CN105797767A - Diesel vehicle oxidized form catalyst having low temperature activity and preparation method thereof - Google Patents
Diesel vehicle oxidized form catalyst having low temperature activity and preparation method thereof Download PDFInfo
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- CN105797767A CN105797767A CN201610144944.5A CN201610144944A CN105797767A CN 105797767 A CN105797767 A CN 105797767A CN 201610144944 A CN201610144944 A CN 201610144944A CN 105797767 A CN105797767 A CN 105797767A
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/78—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
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- 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
- B01D53/944—Simultaneously removing carbon monoxide, hydrocarbons or carbon making use of oxidation catalysts
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- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/20—After treatment, characterised by the effect to be obtained to introduce other elements in the catalyst composition comprising the molecular sieve, but not specially in or on the molecular sieve itself
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- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract
The invention relates to a diesel vehicle oxidized form catalyst having low temperature activity and a preparation method thereof.The catalyst comprises a carrier and a coating applied to the carrier, the coating is loaded with noble metal, the coating comprises tungsten-aluminum silicon composite oxide and molecular sieves, the noble metal is one of Pt and Pd or a mixture of the two types of substances, the coated weight of the coating is 80-180 grams/liter, and the coated weight of the noble metal is 0.5-4.5 grams/liter.The preparation method comprises the steps of firstly, preparing the tungsten-aluminum silicon composite oxide through an equivalent-volume impregnation method, then making slurry with the molecular sieves and the tungsten-aluminum silicon composite oxide according to the mass ratio of 1: (2-10), adding the noble metal Pt and Pd, finally immersing the carrier into the slurry, and conducting drying and sintering, so that the diesel vehicle oxidized form catalyst is obtained.The preparation method of the catalyst is simple, the steps are easy to operate, the prepared diesel vehicle oxidized form catalyst is low in combustion temperature, high in conversion rate and good in thermal stability, good capability for oxidizing HC and CO in tail gas of a diesel vehicle is achieved, and good sulfur resistance is achieved.
Description
Technical field
The present invention relates to a kind of diesel vehicle oxidation catalyst with low temperature active and preparation method thereof, belong to
Catalyst preparation technical field.
Background technology
Along with economic develops rapidly, improving constantly of people's living standard, transportation has obtained front institute
Not some development, yield and the recoverable amount of motor vehicles increase year by year.At fuel-cell vehicle and hybrid electric vehicle still
When universal, diesel vehicle has higher fuel-economy type, the dirt of the lowest tail gas compared with gasoline car
Dye is emitted on the market demand of 21 century and increases quickly.And being continuously increased along with diesel vehicle quantity, diesel oil
The air environmental pollution that tail gas discharge causes the most increasingly causes the extensive concern of people.Emission of diesel engine
Pollutant mainly have carbon monoxide (CO), hydrocarbon (HC), nitrogen oxides (NOX) and particulate matter
(PM), particulate matter mainly has dry carbon, dissolved organic matter (SOF) and a small amount of sulphuric acid and sulfate composition.
Diesel oxidation catalyst (DOC) is the diesel engine vent gas post-processing technology being applied the earliest, and it is main
For eliminating the SOF in HC, CO and the PM in tail gas, generally more than 250 DEG C in the environment of be catalyzed
Eradicating efficacy is preferable.DOC both can be used alone, and can carry with other exhaust aftertreatment technology, diesel oil again
Matter is used in combination with additive technology, emission controls by improving combustion technology.And DOC safeguards simple, it is not necessary to regeneration,
Therefore it is most widely used Diesel Engine After-treatment Technology.But owing in domestic oil product, sulfur content is higher,
Containing more sulfur dioxide (SO in tail gas2), and sulfur dioxide can be oxidized to sulfur trioxide (SO3),
Form sulfate further, cause catalysqt deactivation, poisoning, reduce catalyst in exhaust gas from diesel vehicle
The conversion capability of CO, HC and SOF, so DOC should have certain sulfur resistance.In recent years, with
Abgasgesetz more strict, the catalytic performance of oxidation catalyst is required more and more higher, as low temperature rises
Fire activity, service life etc..
Summary of the invention
The invention aims to solve the problems referred to above, it is provided that a kind of diesel vehicle oxygen with low temperature active
Change type catalyst and preparation method thereof, the diesel vehicle oxidation catalyst initiation temperature prepared is low, conversion
Rate is high, Heat stability is good, HC and CO in exhaust gas from diesel vehicle is had good oxidability, and has
Preferably sulfur resistive ability.
The present invention adopts the following technical scheme that a kind of diesel vehicle oxidation catalyst with low temperature active, bag
Including carrier and the coating coated on carrier, be loaded with noble metal in coating, described coating includes tungsten-sial
Composite oxides and molecular sieve, described noble metal is the mixture of one or both materials in Pt, Pd, institute
The coated weight stating coating is 80-180 grams per liter, and the coated weight of described noble metal is 0.5-4.5 grams per liter.
Further, described molecular sieve is 1:2～10 with the mass ratio of tungsten-sial composite oxides.
Further, in described tungsten-sial composite oxides, the mass ratio of wolfram element and sial composite oxides is
1:19～99.
Further, in described sial composite oxides, silicon dioxide quality mark is 5～25wt%, and remaining is
The sial of aluminium sesquioxide.
Further, described molecular sieve is Hydrogen beta-molecular sieve.
Further, described carrier is cordierite ceramic honeycomb or iron-chromium-aluminum metal honeycomb, the hole of described carrier
Density is 200-600 mesh/square feet.
There is the preparation method of the diesel vehicle oxidation catalyst of low temperature active, comprise the steps:
(1) equi-volume impregnating prepares tungsten-sial composite oxides: by wolfram element and sial composite oxides
Mass ratio is that 1:19-99 weighs ammonium tungstate and sial composite oxides respectively, by the saturated suction of silicon-aluminium compound
Attached amount preparation ammonium tungstate aqueous solution, drops in sial composite oxides also by the ammonium tungstate aqueous solution prepared
Continuously stirred 2～8 hours, then stand, be aged 6～15 hours after under the conditions of 100～170 DEG C dry,
And after 350～550 DEG C of roastings, obtain tungsten-sial composite oxides；
(2) preparation of coating slurry: by the mass ratio of molecular sieve Yu tungsten-sial composite oxides be 1:2～
Tungsten-sial composite oxides and molecular sieve are added separately in deionized water stirring by 10 forms serosity, tungsten-sial
Composite oxides and the gross mass of molecular sieve are 2:3～8 with the mass ratio of deionized water, then use ball milling work
Skill processes serosity, and controlling granule D90 is 5-40 μm, prepares coating slurry；
(3) according to the requirement that the coated weight of noble metal on carrier is 0.5-4.5 grams per liter calculating noble metal, will
Solution containing one or both materials in precious metals pt, Pd joins in coating slurry, stirs,
Form final serosity；
(4) carrier cordierite ceramic honeycomb or iron-chromium-aluminum metal honeycomb are immersed in final serosity, soak
Taking out after 0.5～5min, use compressed air to blow logical by the passage of carrier inside, purge time is 0.5～3min,
Then carrier is dried 3～8 hours under the conditions of 100～170 DEG C, finally by carrier at 350～550 DEG C of bars
Roasting 2～3 hours under part, i.e. obtain diesel vehicle oxidation catalyst.
Preparation method of the present invention is simple, and step is easily operated, and the diesel vehicle oxidation catalyst prepared rises
Temperature is low, conversion ratio is high, Heat stability is good in combustion, HC and CO in exhaust gas from diesel vehicle is had good oxygen
Change ability, and there is preferable sulfur resistive ability.Compared with traditional titania coating, the silicon that the present invention uses
Aluminium composite oxide coating has higher phase transition temperature and good heat stability.
Using the acid sial composite oxides with large specific surface area and loose structure is coated substrate, logical
Crossing equi-volume impregnating and prepared tungsten-sial composite oxides, its acidity relatively sial composite oxides have
Improve further.In the catalyst oxidation reaction that Pt is main active component, the existence of Lewis-acid sites
The oxidation of Pt can be suppressed, and the Pt of zero-valent state is the most active, therefore improve the lewis acid of carrier
Can effectively promote catalyst activity.And the interpolation of wolfram element, the road of sial composite oxides can be increased further
Lewis acid site, and then effectively promote catalyst coat performance.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1: a kind of diesel vehicle oxidation catalyst with low temperature active, catalyst carrier is cordierite
Ceramic honey comb, volume is 1.101 liters, and hole density is 400 mesh/square feet；Coating contains tungsten-sial multiple
Closing oxide and molecular sieve, coating coated weight is 120 grams per liters；Noble metal is platinum, the coated weight of noble metal platinum
It is 3.1 grams per liters.
Preparation method comprises the steps:
(1) equi-volume impregnating prepares tungsten-sial composite oxides: the bodies such as tungsten-sial composite oxides employing
Prepared by long-pending infusion process.In the sial combined oxidation raw material used, the mass fraction of dioxide-containing silica is
15%, remaining is aluminium sesquioxide.Weigh the sial composite oxides that quality is 990 grams, weigh 13.9 grams
Ammonium tungstate dissolves, and is configured to the aqueous solution of sial composite oxides saturated extent of adsorption used, then ammonium tungstate is molten
Drop adds in sial composite oxide powder and continuously stirred 4 hours；Then stand, be aged 10 hours,
Dry 12 hours at 120 DEG C afterwards, obtain tungsten-sial composite oxides 500 DEG C of roastings after 4 hours, system
In the standby tungsten-sial composite oxides obtained, wolfram element is 1:99 with the mass ratio of sial composite oxides.
(2) weigh deionized water 1400 grams, add tungsten-sial composite oxides 800 grams, molecular sieve 200
Gram, stir formation coating slurry, controls serous granule degree D90 and is about 25 microns；
(3) continue platinum nitrate is added in coating paste by whipping process, stir, form final slurry.
(4) take out after cordierite ceramic honeycomb matrix being soaked 1 minute in final slurry at this, then by pressure
Internal to carrier surface and duct unnecessary serosity is blown down by contracting air, and purge time is 2 minutes, is subsequently placed in
Being dried 2 hours at 120 DEG C in baking oven, in Muffle furnace, roasting 2 hours at 500 DEG C, i.e. obtain diesel vehicle oxygen
Change catalyst.
Comparative example: the tungsten in coating-sial composite oxides are changed into tungsten-silicon-titanium coating, preparation method with
Embodiment 1 is identical, uses identical cordierite ceramic honeycomb carrier, identical coated weight, has prepared expensive
The diesel vehicle oxidation catalyst that tenor is identical.
Embodiment 2:
Concrete preparation method is essentially identical with example 1, and difference is, tungsten used-sial composite oxides
In, wolfram element is 1:39 with the mass ratio of sial composite oxides.
Embodiment 3:
Concrete preparation method is essentially identical with example 1, and difference is, tungsten used-sial composite oxides
In, wolfram element is 1:19 with the mass ratio of sial composite oxides.
Embodiment 4:
Concrete preparation method is essentially identical with example 1, and difference is, the sial used by oxide raw material
Composite oxides be the quality mark containing silicon dioxide be the sial composite oxides of 25%.
Embodiment 5:
Concrete preparation method is essentially identical with example 1, and difference is, oxide raw material used is containing two
Siliconoxide mass mark is in the sial composite oxides of 25%, and tungsten used-sial composite oxides, tungsten
Element is 1:39 with the mass ratio of sial composite oxides.
Embodiment 6:
Concrete preparation method is essentially identical with example 1, and difference is, oxide raw material used is containing two
Siliconoxide mass mark is in the sial composite oxides of 25%, and tungsten used-sial composite oxides, tungsten
Element is 1:19 with the mass ratio of sial composite oxides.
Embodiment 7: a kind of diesel vehicle oxidation catalyst with low temperature active, catalyst carrier is ferrum-chromium-aluminum
Metal beehive, volume is 1.101 liters, and hole density is 200 mesh/square feet；Coating contains tungsten-sial multiple
Closing oxide and molecular sieve, coating coated weight is 80 grams per liters；Noble metal is platinum, and the coated weight of noble metal platinum is
0.5 grams per liter.
Preparation method comprises the steps:
(1) equi-volume impregnating prepares tungsten-sial composite oxides: the bodies such as tungsten-sial composite oxides employing
Prepared by long-pending infusion process.In the sial combined oxidation raw material used, the mass fraction of dioxide-containing silica is
5%, remaining is aluminium sesquioxide.Weigh the sial composite oxides that quality is 990 grams, weigh 13.9 grams of tungsten
Acid ammonium dissolves, and is configured to the aqueous solution of sial composite oxides saturated extent of adsorption used, then by ammonium tungstate solution
Drop in sial composite oxide powder and continuously stirred 2 hours；Then stand, be aged 10 hours, it
After dry 12 hours at 100 DEG C, obtain tungsten-sial composite oxides 500 DEG C of roastings after 4 hours, preparation
In the tungsten obtained-sial composite oxides, wolfram element is 1:99 with the mass ratio of sial composite oxides.
(2) weigh deionized water 1400 grams, add tungsten-sial composite oxides 400 grams, molecular sieve 200
Gram, stir formation coating slurry, controls serous granule degree D90 and is about 5 microns；
(3) continue platinum nitrate is added in coating paste by whipping process, stir, form final slurry.
(4) take out after cordierite ceramic honeycomb matrix being soaked 0.5 minute in final slurry at this, then use
Internal to carrier surface and duct unnecessary serosity is blown down by compressed air, and purge time is 2 minutes, then puts
Being dried 3 hours at 100 DEG C in baking oven, in Muffle furnace, roasting 3 hours at 350 DEG C, i.e. obtain diesel vehicle
Oxidation catalyst.
Embodiment 8: a kind of diesel vehicle oxidation catalyst with low temperature active, catalyst carrier is cordierite
Ceramic honey comb, volume is 1.101 liters, and hole density is 600 mesh/square feet；Coating contains tungsten-sial multiple
Closing oxide and molecular sieve, coating coated weight is 180 grams per liters；Noble metal is platinum, the coated weight of noble metal platinum
It is 4.5 grams per liters.
Preparation method comprises the steps:
(1) equi-volume impregnating prepares tungsten-sial composite oxides: the bodies such as tungsten-sial composite oxides employing
Prepared by long-pending infusion process.In the sial combined oxidation raw material used, the mass fraction of dioxide-containing silica is
15%, remaining is aluminium sesquioxide.Weigh the sial composite oxides that quality is 990 grams, weigh 13.9 grams
Ammonium tungstate dissolves, and is configured to the aqueous solution of sial composite oxides saturated extent of adsorption used, then ammonium tungstate is molten
Drop adds in sial composite oxide powder and continuously stirred 8 hours；Then stand, be aged 6 hours,
Dry 12 hours at 170 DEG C afterwards, obtain tungsten-sial composite oxides 550 DEG C of roastings after 4 hours, system
In the standby tungsten-sial composite oxides obtained, wolfram element is 1:99 with the mass ratio of sial composite oxides.
(2) weigh deionized water 1400 grams, add tungsten-sial composite oxides 2000 grams, molecular sieve 200
Gram, stir formation coating slurry, controls serous granule degree D90 and is about 40 microns；
(3) continue platinum nitrate is added in coating paste by whipping process, stir, form final slurry.
(4) take out after cordierite ceramic honeycomb matrix being soaked 5 minutes in final slurry at this, then by pressure
Internal to carrier surface and duct unnecessary serosity is blown down by contracting air, and purge time is 3 minutes, is subsequently placed in
Being dried 2 hours at 170 DEG C in baking oven, in Muffle furnace, roasting 2 hours at 550 DEG C, i.e. obtain diesel vehicle oxygen
Change catalyst.
The catalyst preparing embodiment 1-6 carries out performance evaluation:
The catalyst sample prepared is carried out laboratory simulation distribution evaluation, distribution component list such as table 1 institute
Show.In sample evaluation procedure, temperature controller control electric furnace temperature programming, HC analyser, CO analyze
Instrument and SO2The concentration of each component of gas before and after reacting measured by analyser, obtains the conversion of sample under different temperatures
Rate, and thus obtain the T50 (conversion ratio is temperature when 50%) of sample.The T50 temperature of HC and CO
The lowest, show that the catalytic performance of catalyst is the best；And SO2T50 temperature the highest, then show catalyst
Sulfur resistive ability is the best.
Table 1 diesel vehicle simulation distribution composition
| Gas | Content | Gas | Content |
| HC(C3H8) | 200ppm | O2 | 10% |
| NO | 300ppm | SO2 | 50ppm |
| CO | 500ppm | H2O | 10% |
| CO2 | 6% | N2 | Remaining nitrogen |
T50 (HC, CO, SO of table 2 catalyst2)
| Sample | HC T50(℃) | CO T50(℃) |
| 1 | 229 | 103 |
| 2 | 212 | 101 |
| 3 | 235 | 110 |
| 4 | 215 | 104 |
| 5 | 203 | 98 |
| 6 | 227 | 112 |
| Comparative example | 232 | 110 |
The T50-aged (HC, CO) of table 3 aging state catalyst
| Sample | HC T50-aged(℃) | CO T50-aged(℃) |
| 1 | 279 | 132 |
| 2 | 261 | 129 |
| 3 | 282 | 138 |
| 4 | 264 | 131 |
| 5 | 252 | 125 |
| 6 | 278 | 139 |
| Comparative example | 321 | 152 |
As shown in Table 2, the HC of the diesel vehicle oxidation catalyst that the preparation method in the employing present invention obtains
Relatively low with the T50 temperature of CO, especially embodiment 5 preparation diesel vehicle oxidation catalyst HC and
The T50 temperature of CO reaches minimum and is respectively 203 DEG C and 98 DEG C, and SO2T50Temperature is 349 DEG C, table
This catalyst bright has preferable sulfur resistive ability.
As shown in Table 3, the aging state of diesel vehicle oxidation catalyst that the preparation method in the present invention obtains is used
Performance is obviously improved compared with comparative example, the diesel vehicle oxidation catalyst that wherein prepared by embodiment 5
HC-T50 relatively comparative example reduces 69 DEG C.
Claims (7)
1. a diesel vehicle oxidation catalyst with low temperature active, it is characterized in that: include carrier and the coating coated on carrier, coating is loaded with noble metal, described coating includes tungsten-sial composite oxides and molecular sieve, described noble metal is the mixture of one or both materials in Pt, Pd, the coated weight of described coating is 80-180 grams per liter, and the coated weight of described noble metal is 0.5-4.5 grams per liter.
There is the diesel vehicle oxidation catalyst of low temperature active the most as claimed in claim 1, it is characterised in that: described molecular sieve is 1:2～10 with the mass ratio of tungsten-sial composite oxides.
There is the diesel vehicle oxidation catalyst of low temperature active the most as claimed in claim 1, it is characterised in that: in described tungsten-sial composite oxides, wolfram element is 1:19～99 with the mass ratio of sial composite oxides.
There is the diesel vehicle oxidation catalyst of low temperature active the most as claimed in claim 1, it is characterised in that: in described sial composite oxides, silicon dioxide quality mark is 5～25wt%, and remaining is the sial of aluminium sesquioxide.
There is the diesel vehicle oxidation catalyst of low temperature active the most as claimed in claim 1, it is characterised in that: described molecular sieve is Hydrogen beta-molecular sieve.
There is the diesel vehicle oxidation catalyst of low temperature active the most as claimed in claim 1, it is characterised in that: described carrier is cordierite ceramic honeycomb or iron-chromium-aluminum metal honeycomb, and the hole density of described carrier is 200-600 mesh/square feet.
There is the preparation method of the diesel vehicle oxidation catalyst of low temperature active the most as claimed in claim 1, it is characterised in that: comprise the steps:
(1) equi-volume impregnating prepares tungsten-sial composite oxides: be that 1:19-99 weighs ammonium tungstate and sial composite oxides respectively by the mass ratio of wolfram element Yu sial composite oxides, ammonium tungstate aqueous solution is prepared by the saturated extent of adsorption of silicon-aluminium compound, the ammonium tungstate aqueous solution prepared is dropped in sial composite oxides and continuously stirred 2～8 hours, then stand, be aged 6～15 hours after dry under the conditions of 100～170 DEG C, and after 350～550 DEG C of roastings, obtain tungsten-sial composite oxides；
(2) preparation of coating slurry: to be 1:2～10 be added separately in deionized water stirring by tungsten-sial composite oxides and molecular sieve forms serosity by the mass ratio of molecular sieve Yu tungsten-sial composite oxides, tungsten-sial composite oxides and the gross mass of molecular sieve are 2:3～8 with the mass ratio of deionized water, then ball-milling technology is used to process serosity, controlling granule D90 is 5-40 μm, prepares coating slurry；
(3) according to the requirement that the coated weight of noble metal on carrier is 0.5-4.5 grams per liter calculating noble metal, the solution containing one or both materials in precious metals pt, Pd is joined in coating slurry, stirs, form final serosity；
(4) carrier cordierite ceramic honeycomb or iron-chromium-aluminum metal honeycomb are immersed in final serosity, take out after soaking 0.5～5min, compressed air is used to blow logical by the passage of carrier inside, purge time is 0.5～3min, then carrier is dried 3～8 hours under the conditions of 100～170 DEG C, finally by carrier roasting 2～3 hours under the conditions of 350～550 DEG C, i.e. obtain diesel vehicle oxidation catalyst.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106362792A (en) * | 2016-08-26 | 2017-02-01 | 江苏万路达环保科技有限公司 | Oxidation catalyst repairing sizing agent for light-duty diesel vehicle, preparation method and application thereof |
| CN106807432A (en) * | 2017-02-06 | 2017-06-09 | 无锡威孚环保催化剂有限公司 | A kind of Pt Pd bimetallic catalysts for NO oxidations and preparation method thereof |
| CN106823592A (en) * | 2017-03-15 | 2017-06-13 | 四川绵阳华元航升环保科技有限公司 | A kind of preparation method of light-duty diesel vehicle type oxide particle trap |
| CN106902865A (en) * | 2017-02-13 | 2017-06-30 | 无锡威孚环保催化剂有限公司 | Diesel vehicle particle oxidative catalyst and preparation method thereof |
| CN106902864A (en) * | 2017-03-09 | 2017-06-30 | 无锡威孚环保催化剂有限公司 | A kind of ammoxidation catalyst for diesel engine vent gas cleaning system and preparation method thereof |
| CN111330633A (en) * | 2020-03-10 | 2020-06-26 | 无锡威孚环保催化剂有限公司 | Diesel vehicle oxidation type catalyst with low-temperature adsorption capacity and preparation method thereof |
| CN115555013A (en) * | 2022-10-24 | 2023-01-03 | 华中师范大学 | Pt/silicon modified alumina-based catalyst and preparation method and application thereof |
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| JP2008296224A (en) * | 2008-09-02 | 2008-12-11 | Tokyo Roki Co Ltd | Nitrogen oxide removing catalyst, nitrogen oxide removing method using it, and nitrogen oxide removing device |
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