CN100371072C - Preparation process of selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide - Google Patents
Preparation process of selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide Download PDFInfo
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- CN100371072C CN100371072C CNB2005100865500A CN200510086550A CN100371072C CN 100371072 C CN100371072 C CN 100371072C CN B2005100865500 A CNB2005100865500 A CN B2005100865500A CN 200510086550 A CN200510086550 A CN 200510086550A CN 100371072 C CN100371072 C CN 100371072C
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Abstract
The present invention relates to a preparation process of selective reduction catalyst for lean-burn gasoline automobile exhaust discharge nitrogen oxide, which belongs to the technical field of preparing catalyst for nitrogen oxide reduction in environmental protection. The pseudo-boehmite solid elastomer powder is used as raw material; nitric acid is used as a peptizing agent; urea is used as a dispersing agent; aluminum collosol is obtained by ball milling; a cordierite honeycomb ceramics carrier of 200 to 800 pores/inch2 is immersed into the aluminum collosol liquid, an Al2O3 coating is formed by drying and roasting the aluminum collosol liquid; the Al2O3 coating is excessively submerged in silver nitrate solution and taken out for preparing Ag/Al2O catalyst through roasting. The NOx selective reduction catalyst prepared by the method of the present invention obtains high catalytic conversion efficiency for gaseous contaminants of NOx in the range of lean-burn automobile exhaust discharge temperature, particularly a low temperature range; the catalyst has high reduce selectivity at the same time; the present invention solves the problem of difficult removal of NOx under the condition of oxygen enrichment and reaches the purpose of controlling the lean-burn automobile exhaust discharge, and an environmental benefit is obtained.
Description
Technical field
The present invention relates to a kind of preparation method of selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide, belong to catalyst for reduction of oxides of nitrogen preparing technical field in the environmental protection.
Background technology
Along with increasingly sharpening of global energy crisis situation and greenhouse gases effect, the feasible economy of fuel and the energy and environment problem that reduction CO2 isothermal chamber gas emissions has become the countries in the world common concern of how improving.The gasoline engine that generally uses is to work near theoretical air-fuel ratio at present, and purpose is to make the three-way catalyst that is installed in the tail-gas from gasoline automobiles after-treatment system CO in the engine discharging tail gas, HC and NOx efficiently can be changed into harmless CO
2, H
2O and N
2, but the above-mentioned this several contaminants efficient simultaneously mechanism that transforms is to be based upon the fuel oil imperfect combustion with on the basis that produces reducing agents such as a large amount of CO, HC, therefore becomes the less economical basic reason of gasoline engine fuel.
The gasoline engine that lean-burn gasoline motor car is installed is a kind of engine of working under greater than the chemically correct fuel operating condition in air-fuel ratio.Owing in engine, add excessive air, make fuel can obtain burning more completely, therefore determined this engine to have the fuel economy more superior, lower CO, HC, NOx pollutant and greenhouse gases CO than chemically correct fuel gasoline engine
2Generation.Because gasoline engine discharging tail gas is in the poor gas atmosphere, that is to say at engine discharging tail gas and have excessive oxygen, and be widely used at present contain noble metal such as Pt, Pd, the three-way catalyst of Rh only can be in theoretical air-fuel ratio environs work, could be with CO, three kinds of contaminant gases of HC and NOx effectively transform simultaneously, it is under the exhaust emissions situation of excessive oxygen, can only better conversion CO and HC, but be difficult to effectively carry out the catalytic reduction conversion of NOx, therefore use three-way catalyst to be used for the gasoline engine vent gas treatment, can cause the NOx conversion ratio of being on duty mutually.
The NOx selective reduction catalyst uses hydro carbons as reducing agent, can effectively transform the NOx in the discharging tail gas under the vehicle exhaust excess oxygen.The NOx selective reduction catalyst is applied to the lean-burn gasoline motor car vent gas treatment, is expected to satisfy the strict more automobile exhaust emission standard of issuing and implementation from now on.The discharging exhaust temperature of gasoline engine generally hangs down 200-600 ℃ than the gasoline car of chemically correct fuel, so compare with three-way catalyst, the NOx selective reduction catalyst must have the catalytic reduction reaction activity under lower exhaust temperature condition, can make just that NOx obtains more conversions in the tail gas.
At present the NOx selective reduction catalyst can roughly be divided into three types of noble metal, zeolite and metal oxides.For noble metal type catalyst, its low temperature active is better, but has the deficiency of active temperature narrow range, a large amount of N2O of generation; And there is the problem of hydrothermal stability difference in the zeolite type catalyst; In the metallic oxide type catalyst, some metal oxide oxidation catalyst active components such as Ag, Cu, In etc. show good selectivity and high reaction activity and high to the NOx reduction reaction, therefore have potential application prospect.
For Ag/Al
2O
3Catalyst, with hydro carbons such as the alkane of alkene, high carbon number and alcohols is reducing agent, between middle high-temperature region, show good NOx reduction reaction activity, especially with ethanol as reducing agent, its active temperature scope can drop within the exhaust emissions temperature range of lean-burn automotive engine especially, therefore has the possibility of Application and Development largely.Countries in the world are to Ag/Al at present
2O
3Catalyst has carried out more deep basic theoretical research, but for how optimizing integral catalyzer preparation technology so that the NOx reduction reaction performance of this catalyst improves, the research of this respect report is not a lot.
With microwave technology be applied to the inducing catalysis reaction, Preparation of Catalyst is the latest developments that obtained in catalytic field in the last few years, as in oxidation of the decomposition that aspect the inducing catalysis reaction microwave technology is applied to the halogenated organic hydrocarbon, methane conversion, hydrocarbon etc.; Aspect Preparation of Catalyst, utilize microwave that the dielectric heat effect of water is carried out the synthetic of A type, X type, Y type, ZSM-5 type equimolecular sieve, compare with traditional hydrothermal synthesis method, microwave process for synthesizing can simultaneously a large amount of nucleation and can be shortened crystallization time significantly, obtain evenly tiny crystal grain, specific area increases; Also there are some scholars to utilize microwave technology some inorganic salts to be loaded on the dust carrier such as molecular sieve recently,, thereby catalyst shown than better activity of conventional load mode and selectivity because microwave has improved the active component dispersiveness.Compare with traditional mode of loading, on carriers such as molecular sieve, have the following advantages: the decentralization height with the microwave method load active component; Processing time is short, the efficient height; The processing sample is simple, has avoided mixing, oven dry and the roasting of solution.
In the Preparation of catalysts process, our beyond thought discovery is compared in conjunction with the preparation technology that conventional heat drying combines with incipient impregnation, the Ag/Al for preparing with excessive infusion process and microwave drying or conventional drying process combined
2O
3Integral catalyzer shows the low-temperature reactivity of excellent more NOx conversion performance, especially catalyst.When transforming the simulation lean-burn gasoline tail gas of same composition, the catalyst that the highest transformation efficiency of NOx of the catalyst of invention is prepared in conjunction with the oven drying method than traditional incipient impregnation will exceed more than 30%, and temperature window has also taken place obviously to move to low-temperature space.Therefore, the catalyst of present invention has overcome the Ag/Al of preparation in the past
2O
3The deficiency of integral catalyzer can better be used for the lean-burn vehicle exhaust and handle.
Summary of the invention
The present invention on cordierite honeycomb ceramic carrier coated with the high-specific surface area activated alumina (Al of Prepared by Sol Gel Method
2O
3) coating material, and with excessive infusion process with the Ag spread loads at active A l
2O
3On the coating material,, promptly obtain required catalyst then by step of preparation process such as microwave drying, calcination activations.The constituent content of this catalyst is: Ag, 0.5-4wt% (accounting for the mass percent of coating amount); Al
2O
3Coating material content, 2-50wt% (accounting for the mass percent of ceramic monolith weight).
A kind of preparation process of selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide, this preparation method may further comprise the steps:
(1) be that raw material, nitric acid are that peptizing agent, urea are dispersant with the boehmite dry glue powder, by the aluminium colloidal sol that ball milling obtains having the narrow particle diameter distribution and the viscosity that suits, its solid content is 5-50wt%;
(2) with 200-800 hole/inch
2Cordierite honeycomb ceramic carrier immerses the time of second of 20-180 in the aluminium sol solutions of above-mentioned preparation, takes out the back and blows out colloidal sol unnecessary in the carrier duct gently with compressed air, and at 80-200 ℃ of dry 2-10 hour, 400-800 ℃ formed Al in roasting 2-6 hour
2O
3Coating; The Al that forms
2O
3Coating material is high surface active A l
2O
3, the load capacity of coating is the 2-50wt% of honeycomb ceramic carrier weight;
(3) measure Al on the described honeycomb ceramic carrier
2O
3The saturated water adsorptive value of coating also calculates Al
2O
3The load capacity of silver on the coating, the liquor argenti nitratis ophthalmicus of preparation respective concentration;
(4) will apply Al
2O
3The carrier of coating is excessive to be immersed in the liquor argenti nitratis ophthalmicus of described preparation and to take out after 30-120 minute, redundant nitric acid silver solution residual in the catalyst carrier duct is blown out with compressed air, obtain the catalyst of loaded Ag, its Ag load capacity is the 0.5-4wt% of aluminum oxide coating layer amount;
(5) will carry out drying with microwave drying 5-20 minute or conventional Electric heat oven drying mode in the mode of 60-200 ℃, 2-12 hour with the catalyst of above-mentioned excessive infusion process loaded Ag, in the 300-700 ℃ of air atmosphere calcination process 2-6 hour, promptly prepare Ag/Al
2O
3Catalyst.
Heating using microwave is body phase Fast Heating mode, and the gradient that can reduce integral catalyzer temperature inside and humidity to a considerable extent distributes, and reduces migration and the gathering of Ag active component in dry run, makes the Ag active component at active A l
2O
3The coating material surface evenly distributes, and has improved the decentralization of Ag, thereby the NOx reduction reaction performance of catalyst is improved.
The preparation method of a kind of selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide provided by the invention, the NOx selection type catalytic reduction catalysts for preparing by this kind preparation method, in the scope of lean-burn motor vehicle exhaust emission temperature, especially low temperature range, can obtain the catalytic conversion efficiency very high to gaseous contaminant NOx, catalyst also has very high reduction selectivity simultaneously, both can revert to N fully to NO
2, solved the problem that NOx is difficult to remove under excess oxygen, reach the purpose of control lean-burn motor vehicle exhaust emission, can obtain good benefits in environment.
Description of drawings
Fig. 1 is Ag/Al
2O
3The NOx conversion ratio of catalyst is with the change curve of reaction temperature, and wherein abscissa is a reaction temperature, unit ℃, and ordinate is the NOx conversion ratio, the % of unit.
The specific embodiment
Fig. 1 is Ag/Al
2O
3The NOx conversion ratio of catalyst is with the change curve of reaction temperature, and wherein abscissa is a reaction temperature, unit ℃, and ordinate is the NOx conversion ratio, the % of unit.Three curves in the accompanying drawing 1: the square line is represented the Ag/Al for preparing in conjunction with conventional Electric heat oven drying with incipient impregnation
2O
3The NOx conversion ratio of catalyst is with the change curve of reaction temperature; Round wire is represented the Ag/Al for preparing in conjunction with conventional Electric heat oven drying with excessive dipping
2O
3The NOx conversion ratio of catalyst is with the change curve of reaction temperature; The triangle line is represented the Ag/Al for preparing in conjunction with microwave drying with excessive dipping
2O
3The NOx conversion ratio of catalyst is with the change curve of reaction temperature.
Specify the present invention below in conjunction with embodiment.
Embodiment 1
In the boehmite dry glue powder, add rare HNO
3And urea, promptly obtain the alumina sol that solid content is 21wt% behind the high-speed stirred 5h.The whole samples of 400 hole cordierite honeycomb ceramics are immersed in the above-mentioned colloidal sol 1 minute, take out the back and blow unnecessary colloidal sol in the carrier duct off with compressed air, subsequently the carrier sample is placed at room temperature dry in the shade (32 ℃) 6 hours, 110 ℃ of dryings are 6 hours in the baking oven, 600 ℃ of roastings 2 hours in muffle furnace at last promptly prepare the ceramic monolith of active oxidation aluminized coating.
Certain density silver nitrate aqueous solution is flooded above-mentioned ceramic monolith with aluminum oxide coating layer in isopyknic mode, 110 ℃ of oven dryings then, 600 ℃ of roasting 3h in muffle furnace promptly get Ag/Al at last
2O
3Integral catalyzer, wherein the Ag load capacity is 2wt%.
Embodiment 2
Certain density silver nitrate aqueous solution is flooded the ceramic monolith with aluminum oxide coating layer for preparing in the example 1 in the mode of following excessive dipping: according to the load capacity of silver on the saturated water adsorptive value of aluminum oxide coating layer on the honeycomb ceramic carrier and the aluminum oxide coating layer, calculate the concentration of liquor argenti nitratis ophthalmicus, prepare corresponding liquor argenti nitratis ophthalmicus, will apply Al
2O
3The carrier of coating is immersed in the liquor argenti nitratis ophthalmicus of above-mentioned preparation and after 30-120 minute carrier is taken out, and redundant nitric acid silver solution residual in the catalyst carrier duct is blown out with compressed air.Then with catalyst at 110 ℃ of baking oven heat dryings, 600 ℃ of roasting 3h in muffle furnace promptly get Ag/Al at last
2O
3Integral catalyzer, wherein the Ag load capacity is 2wt%.
Embodiment 3
With the ceramic monolith with aluminum oxide coating layer of certain density silver nitrate aqueous solution to prepare in the excessive impregnation method dipping example 1 described in the example 2, microwave drying is 10 minutes then, and 600 ℃ of roasting 3h in muffle furnace promptly get Ag/Al at last
2O
3Integral catalyzer, wherein the Ag load capacity is 2wt%.
Embodiment 4
With the above-mentioned catalyst sample chamber lean-burn simulative automobile tail gas performance evaluation that experimentizes.The catalyst carrier sample is put into quartz tube reactor, distribution simulation lean-burn motor vehicle exhaust emission composition, with the reducing agent of ethanol as NOx, the reacting gas that uses is 1.01%NO/He (99.995%), O
2(99.995%), N
2(99.995%), absolute ethyl alcohol (analyzing pure), the reaction air inlet consist of 0.07%NOx, 0.19%C
2H
5OH, 8.0%O
2, N
2Be balance gas.Charge flow rate is 564ml/min, and air speed is 21500h
-1In evaluation procedure, keep each gas flow constant, and programme-control catalytic bed temperature, the while is by NO, the NO of process catalyst under the chemiluminescence formula NOx gas analyzer surveying record differential responses temperature
2With the NOx gas component concentrations, the NOx conversion ratio when calculating the differential responses temperature.
The experimental result of above-mentioned example as shown in Figure 1, the catalyst for preparing in the example 3 has 81.5% NOx maximum conversion rate at 375 ℃, the temperature operation window that NOx transforms has taken place obviously to move to low-temperature space, shows that the NOx SCR integral catalyzer that adopts excessive dipping to prepare in conjunction with microwave drying process has the wide and higher NOx conversion ratio of NOx conversion temperature window of very low NOx reduction reaction temperature, broad.In addition, the Preparation of catalysts good process repeatability, technological process is simple, energy consumption is relatively low.The monoblock type Ag/Al that also shows invention by the engine pedestal experiment
2O
3Catalyst can reach the purpose of effective control lean-burn automobile NOx discharge capacity, has the good application development prospect.
Claims (4)
1. the preparation method of a selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide is characterized in that, this preparation method may further comprise the steps:
(1) be that raw material, nitric acid are that peptizing agent, urea are dispersant with the boehmite dry glue powder, ball milling obtains aluminium colloidal sol, and its solid content is 5-50wt%;
(2) with 200-800 hole/inch
2Cordierite honeycomb ceramic carrier immerses 20-180 second in the aluminium sol solutions of above-mentioned preparation, takes out, and blows out colloidal sol unnecessary in the carrier duct gently with compressed air, and at 80-200 ℃ of dry 2-10 hour, 400-800 ℃ formed aluminum oxide coating layer in roasting 2-6 hour;
(3) measure the saturated water adsorptive value of aluminum oxide coating layer on the described cordierite honeycomb ceramic carrier and calculate the load capacity of silver on the aluminum oxide coating layer, the liquor argenti nitratis ophthalmicus of preparation respective concentration;
(4) adopt excessive infusion process the cordierite honeycomb ceramic carrier of covering aluminum oxide coating be immersed in the liquor argenti nitratis ophthalmicus of step (3) preparation and take out after 30-120 minute, redundant nitric acid silver solution residual in the catalyst carrier duct is blown out with compressed air, obtain the catalyst of loaded Ag active component;
(5) catalyst that step (4) is obtained is with microwave drying 5-20 minute, in the 300-700 ℃ of air atmosphere calcination process 2-6 hour, promptly prepares Ag/Al
2O
3Catalyst.
2. the preparation method of a kind of selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide according to claim 1 is characterized in that, the aluminum oxide coating layer load capacity of formation is the 2-50wt% of honeycomb ceramic carrier weight.
3. the preparation method of a kind of selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide according to claim 1 is characterized in that, the catalyst A g load capacity of described loaded Ag active component is the 0.5-4wt% of aluminum oxide coating layer amount.
4. the preparation method of a selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide is characterized in that, this preparation method may further comprise the steps:
(1) be that raw material, nitric acid are that peptizing agent, urea are dispersant with the boehmite dry glue powder, ball milling obtains aluminium colloidal sol, and its solid content is 5-50wt%;
(2) with 200-800 hole/inch
2Cordierite honeycomb ceramic carrier immerses 20-180 second in the aluminium sol solutions of above-mentioned preparation, takes out, and blows out colloidal sol unnecessary in the carrier duct gently with compressed air, and at 80-200 ℃ of dry 2-10 hour, 400-800 ℃ formed aluminum oxide coating layer in roasting 2-6 hour;
(3) measure the saturated water adsorptive value of aluminum oxide coating layer on the described cordierite honeycomb ceramic carrier and calculate the load capacity of silver on the aluminum oxide coating layer, the liquor argenti nitratis ophthalmicus of preparation respective concentration;
(4) adopt excessive infusion process the cordierite honeycomb ceramic carrier of covering aluminum oxide coating be immersed in the liquor argenti nitratis ophthalmicus of step (3) preparation and take out after 30-120 minute, redundant nitric acid silver solution residual in the catalyst carrier duct is blown out with compressed air, obtain the catalyst of loaded Ag active component;
(5) adopt the catalyst of the loaded Ag active component that Electric heat oven obtains step (4) to carry out drying,, under 300-700 ℃ of air atmosphere condition calcination process 2-6 hour at last, promptly prepare Ag/Al 60-200 ℃ temperature range inner drying 2-12 hour
2O
3Catalyst.
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| CNB2005100865500A CN100371072C (en) | 2005-09-30 | 2005-09-30 | Preparation process of selective reduction catalyst for lean-burn gasoline motor car exhausted gas nitrogen oxide |
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| CN100371072C true CN100371072C (en) | 2008-02-27 |
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| US8173574B2 (en) * | 2006-09-20 | 2012-05-08 | Basf Corporation | Catalysts to reduce NOx in an exhaust gas stream and methods of preparation |
| CN102091615A (en) * | 2010-10-15 | 2011-06-15 | 中国科学院生态环境研究中心 | Application of nano cerium dioxide supported nitrogen oxide storage-reduction catalyst in purifying lean-burn tail gases |
| US8844267B2 (en) * | 2011-03-17 | 2014-09-30 | GM Global Technology Operations LLC | Method and system for controlling a nitrogen oxide (NOx) conversion efficiency monitor |
| CN103084218A (en) * | 2013-01-28 | 2013-05-08 | 江苏帕艾尼尔科技有限公司 | Method for loading coating on sponge metal and coating prepared by same |
| CN104148091B (en) * | 2014-08-28 | 2016-08-24 | 华东师范大学 | Integral automobile tail gas clean-up three-way catalyst and preparation method thereof |
| CN105642369B (en) * | 2014-12-04 | 2019-01-25 | 中国石油化工股份有限公司 | A kind of reduction NOxThe alumina support forming processing method of discharge |
| CN105032417B (en) * | 2015-06-05 | 2018-07-20 | 华南理工大学 | A kind of SCR denitration and the preparation method and application thereof of high sulfur resistive |
| CN105854496B (en) * | 2016-06-02 | 2017-11-24 | 浙江农林大学暨阳学院 | A kind of traffic route air cleaning unit |
| KR20190132914A (en) * | 2018-05-21 | 2019-11-29 | 희성촉매 주식회사 | Modified zeolites with thermal stability and a catalyst composite using thereof |
| CN110412091B (en) * | 2019-07-10 | 2024-04-23 | 宁波大学 | Reusable damage identification piezoelectric sensing device |
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