CN109746024A - A kind of NO oxidation catalyst and preparation method thereof based on SCR technology - Google Patents
A kind of NO oxidation catalyst and preparation method thereof based on SCR technology Download PDFInfo
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Abstract
The present invention relates to a kind of NO oxidation catalyst and preparation method thereof based on SCR technology, catalyst is using cordierite honeycomb ceramic as catalyst carrier, first in the coating slurry of the surface of catalyst carrier coating platinum containing noble metal, after drying, roasting, then a certain amount of precious metals pd solution is fixed with using infusion process in one end of catalyst, the precious metals pd amount of solution of dipping is the 1/3 of the catalyst total suction, and coating slurry uses molecular sieve for HC adsorbent material, SiO2For dispersing agent, zirconium acetate is thermostabilization auxiliary agent, and noble metal platinum is active component, and aluminium glue binder is added and is made.Present invention process step is simple, and the catalyst prepared is impregnated with noble metal platinum or Pd in the direction of air inlet, and improved catalyst can be improved the oxygenation efficiency of NO at low temperature, NO is made to be oxidized to NO2Temperature window is more wider between 40%-70%, and the stability of catalyst is more preferable.
Description
Technical field
The present invention relates to a kind of NO oxidation catalyst and preparation method thereof based on SCR technology, belongs to bavin
The preparation technical field of oily vehicle oxidative catalyst.
Background technique
Automobile exhaust pollution has become one of main source of atmosphere pollution.Most NO in cityx, CO, HC and PM
It is all to be generated by vehicle exhaust.NOx, CO, HC, PM not only to human body cause damage and also under certain conditions generate blue
Photochemical fog, keep vegetation dead, the environment of human survival is destroyed.Existing exhaust method regulation, Beijing, Shanghai will implement
Five discharge standard of diesel vehicle state, national implementation date of four discharge standard of diesel vehicle state nearly, therefore, urge diesel vehicle oxidisability
Higher requirements are also raised for the catalytic conversion efficiency of agent.
Diesel vehicle oxidative catalyst (DOC) in the tail gas of oxidated diesel oil vehicle in CO, NO, HC and PM can be dissolved with
Machine ingredient (SOF), coating is mainly made of oxide coating and active noble metal constituent, and noble metal is oxidative catalyst
Key component can exactly reduce the chemistry of HC, CO and SOF in diesel engine vent gas etc. for diesel vehicle DOC using DOC
The activation energy of reaction enables these substances to carry out oxidation reaction at a lower temperature with the oxygen in tail gas, is converted into CO2With
H2O；Oxidation catalyst loads oxide coating and active metal group usually using ceramic honey comb or honeycomb as carrier thereon
Point, common noble metal component is platinum, Pd etc., and it is platinum, the master of platinum that exhaust gas from diesel vehicle, which post-processes widely used noble metal, at present
If for aoxidizing CO, HC.
As discharge standard is gradually stringent, DOC is only used only and has been unable to reach emission request, elimination is used in conjunction in DOC and DPF
PM or with SCR technology be used in conjunction eliminate NOx be increasingly becoming research hotspot.When DOC and DPF are used in conjunction, it is desirable that
NO generates NO2High conversion rate, be conducive to the regeneration of DPF in this way；When DOC and SCR technology are used in conjunction, it is desirable that NO
Generate NO2Conversion ratio between 40%~70%, and the wider window temperature the better, is conducive to accelerating selection catalysis in this way
The reaction rate of reduction technique reduces NOx emission.
There are problems in terms of NO oxidation for current existing diesel vehicle oxidative catalyst, are based on selective catalytic reduction
The NO oxidizing temperature window of the diesel vehicle oxidative catalyst of technical aspect is relatively narrow, the NO conversion ratio when noble metal additional amount improves
It is higher；After aging, catalyst performance decline is obvious.
Summary of the invention
The purpose of the present invention is to solve diesel vehicle oxidative catalysts in the prior art to aoxidize 40% NO~
The relatively narrow problem of temperature window between 70%, provides that preparation method is simple, NO conversion ratio is wider a kind of based on selectivity
NO oxidation catalyst of catalytic reduction technique and preparation method thereof.
The present invention adopts the following technical scheme: a kind of NO oxidation catalyst based on SCR technology, catalysis
Using cordierite honeycomb ceramic as catalyst carrier, the surface of catalyst carrier applies the coating slurry of laminating noble metal platinum for agent, catalysis
One end of agent is fixed with a certain amount of precious metals pd solution using infusion process, and the precious metals pd amount of solution of the fixation is described urges
The 1/3 of agent total suction, the coating slurry use molecular sieve for HC adsorbent material, SiO2For dispersing agent, zirconium acetate is heat
Stabilization aid, noble metal platinum are active component, and aluminium glue binder is added and is made.
A kind of preparation method of the NO oxidation catalyst based on SCR technology, includes the following steps:
(1) River Bank Stability: by a certain percentage by SiO2, molecular sieve, zirconium acetate, aluminium glue binder be added to deionized water
In, weight ratio is 0.4~0.72: 0.25~0.45: 0.02~0.1: 0.01~0.05, is stirred, and nitric acid tune is added
Slurries pH is saved less than 4.0；
(2) slurries ball milling: slurries are ground by planetary ball mill, and the revolving speed of planetary ball mill is 250~380 turns/
Point, runing time is 3~6h, and serous granule degree to D90 is 2~20um；
(3) measurement of solid content: taking 10g slurries in dry pot, and dry pot is placed in 550~600 DEG C of Muffle kiln roasting 10-
20min is cooled to room temperature, and weighs its powder quality, with the quality divided by 10g, just obtains slurry solid content；
(4) addition of noble metal platinum solution: noble metal platinum solution is added in ball milling rear slurry, stirs 2~8h, until
Active component noble metal platinum solution is thoroughly dispersed in slurries, and the amount of added noble metal platinum is 15~30g/ft3；
(5) coating coats: carrier cordierite honeycomb ceramic being immersed in slurries, the carrier cordierite bee for being saturated with slurries is taken out
Nest ceramics, blow away extra slurries with air gun, and by coated weight be 100~180g/L and solid content controls wet weight gain, calculate practical apply
The amount of covering；
(6) dry: the catalyst coated passes through 100~180 DEG C of flash bakings, and drying time is that 3~6h will be in coating
Water evaporation fall；
(7) it roasts: drying rear catalyst is put into Muffle furnace, 450~550 DEG C of 1~2h of roasting are cooling after heat preservation
To room temperature, catalyst weight is weighed；
(8) quantitatively impregnate precious metals pd solution: one end of catalyst impregnates precious metals pd solution, impregnates the amount of precious metals pd
For 5~10g/ft3, noble metal area end is impregnated as airintake direction, catalyst passes through 100~180 DEG C of 3~6h of drying, in
1~2h is roasted under the conditions of 450~550 DEG C to be made.
Further, it takes the slurries 20g with noble metal to be centrifuged after the completion of the step (4), carries out solid liquid phase point
From taking solid fraction to carry out the measurement of noble metal platinum content with ICP.
Further, the mass ratio of the step (4) and noble metal platinum and palladium in (9) is 3: 1.
Present invention process step is simple, and the catalyst prepared is impregnated with precious metals pd in the direction of air inlet, improved
The oxygenation efficiency of NO at low temperature can be improved in catalyst, and NO is made to be oxidized to NO2Temperature window is more more between 40%~70%
The stability of width, catalyst is more preferable.
Specific embodiment
It below will the invention will be further described according to specific embodiment.Three examples are all made of diameter and are below
The cylindrical cordierite honeycomb ceramic carrier of 80mm, a height of 60mm, volume 0.301L, vehicle weight 97g, noble metal platinum
Concentration is 0.138g (noble metal)/g (liquid), and the concentration of precious metals pd is 0.1511g (noble metal)/g (liquid).
Embodiment one: a kind of preparation method of the NO oxidation catalyst based on SCR technology, including it is as follows
Step:
(1) River Bank Stability: by a certain percentage by SiO2, molecular sieve, zirconium acetate, binder be add to deionized water, weight
Amount ratio is 0.72: 0.25: 0.02: 0.01, is stirred, and surveying pH is 3.24；
(2) slurries ball milling: slurries are ground by planetary ball mill, and revolving speed is 250 revs/min, runing time 6h, slurries
Granularity to D90 be 3.22um；
(3) measurement of solid content: taking 10g slurries that dry pot is placed in 600 DEG C of Muffle kiln roasting 10min in dry pot, cold
But to room temperature, weighing its powder quality is 3.95g, and with the quality divided by 10g, just obtaining slurry solid content is 39.5%；
(4) addition of noble metal platinum solution: the slurries 1000g after taking ball milling, noble metal platinum additional amount are 15g/ft3, apply
The amount of covering is 100g/L, and the amount for calculating noble metal platinum is 2.092g, and the amount for weighing noble metal platinum solution is 15.157g, will
Noble metal platinum solution is added in the slurries after ball milling, 2h is stirred, until active component noble metal platinum is thoroughly dispersed in slurries；
(5) it takes 20g slurries to be placed in test tube, puts into a centrifuge centrifugation, carry out Solid-Liquid Separation, measured using ICP solid
The content of noble metal platinum in phase, result are 0.0052g (noble metal)/g (powder)；
(6) coating coats: carrier cordierite honeycomb ceramic being immersed in slurries, the carrier cordierite bee for being saturated with slurries is taken out
Nest ceramics, blow away extra slurries with air gun, control the wet weight gain of target by coated weight requirements of 150g/L and the solid content that measures, count
Calculation catalyst practical coating amount is 77.4g；
(7) dry: the catalyst coated passes through 100 DEG C of drying 6h, and the water evaporation in coating is fallen；
(8) it roasting: drying rear catalyst is put into Muffle furnace, 450 DEG C of roasting 2h are cooled to room temperature after heat preservation,
Weighing catalyst weight is 127.5g；
(9) precious metals pd solution quantitatively impregnates: catalyst impregnates fixed precious metals pd solution at one end, and precious metals pd is added
Amount is 5g/ft3, the amount for calculating precious metals pd is 0.053g, weighs precious metals pd solution 0.3509g, adds water to dipping
Amount target value is 42.5g, and dipping Pd noble metal area end is as airintake direction, and catalyst passes through 100 DEG C of drying 6h, in 450 DEG C
Under the conditions of roasting 2h be prepared；
Embodiment two: a kind of preparation method of the NO oxidation catalyst based on SCR technology, including it is as follows
Step:
(1) River Bank Stability: by a certain percentage by SiO2, molecular sieve, zirconium acetate, aluminium glue binder be added to deionized water
In, weight ratio 0.58: 0.35: 0.04: 0.03 stirs, and surveying pH is 3.29；
(2) slurries ball milling: slurries are ground by planetary ball mill, and revolving speed is 320 revs/min, runing time 4h, slurries
Granularity to D90 be 3.16um；
(3) measurement of solid content: taking 10g slurries in dry pot, and dry pot is placed in 600 DEG C of Muffle kiln roasting 10min,
It is cooled to room temperature, weighing its powder quality is 3.89g, with the quality divided by 10g, just obtains slurry solid content 38.9%；
(4) addition of precious metal solution platinum: taking ball milling rear slurry 1000g, and noble metal platinum additional amount is 20g/ft3, coating
Amount is 140g/L, and the amount for calculating noble metal platinum is 1.9625g, and the amount for weighing noble metal platinum solution is 14.24g, your gold
Belong in the slurries after platinum solution is added to ball milling, 2h is stirred, until active component noble metal platinum is thoroughly dispersed in slurries；
(5) it takes 20g slurries to be placed in test tube, puts into a centrifuge centrifugation, carry out Solid-Liquid Separation, measured using ICP solid
The content of noble metal platinum in phase, result are 0.0050g (noble metal)/g (powder)；
(6) coating coats: carrier cordierite honeycomb ceramic being immersed in slurries, the carrier cordierite bee for being saturated with slurries is taken out
Nest ceramics, blow away extra slurries with air gun, by 140g/L coated weight requirements and measure solid content control the wet weight gain of target
108.3g, practical coating amount are 110.3g；
(7) dry: the catalyst coated passes through 150 DEG C of drying 4h, and the water evaporation in coating is fallen；
(8) it roasts: drying rear catalyst being put into Muffle furnace, 500 DEG C of roasting 1.5h are cooled to room after heat preservation
Temperature, weighing catalyst weight are 139.1g；
(9) precious metals pd solution quantitatively impregnates: catalyst impregnates precious metals pd solution, precious metals pd additional amount at one end
For 6.7g/ft3, the amount for calculating precious metals pd is 0.071g, weighs precious metals pd solution 0.4698g, adds water to dipping
Amount target value is 46.3g, and the impregnation increment of the precious metals pd solution is the 1/3 of the total water absorption rate of catalyst, impregnates precious metals pd solution
Area end passes through 150 DEG C of drying 4h as airintake direction, catalyst, and 1.5h is roasted under the conditions of 500 DEG C and is prepared；
Embodiment three: a kind of preparation method of the NO oxidation catalyst based on SCR technology, including it is as follows
Step:
(1) River Bank Stability: by a certain percentage by SiO2, molecular sieve, zirconium acetate, aluminium glue binder be added to deionized water
In, weight ratio 0.4: 0.45: 0.1: 0.05 stirs, and surveying pH is 3.45；
(2) slurries ball milling: slurries are ground by planetary ball mill, and revolving speed is 380 revs/min, runing time 3h, slurries
Granularity to D90 be 3.08um；
(3) measurement of solid content: taking 10g slurries in dry pot, and dry pot is placed in 580 DEG C of Muffle kiln roasting 20min,
It is cooled to room temperature, weighing its powder quality is 3.97g, with the quality divided by 10g, just obtains slurry solid content 39.7%；
(4) addition of noble metal platinum solution: taking ball milling rear slurry 1000g, and noble metal platinum additional amount is 30g/ft3It calculates,
Coated weight is 180g/L, and it is 16.937g that the amount for calculating noble metal platinum, which is the amount that 2.337g weighs noble metal platinum solution, expensive
Metal platinum solution is added in the slurries after ball milling, 8h is stirred, until active component noble metal platinum is thoroughly dispersed in slurries；
(5) it takes 20g slurries to be placed in test tube, puts into a centrifuge centrifugation, carry out Solid-Liquid Separation, measured using ICP solid
The content of noble metal platinum in phase, result are 0.0057g (noble metal)/g (powder)；
(6) coating coats: carrier cordierite honeycomb ceramic being immersed in slurries, the carrier cordierite bee for being saturated with slurries is taken out
Nest ceramics, blow away extra slurries with air gun, by 180g/L coated weight requirements and measure solid content control target it is wet increase weight be
136.5g practical coating 137.8g；
(7) dry: the catalyst coated passes through 180 DEG C of drying 3h, and the water evaporation in coating is fallen；
(8) it roasts: drying rear catalyst being put into 550 DEG C of roasting 1h in Muffle furnace, is cooled to room temperature, claims after heat preservation
Amount catalyst weight is 151.7g；
(9) precious metals pd solution quantitatively impregnates: catalyst impregnates precious metals pd solution, precious metals pd additional amount at one end
For 10g/ft3, the amount for calculating precious metals pd is 0.106g, weighs precious metals pd solution 0.703g, adds water to impregnation increment
Target value is 50.5g, impregnates the area end of precious metals pd solution as airintake direction, and catalyst passes through 180 DEG C of drying 3h, in
1h is roasted under the conditions of 550 DEG C to be prepared.
Claims (1)
1. a kind of NO oxidation catalyst based on SCR technology, it is characterised in that: catalyst is with cordierite honeycomb
Ceramics are catalyst carrier, and the coating slurry of surface coating platinum containing noble metal of catalyst carrier, one end of catalyst is using leaching
Stain method is fixed with a certain amount of precious metals pd solution, and the precious metals pd amount of solution of the fixation is the catalyst total suction
1/3, the coating slurry uses molecular sieve for HC adsorbent material, SiO2For dispersing agent, zirconium acetate is thermostabilization auxiliary agent, noble metal
Platinum is active component, and aluminium glue binder is added and is made.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110237858A (en) * | 2019-06-25 | 2019-09-17 | 无锡威孚环保催化剂有限公司 | Composite molecular sieves catalyst and preparation method thereof |
| CN115555044A (en) * | 2022-10-10 | 2023-01-03 | 无锡威孚环保催化剂有限公司 | Preparation method of catalyst for NOx pollutants of hydrogen internal combustion engine |
-
2017
- 2017-11-06 CN CN201711079728.8A patent/CN109746024A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110237858A (en) * | 2019-06-25 | 2019-09-17 | 无锡威孚环保催化剂有限公司 | Composite molecular sieves catalyst and preparation method thereof |
| CN115555044A (en) * | 2022-10-10 | 2023-01-03 | 无锡威孚环保催化剂有限公司 | Preparation method of catalyst for NOx pollutants of hydrogen internal combustion engine |
| CN115555044B (en) * | 2022-10-10 | 2024-02-09 | 无锡威孚环保催化剂有限公司 | Application of catalyst in removing NOx pollutants of hydrogen internal combustion engine |
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Application publication date: 20190514 |