CN103861652A - Processing method of diesel engine tail gas oxidation catalytic carrier - Google Patents
Processing method of diesel engine tail gas oxidation catalytic carrier Download PDFInfo
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- CN103861652A CN103861652A CN201210545750.8A CN201210545750A CN103861652A CN 103861652 A CN103861652 A CN 103861652A CN 201210545750 A CN201210545750 A CN 201210545750A CN 103861652 A CN103861652 A CN 103861652A
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- diesel engine
- catalyst
- gas oxidation
- carrier
- tail gas
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Abstract
The invention discloses a processing method of a diesel engine tail gas oxidation catalytic carrier. According to the processing method, the diesel engine tail gas oxidation catalytic carrier is subjected to ultrasonic cleaning. After ultrasonic cleaning, pore walls of the diesel engine tail gas oxidation catalytic carrier are cleaner; loading is more uniform; channel performance is more excellent; pressure drop is lower; and the diesel engine tail gas oxidation catalytic carrier is more suitable to be used as a diesel engine tail gas oxidation catalytic carrier.
Description
Technical field
The invention belongs to diesel engine vent gas and administer field, relate in particular to a kind of processing method of diesel engine vent gas oxidation catalysis carrier.
Background technology
Over nearly 20 years, in the face of the increasingly exhausted pressure bringing to social development of world petroleum resource, in the face of the impact of automobile pollution sharp increase on environment, world car is ceaselessly realized the solution of auto industry sustainable development in searching, in continuous technical development, people have had renewal to diesel engine for automobile and diesel vehicle, more deep understanding, diesel engine compared with gasoline engine economical, under the superior prerequisite of dynamic property, bring certain negative property for the pollution of environment, gasoline engine relatively, the CO that diesel emission goes out, HC is only ten parts of gasoline exhaust, NO
xremain basically stable, but PM(carbon granule thing) be 30～80 times of gasoline exhaust, PM mainly contains solid carbon particulate (following represent with " SOOT "), sulfate (following represent with " sulfates ") and liquid large molecule hydrocarbon particulate (following with " SOF " expression).The particle diameter of PM is generally at 0.01 μ m～10 μ m, and wherein 90% diameter of particle < 1 μ m, so easily float in air and by respiratory tract and enter human body.Therefore, government formulate relevant policies are to strengthen the control to diesel engine PM discharge.Meanwhile, when the optimized operation of diesel engine, the discharge capacity of diesel engine PM has obvious reduction, by adherence pressure and coordinate the Electronic Control of the fuel injection system of timing to realize.But be difficult to reach the satisfaction of expection.How to make a kind of oxidation catalyst in the face of small displacement diesel engine of exploitation, do not changing car load physical state and do not needing under the prerequisite of too much additional auxiliary equipment, CO, HC, PM can be purified at a lower temperature simultaneously, can also face the test of high sulfur content fuel, this can solve the treating tail gas problem of existing diesel.
For the Catalysts and its preparation method (CN1575850A) of purifying waste gas from diesel engine, a kind of Catalysts and its preparation method for purifying waste gas from diesel engine is disclosed, catalyst is removed HC, CO and the SOF in diesel exhaust and is reduced the discharge of particulate.Have for the catalyst of purifying waste gas from diesel engine the catalytic component being deposited on infusibility three-dimensional structure, catalytic component comprises silica-alumina and zeolite, and silica-alumina supports at least one and be selected from the precious metal element of platinum, palladium, rhodium.This catalyst is by joining noble metal component in the slurries of silica-alumina, cause therein chemisorbed, then zeolite is added in the mixture of gained, thereby obtain being loaded with the silica-alumina of noble metal and the mixed serum of zeolite, infusibility three-dimensional structure is immersed in described mixed serum, cause therein the deposition of catalyst component, roasting resulting composition makes subsequently.But the carrier of the catalyst in this application is inhomogeneous, the decentralization of active component in carrier is not high, thereby causes the purifying rate of soot low; And the pressure drop of this catalyst carrier is high.
Reduce the catalyst (CN101056692A) of the not platinum group metal of ignition temperature of particulates on diesel particulate filter, provide a kind of catalytic type diesel particulate filter (CDPF) and a kind of from diesel engine exhaust the method for filtration of particulate matters, wherein catalytic type diesel particulate filter comprises a kind of base material and a kind of carbon monoxide-olefin polymeric, wherein carbon monoxide-olefin polymeric comprises at least one first component, at least one second component and at least one the 3rd component, wherein the first component is at least one selected from cerium, first component of lanthanide series and composition thereof, second component is at least one is selected from cobalt, copper, the second component of manganese and composition thereof: the 3rd component comprises strontium, wherein the first component, after second component and the 3rd component roasting, be oxide form.By particle redox reaction on filter, the Catalysts for Reducing on catalytic type diesel particulate filter remove the temperature of particle from CDPF.Catalytic type diesel particulate filter also can comprise wash coat.The wash coat being made by colloidal alumina has higher surface area and pore volume than the wash coat that contains the aluminium oxide that aluminum nitrate makes.But it is too high that the shortcoming of this catalyst is pressure drop, after long-time use, can cause the obstruction of soot in cell walls, increased considerably the oil consumption of vehicle simultaneously.
A kind of for eliminating the low-temperature combustion catalyst (CN101767012A) of diesel engine carbon black, disclose and a kind ofly do not contained alkali metal and noble metal for eliminating the low-temperature combustion catalyst of diesel engine carbon black, composition is the composite oxides of ferrocerium zirconium, wherein CeO
2molar content be 50%, Fe
2o
3molar content be 5～50%, ZrO
2molar content be 45～0%, the method of preparation has two kinds, method one is co-precipitation hydrothermal synthesis method, method two is mechanical mixing, the concrete steps of method one are: the nitrate of getting Ce, Fe, Zr is configured to by stoichiometric proportion the salting liquid that total concentration is 0.1～0.5mol/L, then adds appropriate H
2o
2, fully stir, evenly mix.Under vigorous stirring, above-mentioned mixed solution is splashed in the ammoniacal liquor of 3～8mol/L with the speed of 2～10mL/min, be precipitated thing.Precipitation completely rear continuation stirs 30～120min, removes part supernatant liquor after aging 30～180min, gained sediment is moved in autoclave (compactedness is 50～70%), in 160～240 ℃ of insulation 24～72h.After products therefrom washs respectively with deionized water and ethanol, 80～120 ℃ of dry 6～24h, obtain target catalyst.This material has very high catalytic activity and heat endurance, and environment is not polluted.The shortcoming of this catalyst is not resistance to sulphur, after long-time use, can cause catalyst poisoning because of the obstruction of the stickums such as thiamines, and this poisoning be irreversible procedure, and be not suitable for diesel engine condition.
The Catalysts and its preparation method (CN1315228) of purifying waste gas from diesel engine, relates to the catalyst of purifying waste gas from diesel engine.This catalyst contains at least one zeolite, and, contain in addition at least one support oxide that is selected from aluminium oxide, silica, titanium dioxide and alumina silicate and at least one noble metal that is selected from platinum, palladium, rhodium and iridium.The feature of this catalyst is that the average oxidation number of precious metal atom is less than 2.5, is to be greater than 3 metal ligand and to be less than the average of 3 oxygen part.In zeolite and support oxide, the microcrystalline form of precious metal atom take average grain diameter as 1～6nm exists.The defect of this invention is that the arresting efficiency of soot is low, and graininess is not suitable for diesel engine condition.
From diesel exhaust, remove catalytic filter and the manufacture method (CN1774285) thereof of soot particulates, a kind of catalytic filter has been described, for removing soot particulates from diesel exhaust, this catalytic filter comprises the monolithic oxidation catalyst of its upstream, can the efficient oxidation gaseous contaminant and volatile organic constituents, also comprise the wall-flow filter of downstream catalyst, for being collected in the low temperature ignition of the soot particulates on filter.The present invention also provides the manufacture method of this catalytic filter, comprises the colloid admixture solution of preparing platinum group metal salts and other slaine with water-soluble polymer and reducing agent, this solution is flooded in catalyst carrier, subsequently high-temperature roasting.In the present invention, adopt this catalytic filter to provide alleviating diesel exhaust pollutant is particulate matter (PM) and gaseous contaminant (HC, CO, NO
x) discharge effective measures.This catalyst-assembly is loaded down with trivial details, and cost is higher, has increased the treating tail gas cost of diesel engine.And this catalyst pressure drop is high, high to oil product requirement, be not suitable for diesel engine condition.
Summary of the invention
First the present invention provides a kind of processing method of diesel engine vent gas oxidation catalysis carrier, and the method is: diesel engine vent gas oxidation catalysis carrier is carried out to ultrasonic cleaning;
Specifically, the method for ultrasonic cleaning is: in cleaning process, regulating pH is 1～3, and frequency is 50Hz, and power is 100W, and the ultrasonic cleaning time is 100～500min; Wherein regulating the reagent that pH uses is hydrofluoric acid.
The method of this ultrasonic cleaning is applicable to the carrier of ceramic honeycomb, is also applicable to metallic carrier or soft metal carrier;
Carrier hole wall after ultrasonic cleaning is cleaner, and load is more even, and passage is better, and pressure drop is lower.
The present invention also provides a kind of carrier of diesel engine vent gas oxidation catalyst, and this carrier is ceramic honeycomb, and this ceramic honeycomb is ultrasonic cleaning.
Wherein ceramic honeycomb is preferably cordierite; Oxide mass ratio in its composition is MgO13.7%, Al
2o
334.9%, SiO
251.4%; Before ultrasonic cleaning, the density of blank cordierite ceramic honeycomb is 400～450g/l;
Wherein the method for ultrasonic cleaning is: in cleaning process, adding hydrofluoric acid and regulating pH is 1～3, and frequency is 50Hz, and power is 100W, and the ultrasonic cleaning time is 100～500min.
Ceramic honeycomb after ultrasonic cleaning, its cell walls specific area improves 40～50m
2/ g.
The present invention also provides a kind of diesel engine vent gas oxidation catalyst, and this catalyst is to prepare take the ceramic honeycomb of above-mentioned ultrasonic cleaning as carrier.
Specifically, this catalyst prepares by the following method:
The ceramic honeycomb carrier of above-mentioned ultrasonic cleaning is inserted in the coating colloid after ageing and soaked load, and soak time is 1-10min; Carrier after load is dried and roasting and obtaining.
Wherein said coating colloid is that modified powder, modified molecular screen, polyvinyl alcohol and water are obtained through high speed shear emulsification, and the speed of wherein shearing is 100-500r/min;
Wherein the mass ratio of modified powder, modified molecular screen, polyvinyl alcohol and water is 40～50:20～40:0.5～1.5:70～90;
Wherein modified powder carries out modification to gama-alumina by precursor Ludox and tetrabutyl titanate simultaneously and obtains, wherein design parameter presoma Ludox is the precursor Ludox of silica and titanium dioxide, and wherein the mass ratio of silica, titanium dioxide and gama-alumina is 28:26:46;
The fresh state of specific area of the gama-alumina of selecting is 260m
2/ g is 180m after 1150 ℃ of aging 24h
2/ g.
Wherein modified molecular screen is: the platinum nitrate solution that is 10-30% by mass concentration carries out modification to molecular sieve and obtains; Wherein in platinum nitrate solution, the weight ratio of platinum simple substance and molecular sieve is 0.5～1:30～60; The silica alumina ratio example of molecular sieve is 60～200; The silica alumina ratio example of preferred molecular sieve is 150;
Modified molecular screen adopts kneader to carry out modification, and wherein the dropping flow of platinum nitrate solution is 0.5～5ml/min, and kneader rotating speed is 24～38r/min, and kneading time is 2～10h.
Coating colloid after ageing refers to above-mentioned coating colloid is added ammonium humate to carry out ageing and obtained; Wherein the addition of ammonium humate is 0.1～1% of coating adhesive body weight, and digestion time is 2～10 days.
In particular, this diesel engine vent gas oxidation catalyst prepares by the following method:
1. with sonic oscillation cleaning ceramic honeycomb; 2. obtain modified powder with the silica sol modified gama-alumina of precursor of silica and titanium dioxide; 3. with platinum nitrate solution, molecular sieve is carried out to modification and obtain modified molecular screen; 4. add polyvinyl alcohol and water to stir modified powder, modified molecular screen, under high speed shear emulsification condition, prepare coating colloid, wherein the mass ratio of modified powder, modified molecular screen, polyvinyl alcohol and water is 40～50:20～40:0.5～1.5:70～90; 5. ammonium humate adds in coating colloid and carries out ageing, and the addition of ammonium humate is 0.1～1% of coating adhesive body weight, and digestion time is 2～10 days; 6. the ceramic honeycomb after ultrasonic cleaning is inserted in the coating colloid after ageing and soaked load, the thickness of load coating is 0.05～0.08mm; 7. be dried, baking temperature is 80～150 ℃, and be 1～5h drying time; 8. carry out roasting, sintering temperature is 400～600 ℃, and roasting time 1～10h, to obtain final product.
The catalyst preparing is oxidation catalyst, can solve carbon soot particles material (PM) and gaseous contaminant (HC, CO, NO
x) emission problem, improved the sulfur resistance of catalyst simultaneously, reduced the oxidizing fire temperature of soot.
The present invention also provides the method for preparing the method for above-mentioned diesel engine vent gas oxidation catalyst carrier and preparing diesel engine vent gas oxidation catalyst.
Ceramic honeycomb is carried out to ultrasonic cleaning, and in cleaning process, adding hydrofluoric acid and regulating pH is 1～3, and frequency is 50Hz, and power is 100W, and the ultrasonic cleaning time is 100～500min.Can obtain diesel engine vent gas oxidation catalyst carrier.
The preparation method of diesel engine vent gas oxidation catalyst is:
The ceramic honeycomb carrier of above-mentioned ultrasonic cleaning is inserted in the coating colloid after ageing and soaked load; Carrier after load is dried and roasting and obtaining.Wherein the ageing of coating colloid and coating colloid sees above.
Object feature of the present invention is: 1. the precursor Ludox of this process using silica, titanium dioxide carries out modification to gama-alumina simultaneously, by precursor Ludox, tetrabutyl titanate, gama-alumina is carried out to modification, sulphur composition in diesel engine vent gas can be adsorbed, avoid the generation of sulfate, improved the sulfur resistance of catalyst; 2. adopt platinum nitrate solution to the quoting of molecular sieve modified and molecular sieve, improved active sites quantity and the sulfur resistance of platinum; 3. adopt ultrasonic washing instrument to process ceramic honeycomb, improved the microcellular structure of cell walls, improved the specific area of micropore; 4. adopt ammonium humate to carry out ageing to coating colloid, improved the density of coating, reduced the thickness of coating, thereby reduced the combustion oxidation temperature of soot; 5. rational coated designs scheme, makes catalyst have low temperature active.The oxidation catalyst processing that the present invention obtains is applied to the test of 1.5L common rail diesel engine tail gas clean-up and shows, gas reaction temperature keeps carbon soot particles to have more than 40% transformation efficiency at 180～420 ℃, carbon monoxide and hydrocarbon have more than 90% transformation efficiency, reduce the oxidizing fire temperature of soot particle simultaneously, solved diesel engine because of the too low technical barrier that cannot administer soot of delivery temperature.
With cordierite (2MgO2Al
2o
35SiO
2) the ceramic honeycomb diesel engine vent gas oxidation catalyst that is carrier, can comprehensive regulation carbon soot particles material (PM) and gaseous contaminant (HC, CO, NO
x) discharge, especially adopt titanium dioxide, silica precursor Ludox gama-alumina to be carried out to modification simultaneously, improved the absorption of coating material to sulphur in diesel engine vent gas, promoted the sulfur resistance of catalyst; Modification by platinum to molecular sieve, has increased the active sites quantity of catalyst, has improved the oxidability of catalyst.There is higher pollutant removing rate, preferably sulfur resistance, longer service life.Catalyst of the present invention also reduces the ignition temperature of soot, by the improvement of cell walls microcellular structure, increase the contact area discharging pollutants with catalyst, reduced catalytic reaction temperature, solved diesel exhaust gas temperature too low and cannot high efficiency carry out the difficult problem of rear waste gas pollution control and treatment.
The specific embodiment
Raw material used in the following example is commercially available prod.
Embodiment 1 Kaolinite Preparation of Catalyst carrier
Cordierite-quality honeycombed ceramics is placed in to ultrasonic instrument and cleans, in cleaning process, adding hydrofluoric acid and regulating pH is 2, and frequency is 50Hz, and power is 100W, and the ultrasonic cleaning time is 200min, obtains the catalyst carrier that hole wall is cleaner.
Embodiment 2 Kaolinite Preparation of Catalyst carriers
Cordierite-quality honeycombed ceramics is placed in to ultrasonic instrument and cleans, in cleaning process, adding hydrofluoric acid and regulating pH is 1, and frequency is 50Hz, and power is 100W, and the ultrasonic cleaning time is 400min, obtains the catalyst carrier that hole wall is cleaner.
The preparation of embodiment 3 diesel engine vent gas oxidation catalysts
Prepare modified powder: gama-alumina is carried out to modification by silica, titanium dioxide precursor Ludox, tetrabutyl titanate simultaneously, temperature is 150 ℃, pressure is 10 MPas, and wherein the mass ratio of silica, titanium dioxide and gama-alumina is 28:26:46;
Prepare modified molecular screen: the platinum nitrate solution that is 10% by mass concentration carries out modification to molecular sieve and obtains; Wherein in platinum nitrate solution, the weight ratio of platinum simple substance and molecular sieve is 1:30; The silica alumina ratio example of molecular sieve is 150;
Be that 45:30:1:80 mix with water according to mass ratio by modified powder, modified molecular screen, polyvinyl alcohol, carry out high speed shear emulsification, the speed of shearing is 150r/min, thereby obtains coating colloid;
Coating colloid is added and in ammonium humate, carries out oldly, and the addition of ammonium humate is 0.5% of coating adhesive body weight, and digestion time is 5 days;
The ceramic honeycomb of the ultrasonic cleaning preparing in embodiment 1 is inserted in the coating colloid after ageing and soaked load, and the thickness of load coating is 0.06mm;
Be dried, baking temperature is 110 ℃, and be 2h drying time;
Carry out roasting, sintering temperature is 550 ℃, and roasting time 6h, to obtain final product.
Prepare with cordierite (2MgO2Al
2o
35SiO
2) diesel engine vent gas oxidation catalyst that ceramic honeycomb is carrier, product size is Φ 118.4mm × 127mm, hole density is 62 holes/cm
2.The contained active component of oxidation catalyst is platinum, and the mass ratio of platinum is 1.0%.
The preparation of embodiment 4 diesel engine vent gas oxidation catalysts
Prepare modified powder: gama-alumina is carried out to modification by silica, titanium dioxide precursor Ludox, tetrabutyl titanate simultaneously, by precursor Ludox, tetrabutyl titanate to gama-alumina modification, temperature is 150 ℃, pressure position 10 MPas, wherein the mass ratio of silica, titanium dioxide and gama-alumina is 25:26:40;
Prepare modified molecular screen: the platinum nitrate solution that is 10% by mass concentration carries out modification to molecular sieve and obtains; Wherein in platinum nitrate solution, the weight ratio of platinum simple substance and molecular sieve is 1:30; The silica alumina ratio example of molecular sieve is 120;
Be that 45:30:1:80 mix with water according to mass ratio by modified powder, modified molecular screen, polyvinyl alcohol, carry out high speed shear emulsification, the speed of shearing is 150r/min, thereby obtains coating colloid;
Coating colloid is added and in ammonium humate, carries out oldly, and the addition of ammonium humate is 0.5% of coating adhesive body weight, and digestion time is 5 days;
Ceramic honeycomb after the ultrasonic cleaning preparing in embodiment 2 is inserted in the coating colloid after ageing and soaked load, and the thickness of load coating is 0.06mm;
Be dried, baking temperature is 140 ℃, and be 1h drying time;
Carry out roasting, sintering temperature is 500 ℃, and roasting time 6h, to obtain final product.
Prepare with cordierite (2MgO2Al
2o
35SiO
2) diesel engine vent gas oxidation catalyst that ceramic honeycomb is carrier, product size is Φ 118.4mm × 127mm, hole density is 31 holes/cm
2.The contained active component of oxidation catalyst is platinum, and the mass ratio of platinum is 1.0%.
Embodiment 5 catalyst activity evaluations
Catalyst activity evaluation adopts rail 1.5L diesel engine altogether to carry out the detection of car load emission testing, and test specification is according to rules IV stage requirement in " light-duty vehicle pollutant emission limit and measuring method (Chinese III, IV stage) ".
Catalyst is installed and complete vehicle test, diesel fuel injection system is high-pressure common rail, waste gas purification technology path is EGR+DOC(EGR+diesel oxidation catalyst), fresh state and aging state emission result are respectively in table 1, table 2, vehicle is SUV, engine fuel injection system is high-pressure common rail, discharge capacity 2.3L, and the durable 80000km of real vehicle is undertaken by car load degradation condition.Wherein, according to the distribution in temperature field in gas extraction system, get two temperature field points at every turn and carry out catalyst installation and measuring while measurement, temperature field point goes respectively 180 ℃, 420 ℃.Remarks: (aging condition: rules IV stage life requirement in " light-duty vehicle pollutant emission limit and measuring method (Chinese III, IV stage) ".）
The catalyst application 1.5L common rail diesel engine cleaning test of embodiment 3 shows, gas reaction temperature all keeps carbon soot particles to have more than 40% transformation efficiency at 180 ℃ and 420 ℃, carbon monoxide and hydrocarbon have more than 90% transformation efficiency, use in conjunction with EGR+DOC overall evaluation of a technical project, can meet Europe IV and above Abgasgesetz.
Finding by embodiment 3, embodiment 4, is 62 holes/cm in carrier hole density
2purification efficiency be 31 holes/cm higher than hole density
2purification efficiency.
The fresh state testing result of table 1
The durable state testing result of table 2 real vehicle 80000km
Claims (2)
1. a processing method for diesel engine vent gas oxidation catalysis carrier, is characterized in that the method is that diesel engine vent gas oxidation catalysis carrier is carried out to ultrasonic cleaning.
2. processing method according to claim 1, is characterized in that the concrete grammar of described ultrasonic cleaning is: in cleaning process, regulating pH is 1～3, and frequency is 50Hz, and power is 100W, and the ultrasonic cleaning time is 100～500min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210545750.8A CN103861652A (en) | 2012-12-14 | 2012-12-14 | Processing method of diesel engine tail gas oxidation catalytic carrier |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210545750.8A CN103861652A (en) | 2012-12-14 | 2012-12-14 | Processing method of diesel engine tail gas oxidation catalytic carrier |
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ID=50901015
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| CN101653730A (en) * | 2009-08-26 | 2010-02-24 | 南京英斯威尔环保科技有限公司 | Three-way catalyst taking cordierite honeycomb ceramics as carrier |
| CN102133537A (en) * | 2010-12-29 | 2011-07-27 | 浙江工业大学 | Honeycomb-ceramic-type monolithic catalyst, and preparation method and application thereof |
| CN102513131A (en) * | 2011-12-09 | 2012-06-27 | 十堰市登喜路实业有限公司 | Catalyst for purification of tail gas produced by military diesel offroad vehicle and coating method thereof |
-
2012
- 2012-12-14 CN CN201210545750.8A patent/CN103861652A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59142851A (en) * | 1983-02-02 | 1984-08-16 | Nippon Shokubai Kagaku Kogyo Co Ltd | Catalyst for cleaning exhaust gas |
| CN1271623A (en) * | 1999-04-09 | 2000-11-01 | 株式会社电装 | Ceramic carrier capable of loading catalyst, catalyst ceramic body and manufacturing method thereof |
| CN1995713A (en) * | 2006-12-13 | 2007-07-11 | 北京英泰世纪环境科技有限公司 | Metal carrier triple-effect catalytic unit and method for making same |
| CN101653730A (en) * | 2009-08-26 | 2010-02-24 | 南京英斯威尔环保科技有限公司 | Three-way catalyst taking cordierite honeycomb ceramics as carrier |
| CN102133537A (en) * | 2010-12-29 | 2011-07-27 | 浙江工业大学 | Honeycomb-ceramic-type monolithic catalyst, and preparation method and application thereof |
| CN102513131A (en) * | 2011-12-09 | 2012-06-27 | 十堰市登喜路实业有限公司 | Catalyst for purification of tail gas produced by military diesel offroad vehicle and coating method thereof |
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Application publication date: 20140618 |
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