CN109590014A - A kind of integral diesel tail gas oxidation catalyst and preparation method thereof - Google Patents
A kind of integral diesel tail gas oxidation catalyst and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J29/076—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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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
- B01D53/92—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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Abstract
The invention discloses a kind of integral diesel tail gas oxidation catalysts and preparation method thereof.Include: by noble-metal-supported additive modification SiO2‑Al2O3Catalyst powder material is obtained on carrier, then catalyst powder material is coated on cordierite substrates and is prepared；Wherein SiO2Mass percentage content in the carrier be 10~30wt%；Noble metal is Pt or/and Pd, 1~3wt% of total load amount.The present invention prepares SiO by additive modifications such as rare earth metal, alkaline-earth metal2‑Al2O3Carrier, the DOC catalyst of carrier preparation can be improved CO, HC, SOF and NO activity and high-temperature aging resisting performance especially NO oxidation activity.
Description
Technical field
The invention belongs to catalyst research preparation technical fields.Especially belong to the preparation of motor-driven vehicle gas disposal catalyst research
Technical field, in particular to a kind of integral diesel tail gas oxidation catalyst and preparation method thereof.
Background technique
Motor-vehicle tail-gas is one of main source of atmosphere pollution, and major pollutants include: carbon monoxide (CO), hydrocarbon
Compound (HC), oxynitrides (NOx) and particulate matter (PM).Serious environmental pollution is not only caused, but also seriously endangers people
The health of class.Diesel vehicle has been used widely because of its fuel economy, high thermal efficiency.Diesel oxidation catalyst
(DOC) carbon monoxide (CO) in main purifying tail gas of diesel vehicles, hydrocarbon compound (HC), oxynitrides (NOx) and
The dissolved organic matter component (SOF) on grain surface object (PM), is oxidized to H for the above-mentioned pollutant in tail gas2O、CO2And NO2.Mesh
Preceding DOC catalyst, using Pt etc. as active component, with high-ratio surface, the Al of high heat stability2O3Sill is used as DOC catalyst
Carrier, to above-mentioned reaction catalytic performance with higher.It is increasingly harsh with regulation, meet the diesel oil of state's VI discharge standard
Vehicle after-treatment system be by exhaust gas from diesel vehicle oxidation catalyst (DOC), diesel vehicle grain catcher (DPF), selective catalysis also
Raw catalyst (SCR) and ammoxidation catalyst (ASC) composition.In DOC+SCR+DPF+ASC after-treatment system, DOC is by NO oxygen
Turn to NO2Reaction can effectively facilitate the catalytic performance of downstream SCR and the oxidation, purification of carbon soot particles, this requires DOC
With higher NO conversion performance, it is just able to satisfy harsh discharge standard.Furthermore it is required that DOC has better CO, HC conversion
Performance and high high-temp stability.Exhaust temperature can be increased sharply in DPF oil spout regenerative process, and DOC outlet temperature is up to 650 DEG C
More than, Pt catalytic active component or carrier sintering can all lead to catalyst activity reduction.The preferable Pt particle of initial dispersion,
Aggregation or crystal grain are grown up under high temperature, and Adsorption is caused to reduce, and catalytic activity reduces.Meanwhile the sintering of carrier can cause hole
Structure collapses, active site are reduced, and existing DOC catalyst is unable to meet demand.
Therefore, it develops a kind of couple of NO and is oxidized to NO2There is better CO, HC conversion performance and high temperature simultaneously with high activity
The DOC catalyst of thermal stability has important meaning for meeting the exploitation of diesel car tail gas refining system of state's VI discharge standard
Justice.
Summary of the invention
The invention discloses a kind of integral diesel tail gas oxidation catalysts and preparation method thereof.The purpose of the present invention is
A kind of NO high conversion efficiency is provided and there is better CO, the integral diesel vehicle DOC of HC conversion performance and high high-temp stability
Catalyst and preparation method thereof.
The invention is realized by the following technical scheme:
Integral diesel tail gas oxidation catalyst of the present invention be by noble-metal-supported additive modification SiO2-
Al2O3Catalyst powder material is obtained on carrier, then catalyst powder material is coated on cordierite substrates and is prepared；Its
Middle SiO2In SiO2-Al2O3Mass percentage content in carrier is 10~30wt%；Noble metal is Pt or/and Pd, total negative
1~3wt% of carrying capacity.
The auxiliary agent is at least one of the oxide of following single metal, after modification the mass percent in carrier
Content is 3~15wt%；Alkaline-earth metal: including Mg, Ca, Sr, Ba；Rare earth metal: including Ce, Pr, La, Y；Transition metal: packet
Include Mn, Co, Ni, Zr.
The preferred Pt of noble metal of the present invention.SiO2-Al2O3Specific surface area be 250-310m2/ gram, Kong Rongwei 0.6-
0.9cm3/ gram.
Catalyst of the present invention is impregnated in SiO by auxiliary agent first2-Al2O3It is thermally treated to obtain modified SiO on carrier2-Al2O3
Carrier, then by precious metal impregnation in modified SiO2-Al2O3Carrier, drying and roasting are prepared.
The preparation of above-mentioned DOC catalyst the following steps are included:
(1) modified support is prepared using equi-volume impregnating, by metering than weighing suitable auxiliary agent presoma, be dissolved in
In ionized water, it is immersed in SiO2-Al2O3On carrier；
(2) sample that (1) obtains is placed in drying box in 60 DEG C of dry 6~12h, finally in roaster in 450~
550 DEG C of roasting 3h obtain modified SiO2-Al2O3The dusty material of carrier；
(3) platinum nitrate solution that will measure ratio, is dissolved in deionized water, is immersed in the modification SiO of (2) preparation2-Al2O3
On carrier；
(4) catalyst obtained in (3) is placed in drying box dry, 450~550 DEG C of roasting 3h and obtains catalyst fines
Material；
(5) on cordierite, through drying, roasting, monoblock type catalysis is made in the catalyst fines coating (4) being prepared
Agent.
The carrier S iO that the present invention uses2-Al2O3It is prepared by the precipitation method, by Al (NO3)3·9H2O is dissolved in deionized water
The aluminum nitrate solution of 1mol/L is obtained, while preparing NH3·H2O:(NH4)2CO3Molar ratio is the NH of 1:13·H2O and (NH4)2CO3Mixed solution, by aluminum nitrate solution, NH3·H2O and (NH4)2CO3Mixed solution and acidic silicasol are with vigorous stirring simultaneously
Precipitation reactor is added in stream, and control pH value is deposited in 60 DEG C and is aged 5 hours, be then filtered, washed 9.0, dry then at 100 DEG C
Dry 12h.Finally obtained powder is gradually warmed up to 900 DEG C of roasting 3h, obtains SiO2-Al2O3。SiO2Matter in the carrier
Degree control is measured in 10~30wt%, prepared SiO2-Al2O3Specific surface area be 250-310m2/ gram, Kong Rongwei
0.6-0.9cm3/ gram, it is able to satisfy requirement of the invention.
DOC catalyst of the invention has good catalytic oxidation activity and thermal stability to CO, HC, SOF and NO, especially
It is the oxidation activity of NO.
Helpfulness of the present invention is: the present invention passes through the preparation of the additive modifications such as rare earth metal, alkaline-earth metal and transition metal
SiO2-Al2O3Carrier, the DOC catalyst of carrier preparation can be improved CO, HC, SOF and NO activity and high-temperature aging resisting performance
Especially NO oxidation activity.
Detailed description of the invention
The conversion ratio of the fresh aging catalyst NO of Fig. 1 embodiment 6 varies with temperature；Wherein, ordinate indicates NO conversion ratio,
Unit %；Abscissa indicates temperature, unit DEG C；Curve A is the variation of the fresh sample of embodiment 6, and curve B is that 6 aging sample of embodiment becomes
Change.
Specific embodiment
The present invention is further described With reference to embodiment, specific embodiment be to the principle of the invention into
One step explanation, does not limit the invention in any way, and same or like technology is protected without departing from the present invention with the present invention
Range.
Embodiment 1
The present embodiment provides Pt/Y2O3/SiO2-Al2O3The preparation method of catalyst, comprising the following steps:
(1) by the yttrium nitrate (15wt%Y of calculation amount2O3) be dissolved in deionized water, using etc. pore volume impregnations method impregnate
In SiO2-Al2O3On carrier, 2h is stood；
(2) sample that (1) obtains is placed in drying box in 60 DEG C of dry 12h, in 550 DEG C of roasting 3h in roaster,
Obtain Y2O3/SiO2-Al2O3Modified support powder；
(3) platinum nitrate solution (1wt%Pt) is suitably diluted, using etc. pore volume impregnations method be impregnated in what (2) obtained
Y2O3/SiO2-Al2O3Powder, dry, roasting is identical as (2), obtains Pt/Y2O3/SiO2-Al2O3Catalyst powder powder material；
(4) acetic acid of the Aluminum sol of catalyst powder powder material and 2~5wt% that (3) obtain, 2~5wt% is ground and is made
Catalyst pulp, and controlling solid content is 35~45%；
(5) catalyst pulp obtained by (4) is uniformly coated on cordierite honeycomb ceramic matrix, controls the upper of catalyst
150~180g/L of carrying capacity；
(6) matrix after coating is gradually warming up to 60 DEG C by room temperature to be dried, then in 550 DEG C of roasting 3h, is obtained
Monoblock type Pt/Y2O3/SiO2-Al2O3Catalyst.
Embodiment 2
(1) by the Ca (NO of calculation amount3)2(10wt%CaO) is dissolved in deionized water, using etc. pore volume impregnations method soak
Stain is in SiO2-Al2O3On carrier, CaO/SiO is made in dry, roasting (identical as (2) the step of embodiment 1)2-Al2O3Carrier material
Material；
(2) according to 1 step of embodiment (3) same procedure, platinum nitrate solution is impregnated in the CaO/SiO of (1) preparation2-
Al2O3On carrier material, dry, roasting obtains Pt/CaO/SiO2-Al2O3Catalyst fines；
(3) according to step (4) in embodiment 1, monoblock type Pt/CaO/SiO is prepared in (5) and (6) same procedure2-
Al2O3Catalyst.
Embodiment 3
(1) by Mn (NO3)2Solution (15wt%MnO2) etc. hole bodies area method be impregnated in SiO2-Al2O3On carrier, dry, roasting
With (with (2) same procedure the step of embodiment 1), MnO is obtainedx/SiO2-Al2O3Carrier material；
(2) according to 1 step of embodiment (3) same procedure, platinum nitrate solution is impregnated in the CaO/SiO of (1) preparation2-
Al2O3On carrier material, dry, roasting obtains that Pt/MnO is preparedx/SiO2-Al2O3Catalyst fines；
(3) according to step (4) in embodiment 1, monoblock type Pt/MnO is prepared in (5) and (6) same procedurex/SiO2-
Al2O3Catalyst.
Embodiment 4
(1) by Ni (NO3)26H2O and Ce (NO3)3·6H2(always upper carrying capacity is 15wt%, NiO:CeO to the mixing of O solution2Rub
You are than 1:1), incipient impregnation is in SiO2-Al2O3On carrier, dry, roasting (with (2) same procedure the step of embodiment 1) is obtained
To CeO2-NiO/SiO2-Al2O3Carrier material；
(2) according to 1 step of embodiment (3) same procedure, platinum nitrate solution is impregnated in the CeO of (1) preparation2-NiO/
SiO2-Al2O3On carrier material, dry, roasting obtains that Pt/CeO is prepared2-NiO/SiO2-Al2O3Catalyst fines；
(3) according to step (4) in embodiment 1, monoblock type Pt/CeO is prepared in (5) and (6) same procedure2-NiO/
SiO2-Al2O3Catalyst.
Embodiment 5
(1) by Mn (NO3)2Solution and Ce (NO3)3·6H2(always upper carrying capacity is 15wt%, MnO to the mixing of O solution2:CeO2's
Molar ratio 1:1), incipient impregnation is in SiO2-Al2O3On carrier, dry, roasting (with (2) same procedure the step of embodiment 1),
Obtain CeO2-MnOx/SiO2-Al2O3Carrier material；
(2) according to 1 step of embodiment (3) same procedure, platinum nitrate solution is impregnated in the CeO of (1) preparation2-MnOx/
SiO2-Al2O3On carrier material, dry, roasting obtains that Pt/CeO is prepared2-MnOx/SiO2-Al2O3Catalyst fines；
(3) according to step (4) in embodiment 1, monoblock type Pt/CeO is prepared in (5) and (6) same procedure2-MnOx/
SiO2-Al2O3Catalyst.
Embodiment 6
(1) by Ce (NO3)3·6H2O, Mn (NO3)2With Ba (NO3)2(always upper carrying capacity is 15wt%, CeO to mixed solution2:
MnO2: the molar ratio 1:1:1 of BaO), incipient impregnation is in SiO2-Al2O3On carrier, drying roasts (the step of with embodiment 1
(2) same procedure), obtain CeO2-MnOx-BaO/SiO2-Al2O3Carrier material；
(2) according to 1 step of embodiment (3) same procedure, platinum nitrate solution is impregnated in the CeO of (1) preparation2-MnOx-
BaO/SiO2-Al2O3On carrier material, dry, roasting obtains that Pt/CeO is prepared2-MnOx-BaO/SiO2-Al2O3Catalyst
Powder；
(3) according to step (4) in embodiment 1, monoblock type Pt/CeO is prepared in (5) and (6) same procedure2-MnOx-
BaO/SiO2-Al2O3Catalyst.
Comparative example 1
(1) by Pt (NO3)2The pore volume impregnations such as solution (load capacity 1wt%) are in Al2O3On carrier, dry, roasting (with
The step of embodiment 1 (2) same procedure), obtain Pt/Al2O3Powder；
(2) according to step (4) in embodiment 1, monoblock type Pt/Al is prepared in (5) and (6) same procedure2O3Catalyst.
Comparative example 2
(1) by Pt (NO3)2The pore volume impregnations such as solution (load capacity 1wt%) are in SiO2-Al2O3On carrier, dry, roasting
It burns (with (2) same procedure the step of embodiment 1), obtains Pt/SiO2-Al2O3Powder；
(2) according to step (4) in embodiment 1, monoblock type Pt/SiO is prepared in (5) and (6) same procedure2-Al2O3It urges
Agent.
Active appraisal experiment
The activity rating of catalyst carries out in the fixed microreactor continuously flowed of multichannel, simulates exhaust gas from diesel vehicle group
Become: NO200ppm, CO1000ppm, C3H6330ppm、O210%, CO28%, N2As carrier gas, air speed 60000h-1.It is all
Catalyst sample 550 DEG C of pretreatment 3h in reaction atmosphere (simulation exhaust gas from diesel vehicle) before the reaction.Then with 5 DEG C/min's
Heating rate test, carries out active testing after each temperature spot is stablized 30 minutes.NO,NO2Concentration use fourier infrared
Gas analyzer (Thermol Fisher Scientific) is tested.
SOF activity rating: lubricating oil is equably loaded on catalyst fines, lubricating oil and catalyst fines sample matter
The ratio between amount is 1:10；Analysis carries out on NETZSCH TG209F1 type thermogravimetric analyzer, the temperature programming in air stream atmosphere,
Air velocity 100ml/min, heating rate are 10 DEG C/min.
Ageing gas volume composition: NO200ppm, CO1500ppm, C3H6600ppm、O25%, CO24%, N2As carrier gas,
Flow velocity is 800mL/min；Senile experiment is that catalyst sample is placed in ageing gas atmosphere, in 670 DEG C of heating 15h, then at
250 DEG C of heating 15h.
Catalyst activity evaluation result is as shown in table 1 before and after aging:
Catalytic activity before and after 1 aging of table
Activity Results before and after embodiment 1 to 6 catalyst aging of embodiment show the present invention by different additive modifications
SiO2-Al2O3The activity and high-temperature aging resisting performance of CO, HC, SOF and NO of the DOC catalyst of carrier preparation are superior to Pt/
Al2O3(comparative example 1) and Pt/SiO2-Al2O3(comparative example 2).NO conversion ratio after embodiment 1 to 6 catalyst aging of embodiment is most
Low is 38%, up to 50%, hence it is evident that higher than the 25% and 32% of 2 catalyst of comparative example 1 and comparative example, in diesel vehicle
In DOC+SCR+DPF+ASC after-treatment system, the oxidation that can more efficiently facilitate the catalytic performance and carbon soot particles of downstream SCR is net
Change.Embodiment 1 to 3 is the SiO of one-component additive modification2-Al2O3Carrier prepares DOC catalyst, and the activity of CO, HC and SOF mention
High significant, the activity after NO aging improves significant；Embodiment 3 and 4 is the SiO of two-component additive modification2-Al2O3Carrier preparation
DOC catalyst, the activity of CO, HC, SOF and NO improve significant before and after aging；Embodiment 6 is CeO2-MnOxThree component of-BaO changes
The SiO of property2-Al2O3Carrier prepares DOC catalyst, and the activity of CO, HC, SOF and NO are best before and after aging, as shown in Figure 1, aging
The high conversion rate of NO up to 50% and has wide temperature window afterwards.
Claims (6)
1. a kind of integral diesel tail gas oxidation catalyst, it is characterised in that: the catalyst is to help noble-metal-supported
The modified SiO of agent2-Al2O3It is prepared on carrier；Wherein SiO2In SiO2-Al2O3Mass percentage content in carrier is
10~30wt%；Noble metal is Pt or/and Pd, 1~3wt% of total load amount.
2. integral diesel tail gas oxidation catalyst shown according to claim 1, it is characterised in that: the auxiliary agent is following
At least one of the oxide of single metal, the mass percentage content in carrier is 3~15wt% after modification；Alkaline earth gold
Belong to: including Mg, Ca, Sr, Ba；Rare earth metal: including Ce, Pr, La, Y；Transition metal: including Mn, Co, Ni, Zr.
3. integral diesel tail gas oxidation catalyst shown according to claim 1, it is characterised in that: the noble metal is preferred
Pt。
4. integral diesel tail gas oxidation catalyst shown according to claim 1, it is characterised in that: the SiO2-Al2O3
The specific surface area of carrier is 250-310m2/ gram, Kong Rongwei 0.6-0.9cm3/ gram.
5. a kind of preparation method of integral diesel tail gas oxidation catalyst, it is characterised in that including following methods: catalyst
It is the described in any item catalyst of Claims 1-4；
(1) modified support is prepared using equi-volume impregnating, by metering than weighing suitable auxiliary agent presoma, is dissolved in deionization
In water, it is immersed in SiO2-Al2O3On carrier；
(2) sample that (1) obtains is placed in drying box in 60 DEG C of dry 6~12h, finally in 450~550 DEG C in roaster
3h is roasted, modified SiO is obtained2-Al2O3The dusty material of carrier；
(3) platinum nitrate or/and palladium nitrate solution that will measure ratio, are dissolved in deionized water, are immersed in the modification of (2) preparation
SiO2-Al2O3On carrier；
(4) catalyst obtained in (3) is placed in drying box dry, 450~550 DEG C of roasting 3h and obtains catalyst fines material
Material；
(5) on cordierite, through drying, roasting, integral catalyzer is made in the catalyst fines coating (4) being prepared.
6. the preparation method of integral diesel tail gas oxidation catalyst according to claim 5, it is characterised in that: described
Carrier S iO2-Al2O3It is prepared by the precipitation method, including following methods:
(1) by Al (NO3)3·9H2O is dissolved in the aluminum nitrate solution that 1mol/L is obtained in deionized water, while preparing NH3·H2O:
(NH4)2CO3Molar ratio is the NH of 1:13·H2O and (NH4)2CO3Mixed solution；
(2) by aluminum nitrate solution, NH3·H2O and (NH4)2CO3Cocurrent is added with vigorous stirring for mixed solution and acidic silicasol
Precipitation reactor, control pH value are deposited in 60 DEG C and are aged 5 hours, be then filtered, washed, then at 100 DEG C of dry 12h 9.0；
(3) obtained powder is gradually warmed up to 900 DEG C of roasting 3h, obtains SiO2-Al2O3Carrier；SiO2Quality in the carrier
Degree is 10~30wt%.
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| CN112058261A (en) * | 2020-08-17 | 2020-12-11 | 四川大学 | Integral diesel exhaust oxidation catalyst, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114423521A (en) * | 2019-09-23 | 2022-04-29 | 喜星触媒株式会社 | Oxidation catalyst composition doped with manganese on a support |
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| CN112934234A (en) * | 2021-01-19 | 2021-06-11 | 惠州市瑞合环保科技有限公司 | DOC catalyst for diesel tail gas after-treatment system |
| CN114534776A (en) * | 2022-01-19 | 2022-05-27 | 中自环保科技股份有限公司 | Sulfur-resistant diesel vehicle oxidation type catalyst and preparation method thereof |
| CN115382543A (en) * | 2022-08-30 | 2022-11-25 | 惠州市瑞合环保科技有限公司 | Diesel oil oxidation catalyst containing strontium and tungsten and preparation method thereof |
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