CN108561211B - It is a kind of with low back pressure, the DPF of low light-off temperature Catalytic Layer and its preparation process - Google Patents

It is a kind of with low back pressure, the DPF of low light-off temperature Catalytic Layer and its preparation process Download PDF

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CN108561211B
CN108561211B CN201810362151.XA CN201810362151A CN108561211B CN 108561211 B CN108561211 B CN 108561211B CN 201810362151 A CN201810362151 A CN 201810362151A CN 108561211 B CN108561211 B CN 108561211B
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dpf
back pressure
glue
preparation process
low
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CN108561211A (en
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魏宽
王云
王瑞芳
杨娅
吴干学
冯锡
张艳华
李云
陈启章
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Sinocat Environmental Technology Co Ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
    • F01N3/033—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices
    • F01N3/035—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices with catalytic reactors, e.g. catalysed diesel particulate filters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/0001—Making filtering elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/66—Regeneration of the filtering material or filter elements inside the filter
    • B01D46/80—Chemical processes for the removal of the retained particles, e.g. by burning
    • B01D46/82—Chemical processes for the removal of the retained particles, e.g. by burning with catalysts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/9404—Removing only nitrogen compounds
    • B01D53/9409—Nitrogen oxides
    • B01D53/9413—Processes characterised by a specific catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44—Palladium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0234—Impregnation and coating simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/10—Noble metals or compounds thereof
    • B01D2255/102—Platinum group metals
    • B01D2255/1021—Platinum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/10—Noble metals or compounds thereof
    • B01D2255/102—Platinum group metals
    • B01D2255/1023—Palladium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/206—Rare earth metals
    • B01D2255/2065—Cerium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20715—Zirconium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/209—Other metals
    • B01D2255/2092—Aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/01—Engine exhaust gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/01—Engine exhaust gases
    • B01D2258/012—Diesel engines and lean burn gasoline engines

Abstract

The invention discloses a kind of PM, PN particulate matters for trapping, purifying, in low-temperature catalytic oxidation exhaust gas from diesel vehicle, and DPF and its preparation process with low back pressure Catalytic Layer.Including aluminum soluble salt or aluminium oxide to be added in water-alcohol solvent system, slurries A is obtained by high-energy ball milling；Ionic mixed solution is made in the soluble-salt of cerium, zirconium, is added in slurries A, agitated that slurries B is made, slurries B ageing simultaneously carries out high-energy ultrasonic oscillation simultaneously, forms the glue C with gel particles；Then impregnation technology is used, glue C is impregnated on wall-flow type DPF air inlet wall surface and in wall inner pore, blowback is finally carried out using air-flow, dispose extra glue C, after drying, by active precious metal ion solution by way of aerosol sprays, it is impregnated into the DPF with coat after drying, obtaining one kind through drying, roasting again has low-temperature catalytic oxidation PM, PN, and the diesel particulate trap with low back pressure feature.

Description

It is a kind of with low back pressure, the DPF of low light-off temperature Catalytic Layer and its preparation process
Technical field
The invention belongs to catalyst research preparation technical fields, especially belong to the preparation of motor-driven vehicle gas disposal catalyst research Technical field, in particular to it is a kind of with low back pressure, the DPF of low light-off temperature Catalytic Layer and its preparation process.
Background technique
Diesel engine has the thermal efficiency high, and the remarkable advantage of good economy performance can generate a large amount of soot under lean burn conditions Grain, i.e., so-called soot particulate (Particulate Matter, referred to as: PM), and its a large amount of PN (Particulate Number, abbreviation PN), serious harm is caused to the health of the mankind, serious damage especially will cause to human respiratory and lung Wound, therefore with the continuous development of car industry, the reinforcement of people's environmental consciousness, PM and PN of the national legislation to motor vehicle exhaust emission Also it is made that stringent restriction.
In order to realize to PM, especially enormous amount, and its size reaches nanoscale PN particle, using flow honeycomb filter Device, for diesel vehicle, then using DPF (diesel particle filter) diesel particulate filter, as representative, realization is caught Collection and purification function, it is desirable that capture rate reaches 99% or more, purifies to it, that is to say, that is catalyzed the PM trapped and PN Oxidation, mainly passes through NO2And/or O2In the case where auxiliary, realize that PM and PN is converted into CO2, the final circulation for realizing DPF Trapping.
For all heavy goods vehicles, because its engine Raw exhaust temperature is higher relative to Light-duty Vehicle, usually with NO2It is auxiliary It helps based on regeneration, reacts: PM/PN+NO2→CO2+ NO realizes that the catalysis oxidation of PM and PN, temperature requirement range are usual In 200 DEG C~450 DEG C, by reducing the initiation temperature of PM/PN, its transformation efficiency is improved, on the one hand increases to improve and start The efficiency of combustion of machine and the economy of fuel oil, on the other hand due to needing a large amount of NO2, therefore filtered in catalytic type diesel particulate The surface device (Catalytic Diesel Particulate Filter, abbreviation CDPF) can generate a large amount of NO in situ2, for It is regenerated；And for the medium and heavy vehicle of all Light-duty Vehicles and part, mainly rely on O2It assists, realizes PM and PN Regeneration, i.e., so-called initiative regeneration, react PM/PN+O2→CO2, 450 DEG C~650 DEG C of typical temperature claimed range.
It is required that improving DPF trapping, the capture rate for requiring DPF that there is good PM and PN that is to say, that is, require to improve The porosity of DPF reduces pore-size, while improving DPF to the limit carbon carrying capacity of PM and PN, but this increases the back pressure of DPF Added with directly affecting, the deterioration of engine fuel efficiency of combustion is eventually led to, in turn, and increases the discharge of PM and PN.
In order to which while improving the capture rate of PM and PN, the back pressure that reduction air-flow generates as far as possible fires engine fuel The influence of efficiency degradation is burnt, one layer of filter layer of coating in hole path surface and wall inner pore on the one hand is entered to DPF, improves soot Capture rate, the catalysis oxidation for accelerating PM and PN is on the other hand required, therefore it is required that having good catalysis oxidation PM and PN and low The DPF of back pressure Catalytic Layer, i.e. catalytic type diesel particulate filter (catalytic Diesel Particle Filter, referred to as CDPF), wherein catalytic efficiency and its structural stability to filter layer require height.
United States Patent (USP) 9517454B2 discloses a kind of diesel particulate trap, it is mentioned that on DPF air flow inlet channel surface One layer of porous coating with bridged-style is formed, is mainly characterized by forming collosol and gel in terms of the preparation of coating material Particle, this is beneficial to slurry on DPF entrance wall surface, realize uniformly coating, entirely post-processing operational process in, will have Conducive to back pressure reduction, major defect be it is inadequate to the catalysis oxidation ability of PM and PN and its ability resistant to high temperature, structure it is steady It is qualitative have it is to be strengthened.
A kind of band coating diesel particulate filter is disclosed in United States Patent (USP) 9346019B2 etc., contains oxidized form in coating Catalytic activity, and precious metals pt is subjected to region coating, sufficiently to realize active noble metals Pt to the catalysis oxidation of PM and PN Function, but be not very well that is, when vehicle exhaust air-flow passes through DPF, high back pressure easy to form is led in terms of the control of back pressure Engine is caused to deteriorate the efficiency of combustion of fuel oil.
In diesel exhaust after-treatment system, to realize the good trapping filter efficiency to PM and PN, at the same guarantee PM and PN realizes good power of regeneration, then, on the one hand require DPF itself to have good arresting efficiency, it is on the other hand then more Requirement be that its back pressure wants low, have good low temperature ignition performance to PM and PN, coating can resist the height generated during regeneration Temperature influences the deterioration of catalytic performance.
Summary of the invention
The present invention is insufficient according to prior art to be disclosed with low back pressure, the DPF of low light-off temperature Catalytic Layer and its system Standby technique.It is an object of the present invention to provide a kind of DPF with low back pressure coating filter layer, are a kind of steady with low back pressure, structure Fixed and low-temperature catalytic oxidation PM and PN diesel particulate filter；DPF prepared by the present invention is applied in exhaust gas from diesel vehicle processing, PN ultrafine to the particle size and PM of larger particle size has good trapping ability, in NO2And/or O2Auxiliary Under, it is able to achieve the good catalysis oxidation of PN and PM, the final regeneration for realizing DPF, DPF preparation process is easy to control, Yi Shixian Industrialized production.
The invention is realized by the following technical scheme:
It is a kind of with low back pressure, the DPF preparation process of low light-off temperature Catalytic Layer, comprising the following steps:
1) preparation of coat glue, by containing aluminium oxide or aluminum soluble salt be added in water-alcohol solvent system, with Aluminum oxide weight note, concentration in a solvent are 10-30wt%, and the concentration of alcohol is 1.0~50.0wt% in solvent, soluble The concentration of acid is 0.1~1.0wt%, at normal temperature high-energy ball milling 20min~120min, obtains slurries A；Then by cerous nitrate, Zirconium nitrate is pre-mixed to form ionic soln according to molar ratio Ce:Zr=1:1~6:1, is added in slurries A, with cerium oxide and The zirconium oxide weight note total butt coated weight ratio of Zhan is 10~50wt%, 30~180min of electromagnetic agitation, forms slurries B, adjustment Solid content is 15~20wt%；Under the conditions of 30~80 DEG C of temperature, to slurries B ageing 12~for 24 hours, while high-energy ultrasonic vibration is carried out It swings, forms glue C；
2) glue coats, and by glue C by grouting immersion coating, deposits it into wall-flow diesel particulate filter air inlet In end wall surface and in wall inner pore, and blowback being carried out with compressed air stream, air-flow enters from outlet side, extra glue C is disposed, Then it is dried；
3) active noble metals particle impregnates, and using aerosolization spray immersion, the solution of the ion containing active noble metals is passed through Air-flow, which is crushed, to nebulize, in the DPF that then spray immersion to step 2) obtains, air-dry it is dry, Muffle furnace roasting, obtain diesel oil Grain catcher DPF finished product.
The coating catalysis material is the composite oxides of aluminium oxide, cerium oxide or/and zirconium oxide.
The alcohols is the mixing of one or more of methanol, ethyl alcohol, glycerine, polyethylene glycol, propyl alcohol or isopropanol Object.
The soluble acids are the mixtures of one or more of formic acid, citric acid, nitric acid, acetic acid.
The aerosolization spray immersion is compressed air pressure >=3MPa, noble metal solution flow velocity≤1L/min, spray It penetrates direction and center line angle in duct is greater than 20 °.
The high-energy ball milling revolving speed is 500~2000r/min, time 20min~120min；The electromagnetic agitation revolving speed is 200~500r/min, time 30min~180min.
Step 3) the apoplexy is dry, roasting is dry 0.5h~3h in the hot wind for be placed in DPF 100 DEG C~150 DEG C, so Muffle furnace roasting, calcining time 2h~6h are carried out under the conditions of 450 DEG C~650 DEG C afterwards.
The DPF that the present invention prepares preparation process is applied in exhaust gas from diesel vehicle processing.
The present invention enables catalysis material sufficiently and evenly to deposit to DPF inlet end table by improving pulping process Among face and inner duct, while coating porosity is higher, this is provided to reduce back pressure as far as possible, with traditional incipient impregnation Then noble metal is compared by ball milling pulping process, this technique state aspects such as slurry partial size needed for realizing reduce technique stream Journey, it is often more important that the slurry of the appropriate particle size needed for capable of obtaining, the uniformity of easily controllable coat realize that catalysis material exists Uniform coating in DPF.
By improving precious metal impregnation technique, meets using lower noble metal amount, realize noble metal It makes full use of, while noble metal being allowed to be distributed in the outside of catalysis material as much as possible, promoted urging containing noble metal in this way The PM/PN for changing coating and trapping is sufficiently physically contacted, and when the NO atmosphere of upstream transmitting, which enters CDPF, enters gas channel, noble metal is living Property particle is oxidized as NO2, to realize enough NO2Passive regeneration catalysis oxidation occurs with PM/PN, is passing through passive regeneration The NO generated after oxidation, and noble metal oxidation can be continued through, it realizes the NO oxidation process of circulation, on the one hand reduces gas The dissipation of heat in stream, on the other hand increases the rate of reaction, to realize under lower temperature in entire after-treatment system PM/PN ignition, increase passive regeneration generation frequency.
Helpfulness of the present invention:
By optimizing the gentle atomized spray infusion process technique of sol-gel method, DPF coat coating uniformity, drop are improved Low coat back pressure increases the stability and low-temperature catalytic oxidation performance of coating layer；
To glue needed for coat, by high-energy ball milling, after electromagnetic agitation and high-energy ultrasonic oscillation ageing, make its flowing Property it is good, grain diameter is moderate, and uniformly, phenomena such as no plug-hole, no holiday, no spray is grey occurs for final coating, for the low back of coat Pressure, stable hole coating structure lay the foundation.
Using aerosolization spray immersion method, dipping noble metal solution is carried out, simple process, at low cost, process can Control, noble metal are evenly distributed, and noble metal utilisation are improved, to obtain the property of excellent low-temperature catalytic oxidation PM and PN Energy；
Detailed description of the invention
Fig. 1 is CDPF of the present invention and traditional handicraft prepares the comparison of CDPF back pressure；In figure, abscissa indicates air speed, single Position wh-1；Ordinate indicates back pressure, unit kpa；PM loading capacity is 4.2g/L in experiment；1 to 4 is 1 to 4 point of the embodiment of the present invention The sample not prepared, 5 be the sample of traditional handicraft preparation.
Fig. 2 is CDPF of the present invention and traditional handicraft prepares CDPF initiation temperature and compares, and in figure, abscissa indicates various kinds Product, 1 to 4 is the sample that the embodiment of the present invention 1 to 4 is prepared respectively, and 5 be the sample of traditional handicraft preparation；Ordinate indicates ignition Temperature, unit DEG C.
Specific embodiment
The present invention is specifically described below by example, the present embodiment is served only for carrying out the present invention further Illustrate, but should not be understood as limiting the scope of the invention, those skilled in the art is according to the content of aforementioned present invention The some nonessential modifications and adaptations made also belong to the scope of protection of the invention.
Noble metal total amount 2.0g/ft in this example DPF3, white carrier used is the honeycomb ceramic carrier of cordierite.
DPF preparation process of the present invention includes the following steps:
1) aluminum soluble salt or aluminium oxide that require according to certain mass concentration are added to by the preparation of coat glue In water-alcohol solvent system, then the solvable of weight of solvent 0.1wt%~1wt% is added in mass ratio≤30% with dicyandiamide solution Property acid, after high-energy-milling, obtain slurries A；By cerium, zirconium soluble-salt according to certain molar ratio, formation from Subtype mixed solution is added in slurries A, by electromagnetic agitation, is formed slurries B, is then aged to slurries B, while into The oscillation of row high-energy ultrasonic, forms the glue C with gel particles.
2) glue coats: will be on glue C immersion coating to wall-flow diesel particulate filter DPF air inlet wall surface and in wall In hole, and blowback is carried out with compressed air stream, i.e. air-flow enters from outlet side, disposes extra glue C, is then done It is dry.
3) active noble metals particle impregnates, using aerosolization spray immersion method: active precious metal ion solution is led to Air-flow is crossed, is crushed and is nebulized, then spray immersion is into the DPF with coat after drying, finally through overdrying Dry, Muffle furnace roasting coats filter layer, and the diesel oil with good catalysis oxidation ability with low back pressure to get to a kind of Grain catcher.
The present invention coat catalysis material be alumina-ceria-zirconia composite oxides, mainly comprising aluminium oxide, Cerium oxide and zirconium oxide, compound phase composition may is that alumina-thoria, Ceria-zirconia, aluminium oxide-zirconium oxide, Alumina-ceria-zirconia etc., two kinds therein and its more than compound phase oxide.
Aluminum soluble salt or aluminium oxide of the present invention include oxide containing aluminium or the aluminium salt for dissolving in acid or alkali, the band crystallization water Aluminum oxide or hydrate and one of rare earth and alkali-earth metal modified aluminium oxide, with aluminium ion weight note, in solvent In concentration be 10-30wt%, be mainly characterized by and cerium and zirconium composition composite oxides, have high-ratio surface, high temperature resistant sintering Feature；For cerium zirconium material then mainly with having soluble cerium salt and soluble zirconates, cerous nitrate, nitric acid are specifically included that Zirconium, atomic molar ratio are as follows: Ce:Zr=1:1~6:1；After forming composite oxides, the total butt coating of cerium oxide, zirconium oxide Zhan Amount ratio, it is desirable that 10~50wt%.
Alcohols of the present invention includes the alcohols such as methanol, ethyl alcohol, glycerine, polyethylene glycol, propyl alcohol, isopropanol, includes at least it Middle one kind, dosage is in 1.0wt%~50.0wt%.
Acids of the present invention includes at least one of soluble acids of non-volatility, including formic acid, citric acid, nitric acid, acetic acid, Dosage is in 0.1wt%~1.0wt%.
High-energy-milling in sol-gel method of the present invention, revolving speed requirement 500~2000r/min, time 20min~ 120min。
Electromagnetic agitation technique in sol-gel method of the present invention, revolving speed requirement 200~500r/min, time 30min~ 180min。
Ageing process in sol-gel method of the present invention, it is desirable that the working frequency 20KHz of high-energy ultrasonic oscillation~ 100KHz, power is between 100W~500W, and temperature range is in 30 DEG C~80 DEG C, digestion time 12h~for 24 hours, and solid content is wanted It asks in 15wt%~20wt%.
Air-dried technique in dipping of the present invention-roasting method technique, it is desirable that the DPF for having coat is placed in 100 DEG C~150 DEG C Hot wind in dry 0.5h~3h.
Aerosolization spray immersion method of the present invention, it is desirable that compressed air pressure >=3MPa, noble metal solution flow velocity≤1L/ Min, injection direction and duct center line angle are greater than 20 °.
Aerosolization spray immersion method of the present invention air-dries dry, roasting technique requirement and is placed in 100 DEG C~150 DEG C of hot wind and does Then dry 0.5h~3h carries out Muffle furnace roasting, calcining time 2h~6h under the conditions of 450 DEG C~650 DEG C.
The present invention specifically prepares the DPF of following embodiment and is detected.
Embodiment 1
Coating slurry configuration, coating and noble metal impregnation technology:
1) boehmite: being added in deionized water by 20wt%, 0.1wt% citric acid be added by the configuration of glue, into Row high-energy ball milling, revolving speed requires 1000r/min, after about 60min, is added the mixed solution of cerous nitrate and zirconium nitrate, cerous nitrate and The molar ratio 4:1 of zirconium nitrate feeds intake, and then proceedes to electromagnetic agitation, stirring rate 200r/min, time about 30min, finally It is aged, high-energy ultrasonic oscillation, working frequency 50KHz, power is controlled in 100W, temperature at 50 DEG C, and solid content is adjusted to 15wt%, time 12h.
2) glue coats: the glue after ageing is dipped into being coated to wall-flow diesel particle filtering using infusion process On the air inlet wall surface of device and in wall inner pore, and blowback is carried out with compressed air stream, to dispose extra glue, then will had The DPF of coat is placed in 120 DEG C of air-heater dry 1h.
3) aerosolization spray immersion active noble metals particle: by active precious metal ion solution by air-flow, by it Broken to nebulize, then spray immersion is into the DPF with coat after roasting, it is desirable that compressed air pressure 4MPa, Noble metal solution flow velocity 0.5L/min, injection direction and duct centerlines are 30 °, mole of platinum nitrate and palladium nitrate Than=2:1.Then DPF is placed in the dry 1h of 120 DEG C of hot air drying machines, is finally placed in Muffle furnace, carries out roasting technique, temperature requirement 550 DEG C, time 4h.
Embodiment 2
Coating slurry configuration, coating and noble metal impregnation technology:
1) boehmite: being added in deionized water by 20wt%, 1.0wt% citric acid be added by the configuration of glue, into Row high-energy ball milling, revolving speed requires 1000r/min, after about 60min, is added the mixed solution of cerous nitrate and zirconium nitrate, cerous nitrate and The molar ratio 1:1 of zirconium nitrate feeds intake, and then proceedes to electromagnetic agitation, stirring rate 200r/min, time about 30min, finally Ripening is carried out, high-energy ultrasonic oscillation, working frequency 50KHz, power is in 100W, and at 50 DEG C, solid content is adjusted for temperature control For 15wt%, time 12h.
2) glue coats: the glue after ageing using infusion process, is dipped into being coated to wall-flow diesel particle filtering On the air inlet wall surface of device and in wall inner pore, and blowback is carried out with compressed air stream, to dispose extra glue, then will had The DPF of coat is placed in 120 DEG C of air-heater dry 0.5h.
3) aerosolization spray immersion active noble metals particle: by active precious metal ion solution by air-flow, by it Broken to nebulize, then spray immersion is into the DPF with coat after roasting, it is desirable that compressed air pressure 4MPa, Noble metal solution flow velocity 0.5L/min, molar ratio=4:1 of platinum nitrate and palladium nitrate, injection direction and duct center wire clamp Angle is 45 °.Then DPF is placed in 120 DEG C of hot air drying machines, time 2h, is finally placed in Muffle furnace, carry out roasting technique, temperature It is required that 550 DEG C, time 4h.
Embodiment 3
Coating slurry configuration, coating and noble metal impregnation technology:
1) boehmite: being added in deionized water by 10wt%, 1.0wt% citric acid be added by the configuration of glue, into Row high-energy ball milling, revolving speed requires 1000r/min, after about 60min, is added the mixed solution of cerous nitrate and zirconium nitrate, cerous nitrate and The molar ratio 3:1 of zirconium nitrate feeds intake, and then proceedes to electromagnetic agitation, stirring rate 200r/min, time about 30min, finally Ripening is carried out, high-energy ultrasonic oscillation, working frequency 100KHz, power is in 100W, and at 50 DEG C, solid content is adjusted for temperature control For 15wt%, time 20h.
2) glue coats: the glue after ageing using infusion process, is dipped into being coated to wall-flow diesel particle filtering On the air inlet wall surface of device and in wall inner pore, and blowback is carried out with compressed air stream, to dispose extra glue, then will had The DPF of coat is placed in 120 DEG C of air-heater dry 2h.
3) aerosolization spray immersion active noble metals particle: by active precious metal ion solution by air-flow, by it Broken to nebulize, then spray immersion is into the DPF with coat after roasting, it is desirable that compressed air pressure 5MPa, Noble metal solution flow velocity 0.3L/min, molar ratio=4:1 of platinum nitrate and palladium nitrate, injection direction and duct center wire clamp Angle is 60 °.Then DPF is placed in 120 DEG C of hot air drying machines, time 2h, is finally placed in Muffle furnace, carry out roasting technique, temperature It is required that 550 DEG C, time 2h.
Embodiment 4
Coating slurry configuration, coating and noble metal impregnation technology:
1) boehmite: being added in deionized water by 10wt%, 1.0wt% citric acid be added by the configuration of glue, into Row high-energy ball milling, revolving speed requires 1500r/min, after about 30min, is added the mixed solution of cerous nitrate and zirconium nitrate, cerous nitrate and The molar ratio 7:1 of zirconium nitrate feeds intake, and then proceedes to electromagnetic agitation, stirring rate 200r/min, time about 30min, finally Ripening is carried out, high-energy ultrasonic oscillation, working frequency 100KHz, power is in 100W, and at 50 DEG C, solid content is adjusted for temperature control For 15wt%, the time is for 24 hours.
2) glue coats: the glue after ageing using infusion process, is dipped into being coated to wall-flow diesel particle filtering On the air inlet wall surface of device and in wall inner pore, and blowback is carried out with compressed air stream, to dispose extra glue, then will had The DPF of coat is placed in 120 DEG C of air-heater dry 2h.
3) aerosolization spray immersion active noble metals particle: by active precious metal ion solution by air-flow, by it Broken to nebulize, then spray immersion is into the DPF with coat after roasting, it is desirable that compressed air pressure 5MPa, Molar ratio=2:1 injection direction of noble metal solution flow velocity 0.3L/min, platinum nitrate and palladium nitrate and duct center are one On horizontal line.Then DPF is placed in 120 DEG C of hot air drying machines, time 2h, is finally placed in Muffle furnace, carry out roasting technique, temperature Degree requires 550 DEG C, time 2h.
Detect example
The cPDF that embodiment 1 to 4 is obtained is detected, and detection method is as follows:
As shown in Figure 1, being prepared with the DPF carrier of a batch of certain specification by present invention process technology, pass through Engine is crossed, realizes the load of PM, loading capacity requires 4.0 ± 0.5g/L, then under normal temperature state, in self-control back pressure tester On device, back pressure test is carried out, the curve that back pressure changes with the variation of air speed is obtained.
From Fig. 1 the result shows that, through the invention in the catalyst coatings material of preparation process and its design mentioned, by changing Become corresponding technological parameter, relative to traditional handicraft, be able to achieve the purpose of low back pressure, this is beneficial to the power for improving engine Performance.
As shown in Fig. 2, be prepared with the DPF carrier of a batch of certain specification by this patent technology, it is first It is first activated on engine pedestal, then carries out PM load, loading capacity requires 4.0 ± 0.5g/L, then one Under fixed engine operation condition, promoted CDPF inlet temperature (initial temperature is set as 250 DEG C), as the temperature increases, PM Gradually catalysis oxidation occurs, when back pressure is substantially reduced, that is, determines that temperature is the initiation temperature of PM at this time；
After the completion of carrying out initiation temperature testing experiment to the carrier of fresh state, aging process, treatment conditions 900 are carried out DEG C, 20h contains 10%H2Under the conditions of the air atmosphere of O, hydrothermal aging processing is carried out, then with above-mentioned same method, carries out PM Initiation temperature test.
From Fig. 2 the result shows that, through the invention in the catalyst coatings material of preparation process and its design mentioned, by changing Become corresponding technological parameter, relative to traditional handicraft, about 30 DEG C can be reduced to the initiation temperature of its fresh state and aging state, this It will be very beneficial for the generation of PM passive regeneration in CDPF, can effectively be able to achieve NO at a lower temperature2Assist PM catalysis oxidation.

Claims (8)

1. a kind of with low back pressure, the DPF preparation process of low light-off temperature Catalytic Layer, it is characterised in that the following steps are included:
1) preparation of coat glue, by containing aluminium oxide or aluminum soluble salt be added in water-alcohol solvent system, with alumina Compound weight note, concentration in a solvent are 10-30wt%, and the concentration of alcohol is 1.0~50.0wt% in solvent, soluble acid Concentration is 0.1~1.0wt%, at normal temperature high-energy ball milling 20min~120min, obtains slurries A；Then by cerous nitrate, nitric acid Zirconium is pre-mixed to form ionic soln according to molar ratio Ce:Zr=1:1~6:1, is added in slurries A, with cerium oxide and oxidation The zirconium weight note total butt coated weight ratio of Zhan is 10~50wt%, 30~180min of electromagnetic agitation, forms slurries B, and adjustment contains admittedly Amount is 15~20wt%；Under the conditions of 30~80 DEG C of temperature, to slurries B ageing 12~for 24 hours, while high-energy ultrasonic oscillation is carried out, Form glue C；
2) glue coats, and by glue C by grouting immersion coating, deposits it into wall-flow diesel particulate filter air inlet end wall On face and in wall inner pore, and blowback is carried out with compressed air stream, air-flow enters from outlet side, disposes extra glue C, then It is dried；
3) active noble metals particle impregnates, and using aerosolization spray immersion, the solution of the ion containing active noble metals is passed through air-flow Be crushed and nebulized, in the filter that then spray immersion to step 2) obtains, air-dry it is dry, Muffle furnace roasting, obtain DPF at Product.
2. according to claim 1 have low back pressure, the DPF preparation process of low light-off temperature Catalytic Layer, it is characterised in that: The coating catalysis material is the composite oxides of aluminium oxide, cerium oxide or/and zirconium oxide.
3. according to claim 1 have low back pressure, the DPF preparation process of low light-off temperature Catalytic Layer, it is characterised in that: The alcohol is the mixture of one or more of methanol, ethyl alcohol, glycerine, polyethylene glycol, propyl alcohol or isopropanol.
4. according to claim 1 have low back pressure, the DPF preparation process of low light-off temperature Catalytic Layer, it is characterised in that: The soluble acids are the mixtures of one or more of formic acid, citric acid, nitric acid, acetic acid.
5. according to claim 1 have low back pressure, the DPF preparation process of low light-off temperature Catalytic Layer, it is characterised in that: The aerosolization spray immersion is compressed air pressure >=3MPa, noble metal solution flow velocity≤1L/min, injection direction with Duct centerlines are greater than 20 degree.
6. according to claim 1 have low back pressure, the DPF preparation process of low light-off temperature Catalytic Layer, it is characterised in that: The high-energy ball milling revolving speed is 500~2000r/min, 20~120min of time；The electromagnetic agitation revolving speed is 200~500r/ Min, 30~180min of time.
7. according to claim 1 have low back pressure, the DPF preparation process of low light-off temperature Catalytic Layer, it is characterised in that: Step 3) the apoplexy is dry, roasting is dry 0.5~3h in the hot wind for be placed in DPF 100~150 DEG C, then 450~ Muffle furnace roasting, 2~6h of calcining time are carried out under the conditions of 650 DEG C.
8. a kind of DPF with low back pressure, low light-off temperature Catalytic Layer, it is characterised in that: the DPF is claim 1 to 7 times The DPF of the preparation of preparation process described in one.
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CN109999803A (en) * 2019-04-16 2019-07-12 中自环保科技股份有限公司 A kind of the cerium base catalyst and preparation process of low-temperature catalytic oxidation soot
CN110124659B (en) * 2019-06-20 2021-03-23 中自环保科技股份有限公司 Cerium-zirconium-aluminum-based composite material, cGPF catalyst and preparation method thereof
CN110152721A (en) * 2019-06-25 2019-08-23 无锡威孚环保催化剂有限公司 The preparation method of wall-flow particulate trap catalyst
CN111330363B (en) * 2020-03-13 2021-08-24 苏州德中创恒软件科技有限公司 Vehicle DPF washs regeneration facility
CN111821971B (en) * 2020-07-30 2023-08-18 中自环保科技股份有限公司 Integral catalyst for catalytic regeneration of carbon smoke and preparation method thereof
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CN114653396B (en) * 2022-03-09 2023-11-24 同济大学 DPF catalyst coating method capable of achieving low exhaust back pressure and high catalytic efficiency
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