CN109012666A - A kind of preparation method of cleaning catalyst for tail gases of automobiles - Google Patents
A kind of preparation method of cleaning catalyst for tail gases of automobiles Download PDFInfo
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- CN109012666A CN109012666A CN201811077198.8A CN201811077198A CN109012666A CN 109012666 A CN109012666 A CN 109012666A CN 201811077198 A CN201811077198 A CN 201811077198A CN 109012666 A CN109012666 A CN 109012666A
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- 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
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- 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
- B01D53/922—Mixtures of carbon monoxide or hydrocarbons and nitrogen oxides
- B01D53/925—Simultaneous elimination of carbon monoxide or hydrocarbons and nitrogen oxides
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Abstract
The invention discloses a kind of preparation methods of cleaning catalyst for tail gases of automobiles, the load of the preparation of pretreatment, hydrogen-storing material, the preparation of activated aluminum and active aluminium layer including carrier；It is handled during vehicle treated using malic acid and polyethylene glycol, hydrogen-storing material is prepared by the precipitation method, joined the auxiliary agent of optimization in the dipping process of active aluminium layer.Carrier of the invention improves the specific surface area of carrier by acid etching using preceding being pre-processed, while in order to reduce influence of the acid etching to support strength, polyethylene glycol is added as protection auxiliary agent, so that intensity is lower by being influenced in acid corrosion process.
Description
Technical field
The present invention relates to automobile catalytic devices, and in particular to a kind of preparation method of cleaning catalyst for tail gases of automobiles.
Background technique
The tail gas of locomotive emissions is one of primary pollution source of atmosphere pollution.Medium and heavy diesel vehicle major pollutants are nitrogen oxygen
Compound is discharged extremely serious to the injury of ecological environment and human health.Nitrogen oxides in burning waste gas is usually by firing
The nitrogen in nitride and air in material reacts generation with oxygen at high temperature.With internal combustion engine especially diesel engine and other richnesses
It include pollutant carbon monoxide (CO), hydrocarbon (HC), soot particulate matter and nitrogen oxidation in exhaust gas for oxygen combustion engine
Object.In the case of gasoline engines, the oxygen in air and fuel are mixed and burned by chemical ratios, do not have carbon in pollutant
Grain object, can be purified by so-called three-way catalyst (TWC).
Auto-exhaust catalyst commonly used in the prior art mainly includes following four part: carrier, active oxidation aluminium layer with
And active component.The surface of cordierite honeycomb structure is usually glassy, smoother, and specific surface area is smaller.It is urged to reduce
Change device product, load more active components to improve tail gas clean-up effect, needs to improve the ratio of cordierite honeycomb structure as far as possible
Surface area and the adhesive force of raising and active aluminium layer.
The catalyst converter erosion by high temperature gas flow for a long time when in use, the load so that the active aluminium layer on surface gradually falls off
Body causes catalytic performance to gradually decrease.When slurry is adsorbed on carrier by the method impregnated in the prior art, carrier and aluminium layer
Between adsorption capacity it is to be improved, activated aluminum can be strengthened and active catalytic components are resisted by high temperature gas flow by improving adsorption capacity
Erosion property, and then improve the catalytic performance after long-time use.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of cleaning catalyst for tail gases of automobiles, can be improved the ratio table of carrier
Area enhances adsorption capacity and firmness of the carrier between active aluminium layer.
In order to achieve the above object, providing a kind of preparation side of cleaning catalyst for tail gases of automobiles in one embodiment of the present of invention
Method, comprising the following steps:
(1) pretreatment of carrier: being placed in 5h ~ 10h in the mixed solution of malic acid and polyethylene glycol for carrier, then takes out clear
It washes, be dried for standby；
(2) preparation of hydrogen-storing material:
Cerous nitrate, zirconium nitrate, yttrium nitrate are dissolved in water according to molar ratio 100:50 ~ 80:10 ~ 20, ammonium hydroxide is added and adjusts pH
To alkalinity, make rare earth element precipitating complete；Will after obtained sediment filtering and washing successively at 80 DEG C ~ 100 DEG C dry 5h ~
10h, 500 DEG C ~ 550 DEG C roasting 3h ~ 5h；Obtain storage oxygen powder；
(3) preparation of activated aluminum:
By lanthana, cerium oxide 30 ~ 50h of ball milling, aluminium oxide continuation ball milling 20h ~ 30h is then added and obtains activated aluminium-hydrogen-oxygen lanthanum-
The activated aluminum powder of cerium oxide；The molar ratio of aluminium oxide, lanthana and cerium oxide is 100:5 ~ 10:5 ~ 15 in activated aluminum powder；
(4) load of active aluminium layer:
Storage oxygen powder and activated aluminum powder are added in the water containing auxiliary agent 1,4-butyrolactone to be uniformly mixed and form mixed liquid, then will
Step (1) treated carrier impregnation 1min ~ 3min in mixed liquid；Dry 2 ~ 3h, drying finish in hot wind after dipping
2h ~ 5h is roasted at 500 DEG C ~ 600 DEG C afterwards；Obtain active aluminium layer carrier；
(5) it is catalyzed the load of slurry
By active aluminium layer carrier impregnation in precious metal solution, dry 2 ~ 3h in hot wind is taken out after impregnating 1min ~ 3min, it is dry
After at 500 DEG C ~ 600 DEG C roast 5h ~ 10h, obtain the catalyst of finished product.
Preferably, carrier is cordierite honeycomb carrier；The mass fraction of malic acid is 15% ~ 25% in mixed solution, poly- second
The mass fraction of glycol is 5% ~ 10%.
Preferably, ammonium hydroxide, which is added, adjusts pH to 10.
Preferably, the revolving speed of ball milling is 200r/min ~ 300r/min.
Preferably, whole content of the auxiliary agent 1,4-butyrolactone in mixed liquid is 0.2mol/L ~ 0.1mol/L.
Preferably, precious metal element is one of Metal Palladium, platinum and rhodium or several mixing；Noble metal member on catalyst converter
The load capacity of element is 2% ~ 3%.
Preferably, mixing in liquid further includes dispersing agent, and dispersing agent is polyvinyl alcohol, and dispersing agent mixes the concentration in liquid in activated aluminum
For 1mol/L.
Storage oxygen powder 10g ~ 50g, activated aluminum powder 100g ~ 200g is added in step (4) in every kilogram of water.
In conclusion the invention has the following advantages that
1, carrier improves the specific surface area of carrier, while by acid etching using preceding being pre-processed in order to reduce acid etching to load
Polyethylene glycol is added as protection auxiliary agent, so that intensity is lower by being influenced in acid corrosion process in the influence of body intensity.
2, when activated aluminum mixes liquid coated in carrier, joined 1,4-butyrolactone, can be improved mixed slurry material and carrier it
Between adsorption capacity, reduce use process in obscission.
Specific embodiment
Embodiment 1
A kind of preparation method of cleaning catalyst for tail gases of automobiles, comprising the following steps:
(1) it is molten that cordierite honeycomb carrier the pretreatment of carrier: is placed in the mixing containing 20% malic acid and 6% polyethylene glycol
6h in liquid then takes out cleaning, is dried for standby；
(2) preparation of hydrogen-storing material:
It takes cerous nitrate 100mol, zirconium nitrate 60mol, yttrium nitrate 15mol to be dissolved in water, ammonium hydroxide is added and adjusts pH to 10, allows dilute
Earth elements precipitating is complete；6h, 550 DEG C of roasting 3h will be successively dried after obtained sediment filtering and washing at 100 DEG C；It obtains
Store up oxygen powder；
(3) preparation of activated aluminum:
By lanthana 10mol, cerium oxide 15mol revolving speed be 250r/min ball mill in ball milling 40h, aluminium oxide is then added
100mol continues ball milling 20h and obtains activated aluminium-hydrogen-oxygen lanthanum-cerium oxide activated aluminum powder；
(4) load of active aluminium layer:
20g is stored up into oxygen powder and 150g activated aluminum powder is added and contains auxiliary agent 1,4- butyrolactone 0.3mol, polyethylene of dispersing agent alcohol
It in the 1000g water of 5mol, is uniformly mixed and forms mixed liquid, then by step (1) treated carrier impregnation 2min in mixed liquid；Leaching
2h is dried after stain in 100 DEG C of hot winds, roasts 3h at 550 DEG C after dry；Obtain active aluminium layer carrier；
(5) it is catalyzed the load of slurry
By active aluminium layer carrier impregnation in palladium chloride solution, dry 2 ~ 3h in hot wind is taken out after impregnating 1min ~ 3min, it is dry
After at 500 DEG C ~ 600 DEG C roast 5h ~ 10h, obtain the catalyst of finished product, the load capacity of precious metal element is on catalyst
2%。
One, influence research of the different pretreatments method to carrier specific surface area
Cordierite is common containing alumina supporter, with good mechanical performance and thermal stability, therefore is three-way catalyst
Preferred carrier.The surface of cordierite honeycomb carrier is smooth, and specific surface area is smaller, and logical peracid treatment is able to carry out at corrosivity
Reason obtains more high-specific surface area.
Experimental example 1
Experimental method:
More cordierite honeycomb carriers are taken, clear water washing is taken out surface dust and impurity, is separately immersed in as shown in table 1 not
8h in same treatment fluid, then takes out cleaning, drying.Specific area measuring and strength detection, testing result such as table are carried out after drying
Shown in 1.Wherein control group is untreated carrier.
Specific area measuring: health tower Quantachrome direct-reading dynamic flow method specific surface area analysis instrument Monosorb；
The present invention sets its specific surface area and intensity as 100% using control group as reference, the specific surface area amplification degree of remaining experimental group
Calculation is: using same instruments and method, the difference and control group of the parameter of experimental group specific surface area parameter and control group
The ratio of parameter.
Strength detection: WSY-400A type pressure test machine testing.
The calculation of intensity decrease rate is: with the difference and control group of experimental group intensive parameter and control group intensive parameter
The absolute value of the ratio of parameter.
Table 1: the processing result of different disposal liquid
It can be learnt from above-mentioned experimental result:
It A,, can be with hydrogen ion in acid solution since carrier is actually magnesium aluminum compounds after being handled using acid solution
Certain reaction occurs, substance is dissolved into acid solution in carrier during the reaction, more holes is formd, so that the ratio of carrier
Surface area increases.In the case where no other reagents protection, this acid etching can be significantly reduced the intensity of carrier, carrier
It is reduced to the requirement for being not suitable for catalyst to carrier after such intensity.
B, the difference of experimental group 1 and 2 is, the acidity of hydrochloric acid is better than malic acid, and corrosive power is stronger, therefore it expands
Rate is higher, and then intensity also reduces more.Any effect is not shown when polyethylene glycol in experimental group 3 individually uses.
C, experimental group 1 is compared with experimental group 4, and experimental group 4 increases polyethylene glycol, and amplification degree has a degree of drop
It is low, but still have larger impact to the raising of the specific surface area of carrier, but its intensity decrease rate is very low, illustrates in poly- second
Under the protection of glycol, although the expansion of specific surface area receives certain restrictions, support strength obtains good protection, can
It is satisfied with requirement of the catalyst converter to support strength.The polyethylene glycol of experimental group 5 can also play the role of centainly protecting support strength,
But its effect is no and malic acid cooperates advantageously, illustrates that the cooperation of both malic acid and polyethylene glycol is more excellent.
D, it selects the carrier of experimental group 4 as catalyst converter carrier, obtains bigger specific surface area parameter, can more hold
Easily and the more catalyst of load, the efficient and diminution volume of this catalyst provide further possibility.
Two, activated aluminum mixes influence of the auxiliary agent to carrier adsorption power in liquid
It needs to keep good adsorption capacity between the mixed liquid and carrier of activated aluminum, be conducive to so living in long-time use process
Property aluminium layer will not be by high temperature gas flow erosion, the case where avoiding catalytic effect from reducing appearance.
Experimental method:
Hydrogen-storing material and activated aluminum powder in Example 1；It is added in the deionized water containing auxiliary agent and is made containing activated aluminum
Mixed liquid.Then by step (1) treated carrier impregnation in mixed liquid 2min；It is dry in 100 DEG C of hot winds after dipping
2h roasts 3h at 550 DEG C after dry；Obtain active aluminium layer carrier.
Detect the adsorption capacity between carrier and active aluminium layer:
Adsorption capacity detection method: active alumina supporter is placed in 85 DEG C of hot water of flowing, and is washed away for 24 hours under ultrasonic wave effect；
Drying is then taken out, calculates the quality for the loss for washing away rear active alumina supporter and the ratio for washing away preceding active aluminium layer quality, as
Mass loss ratio.Mass loss ratio is bigger, and it is about serious to illustrate that active aluminium layer falls off.Before the quality of active aluminium layer can be by washing away
The difference of the quality of the quality and carrier of active alumina supporter is calculated, due to having good stability for carrier, in the case not
It is easy to fall off, therefore mass loss is than being mainly caused by active aluminium layer falls off.
Table 2: influence of the different auxiliary agents to mass loss ratio
From table 2 it is known that any auxiliary agent is not added in control group, so that the adsorption capacity between mixed liquid and carrier is general, activity
Aluminium layer loss is larger, and dispersing agent is added in experimental group 1, can play the role of dispersing activated aluminum to mix liquid, therefore can allow absorption
It is more uniform, adsorption capacity can be also improved to a certain extent.Joined 1,4-butyrolactone in experimental group 2, can to carrier and
Facilitation is played in the suction-operated of mixed liquid, so that absorption between the two is stronger, by still being able to after water erosion
Keep good active aluminium layer；Facilitate catalyst converter so still can in the case where being used for a long time and being corroded by high temperature gas flow
Obtain good catalytic capability.
Claims (8)
1. a kind of preparation method of cleaning catalyst for tail gases of automobiles, comprising the following steps:
(1) pretreatment of carrier: being placed in 5h ~ 10h in the mixed solution of malic acid and polyethylene glycol for carrier, then takes out clear
It washes, be dried for standby；
(2) preparation of hydrogen-storing material:
Cerous nitrate, zirconium nitrate, yttrium nitrate are dissolved in water according to molar ratio 100:50 ~ 80:10 ~ 20, ammonium hydroxide is added and adjusts pH
To alkalinity, make rare earth element precipitating complete；Will after obtained sediment filtering and washing successively at 80 DEG C ~ 100 DEG C dry 5h ~
10h, 500 DEG C ~ 550 DEG C roasting 3h ~ 5h；Obtain storage oxygen powder；
(3) preparation of activated aluminum:
By lanthana, cerium oxide 30 ~ 50h of ball milling, aluminium oxide continuation ball milling 20h ~ 30h is then added and obtains activated aluminium-hydrogen-oxygen lanthanum-
The activated aluminum powder of cerium oxide；The molar ratio of aluminium oxide, lanthana and cerium oxide is 100:5 ~ 10:5 ~ 15 in activated aluminum powder；
(4) load of active aluminium layer:
Storage oxygen powder and activated aluminum powder are added in the water containing auxiliary agent 1,4-butyrolactone to be uniformly mixed and form mixed liquid, then will
Step (1) treated carrier impregnation 1min ~ 3min in mixed liquid；Dry 2 ~ 3h, drying finish in hot wind after dipping
2h ~ 5h is roasted at 500 DEG C ~ 600 DEG C afterwards；Obtain active aluminium layer carrier；
(5) it is catalyzed the load of slurry
By active aluminium layer carrier impregnation in precious metal solution, dry 2 ~ 3h in hot wind is taken out after impregnating 1min ~ 3min, it is dry
After at 500 DEG C ~ 600 DEG C roast 5h ~ 10h, obtain the catalyst of finished product.
2. preparation method as described in claim 1, it is characterised in that: the carrier is cordierite honeycomb carrier；The mixing
The mass fraction of malic acid is 15% ~ 25% in solution, and the mass fraction of polyethylene glycol is 5% ~ 10%.
3. preparation method as described in claim 1, it is characterised in that: the ammonium hydroxide, which is added, adjusts pH to 10.
4. preparation method as described in claim 1, it is characterised in that: the revolving speed of the ball milling is 200r/min ~ 300r/min.
5. preparation method as described in claim 1, it is characterised in that: whole content of the auxiliary agent 1,4-butyrolactone in mixed liquid
For 0.2mol/L ~ 0.1mol/L.
6. preparation method as described in claim 1, it is characterised in that: the precious metal element is in Metal Palladium, platinum and rhodium
One or several kinds mixing；The load capacity of precious metal element is 2% ~ 3% on the catalyst converter.
7. preparation method as described in claim 1, it is characterised in that: further include dispersing agent in the mixed liquid, dispersing agent is poly-
Vinyl alcohol, it is 1mol/L that dispersing agent, which mixes the concentration in liquid in activated aluminum,.
8. preparation method as described in claim 1, it is characterised in that: storage oxygen powder is added in the step (4) in every kilogram of water
Last 10g ~ 50g, activated aluminum powder 100g ~ 200g.
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Cited By (5)
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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 |
| CN111632588A (en) * | 2020-06-09 | 2020-09-08 | 合肥神舟催化净化器股份有限公司 | Preparation method of automobile exhaust purification catalyst |
| CN111632589A (en) * | 2020-06-09 | 2020-09-08 | 合肥神舟催化净化器股份有限公司 | Preparation method of high-stability automobile exhaust purification catalyst |
| CN112588285A (en) * | 2020-12-14 | 2021-04-02 | 西安凯立新材料股份有限公司 | Hydrothermally stable acrylic acid waste gas catalytic combustion catalyst and preparation method thereof |
| CN114361482A (en) * | 2022-01-06 | 2022-04-15 | 江苏科技大学 | Preparation method of high-permeability carbon paper for fuel cell |
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Cited By (6)
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| CN111632589A (en) * | 2020-06-09 | 2020-09-08 | 合肥神舟催化净化器股份有限公司 | Preparation method of high-stability automobile exhaust purification catalyst |
| CN112588285A (en) * | 2020-12-14 | 2021-04-02 | 西安凯立新材料股份有限公司 | Hydrothermally stable acrylic acid waste gas catalytic combustion catalyst and preparation method thereof |
| CN112588285B (en) * | 2020-12-14 | 2023-02-10 | 西安凯立新材料股份有限公司 | Hydrothermally stable acrylic acid waste gas catalytic combustion catalyst and preparation method thereof |
| CN114361482A (en) * | 2022-01-06 | 2022-04-15 | 江苏科技大学 | Preparation method of high-permeability carbon paper for fuel cell |
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Denomination of invention: A preparation method of automobile exhaust purification catalyst Effective date of registration: 20221013 Granted publication date: 20210511 Pledgee: Mianyang Rural Commercial Bank Co.,Ltd. Changxing Sub branch Pledgor: SICHUAN XINYUANRUI TECHNOLOGY Co.,Ltd. Registration number: Y2022980018284 |
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