CN107537558A - Strengthen the carried catalyst preparation method for removing NOx with grappling - Google Patents
Strengthen the carried catalyst preparation method for removing NOx with grappling Download PDFInfo
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- CN107537558A CN107537558A CN201710501349.7A CN201710501349A CN107537558A CN 107537558 A CN107537558 A CN 107537558A CN 201710501349 A CN201710501349 A CN 201710501349A CN 107537558 A CN107537558 A CN 107537558A
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- grappling
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Abstract
The present invention relates to a kind of carried catalyst preparation method that NOx is removed with grappling enhancing, i.e. at a certain temperature, copper and iron ion, transition metal ions, molecular sieve, reacted by the chemical action of aminoquinoxaline, so that active component load is uniformly dispersed, the final activated product formed in combustion has the efficient selective effect to NOx grapplings enhancing, and then has preferable conversion rate of NOx.Carried catalyst with grappling enhancing De NO X prepared by present invention conversion rate of NOx under B50 operating modes is up to 96.1%, 548 DEG C of C100 conversion rate of NOx are 82.9%, 198 DEG C of C25 conversion rate of NOx are 86.8%, show that higher NOx activity, the cated expulsion rate of tool are low in 198~548 DEG C.Meanwhile the preparation process is simple, it is easy to industrialize.
Description
Technical field
The present invention relates to the carried catalyst preparation method for strengthening removal NOx with grappling, belongs to motor vehicle emission technology neck
Domain.
Background technology
To meet Abgasgesetz, Urea-SCR technologies have turned into the preferred reduction NOx technologies road of medium and heavy-duty engines enterprise
Line, when its principle is that the NOx in ammonia and vehicle exhaust caused by hydrolysis of urea passes through the carrier for scribbling active coating, NOx is fast
Speed is reduced to nitrogen and water by ammonia, and ammonia and NOx can quickly be chemically reacted on post processing carrier, be and load
The composition interwoveness of body.With active coating carrier be made up of carrier and catalyst, carrier carry first coating and
Active component, suitable catalytic reaction passage is also secondly provided, without the support of carrier, catalyst fines is can not to play its property
Can, cordierite honeycomb carrier is because with high surface area, high density holes, hole wall is thin, thermal coefficient of expansion is low and resistance to sudden heating
Good wait presents superior performance in vehicle exhaust denitration field.Main active component of the catalyst as denitration, it is necessary to load
Competence exertion acts on to carrier, therefore how to organically combine catalyst and carrier, and it is most preferably mesh to reach its denitration effect
The focus of preceding research.
Patent of invention CN201110275543.0 discloses a kind of NOx selective catalytic reduction molecular sieve catalyst and preparation
Method.Catalyst forms：(10%~30%) CeO2- M+ (90%~70%) Fe/ZSM-5, wherein M are TiO2Or WO3,
CeO2/ M mass ratio=3: 1~1: 1；Molecular sieve ZSM-5 SiO2/Al2O3=15~150.With soluble cerium salt and titanium salt
Or tungsten salt is raw material, alkali is coprecipitator, and polyethylene glycol is thickener, and using molecular sieve HZSM-5 as raw material, soluble ammonium salt is
NH4/ZSM-5 is made in source of ammonium, ion exchange.Using soluble ferric iron salt as raw material, Fe, ZSM-5 is made in ion exchange.It is molten with aluminum oxide
One or more in glue, Ludox or acetic acid zirconium are binding agent, and Fe/ZSM-5 is first coated on cordierite honeycomb ceramic carrier, then
Painting is covered with CeO2-M, dries, roasting.Catalyst wide active temperature windows conversion ratio is more than 80%, in 190-600 DEG C of temperature range
Interior achievable efficient catalytic removing nitrogen oxides.
Patent of invention CN201110057115.0 discloses the molecular sieve type use for diesel engine selective catalysis that a kind of manganese is modified
Reducing catalyst.Catalyst is using cordierite honeycomb ceramic as carrier material；Main active component is to enter to divide through ion exchange
The Mn2+ ions and manganese oxide particle of son sieve；The remaining H+ not exchanged and sial skeleton structure are urged respectively as helping in molecular sieve
Agent and coated substrate.In molecular sieve powder after ion-exchanged, manganese element percentage by weight is 0.6~9.2%；Load
In cordierite honeycomb ceramic carrier and coat composed loaded catalyst after coating, coating weight percentage is 5~15%.
Preparation includes molecular sieve modified and loaded catalyst preparation.
The molecular sieve type use for diesel engine selectivity that a kind of manganese of patent of invention CN 201410643551.X, zirconium double metal are modified
Catalytic reduction catalysts.Manganese, zr element are to be entered by liquid ion exchange-infusion process in molecular sieve.With by modified
Powder catalyst gross weight on the basis of, manganese element accounts for percentage by weight 4.5~7.5%, and zr element accounts for percentage by weight 4.5
~15%.On the basis of loaded catalyst gross weight, percentage by weight 5~15% shared by coating.Due to using nontoxic molecule
The manganese element and zr element of sieve and low toxicity prepare the automobile-used SCR catalyst of novel diesel, reduce murder by poisoning of the catalyst to human body；
The high activity of catalyst temperature window in diesel vehicle SCR reactions is expanded simultaneously.Method of modifying is improved load capacity, load
Ratio is more flexible adjustable, is advantageous to the further optimization of catalyst performance.
It is as follows problem to be present in the preparation method of above-mentioned preparation denitration carried catalyst：(1) catalyst temperature window narrows, selection
Poor, the NO of propertyXConversion ratio is low;（2）Active component coating is uneven, and enrichment locally occurs or coated weight is very few；（3）Active component
Coating is low with carrier-bound firmness, and coating is easy to fall off；（4）Preparation technology very complicated.
The content of the invention
It is an object of the invention to provide one kind, and there is grappling enhancing to remove NOXCarried catalyst preparation method, that is, exist
Under certain temperature, copper and iron ion, transition metal ions, molecular sieve, reacted by the chemical action of aminoquinoxaline so that
Active component load is uniformly dispersed, and the activated product finally formed in combustion has the efficient choosing to NOx grapplings enhancing
Selecting property effect, and then there is preferable conversion rate of NOx.Prepared by the present invention has the carried catalyst of grappling enhancing De NO X
Conversion rate of NOx is up to 96.1% under B50 operating modes, and 548 DEG C of C100 conversion rate of NOx are 82.9%, 198 DEG C of C25 conversion rate of NOx
For 86.8%, show that higher NOx activity, the cated expulsion rate of tool are low in 198~548 DEG C.Meanwhile the preparation technology mistake
Journey is simple, is easy to industrialize.
The technical proposal of the invention is realized in this way：Strengthen the carried catalyst preparation method for removing NOx with grappling,
It is characterized in that comprise the following steps that：(1) cordierite honeycomb carrier pre-treatment：Carrier is immersed in mass fraction at room temperature is
20min~60min in 2%~3.8% ammoniacal liquor, carrier cordierite ceramic is taken out, rinsed repeatedly with deionized water to PH in neutrality
By drying, 500 DEG C of calcining 2h~4h；（2）Grappling strengthens the preparation of mixed liquor：A. by 3.6~5.7 parts of molysite, 2.8~
5.2 parts of mantoquitas, 1.4~2.3 parts of metal promoters are dissolved in deionized water, stirring and dissolving；B. 11.3~14.3 parts of molecular sieves are added
Carrier, mix 2~4h；C. 0.3~0.4 part of aminoquinoxaline is added, at 45~60 DEG C, stirs 1~3h；C. add and contain
2.1~4.7 parts of Ludox (SiO2Content be 40%), 2.4~5.3 parts of Alumina gels（Al2O3Content is 40%）, 1.9~6.6 parts of carboxylics
Methylcellulose sodium water solution（Mass fraction 1%）Hybrid adhesive, stir, obtain mixed liquor, until being uniformly mixing to obtain
Contain molecular sieve activity mixed liquor；（3）Cordierite honeycomb carrier activates：Treated carrier cordierite ceramic is placed in and prepared
Contain in molecular sieve activity mixed liquor after 5~10min, take out carrier, blow away remained on surface liquid with purge gas, be placed in baking oven
80~105 DEG C of drying, finally calcine 2~4h at 450 DEG C~530 DEG C and obtain molecular sieve cordierite honeycomb carrier catalyst.
Metal promoter is the one or more in La, Mn, Ni, Ce salt in the grappling enhancing mixed liquor.
The positive effect of the present invention is to be reacted copper and iron ion, transition metal ions, molecular sieve, makes part mixing gold
Category ion enters molecular sieve pore passage, and at a certain temperature by the chemical action of aminoquinoxaline, finally makes molecular sieve and more
Composition activity metal component is formed in calcination process and imitated with the efficient selective to NOx grapplings enhancing by chemical action
Fruit, and there is wider temperature window；Add the binding agent containing high temperature Ludox, high temperature Alumina gel and carboxymethyl cellulose
System, the firmness of active component and carrier combination can be strengthened, solve active component coating and carrier-bound firmness
It is low, coating problem easy to fall off；The monoblock type that grappling enhancing mixed liquor, cordierite honeycomb carrier single step are prepared by burning
Carried catalyst, it is uneven to efficiently solve catalyst activity component coating, and enrichment locally occurs or coated weight is very few asks
Topic.
Brief description of the drawings
Fig. 1 is tested in vibration mechine structural representation to prepare containing non-noble metal monolithic substrate catalyst expulsion rate
Figure.
Embodiment
In following specific example descriptions, a large amount of concrete details are given in order to the more deep understanding present invention.So
And it will be apparent to one skilled in the art that the present invention can be able to without one or more of these details
Implement.
Embodiment 1
(1) cordierite honeycomb carrier pre-treatment
Carrier cordierite ceramic is immersed at room temperature in the ammoniacal liquor of mass fraction 2%, takes out after 60min, rushed repeatedly with deionized water
Wash, untill the PH displays of solution are neutral after the washing lotion, drying, 500 DEG C of calcining 4h at 105 DEG C.
(2) preparation of grappling enhancing mixed liquor
A. 300g copper nitrates, 240g ferric nitrates, 120g cerous nitrates is weighed to be dissolved in 5300g deionized waters；B. add
1200gSapo34 molecular sieve powders, stir 2h；C. add 21.2g aminoquinoxaline, 1h is stirred at 60 DEG C；Add 400g
Ludox (SiO2Content be 40%), 450g Alumina gels（Al2O3Content is 40%）, 400g sodium carboxymethyl cellulose solutions（Quality
Fraction 1%）, stir, obtain mixed liquor.
(3) cordierite honeycomb carrier activates
Will（1）The cordierite honeycomb carrier obtained after middle pretreatment is placed in（2）In in the molecular sieve activity mixed liquor for preparing,
Carrier is taken out after 5min, remained on surface liquid is blown away with compressed air, is placed in 80 DEG C of drying in baking oven, 450 DEG C of calcining 4h are obtained
Strengthen with grappling and remove NOXCarried catalyst.
Molecular sieve cordierite honeycomb carrier catalyst is prepared in embodiment 1 and carries out coating shedding rate experiment, is claimed first
There to be grappling enhancing to remove NO after measuring qualityXCarried catalyst 3 be arranged on vibration mechine 4 on fixture 2 in fix
Bolt 1 is fixed, as shown in Figure 1.Using vibration acceleration 10g, vibration frequency is（100±5）Hz, test period 5h, experiment
Carried catalyst is removed after end and claims its quality, it is 2.95% to be computed coating shedding rate, and this shows active component coating and carrier
With reference to firmness it is high, solve coating problem easy to fall off.
Monolithic substrate catalyst is prepared in embodiment 1 and carries out engine rig test, experiment condition and test knot
Fruit is as shown in table 1, and preparation contains non-noble metal monolithic substrate catalyst engine bench test.
It can be seen that conversion rate of NOx is up to 96.1% under B50 operating modes, 548 DEG C, conversion rate of NOx is minimum under C100 operating modes
82.9%, 198 DEG C of C25 conversion rate of NOx are 86.8%, and higher NOx activity is shown in 198~548 DEG C.
Embodiment 2
(1) cordierite honeycomb carrier pre-treatment
Carrier cordierite ceramic is immersed at room temperature in the ammoniacal liquor of mass fraction 3.8%, is taken out after 60min, use deionized water repeatedly
Rinse, until untill the PH displays of solution are neutral after washing lotion, at 105 DEG C drying, 500 DEG C calcine 4h.
(2) preparation of grappling enhancing mixed liquor
A. 480g copper nitrates, 400g ferric nitrates, 150g lanthanum nitrates is weighed to be dissolved in 5200g deionized waters；B. 1200gZSM5 is added
Molecular sieve powder, stir 4h；C. add 34.2g aminoquinoxaline, 3h is stirred at 45 DEG C；Add 180g Ludox (SiO2
Content be 40%), 200g Alumina gels（Al2O3Content is 40%）, 550g sodium carboxymethyl cellulose solutions（Mass fraction 1%）, stir
Mix uniformly, obtain mixed liquor.
(3) cordierite honeycomb carrier activates
Will（1）The cordierite honeycomb carrier obtained after middle pretreatment is placed in（2）In in the molecular sieve activity mixed liquor for preparing,
Carrier is taken out after 10min, remained on surface liquid is blown away with compressed air, is placed in 105 DEG C of drying in baking oven, 530 DEG C of calcining 4h are produced
NO is removed to strengthening with grapplingXCarried catalyst.
Embodiment 3
(1) cordierite honeycomb carrier pre-treatment
Carrier cordierite ceramic is immersed at room temperature in the ammoniacal liquor of mass fraction 2%, takes out after 30min, rushed repeatedly with deionized water
Wash, untill the PH displays of solution are neutral after the washing lotion, drying, 500 DEG C of calcining 3h at 105 DEG C.
(2) preparation of grappling enhancing mixed liquor
A. 400g copper nitrates, 400g ferric nitrates, 180g manganese nitrates is weighed to be dissolved in 6200g deionized waters；B. add
1200gSapo34 molecular sieve powders, stir 2h；C. add 32.8g aminoquinoxaline, 2h is stirred at 55 DEG C；Add 350g
Ludox (SiO2Content be 40%), 300g Alumina gels（Al2O3Content is 40%）, 180g sodium carboxymethyl cellulose solutions（Quality
Fraction 1%）, stir, obtain mixed liquor.
(3) cordierite honeycomb carrier activates
Will（1）The cordierite honeycomb carrier obtained after middle pretreatment is placed in（2）In in the molecular sieve activity mixed liquor for preparing,
Carrier is taken out after 6min, remained on surface liquid is blown away with compressed air, is placed in 105 DEG C of drying in baking oven, 450 DEG C of calcining 2h are obtained
Strengthen with grappling and remove NOXCarried catalyst.
Embodiment 4
(1) carrier cordierite ceramic pre-treatment
Carrier cordierite ceramic is immersed at room temperature in the ammoniacal liquor of mass fraction 2%, takes out after 30min, rushed repeatedly with deionized water
Wash, untill the PH displays of solution are neutral after the washing lotion, drying, 500 DEG C of calcining 4h at 105 DEG C.
(2) preparation of grappling enhancing mixed liquor
A. 440g copper nitrates, 480g ferric nitrates and 150g nickel nitrates is weighed to be dissolved in 6000g deionized waters；B. add
1200gBeta25 molecular sieve powders, stir 2h；C. add 35.2g aminoquinoxaline, 2h is stirred at 55 DEG C；Add 300g
Ludox (SiO2Content be 40%), 300g Alumina gels（Al2O3Content is 40%）, 250g sodium carboxymethyl cellulose solutions（Quality
Fraction 1%）, stir, obtain mixed liquor.
(3) cordierite honeycomb carrier activates
Will（1）The cordierite honeycomb carrier obtained after middle pretreatment is placed in（2）In in the molecular sieve activity mixed liquor for preparing,
Carrier is taken out after 5min, remained on surface liquid is blown away with compressed air, is placed in 105 DEG C of drying in baking oven, 500 DEG C of calcining 3h are obtained
Strengthen with grappling and remove NOXCarried catalyst.
Embodiment 5
(1) carrier cordierite ceramic pre-treatment
Carrier cordierite ceramic is immersed at room temperature in the ammoniacal liquor of mass fraction 2%, takes out after 30min, rushed repeatedly with deionized water
Wash, untill the PH displays of solution are neutral after the washing lotion, drying, 500 DEG C of calcining 4h at 105 DEG C.
(2) preparation of grappling enhancing mixed liquor
A. 400g copper nitrates, 350g ferric nitrates, 80g cerous nitrates, 80g lanthanum nitrates, 80g manganese nitrates are weighed and is dissolved in 7000g deionizations
In water；B. 1200gSSZ -13 molecular sieve powders are added, stir 2h；C. add 31.8g aminoquinoxaline, stirred at 60 DEG C
2h；Add 480g Ludox (SiO2Content be 40%), 520g Alumina gels（Al2O3Content is 40%）, 380g sodium carboxymethylcelluloses
The aqueous solution（Mass fraction 1%）, stir, obtain mixed liquor.
(3) cordierite honeycomb carrier activates
Will（1）The cordierite honeycomb carrier obtained after middle pretreatment is placed in（2）In in the molecular sieve activity mixed liquor for preparing,
Carrier is taken out after 5min, remained on surface liquid is blown away with compressed air, is placed in 105 DEG C of drying in baking oven, 530 DEG C of calcining 2h are obtained
Strengthen with grappling and remove NOXCarried catalyst.
Claims (4)
1. NOx carried catalyst preparation method is removed with grappling enhancing, it is characterised in that comprise the following steps that：(1) violet is blue or green
Stone honeycomb substrate pre-treatment：Carrier is immersed in 20min~60min in the ammoniacal liquor that mass fraction is 2%~3.8% at room temperature, taken
Go out carrier cordierite ceramic, rinsed repeatedly with deionized water to PH and calcine 2h~4h through drying, 500 DEG C in after neutrality；（2）Grappling
Strengthen the preparation of mixed liquor：A. the molysite, mantoquita, metal promoter of certain mass are dissolved in deionized water, stirring and dissolving；b.
Molecular sieve carrier is added, mixes 2~4h；C. add aminoquinoxaline, at 45~60 DEG C, stir 1~3h；C. add and bond
Agent, until being uniformly mixing to obtain mixed liquor；（3）Cordierite honeycomb carrier activates：Treated carrier cordierite ceramic is placed in
What is prepared contains in molecular sieve activity mixed liquor after 5~10min, takes out carrier, blows away remained on surface liquid with purge gas, put
In 80~105 DEG C of drying of baking oven, finally calcine 2~4h at 450 DEG C~530 DEG C and obtain molecular sieve cordierite honeycomb carrier carrier
Carried catalyst.
2. the carried catalyst preparation method according to claim 1 that NOx is removed with grappling enhancing, it is characterised in that institute
State grappling enhancing mixed liquor in molysite be 3.6~5.7 parts, mantoquita is 2.8~5.2 parts, metal promoter is 1.4~2.3 parts, molecule
To sieve as 11.3~14.3 parts, aminoquinoxaline be 0.3~0.4 part, binding agent is 9.0~14.8 parts.
3. the carried catalyst preparation method body according to claim 1 that NOx is removed with grappling enhancing, it is characterised in that
Metal promoter is the one or more in La, Mn, Ni, Ce salt in the grappling enhancing mixed liquor.
4. the carried catalyst preparation method body according to claim 1 that NOx is removed with grappling enhancing, it is characterised in that
Binding agent is the mixture of Ludox, Alumina gel and sodium carboxymethylcellulose in the grappling enhancing mixed liquor, wherein 2.1~
4.7 parts of Ludox, SiO2Content is 40%, 2.4~5.3 part of Alumina gel, Al2O3Content is 40%, 1.9~6.6 part of carboxymethyl cellulose
Plain sodium water solution, mass fraction 1%.
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