CN104117381B - Diesel vehicle oxidative catalyst containing Al-Si-Ti composite oxides - Google Patents
Diesel vehicle oxidative catalyst containing Al-Si-Ti composite oxides Download PDFInfo
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- CN104117381B CN104117381B CN201410396471.9A CN201410396471A CN104117381B CN 104117381 B CN104117381 B CN 104117381B CN 201410396471 A CN201410396471 A CN 201410396471A CN 104117381 B CN104117381 B CN 104117381B
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Abstract
The present invention relates to a kind of diesel vehicle oxidative catalyst containing Al Si Ti composite oxides, with cordierite honeycomb ceramic as carrier, with TiO2Being dispersant with Al Ti Si composite oxides, with molecular sieve as adsorbing material, zirconium nitrate is thermally-stabilised auxiliary agent, the catalyst with citric acid as binding agent, made by with precious metals pt and Pd as active component；The addition of noble metal is 5 ~ 200g/ft3.Preparation method of the present invention is simple, and the catalyst prepared uses mixed coating noble metal-coating active component, is possible not only to accurately control the content of noble metal and makes noble metal be evenly distributed, and catalyst effect is more preferable.
Description
Technical field
The present invention relates to a kind of diesel vehicle oxidative catalyst containing Al-Si-Ti composite oxides, belong to diesel vehicle oxygen
The property changed catalyst preparation technical field.
Background technology
Diesel vehicle oxidative catalyst (DOC) is a part of organic in CO, NO, HC and PM in the tail gas of oxidated diesel oil car
Dissolving in SOF, its coating is mainly made up of oxide coating and active noble metal constituent, and noble metal is the pass of oxidative catalyst
Key component, for diesel vehicle DOC, it is simply that utilize DOC can reduce the chemistry of HC, CO and SOF etc. in diesel engine vent gas anti-
The activation energy answered, makes these materials can carry out oxidation reaction at a lower temperature with the oxygen in tail gas, is converted into CO2With
H2O。
Oxygen diesel car tail gas refining catalyst generally comprises carrier, active coating two parts.Traditional diesel vehicle oxidized form
Catalyst mostly is Ti-base catalyst, and owing to Ti-base catalyst absorption noble metal ability is poor, noble metal can only use immersion coating
Technique, so that noble metal is difficult to accurately control, and owing to noble metal is concentrated mainly on coating surface, the most easily because of your gold
Belong to sintering and make catalysqt deactivation, the most easily make catalysqt deactivation because of sulfur poisoning so that durable not the reaching of catalyst is wanted
Ask, in order to meet the requirement of the Abgasgesetz of increasingly stringent, use mixed coating coating catalyst thus improve the durable of catalyst
Performance becomes inevitable requirement.
Summary of the invention
Present invention aims to existing diesel vehicle oxidative catalyst be not suitable for doing the mixed painting of serosity, noble metal
Absorbability difference and the shortcoming of skewness；Providing a kind of preparation method simple, in catalyst, the load capacity of noble metal can
Accurately control, the diesel vehicle oxidative catalyst that catalyst activity is high.
The present invention uses following technical scheme: a kind of diesel vehicle oxidisability containing Al-Si-Ti composite oxides is urged
Agent, with cordierite honeycomb ceramic as carrier, with TiO2It is dispersant with Al-Ti-Si composite oxides, with molecular sieve for absorption
Material, zirconium nitrate is thermally-stabilised auxiliary agent, the catalysis with citric acid as binding agent, made by with precious metals pt or Pd as active component
Agent, the addition of noble metal is 5～200g/ft3。
Further, described Al-Ti-Si composite oxides are made up of aluminium sesquioxide, titanium dioxide, silicon dioxide, its
Mass ratio is 0.5～0.7:0.2～0.4:0.05～0.2.
A kind of preparation method of the diesel vehicle oxidative catalyst containing Al-Si-Ti composite oxides, it is characterised in that:
Comprise the steps:
(1) River Bank Stability: TiO by a certain percentage2, AL-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide, lemon
Lemon acid, platinum nitrate solution and palladium nitrate solution join in deionized water, described component TiO2, AL-Ti-Si composite oxides,
ZSM-5 molecular sieve, zirconium dioxide, citric acid, platinum nitrate and Palladous nitrate. quality proportioning are 0.2～0.37:0.2～0.35:0.25
～0.45:0.02～0.1:0.01～0.05:0.00316～0.04295:0.0006043～0.02843, stir；
(2) ball milling: the serosity that configured is ground through planetary ball mill, the rotating speed of planetary ball mill be 250～
380 revs/min, the operation time is 3～6h, and serous granule degree to D90 is 2～20um；
(3) mensuration of solid content: take 10g serosity in dry pot, dry pot is placed in 550～600 DEG C of Muffle kiln roastings 10
～20min, it is cooled to room temperature, weighs its powder quality, by this quality divided by 10g, obtain slurry solid content；
(4) coating coating: be coated with quantitatively coating special plane, catalyst carrier be positioned at application chamber, according to painting
The amount of covering is that the 80～180g/L solid contents requiring and recording calculate the wet weightening finish of target, and the serosity calculated is joined slurry dish
In, quantitatively coat；
(5) dry: the catalyst coated, through 100 DEG C～180 DEG C of flash bakings, dries 3～6h, by the water in coating
Evaporate；
(6) roasting: drying rear catalyst is put in Muffle furnace, 450 DEG C～550 DEG C of roasting 1h～2h, after insulation terminates
It is cooled to room temperature, calculates catalyst practical coating amount.
Further, the bullion content in serosity is measured after (3) by described step, by the serosity with noble metal
Take 20g to be centrifuged, carry out Solid-Liquid Separation, take solid phase and use ICP to carry out the mensuration of content.
Further, the mass ratio of described precious metals pt and Pd is 1/2～1/7.
Further, described molecular sieve uses ZSM-5 molecular sieve.
Preparation method of the present invention is simple, and the catalyst prepared uses mixed coating noble metal-coating active component, not only may be used
Making noble metal be evenly distributed accurately to control the content of noble metal, catalyst effect is more preferable.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated.Three below example all uses a diameter of
The cylindrical ceramic carrier of 80mm, a height of 60mm, volume is 0.301L, and vehicle weight is 97g, and the concentration of precious metals pt is
0.138g (noble metal)/g (liquid), the concentration of precious metals pd is 0.1511g (noble metal)/g (liquid).
Embodiment one: a kind of preparation containing Al-Ti-Si composite oxides oxidation catalyst, noble metal addition according to
5g/ft3Calculate, precious metals pt/precious metals pd is 7/1, coated weight according to 80g/L, the wherein group of Al-Ti-Si composite oxides
Become aluminium sesquioxide, titanium dioxide, silicon dioxide quality than for 0.5:0.2:0.05, comprise the steps:
(1) River Bank Stability: by a certain percentage by TiO2, Al-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide,
Citric acid, platinum nitrate solution, palladium nitrate solution join in deionized water, and its mass ratio is 0.3:0.2:0.35:0.1:0.05:
0.01399:0.001826, stirs；
(2) serosity ball milling: serosity grinds through planetary ball mill, and the rotating speed of planetary ball mill is 250 revs/min, fortune
The row time is 6h, serous granule degree to D90 be 3.23um, pH be 3.14；
(3) mensuration of solid content: take 10g serosity in dry pot, dry pot is placed in 600 DEG C of Muffle kiln roasting 10min, cold
But to room temperature, weighing its powder quality is 3.86g, and by this quality divided by 10g, just obtaining slurry solid content is 38.6%；
(4) bullion content measures: takes 20g serosity and is placed in test tube, puts in centrifuge centrifugal, carries out solid liquid phase and divide
From, use ICP to measure precious metals pt, the content of Pd in solid phase, the content recording precious metals pt is 0.00192g (noble metal)/g
(powder body), the content of precious metals pd is 0.000275g (noble metal)/g (powder body).
(5) coating coating: be coated with quantitatively coating special plane, is 80g/L requirement according to coated weight and consolidating of recording contains
It is 62.4g that amount calculates the wet weightening finish of target, is joined by serosity in slurry dish and quantitatively coats；
(6) dry: the catalyst coated dries 6h through 100 DEG C, is evaporated by the water in coating；
(7) roasting: drying rear catalyst is put in Muffle furnace, 450 DEG C of roasting 2h, insulation is cooled to room temperature after terminating,
Weighing catalyst weight is 121.2g.
Embodiment two: a kind of preparation containing Al-Ti-Si composite oxides oxidation catalyst, noble metal addition according to
34g/ft3Calculating, precious metals pt/precious metals pd ratio uses 3/1, coated weight according to 120g/L, wherein Al-Ti-Si composite oxygen
Compound consist of aluminium sesquioxide, titanium dioxide, silicon dioxide quality than for 0.6:0.3:0.1, comprise the steps:
(1) River Bank Stability: by a certain percentage by TiO2, Al-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide,
Citric acid, platinum nitrate solution, palladium nitrate solution join in deionized water, and its ratio is 0.37:0.35:0.25:0.02:
0.01:0.0891:0.03599, stirs；
(2) serosity ball milling: serosity grinds through planetary ball mill, and the rotating speed of planetary ball mill is 330 revs/min, fortune
The row time is 4h, serous granule degree to D90 be 3.33um, pH be 3.23；
(3) mensuration of solid content: take 10g serosity in dry pot, dry pot is placed in 600 DEG C of Muffle kiln roasting 10min, cold
But to room temperature, weighing its powder quality is 3.96g, and by this quality divided by 10g, just obtaining slurry solid content is 39.6%；
(4) in serosity, bullion content measures: takes 20g serosity and is placed in test tube, puts in centrifuge centrifugal, carries out solid-liquid
Being separated, use ICP to measure precious metals pt, the content of Pd in solid phase, the content recording precious metals pt is 0.00743g (your gold
Belong to)/g (powder body), the content of precious metals pd is 0.00245g (noble metal)/g (powder body)；
(5) coating coating: be coated with quantitatively coating special plane, serosity joined in slurry dish and be coated, according to painting
The amount of covering be 120g/L require and the solid content that records to calculate the wet weightening finish of target be 91.2g, serosity is joined slurry dish is carried out fixed
Amount coating；
(6) dry: the catalyst coated dries 4h through 150 DEG C, is evaporated by the water in coating；
(7) roasting: put in Muffle furnace by drying rear catalyst, 500 DEG C of roasting 1.5h, insulation is cooled to room after terminating
Temperature, weighing catalyst weight is 132.5g.
Embodiment three: a kind of preparation containing Al-Ti-Si composite oxides oxidation catalyst, noble metal addition according to
200g/ft3Calculate, its precious metals pt/precious metals pd is 2/1, coated weight according to 180g/L, wherein Al-Ti-Si composite oxides
Consist of aluminium sesquioxide, titanium dioxide, silicon dioxide quality than for 0.7:0.4:0.2, comprise the steps:
(1) River Bank Stability: by a certain percentage by TiO2, Al-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide,
Citric acid, platinum nitrate solution, palladium nitrate solution join in deionized water, and its ratio is 0.2:0.29:0.45:0.03:0.03:
0.31076:0.18818, stirs；
(2) serosity ball milling: serosity grinds through planetary ball mill, and the rotating speed of planetary ball mill is 380 revs/min, fortune
The row time is 3h, and serous granule degree is 3.13um, and surveying pH is 3.17；
(3) mensuration of solid content: take 10g serosity in dry pot, dry pot is placed in 550 DEG C of Muffle kiln roasting 20min, cold
But to room temperature, weighing its powder quality is 3.88g, and by this quality divided by 10g, just obtaining slurry solid content is 38.8%；
(4) serosity solid phase bullion content measures: takes 20g serosity and is placed in test tube, puts in centrifuge centrifugal, carries out solid
Liquid phase separation, uses ICP to measure precious metals pt, the content of Pd in solid phase, and the content recording precious metals pt is 0.02942g (your gold
Belong to)/g (powder body), the content of precious metals pd is 0.0130g (noble metal)/g (powder body)；
(5) coating coating: be coated with quantitatively coating special plane, joins serosity in slurry dish and according to coated weight is
It is 139.6g that the solid content that 180g/L requires and records calculates the wet weightening finish of target, is joined by serosity in slurry dish and is quantitatively coated with
Cover；
(6) dry: the catalyst coated dries 3h through 180 DEG C, is evaporated by the water in coating；
(7) roasting: drying rear catalyst is put in Muffle furnace, 550 DEG C of roasting 1h, insulation is cooled to room temperature after terminating,
Weighing catalyst weight is 150.6g.
The catalyst of embodiment two preparation is carried out activity rating.
One, catalyst fresh state activity rating
Test is carried out in tube furnace.
Method of testing: will be containing NO, CO2、H2O、C3H8, the gaseous mixture of CO be passed through in high temperature reaction stove, wherein NO:
300ppm, CO:500ppm, C3H8: 300ppm, H2O:6%, CO2: 6%；Heating rate is 10 DEG C/min, is eventually raised to 500 DEG C.
Test result is shown in Table 1
Table 1 fresh state catalyst activity evaluation result
As shown in Table 1, the initiation temperature T50 of HC and CO of the catalyst prepared by embodiment two is respectively 318 DEG C and 136
℃；NO is converted into NO2Maximum conversion be 78.5%.
Two, heat ageing rear catalyst activity rating is investigated:
Pre-treatment: be first placed in Muffle furnace by catalyst aging, aging temperature is 750 DEG C, and ageing time is 20h, so
After again the conversion ratio of NO, CO and HC in vehicle exhaust respectively is investigated.
Test is carried out in high temperature reaction stove.
Method of testing: will be containing NO, CO2、H2O、C3H8, the gaseous mixture of CO be passed through in high temperature reaction stove, wherein NO:
300ppm, CO:500ppm, C3H8: 300ppm, H2O:6%, CO2: 6%；Heating rate is 10 DEG C/min, is eventually raised to 500 DEG C.
Test result is shown in Table 2.
Table 2 heat ageing state catalyst activity evaluation result
As shown in Table 2, the HC initiation temperature T50 after heat ageing of the catalyst prepared by embodiment two is 360 DEG C, CO
Initiation temperature T50 is 159 DEG C, and NO generates NO2Conversion ratio be 70%, NO2Granule can be carried out effectively by the raising of conversion ratio
Process.
Three, sulfur aging rear catalyst activity rating
Pre-treatment: the catalyst of preparation is placed in Muffle furnace, is passed through SO2, 100ppm, heating-up temperature 350 DEG C, the time
10h, investigates the conversion ratio of NO, CO and HC in vehicle exhaust the most respectively.
Test is to carry out in high temperature reaction stove.
Method of testing: will be containing NO, CO2、H2O、C3H8, the gaseous mixture of CO be passed through in high temperature reaction stove, wherein NO:
300ppm, CO:500ppm, C3H8: 300ppm, H2O:6%, CO2: 6%；Heating rate is that every min heats up 10 DEG C, is eventually raised to
500℃。
Test result is shown in Table 3.
Table 3 sulfur aging catalyst Activity evaluation
From the data in table 3, it can be seen that the catalyst of embodiment two preparation is 345 DEG C to HC initiation temperature T50 after over cure is aging,
CO initiation temperature is 140 DEG C；NO generates NO2Maximum conversion be 73%.
Four, the evaluation of car load catalyst activity is investigated:
Use the catalyst of preparation in embodiment two to carry out complete vehicle test, detect the quality of the pollutant of every kilometer of discharge.
Table 4, car load Catalyst test results
From table 4 experimental result, the catalyst prepared by embodiment two contributes to the minimizing of HC, CO pollutant, PM
Grain thing also has significantly minimizing, it is seen that prepared by the present invention has preferably containing Al-Ti-Si composite oxides oxidation catalyst
Catalytic effect.
Claims (4)
1. a preparation method for the diesel vehicle oxidative catalyst containing Al-Si-Ti composite oxides, described containing Al-Si-
The diesel vehicle oxidative catalyst of Ti composite oxides, with cordierite honeycomb ceramic as carrier, with TiO2It is combined with Al-Ti-Si
Oxide is dispersant, and with molecular sieve as adsorbing material, zirconium dioxide is thermally-stabilised auxiliary agent, with citric acid as binding agent, with expensive
Pt metal and Pd are the catalyst made by active component, and the addition of noble metal is 5 ~ 200g/ft3；It is characterized in that, including
Following steps:
(1) River Bank Stability: TiO by a certain percentage2, Al-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide, citric acid,
Platinum nitrate solution and palladium nitrate solution join in deionized water, described component TiO2, Al-Ti-Si composite oxides, ZSM-5
Molecular sieve, zirconium dioxide, citric acid, noble metal platinum nitrate and noble metal Palladous nitrate. mass ratio are 0.2 ~ 0.37:0.2 ~ 0.35:
0.25 ~ 0.45:0.02 ~ 0.1:0.01 ~ 0.05:0.00316 ~ 0.04295:0.0006043 ~ 0.02843, stirs；
(2) ball milling: the serosity that configured is ground through planetary ball mill, the rotating speed of planetary ball mill is 250 ~ 380 turns/
Point, the operation time is 3 ~ 6h, and serous granule degree to D90 is 2 ~ 20 μm；
(3) mensuration of solid content: take 10g serosity in crucible, crucible is placed in 550 ~ 600 DEG C of Muffle kiln roastings 10 ~
20min, is cooled to room temperature, weighs its powder quality, by this quality divided by 10g, obtains slurry solid content；
(4) coating coating: be coated with quantitatively coating special plane, catalyst carrier be positioned at application chamber, according to coated weight
It is that the solid content that 80 ~ 180g/L requires and records calculates the wet weightening finish of target, the serosity calculated is joined in slurry dish, carry out
Quantitatively coating；
(5) dry: the catalyst coated, through 100 ~ 180 DEG C of flash bakings, is dried 3 ~ 6h, evaporated by the water in coating；
(6) roasting: put in Muffle furnace by drying rear catalyst, 450 ~ 550 DEG C of roasting 1 ~ 2h, insulation is cooled to room after terminating
Temperature, calculates catalyst practical coating amount.
A kind of preparation side of the diesel vehicle oxidative catalyst containing Al-Si-Ti composite oxides
Method, it is characterised in that: after described (3), the bullion content in serosity is measured, the serosity with noble metal is taken 20g and enters
Row is centrifugal, carries out Solid-Liquid Separation, takes solid phase and uses ICP to carry out the mensuration of content.
A kind of preparation side of the diesel vehicle oxidative catalyst containing Al-Si-Ti composite oxides
Method, it is characterised in that: the mass ratio of described precious metals pd and Pt is 1/2 ~ 1/7.
A kind of preparation side of the diesel vehicle oxidative catalyst containing Al-Si-Ti composite oxides
Method, it is characterised in that: described Al-Ti-Si composite oxides are made up of aluminium sesquioxide, titanium dioxide, silicon dioxide, its quality
Ratio is 0.5 ~ 0.7:0.2 ~ 0.4:0.05 ~ 0.2.
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| CN105435819B (en) * | 2016-01-06 | 2018-03-16 | 武汉理工大学 | A kind of cordierite loads MnOxF adulterates TiO2The method of active component and the MnO of preparationxF adulterates TiO2Cordierite composite catalyst |
| CN108722390A (en) * | 2018-05-31 | 2018-11-02 | 合肥神舟催化净化器股份有限公司 | A kind of oxidation catalyzer and preparation method thereof of Ce-Si-Al composite oxides |
| CN109225210B (en) * | 2018-09-30 | 2019-09-13 | 中自环保科技股份有限公司 | A kind of low noble metal diesel vehicle oxidation catalyst preparation method and its catalyst of preparation |
| CN113731479A (en) * | 2021-09-28 | 2021-12-03 | 无锡威孚环保催化剂有限公司 | HCHO catalyst capable of efficiently and rapidly degrading at room temperature and preparation method thereof |
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| TWI449572B (en) * | 2006-11-29 | 2014-08-21 | Umicore Shokubai Japan Co Ltd | Oxidation catalyst and the oxidation catalyst using an exhaust gas purification system |
| CN101530787B (en) * | 2009-04-13 | 2011-04-27 | 无锡威孚环保催化剂有限公司 | Oxidation catalyst for purifying tail gas of diesel vehicles and preparation method thereof |
| CN102574055B (en) * | 2009-11-12 | 2015-11-25 | 尤米科尔股份公司及两合公司 | The diesel oxidation catalyst improved |
| JP5664918B2 (en) * | 2011-04-08 | 2015-02-04 | トヨタ自動車株式会社 | Exhaust gas purification catalyst |
| CN103752338B (en) * | 2014-02-08 | 2015-08-19 | 无锡威孚力达催化净化器有限责任公司 | For the preparation method of the oxidation catalyst of purification of diesel tail gas |
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