck flask of 50 mL diglycols, in temperature is 100 ℃ of following condensing reflux 30 min, continue to be warming up to 190 ℃ and remain on condensing reflux 60 min under this temperature, obtain the following ferrocerium composite oxides colloid of 5 nm, wherein the atomic ratio of Fe/ (Ce+Fe) is 1%.
Embodiment 9
Raw materials used and method is with embodiment 6, and different is, adds the ratio difference of ferrocerium, and the atomic ratio that obtains Fe/ (Ce+Fe) at last is 25%.
Embodiment 10
Raw materials used and method is with embodiment 7, and different is, adds the ratio difference of ferrocerium, and the atomic ratio that obtains Fe/ (Ce+Fe) at last is 15%.
Embodiment 11
Raw materials used and method is with embodiment 8, and different is, adds the ratio difference of ferrocerium, and the atomic ratio that obtains Fe/ (Ce+Fe) at last is 5%.
Embodiment 12
Adopt deposition-precipitation method, the Ce-Fe composite oxides are deposited on the soot, to reach the effect that soot and catalyst closely contact, wherein the ratio of soot and catalyst is 1:9.Specific practice is, 0.0396 g soot is joined in the 50 mLCe-Fe composite oxides colloids, ultrasonic dispersion 30 min mix, ratio according to 1:1:1.5 adds absolute ethyl alcohol and ammoniacal liquor in this mixture then, with centrifugal 60 min of 9000 r/min, gained is deposited in 80 ℃ of vacuum drying 24 h in the vacuum drying chamber, obtains the sample that Ce-Fe composite oxides and soot closely contact.O
2Temperature programmed oxidation test and NO/O
2The temperature programmed oxidation test is carried out on fixed bed reactors, and experiment condition the results are shown in Figure 7 with embodiment 3.
Claims (9)
1. nano-quantum point level diesel vehicle fuel addition type Preparation of catalysts method is characterized in that may further comprise the steps:
(1) with in trivalent cerium slaine or trivalent cerium and the ferric iron metal salt mixture adding alcohol ether, is made into the solution that the cation total concentration is 0.001 ~ 0.04 mol/L;
(2) adopt two sections temperature-raising methods that above-mentioned solution is added thermal response, at first be warming up to 100 ℃, condensing reflux to solution mixes, and is warming up to 160 ~ 200 ℃ then, reacts to solution changes color promptly to get cerium oxide catalyst or ferrocerium composite oxide catalysts.
2. preparation method according to claim 1 is characterized in that: described trivalent cerium slaine is cerous nitrate, cerous acetate or cerium chloride; Described ferric iron slaine is ferric nitrate, ferric acetate, iron chloride or ferric acetyl acetonade.
3. preparation method according to claim 2, it is characterized in that: in the step (1), during trivalent cerium slaine wiring solution-forming, have the crystallization water in the used trivalent cerium slaine, during the common wiring solution-forming of trivalent cerium slaine and ferric iron slaine, at least a crystallization water that has in trivalent cerium slaine and the ferric iron slaine.
4. preparation method according to claim 1 is characterized in that: described alcohol ether is diglycol or triethylene-glycol.
5. preparation method according to claim 1 is characterized in that: in the gained ferrocerium composite oxide catalysts, the atomic ratio of Fe/ (Ce+Fe) is between 1 ~ 30 %.
6. preparation method according to claim 1, it is characterized in that: in the step (2), when only containing cerium ion in the solution, reactant liquor gets the cerium oxide catalyst when faint yellow by colourless becoming, when containing cerium ion and iron ion simultaneously in the solution, reactant liquor is by the faint yellow ferrocerium composite oxide catalysts that gets when becoming yellowish-brown.
7. according to each described preparation method among the claim 1-6, it is characterized in that: during two sections temperature-raising methods, the 30 min times of insulation reaction in the time of 100 ℃ are then at 160 ~ 200 ℃ of following condensing reflux 30 ~ 90 min.
8. nano-quantum point level diesel vehicle fuel addition type catalyst that adopts the described preparation method of claim 1 to make.
9. the described nano-quantum point level of claim 8 diesel vehicle fuel addition type Application of Catalyst.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479764A (en) * | 2014-11-06 | 2015-04-01 | 金景达(北京)环保热力科技有限公司 | Nonmetal nanometer quantum-dot composite additive and modified efficient environment-friendly methanol fuel thereof |
| CN113877586A (en) * | 2021-10-12 | 2022-01-04 | 淮阴师范学院 | Preparation method and application of morphology-controllable hierarchical cerium-iron bimetal composite oxide |
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| US20070287626A1 (en) * | 2003-12-09 | 2007-12-13 | William Jones | Process For The Preparation Of An Oxidic Catalyst Composition Comprising A Divalent And A Trivalent Metal |
| US20080280750A1 (en) * | 2007-05-09 | 2008-11-13 | Pao-Chu Liu | Catalysts for treating acid and halogen gases and production methods thereof |
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2010
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479764A (en) * | 2014-11-06 | 2015-04-01 | 金景达(北京)环保热力科技有限公司 | Nonmetal nanometer quantum-dot composite additive and modified efficient environment-friendly methanol fuel thereof |
| CN104479764B (en) * | 2014-11-06 | 2016-03-16 | 金景达(北京)环保热力科技有限公司 | A kind of non pinetallic nano quantum dot composite additive and modified high-efficient environmental-protective methanol fuel thereof |
| CN113877586A (en) * | 2021-10-12 | 2022-01-04 | 淮阴师范学院 | Preparation method and application of morphology-controllable hierarchical cerium-iron bimetal composite oxide |
| CN113877586B (en) * | 2021-10-12 | 2023-10-31 | 淮阴师范学院 | Preparation method and application of cerium-iron bimetallic composite oxide with hierarchical structure and controllable morphology |
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