CN104117381A - Diesel vehicle oxidation catalyst containing Al-Si-Ti composite oxide - Google Patents
Diesel vehicle oxidation catalyst containing Al-Si-Ti composite oxide Download PDFInfo
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- CN104117381A CN104117381A CN201410396471.9A CN201410396471A CN104117381A CN 104117381 A CN104117381 A CN 104117381A CN 201410396471 A CN201410396471 A CN 201410396471A CN 104117381 A CN104117381 A CN 104117381A
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Abstract
The invention relates to a diesel vehicle oxidation catalyst containing Al-Si-Ti composite oxide. The diesel vehicle oxidation catalyst is prepared by taking cordierite honeycomb ceramics as a carrier, TiO2 and Al-Ti-Si composite oxide as a dispersing agent, a molecular sieve as adsorbing material, zirconium nitrate as a thermal stabilizing auxiliary agent, citric acid as a binding agent and precious metals Pt and Pd as active components; the feeding amount of the precious metals is 5-200g/ft<3>. The preparation method is simple; the prepared catalyst are coated by the precious metal active components by a mixed coating method, so that the content of the precious metals can be accurately controlled, the precious metals are evenly distributed, and the effect of the catalyst is better.
Description
Technical field
The present invention relates to a kind of diesel vehicle oxidative catalyst of the Al-Si-Ti of containing composite oxides, belong to diesel vehicle oxidative catalyst preparing technical field.
Background technology
Diesel vehicle oxidative catalyst (DOC) for a part of Identification of Soluble Organic in tail gas CO, NO, HC and the PM of oxidated diesel oil car in SOF, its coating is mainly comprised of oxide coating and active noble metals component, noble metal is the key component of oxidative catalyst, for diesel vehicle DOC, utilize exactly DOC can reduce the activation energy of the chemical reaction of HC, CO in diesel engine vent gas and SOF etc., make the oxygen in these substances and tail gas at lower temperature, carry out oxidation reaction, be converted into CO
2and H
2o.
Oxygen diesel car tail gas refining catalyst generally comprises carrier, active coating two parts.Traditional diesel vehicle oxidation catalyst mostly is Ti-base catalyst, because Ti-base catalyst absorption noble metal ability is poor, noble metal can only adopt immersion coating technique, thereby make noble metal be difficult to accurate control, and because noble metal mainly concentrates on coating surface, on the one hand easily because noble metal sintering makes catalysqt deactivation, on the other hand easily because sulfur poisoning makes catalysqt deactivation, make that catalyst is durable does not reach requirement, in order to meet the requirement of the Abgasgesetz of increasingly stringent, thereby the endurance quality that adopts mixed painting method coated catalysts to improve catalyst becomes inevitable requirement.
Summary of the invention
The object of the invention is to not to be suitable for doing for existing diesel vehicle oxidative catalyst that slurries are mixed is coated with, the shortcoming of the poor and skewness of noble metal adsorption capacity; Provide a kind of preparation method simple, the diesel vehicle oxidative catalyst that in catalyst, the load capacity of noble metal can accurately be controlled, catalyst activity is high.
The present invention adopts following technical scheme: a kind of diesel vehicle oxidative catalyst of the Al-Si-Ti of containing composite oxides, take cordierite honeycomb ceramic as carrier, with TiO
2with Al-Ti-Si composite oxides be dispersant, take molecular sieve as sorbing material, zirconium nitrate is thermally-stabilised auxiliary agent, take citric acid as binding agent, take precious metals pt or Pd as the made catalyst of active component, the addition of noble metal is 5～200g/ft
3.
Further, described Al-Ti-Si composite oxides are comprised of alundum (Al2O3), titanium dioxide, silica, and its mass ratio is 0.5～0.7:0.2～0.4:0.05～0.2.
A preparation method for the diesel vehicle oxidative catalyst that contains Al-Si-Ti composite oxides, is characterized in that: comprise the steps:
(1) slurries preparation: TiO by a certain percentage
2, 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 TiO
2, AL-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide, citric acid, platinum nitrate and palladium nitrate quality proportioning be 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 slurries that configure are ground through planetary ball mill, and the rotating speed of planetary ball mill is 250～380 revs/min, and be 3～6h running time, serous granule degree to D90 be 2～20um;
(3) mensuration of solid content: get 10g slurries in dry pot, will do pot and be placed in 550～600 ℃ of Muffle furnace roasting 10～20min, be cooled to room temperature, weigh its powder quality, divided by 10g, obtain slurry solid content by this quality;
(4) coating applies: with quantitatively applying special plane, apply, catalyst carrier is positioned over to application chamber place, according to coated weight, be that the solid content that 80～180g/L requires and records calculates the wet weightening finish of target, the slurries that calculate are joined in slurry dish, quantitatively apply;
(5) dry: the catalyst having applied, through 100 ℃～180 ℃ flash bakings, is dried 3～6h, and the water in coating is evaporated;
(6) roasting: oven dry rear catalyst is put into Muffle furnace, and 450 ℃～550 ℃ roasting 1h～2h, are cooled to room temperature after insulation finishes, and calculate catalyst practical coating amount.
Further, described step is measured the bullion content in slurries after (3), by get 20g with the slurries of noble metal, is undertaken centrifugally, carries out Solid-Liquid Separation, gets solid phase and adopts 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 adopts ZSM-5 molecular sieve.
Preparation method of the present invention is simple, and the catalyst of preparing adopts mixed painting method noble metal-coating active component, not only can accurately control the content of noble metal but also noble metal is evenly distributed, and catalyst effect is better.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.All to adopt diameter be 80mm to three examples below, height is the cylindrical ceramic carrier of 60mm, volume is 0.301L, vehicle weight is 97g, the concentration of precious metals pt is 0.138g (noble metal)/g (liquid), and the concentration of precious metals pd is 0.1511g (noble metal)/g (liquid).
Embodiment mono-: a kind of preparation that contains Al-Ti-Si composite oxides oxidation catalyst, noble metal addition is according to 5g/ft
3calculate, precious metals pt/precious metals pd is 7/1, and coated weight is according to 80g/L, wherein Al-Ti-Si composite oxides consist of alundum (Al2O3), titanium dioxide, silica quality than being 0.5:0.2:0.05, comprise the steps:
(1) slurries preparation: by a certain percentage by TiO
2, Al-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide, citric acid, platinum nitrate solution, palladium nitrate solution join in deionized water, its mass ratio is 0.3:0.2:0.35:0.1:0.05:0.01399:0.001826, stirs;
(2) slurries ball milling: slurries grind through planetary ball mill, and the rotating speed of planetary ball mill is 250 revs/min, and be 6h running time, and serous granule degree is 3.23um to D90, and pH is 3.14;
(3) mensuration of solid content: get 10g slurries in dry pot, will do pot and be placed in 600 ℃ of Muffle furnace roasting 10min, be cooled to room temperature, weighing its powder quality is 3.86g, and divided by 10g, just obtaining slurry solid content is 38.6% by this quality;
(4) bullion content is measured: get 20g slurries and be placed in test tube, put into centrifuge centrifugal, carry out Solid-Liquid Separation, adopt ICP to measure the content of precious metals pt, Pd in solid phase, the content that records precious metals pt is 0.00192g (noble metal)/g (powder), and the content of precious metals pd is 0.000275g (noble metal)/g (powder).
(5) coating applies: with quantitatively applying special plane, applying, is that the solid content that 80g/L requires and records calculates the wet weightening finish of target for 62.4g according to coated weight, slurries is joined in slurry dish and quantitatively apply;
(6) dry: the catalyst having applied is dried 6h through 100 ℃, and the water in coating is evaporated;
(7) roasting: oven dry rear catalyst is put into Muffle furnace, and 450 ℃ of roasting 2h, are cooled to room temperature after insulation finishes, and weighing catalyst weight is 121.2g.
Embodiment bis-: a kind of preparation that contains Al-Ti-Si composite oxides oxidation catalyst, noble metal addition is according to 34g/ft
3calculate, precious metals pt/precious metals pd ratio adopts 3/1, and coated weight is according to 120g/L, wherein Al-Ti-Si composite oxides consist of alundum (Al2O3), titanium dioxide, silica quality than being 0.6:0.3:0.1, comprise the steps:
(1) slurries preparation: by a certain percentage by TiO
2, Al-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide, citric acid, platinum nitrate solution, palladium nitrate solution join in deionized water, its ratio is 0.37:0.35:0.25:0.02:0.01:0.0891:0.03599, stirs;
(2) slurries ball milling: slurries grind through planetary ball mill, and the rotating speed of planetary ball mill is 330 revs/min, and be 4h running time, and serous granule degree is 3.33um to D90, and pH is 3.23;
(3) mensuration of solid content: get 10g slurries in dry pot, will do pot and be placed in 600 ℃ of Muffle furnace roasting 10min, be cooled to room temperature, weighing its powder quality is 3.96g, and divided by 10g, just obtaining slurry solid content is 39.6% by this quality;
(4) in slurries, bullion content is measured: get 20g slurries and be placed in test tube, put into centrifuge centrifugal, carry out Solid-Liquid Separation, adopt ICP to measure the content of precious metals pt, Pd in solid phase, the content that records precious metals pt is 0.00743g (noble metal)/g (powder), and the content of precious metals pd is 0.00245g (noble metal)/g (powder);
(5) coating applies: with quantitatively applying special plane, applying, slurries are joined in slurry dish and applied, is that the solid content that 120g/L requires and records calculates the wet weightening finish of target for 91.2g according to coated weight, slurries is joined in slurry dish and quantitatively apply;
(6) dry: the catalyst having applied is dried 4h through 150 ℃, and the water in coating is evaporated;
(7) roasting: oven dry rear catalyst is put into Muffle furnace, and 500 ℃ of roasting 1.5h, are cooled to room temperature after insulation finishes, and weighing catalyst weight is 132.5g.
Embodiment tri-: a kind of preparation that contains Al-Ti-Si composite oxides oxidation catalyst, noble metal addition is according to 200g/ft
3calculate, its precious metals pt/precious metals pd is 2/1, and coated weight is according to 180g/L, wherein Al-Ti-Si composite oxides consist of alundum (Al2O3), titanium dioxide, silica quality than being 0.7:0.4:0.2, comprise the steps:
(1) slurries preparation: by a certain percentage by TiO
2, Al-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide, citric acid, platinum nitrate solution, palladium nitrate solution join in deionized water, its ratio is 0.2:0.29:0.45:0.03:0.03:0.31076:0.18818, stirs;
(2) slurries ball milling: slurries grind through planetary ball mill, and the rotating speed of planetary ball mill is 380 revs/min, and be 3h running time, and serous granule degree is 3.13um, surveying pH is 3.17;
(3) mensuration of solid content: get 10g slurries in dry pot, will do pot and be placed in 550 ℃ of Muffle furnace roasting 20min, be cooled to room temperature, weighing its powder quality is 3.88g, and divided by 10g, just obtaining slurry solid content is 38.8% by this quality;
(4) slurries solid phase bullion content is measured: get 20g slurries and be placed in test tube, put into centrifuge centrifugal, carry out Solid-Liquid Separation, adopt ICP to measure the content of precious metals pt, Pd in solid phase, the content that records precious metals pt is 0.02942g (noble metal)/g (powder), and the content of precious metals pd is 0.0130g (noble metal)/g (powder);
(5) coating applies: with quantitatively applying special plane, apply, it is that the solid content that 180g/L requires and records calculates the wet weightening finish of target for 139.6g according to coated weight that slurries are joined in slurry dish, slurries is joined in slurry dish and quantitatively apply;
(6) dry: the catalyst having applied is dried 3h through 180 ℃, and the water in coating is evaporated;
(7) roasting: oven dry rear catalyst is put into Muffle furnace, and 550 ℃ of roasting 1h, are cooled to room temperature after insulation finishes, and weighing catalyst weight is 150.6g.
Catalyst to embodiment bis-preparations carries out activity rating.
One, the fresh state activity rating of catalyst
Test is carried out in tube furnace.
Method of testing: will contain NO, CO
2, H
2o, C
3h
8, CO gaseous mixture pass in high temperature reaction stove, NO:300ppm wherein, CO:500ppm, C
3h
8: 300ppm, H
2o:6%, CO
2: 6%; Heating rate is 10 ℃/min, finally rises to 500 ℃.
Test result is in Table 1
The fresh state catalyst activity of table 1 evaluation result
As shown in Table 1, the prepared HC of catalyst and the initiation temperature T50 of CO of embodiment bis-is respectively 318 ℃ and 136 ℃; NO is converted into NO
2maximum conversion be 78.5%.
Two, heat ageing rear catalyst activity rating is investigated:
Pre-treatment: first catalyst is placed in to Muffle furnace aging, aging temperature is 750 ℃, and ageing time is 20h, and then NO, CO in vehicle exhaust respectively and the conversion ratio of HC are investigated.
Test is carried out in high temperature reaction stove.
Method of testing: will contain NO, CO
2, H
2o, C
3h
8, CO gaseous mixture pass in high temperature reaction stove, NO:300ppm wherein, CO:500ppm, C
3h
8: 300ppm, H
2o:6%, CO
2: 6%; Heating rate is 10 ℃/min, finally rises to 500 ℃.
Test result is in Table 2.
Table 2 heat ageing state catalyst activity evaluation result
As shown in Table 2, the HC initiation temperature T50 of the prepared catalyst of embodiment bis-after heat ageing is 360 ℃, and CO initiation temperature T50 is 159 ℃, and NO generates NO
2conversion ratio be 70%, NO
2the raising of conversion ratio can effectively be processed particle.
Three, the aging rear catalyst activity rating of sulphur
Pre-treatment: the catalyst of preparation is placed in to Muffle furnace, passes into SO
2, 100ppm, 350 ℃ of heating-up temperatures, time 10h, and then respectively the conversion ratio of the NO in vehicle exhaust, CO and HC is investigated.
Test is to carry out in high temperature reaction stove.
Method of testing: will contain NO, CO
2, H
2o, C
3h
8, CO gaseous mixture pass in high temperature reaction stove, NO:300ppm wherein, CO:500ppm, C
3h
8: 300ppm, H
2o:6%, CO
2: 6%; Heating rate is that every min heats up 10 ℃, finally rises to 500 ℃.
Test result is in Table 3.
Table 3 sulphur aging catalyst activity rating result
From table 3 data, the catalyst of embodiment bis-preparations is 345 ℃ to HC initiation temperature T50 after over cure is aging, and CO initiation temperature is 140 ℃; NO generates NO
2maximum conversion be 73%.
Four, the evaluation of car load catalyst activity is investigated:
Adopt the catalyst of preparation in embodiment bis-to carry out complete vehicle test, detect the quality of the pollutant of every kilometer of discharge.
Table 4, car load catalyst test result
From table 4 experimental result, the prepared catalyst of embodiment bis-contributes to the minimizing of HC, CO pollutant, and PM particle also has obvious minimizing, and the Al-Ti-Si composite oxides oxidation catalyst that contains prepared by visible the present invention has good catalytic effect.
Claims (6)
1. a diesel vehicle oxidative catalyst that contains Al-Si-Ti composite oxides, is characterized in that: take cordierite honeycomb ceramic as carrier, with TiO
2with Al-Ti-Si composite oxides be dispersant, take molecular sieve as sorbing material, zirconium nitrate is thermally-stabilised auxiliary agent, take citric acid as binding agent, take precious metals pt and Pd as the made catalyst of active component, the addition of noble metal is 5 ~ 200g/ft
3.
2. a kind of diesel vehicle oxidative catalyst that contains Al-Si-Ti composite oxides as claimed in claim 1, it is characterized in that: described Al-Ti-Si composite oxides are comprised of alundum (Al2O3), titanium dioxide, silica, its mass ratio is 0.5 ~ 0.7:0.2 ~ 0.4:0.05 ~ 0.2.
3. the preparation method of a kind of diesel vehicle oxidative catalyst that contains Al-Si-Ti composite oxides as claimed in claim 1, is characterized in that: comprise the steps:
(1) slurries preparation: TiO by a certain percentage
2, 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 TiO
2, AL-Ti-Si composite oxides, ZSM-5 molecular sieve, zirconium dioxide, citric acid, noble metal platinum nitrate and noble metal palladium nitrate mass ratio be 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 slurries that configure are ground through planetary ball mill, and the rotating speed of planetary ball mill is 250 ~ 380 revs/min, and be 3 ~ 6h running time, serous granule degree to D90 be 2 ~ 20um;
(3) mensuration of solid content: get 10g slurries in dry pot, will do pot and be placed in 550 ~ 600 ℃ of Muffle furnace roasting 10 ~ 20min, be cooled to room temperature, weigh its powder quality, divided by 10g, obtain slurry solid content by this quality;
(4) coating applies: with quantitatively applying special plane, apply, catalyst carrier is positioned over to application chamber place, according to coated weight, be that the solid content that 80 ~ 180g/L requires and records calculates the wet weightening finish of target, the slurries that calculate are joined in slurry dish, quantitatively apply;
(5) dry: the catalyst having applied, through 100 ~ 180 ℃ of flash bakings, is dried 3 ~ 6h, and the water in coating is evaporated;
(6) roasting: oven dry rear catalyst is put into Muffle furnace, and 450 ~ 550 ℃ of roasting 1 ~ 2h, are cooled to room temperature after insulation finishes, and calculate catalyst practical coating amount.
4. the preparation method of a kind of diesel vehicle oxidative catalyst that contains Al-Si-Ti composite oxides as claimed in claim 3, it is characterized in that: after described (3), the bullion content in slurries is measured, by getting 20g with the slurries of noble metal, undertaken centrifugal, carry out Solid-Liquid Separation, get solid phase and adopt ICP to carry out the mensuration of content.
5. a kind of diesel vehicle oxidative catalyst that contains Al-Si-Ti composite oxides as claimed in claim 1, is characterized in that: the mass ratio of described precious metals pd and Pt is 1/2 ~ 1/7.
6. a kind of diesel vehicle oxidative catalyst that contains Al-Si-Ti composite oxides as claimed in claim 1, is characterized in that: described molecular sieve adopts ZSM-5 molecular sieve.
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| CN105435819A (en) * | 2016-01-06 | 2016-03-30 | 武汉理工大学 | Method for loading MnOx-F doped TiO2 active component on cordierite and prepared MnOx-F doped TiO2-cordierite 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 |
| CN109225210A (en) * | 2018-09-30 | 2019-01-18 | 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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| CN105435819A (en) * | 2016-01-06 | 2016-03-30 | 武汉理工大学 | Method for loading MnOx-F doped TiO2 active component on cordierite and prepared MnOx-F doped TiO2-cordierite composite catalyst |
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| CN109225210A (en) * | 2018-09-30 | 2019-01-18 | 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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