CN104190413A - SCR-based NO oxidation catalyst and preparation method thereof - Google Patents
SCR-based NO oxidation catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a SCR-based NO oxidation catalyst and a preparation method thereof. The preparation method of the SCR-based NO oxidation catalyst comprises the following steps: firstly coating the surface of a catalyst carrier with coating slurry containing noble metal Pt by taking cordierite honeycomb ceramic as the catalyst carrier, drying and roasting; and subsequently fixing a certain amount of noble metal Pd solution at one end of the catalyst by using an impregnation method, wherein the amount of the impregnated noble metal Pd solution accounts for 1/3 of the total water absorption amount of the catalyst; the coating slurry is prepared by taking a molecular sieve as an HC adsorption material, taking SiO2 as a dispersing agent, taking zirconium acetate as a thermal stability additive, taking noble metal Pt as an active component and adding an alumina gel adhesive. The preparation method of the SCR-based NO oxidation catalyst is simple in processing steps; the noble metal Pt or Pd is impregnated in the air inlet direction of the prepared catalyst; by virtue of the improved catalyst, the oxidation rate of the NO at the low temperature can be improved, so that the and the temperature window is relatively wide when the NO is oxidized to between 40%-70% in the process of oxidizing NO into NO2; the catalyst is relatively high in stability.
Description
Technical field
The present invention relates to a kind of NO oxidation catalyst based on SCR and preparation method thereof, belong to the preparing technical field of diesel vehicle oxidative catalyst.
Background technology
Automobile exhaust pollution has become one of main source of atmosphere pollution.Most NO in city
x, CO, HC and PM produce by vehicle exhaust.NO
x, CO, HC, PM not only cause damage but also produce under certain conditions blue photochemical fog human body, makes vegetation dead, the environment of human survival is destroyed.Existing exhaust method regulation, diesel vehicle state five discharge standards will be implemented in Beijing, Shanghai, and the national implementation date of diesel vehicle state four discharge standards nearly, therefore, also has higher requirement to the catalytic conversion efficiency of diesel vehicle oxidative catalyst.
Diesel vehicle oxidative catalyst (DOC) is for the SOF Soluble Organic Fraction (SOF) in tail gas CO, NO, HC and the PM of oxidated diesel oil car, 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; It is carrier that oxidation catalyst be take ceramic honey comb or honeycomb metal conventionally, load oxide coating and active metal component on it, conventional noble metal component is Pt, Pd etc., and at present the widely used noble metal of exhaust gas from diesel vehicle post processing is Pt, and Pt is mainly used for being oxidized CO, HC.
Along with discharge standard is strict gradually, only use DOC cannot reach emission request, DOC and DPF are used in conjunction to eliminate PM or be used in conjunction elimination NOx with SCR becomes study hotspot gradually.When DOC and DPF are used in conjunction, require NO to generate NO
2conversion ratio high, be conducive to like this regeneration of DPF; When DOC and SCR are used in conjunction, require NO to generate NO
2conversion ratio between 40%～70%, and window temperature is more wide better, is conducive to like this accelerate the reaction rate of SCR, falls low NOx drainage.
There are problems aspect NO oxidation in current existing diesel vehicle oxidative catalyst, the NO oxidizing temperature window of the diesel vehicle oxidative catalyst based on SCR aspect is narrower, and when noble metal addition improves, NO conversion ratio is higher; After overaging, catalyst performance declines obviously.
Summary of the invention
The object of the invention is, in order to solve diesel vehicle oxidative catalyst in prior art, NO is oxidized to the narrower problem of temperature window between 40%～70%, a kind of NO oxidation catalyst based on SCR that preparation method is simple, NO conversion ratio is wider and preparation method thereof is provided.
The present invention adopts following technical scheme: a kind of NO oxidation catalyst based on SCR, catalyst be take cordierite honeycomb ceramic as catalyst carrier, the surface of catalyst carrier applies the coating slurries containing precious metals pt, one end of catalyst adopts infusion process to be fixed with a certain amount of precious metals pd solution, described fixing precious metals pd solution amount is 1/3 of described catalyst total suction, it is HC sorbing material that described coating slurries adopt molecular sieve, SiO
2for dispersant, zirconium acetate is thermally-stabilised auxiliary agent, and precious metals pt is active component, adds aluminium glue binding agent to make.
A preparation method for NO oxidation catalyst based on SCR, comprises the steps:
(1) slurries preparation: by a certain percentage by SiO
2, molecular sieve, zirconium acetate, aluminium glue binding agent join in deionized water, weight ratio is 0.4～0.72:0.25～0.45:0.02～0.1:0.01～0.05, stirs, and adds nitric acid to regulate slurries pH to be less than 4.0;
(2) slurries ball milling: slurries grind 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, just obtain slurry solid content by this quality;
(4) adding of precious metals pt solution: precious metals pt solution is joined in ball milling rear slurry, stirs 2～8h, be dispersed in completely in slurries to active component precious metals pt solution, add precious metals pt amount be 15～30g/ft
3;
(5) coating applies: carrier cordierite honeycomb ceramic being immersed in slurries, take out the carrier cordierite honeycomb ceramic that soaks full slurries, with air gun, blow away unnecessary slurries, is that 100～180g/L and solid content are controlled wet weightening finish by coated weight, calculates practical coating amount;
(6) dry: the catalyst having applied is through 100～180 ℃ of flash bakings, and drying time is that 3～6h evaporates the water in coating;
(7) 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 weigh catalyst weight;
(8) quantitatively flood precious metals pd solution: one end dipping precious metals pd solution of catalyst, the amount of dipping precious metals pd is 5～10g/ft
3, dipping noble metal area end is as airintake direction, and catalyst is dried 3～6h through 100～180 ℃, and under 450～550 ℃ of conditions, roasting 1～2h makes.
Further, after described step (4) completes, get slurries 20g with noble metal and carry out centrifugally, carry out Solid-Liquid Separation, get solid phase part and with ICP, carry out the mensuration of precious metals pt content.
Further, the mass ratio of the noble metal platinum in described step (4) and (9) and palladium is 3:1.
Processing step of the present invention is simple, and the catalyst of preparing is impregnated with precious metals pd in the direction of air inlet, and the catalyst after improvement can improve NO oxygenation efficiency at low temperatures, makes NO be oxidized to NO
2between 40%～70%, temperature window is wider, and the stability of catalyst is better.
The specific embodiment
Below will according to specific embodiment, the invention will be further described.All to adopt diameter be 80mm to three examples below, height is the cylindrical cordierite honeycomb 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 method of the NO oxidation catalyst based on SCR, comprises the steps:
(1) slurries preparation: by a certain percentage by SiO
2, molecular sieve, zirconium acetate, binding agent join in deionized water, part by weight is 0.72:0.25:0.02:0.01, stirs, surveying pH is 3.24;
(2) slurries ball milling: slurries grind through planetary ball mill, and rotating speed is 250 revs/min, and be 6h running time, serous granule degree to D90 be 3.22um;
(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 3.95g, and divided by 10g, just obtaining slurry solid content is 39.5% by this quality;
(4) adding of precious metals pt solution: get the slurries 1000g after ball milling, precious metals pt addition is 15g/ft
3, coated weight is 100g/L, and the amount that calculates precious metals pt is 2.092g, and the amount that takes precious metals pt solution is 15.157g, and precious metals pt solution is joined in the slurries after ball milling, stirs 2h, is dispersed in slurries completely to active component noble metal platinum;
(5) 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 in solid phase, result is 0.0052g (noble metal)/g (powder);
(6) coating applies: carrier cordierite honeycomb ceramic is immersed in slurries, the carrier cordierite honeycomb ceramic of full slurries is soaked in taking-up, with air gun, blow away unnecessary slurries, by the coated weight requirement of 150g/L and the solid content that records, control the wet weightening finish of target, calculating catalyst practical coating amount is 77.4g;
(7) dry: the catalyst having applied is dried 6h through 100 ℃, and the water in coating is evaporated;
(8) 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 127.5g;
(9) precious metals pd solution quantitatively floods: catalyst at one end floods fixedly precious metals pd solution, and precious metals pd addition is 5g/ft
3, the amount that calculates precious metals pd is 0.053g, takes precious metals pd solution 0.3509g, adding water to pickup desired value is 42.5g, dipping Pd noble metal area end is as airintake direction, and catalyst is dried 6h through 100 ℃, and under 450 ℃ of conditions, roasting 2h is prepared from;
Embodiment bis-: a kind of preparation method of the NO oxidation catalyst based on SCR, comprises the steps:
(1) slurries preparation: by a certain percentage by SiO
2, molecular sieve, zirconium acetate, aluminium glue binding agent join in deionized water, its weight ratio is 0.58:0.35:0.04:0.03, stirs, surveying pH is 3.29;
(2) slurries ball milling: slurries grind through planetary ball mill, and rotating speed is 320 revs/min, and be 4h running time, serous granule degree to D90 be 3.16um;
(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 3.89g, divided by 10g, just obtains slurry solid content 38.9% by this quality;
(4) adding of precious metal solution Pt: get ball milling rear slurry 1000g, precious metals pt addition is 20g/ft
3, coated weight is 140g/L, and the amount that calculates precious metals pt is 1.9625g, and the amount that takes precious metals pt solution is 14.24g, and precious metals pt solution joins in the slurries after ball milling, stirs 2h, is dispersed in slurries completely to active component precious metals pt;
(5) 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 in solid phase, result is 0.0050g (noble metal)/g (powder);
(6) coating applies: carrier cordierite honeycomb ceramic is immersed in slurries, the carrier cordierite honeycomb ceramic of full slurries is soaked in taking-up, with air gun, blow away unnecessary slurries, by the coated weight requirement of 140g/L and the solid content that records, control the wet weightening finish of target 108.3g, practical coating amount is 110.3g;
(7) dry: the catalyst having applied is dried 4h through 150 ℃, and the water in coating is evaporated;
(8) 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 139.1g;
(9) precious metals pd solution quantitatively floods: catalyst at one end floods precious metals pd solution, and precious metals pd addition is 6.7g/ft
3the amount that calculates precious metals pd is 0.071g, take precious metals pd solution 0.4698g, adding water to pickup desired value is 46.3g, the pickup of this precious metals pd solution is 1/3 of the total water absorption rate of catalyst, dipping precious metals pd solution area end is as airintake direction, and catalyst is dried 4h through 150 ℃, and under 500 ℃ of conditions, roasting 1.5h is prepared from;
Embodiment tri-: a kind of preparation method of the NO oxidation catalyst based on SCR, comprises the steps:
(1) slurries preparation: by a certain percentage by SiO
2, molecular sieve, zirconium acetate, aluminium glue binding agent join in deionized water, its weight ratio is 0.4:0.45:0.1:0.05, stirs, surveying pH is 3.45;
(2) slurries ball milling: slurries grind through planetary ball mill, and rotating speed is 380 revs/min, and be 3h running time, serous granule degree to D90 be 3.08um;
(3) mensuration of solid content: get 10g slurries in dry pot, will do pot and be placed in 580 ℃ of Muffle furnace roasting 20min, be cooled to room temperature, weighing its powder quality is 3.97g, divided by 10g, just obtains slurry solid content 39.7% by this quality;
(4) adding of precious metals pt solution: get ball milling rear slurry 1000g, precious metals pt addition is 30g/ft
3calculate, coated weight is 180g/L, and the amount that calculates precious metals pt is 2.337g, and the amount that takes precious metals pt solution is 16.937g, and precious metals pt solution joins in the slurries after ball milling, stirs 8h, is dispersed in slurries completely to active component precious metals pt;
(5) 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 in solid phase, result is 0.0057g (noble metal)/g (powder);
(6) coating applies: carrier cordierite honeycomb ceramic is immersed in slurries, the carrier cordierite honeycomb ceramic of full slurries is soaked in taking-up, with air gun, blow away unnecessary slurries, by the coated weight requirement of 180g/L and the solid content that records, controlling the wet weightening finish of target is 136.5g, practical coating 137.8g;
(7) dry: the catalyst having applied is dried 3h through 180 ℃, and the water in coating is evaporated;
(8) roasting: oven dry rear catalyst is put into 550 ℃ of roasting 1h of Muffle furnace, be cooled to room temperature after insulation finishes, weighing catalyst weight is 151.7g;
(9) precious metals pd solution quantitatively floods: catalyst at one end floods precious metals pd solution, and precious metals pd addition is 10g/ft
3, the amount that calculates precious metals pd is 0.106g, takes precious metals pd solution 0.703g, adding water to pickup desired value is 50.5g, the area end of dipping precious metals pd solution is as airintake direction, and catalyst is dried 3h through 180 ℃, and under 550 ℃ of conditions, roasting 1h is prepared from.
Catalyst to embodiment bis-preparations carries out activity rating.
One, fresh state catalyst activity evaluation is investigated:
Test is carried out in high temperature 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 that every min heats up 10 ℃, finally rises to 500 ℃.
Test result is in Table 1
The fresh state catalyst activity of table 1 evaluation result
By table 1 Data Comparison, found, NO is converted into NO
2temperature window at 40%-70% is 170 ℃-425 ℃.
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 NOX, CO in vehicle exhaust respectively and the conversion ratio of HC are 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 2.
Table 2 heat ageing rear catalyst activity rating result
From table 2 data, NO is converted into NO
2temperature window 40%～70% is 202 ℃～407 ℃, and low temperature window comparatively fresh state improves nearly 32 ℃, is 202 ℃, 200 ℃ of left and right, can reach more than 40%, reaches requirement, and high temperature window still keeps more than 40% at 400 ℃.
Three, the aging rear catalyst activity rating of sulphur is investigated:
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 to the NO in vehicle exhaust
x, CO and HC conversion ratio investigate.
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
As seen from the results in Table 3, NO is converted into NO
2temperature window at 40%-70% is 206～396 ℃, and low temperature window comparatively fresh state improves nearly 36 ℃, is 206 ℃, and high temperature window reaches more than 40% 396 ℃ of NO oxidations.
Claims (4)
1. the NO oxidation catalyst based on SCR, it is characterized in that: catalyst be take cordierite honeycomb ceramic as catalyst carrier, the surface of catalyst carrier applies the coating slurries containing precious metals pt, one end of catalyst adopts infusion process to be fixed with a certain amount of precious metals pd solution, described fixing precious metals pd solution amount is 1/3 of described catalyst total suction, it is HC sorbing material that described coating slurries adopt molecular sieve, SiO
2for dispersant, zirconium acetate is thermally-stabilised auxiliary agent, and precious metals pt is active component, adds aluminium glue binding agent to make.
2. the preparation method of the NO oxidation catalyst based on SCR described in claim 1, is characterized in that: comprise the steps:
(1) slurries preparation: in proportion by SiO
2, molecular sieve, zirconium acetate, aluminium glue binding agent join in deionized water, weight ratio is 0.4 ~ 0.72:0.25 ~ 0.45:0.02 ~ 0.1:0.01 ~ 0.05, stirs, and adds nitric acid to regulate slurries PH to be less than 4.0;
(2) slurries ball milling: slurries grind 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, just obtain slurry solid content by this quality;
(4) adding of precious metals pt solution: precious metals pt solution is joined in ball milling rear slurry, stirs 2 ~ 8h, be dispersed in completely in slurries to active component precious metals pt solution, add precious metals pt amount be 15 ~ 30g/ft
3;
(5) coating applies: carrier cordierite honeycomb ceramic being immersed in slurries, take out the carrier cordierite honeycomb ceramic that soaks full slurries, with air gun, blow away unnecessary slurries, is that 100 ~ 180g/L and solid content are controlled wet weightening finish by coated weight, calculates practical coating amount;
(6) dry: the catalyst having applied is through 100 ~ 180 ℃ of flash bakings, and drying time is that 3 ~ 6h evaporates the water in coating;
(7) 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 weigh catalyst weight;
(8) quantitatively flood precious metals pd solution: one end dipping precious metals pd solution of catalyst, the amount of dipping precious metals pd is 5 ~ 10g/ft
3, dipping noble metal area end is as airintake direction, and catalyst is dried 3 ~ 6h through 100 ~ 180 ℃, and under 450 ~ 550 ℃ of conditions, roasting 1 ~ 2h makes.
3. the preparation method of a kind of NO oxidation catalyst based on SCR as claimed in claim 2, it is characterized in that: the slurries 20g getting with precious metals pt after described step (4) completes carries out centrifugal, carry out Solid-Liquid Separation, get solid phase part and with ICP, carry out the mensuration of precious metals pt content.
4. the preparation method of a kind of NO oxidation catalyst based on SCR as claimed in claim 2, is characterized in that: the noble metal platinum in described step (4) and (9) and the mass ratio of palladium are 3:1.
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