CN102151564A - Preparation method and slurry of denitration integral type catalyst - Google Patents
Preparation method and slurry of denitration integral type catalyst Download PDFInfo
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- CN102151564A CN102151564A CN2011100347117A CN201110034711A CN102151564A CN 102151564 A CN102151564 A CN 102151564A CN 2011100347117 A CN2011100347117 A CN 2011100347117A CN 201110034711 A CN201110034711 A CN 201110034711A CN 102151564 A CN102151564 A CN 102151564A
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Abstract
The invention provides slurry for preparing a denitration integral type catalyst, which comprises a catalyst, silica gel and water. The invention also provides a method for preparing the denitration integral type catalyst by using a dipping method. Compared with the prior art, the slurry of the invention does not include any organic solvent, is simple and environmental-friendly and can reduce the production cost. The prepared integral type catalyst has higher denitration activity and wider temperature window, the coating amount of the catalyst can be realized by adjusting the concentration of the catalyst in the slurry liquor and the target coating amount can be obtained by only one-time coating so that the preparation process is greatly shortened, the production cost is greatly reduced and large-scale production can be carried out.
Description
Technical field
The present invention relates to a kind of catalysis material field of nitrogen oxide reduction, especially a kind of preparation method of denitrating integral catalyst and slurry simple, environmental protection thereof.
Background technology
In recent years, diesel engine enjoys favor with its good fuel economy and power performance, but the greatest problem that diesel engine exists is exactly that discharged nitrous oxides is serious.Nitrogen oxide includes NO, NO
2, N
2O, N
2O
3, N
2O
4And N
2O
5Deng, the NO that produces in the various fuel combustion process
xMainly be NO, account for 90%~95%, NO
2Account for 5%~10%, N
2O only accounts for about 1%, NO and NO
2Be referred to as NO
xNitrogen oxide (NO
x) be a global environmental problem to the pollution of atmosphere, its influence mainly shows as and forms acid rain, causes photochemical fog, causes the surface layer atmospheric ozone to pollute, produce greenhouse effects, destroys natural ecological environment etc.In addition, NO
xAlso participate in forming airborne floating dust (PM
2.5), the serious harm human health.Therefore, restriction diesel engine NO
xThe rules of discharging are also grown out of nothing, and to strictness, how to reduce diesel engine for automobile NO from loose
xThe research of discharging seems particularly important.
At present, SCR (SCR, i.e. selective catalytic reduction) denitration technology becomes the denitration technology of main flow on the our times with it up to 90% denitration rate.The SCR denitration is under the situation that catalyst exists, and adopting Ammonia material, CO, hydrocarbon is reducing agent, and the reducing substances that also can utilize tail gas self is with the NO in the tail gas
xBe reduced into N
2In recent years, the diesel vehicle SCR technology of external practicability mainly is that employing ammonia is the catalyst system and catalyzing of reducing agent, in view of NH
3Toxicity, the researcher generally adopts 32.5% aqueous solution of urea to replace ammonia to carry out Selective Catalytic Reduction of NO x, i.e. the Urea-SCR system.For example, be that the center begins to carry out the exemplary detection test of SCR the nineties with Europe on truck or motor bus, and this technology has been known as the preferred option of Europe up to standard IV, Europe V by European countries.U.S. automotive engineer association (SAE) announces that also it is one of candidate technologies of suitable Abgasgesetz in recent years.
Catalyst is the core of NH3-SCR technology, and the SCR catalyst divides by operating temperature, can be divided into low temperature (<300 ℃), middle temperature (300-400 ℃) and high temperature section (>400 ℃) catalyst.High temperature section catalyst during research at present and using mostly is is announced PILC (the pillared interlayered clay) catalyst that discloses a kind of metal ion exchanged for No. 6521559 as United States Patent (USP), and wherein Jiao Huan metal ion comprises Cr
3+, Mn
2+, Co
2+, Cu
2+, Ni
2+Deng, carrier is PILC or is the Al of coupling
2O
3-PILC, TiO
2-PILC, ZrO
2-PILC and SiO
2-PILC, and auxiliary agent Ce, La, Pr, Th, Nd etc. in addition, this catalyst has improved the catalytic activity of catalyst greatly, and has strengthened its anti-sulphur ability.United States Patent (USP) is announced and is disclosed the technology that a modification by carrier improves the catalyst activity for No. 4975256, for example, titanium salt is deposited in the inorganic oxide SiO of porous
2, Al
2O
3And ZrO
2Deng on, macropore (aperture>600 that increase catalyst carrier
) number, rational pore-size distribution is provided, thereby has significantly improved catalytic activity, and than using Detitanium-ore-type TiO separately
2The cost of making carrier is low.
But, though granular catalyst has shown catalysis behavior preferably in little anti-test, but in the actual application of SCR technology, because the catalyst fluid resistance of nutty structure greatly, easily stopped up by the tail gas dust, cause pressure drop to increase, feasible operation can not move continuously, so the catalyst that adopts is an integral catalyzer usually.Integral catalyzer has the bigger parallel channels of percent opening, help dust pass through be difficult for stopping up, wear-resistant, and have pressure and reduce, can utilize advantages such as surface height, heat transfer and mass transfer ability are good, easy to loading and unloading, so be widely used in the processing of motor-vehicle tail-gas.By wide coverage and to be applied to the integral catalyzer of exhaust gas from diesel vehicle in removing generally be to adopt immersion process for preparing, and the key technology of immersion process for preparing integral catalyzer is exactly the preparation of the used slurries of dipping.In order to make coating have better caking property and uniformity, generally can use a large amount of organic solvents in the slurries preparation of traditional integral catalyst, this not only can significantly increase production cost, and production process also is easy to cause environmental pollution.
In view of this, a kind of simply, the integral catalyzer slurry that do not contain organic solvent of necessary research and development and the preparation method of integral catalyzer.
Summary of the invention
The objective of the invention is to: a kind of slurry of preparation denitrating integral catalyst of simple, environmental protection is provided, and the method for utilizing this slurry efficient production denitrating integral catalyst is provided.
In order to solve the problems of the technologies described above, the invention provides a kind of slurry for preparing denitrating integral catalyst, it comprises catalyst, silica gel and water.
The mass percent of each composition is in the above-mentioned slurry: silica gel is with SiO
2Count 5-10%, preferably 6-7%; Catalyst 10-50%, preferably 30-35%; Water 40-85%, preferably 58-64%.
Described water is deionized water, and silica gel is 20% silica gel.
Described catalyst is the catalytic component based on vanadium of titania supported, and wherein content of vanadium is with V
2O
5Quality meter 0.5-10%, and contain with WO
3The tungsten auxiliary agent of meter 0.5-10%.
In order to solve the problems of the technologies described above, the present invention also provides a kind of method for preparing denitrating integral catalyst, it is the slurry that utilizes in above-mentioned arbitrary paragraph, adopt the immersion process for preparing denitrating integral catalyst, concrete steps are: after catalyst is ground, be dispersed in the aqueous solution of silica gel, solid content is determined by the final coated weight of catalyst, stirred 0.5-2 hour, and made slurry; Carrier is dipped in the slurry, slowly takes out after 5 minutes, dry up raffinate with ear washing bulb, wore out 6-10 hour under the room temperature, at 80-110 ℃ of dry 3-5 hour, then in Muffle furnace with 1-5 ℃ of/minute temperature programming to 450-600 ℃ the calcining 1-5 hour, make denitrating integral catalyst.
Described carrier is a cellular structure ceramic carrier.
The above-mentioned method for preparing denitrating integral catalyst, also comprise to before applying and the cellular structure ceramic carrier after applying weigh, to determine the step of coated weight.
With respect to prior art, do not contain any organic solvent in the slurry of the present invention, not only simple, environmental protection, and can reduce production costs; The integral catalyzer that the present invention prepares has the higher denitration activity and the temperature window of broad, and the coated weight of catalyst can be realized by catalyst concentration in the modulation slurries, only need primary coating just can obtain the target coated weight, thereby shorten preparation process greatly, significantly reduce production costs, also just be more suitable for large-scale production.
Description of drawings
Fig. 1 is the denitration effect figure of the prepared denitrating integral catalyst of various embodiments of the present invention.
Fig. 2 is the catalyst denitration effect comparison diagram of the embodiment of the invention 2 prepared denitrating integral catalysts and prior art.
The specific embodiment
Embodiment 1
Cordierite honeycomb ceramic after the roasting is weighed.With catalyst V
2O
5/ WO
3/ TiO
2After the grinding, get 8 grams and be dispersed in 4 gram water, the solution made of 8 grams, 20% silica gel, stirred 0.5 hour, make catalyst content and be 40% slurry.The carrier cordierite honeycomb ceramic is dipped in the above-mentioned slurry, slowly take out after 5 minutes, dry up raffinate with ear washing bulb, wore out 8 hours under the room temperature, 110 ℃ of dryings 4 hours, then in Muffle furnace with 2 ℃ of/minute temperature programmings to 550 ℃ calcining 2 hours, make denitrating integral catalyst, and it weighed to determine coated weight.
Embodiment 2
Cordierite honeycomb ceramic after the roasting is weighed.With catalyst V
2O
5/ WO
3/ TiO
2After the grinding, get 8 grams and be dispersed in 8 gram water, the solution made of 8 grams, 20% silica gel, stirred 1.5 hours, make catalyst content and be 33.3% slurry.The carrier cordierite honeycomb ceramic is dipped in the above-mentioned slurry, slowly take out after 5 minutes, dry up raffinate with ear washing bulb, wore out 8 hours under the room temperature, 110 ℃ of dryings 4 hours, then in Muffle furnace with 2 ℃ of/minute temperature programmings to 550 ℃ calcining 2 hours, make denitrating integral catalyst, and it weighed to determine coated weight.
Embodiment 3
Cordierite honeycomb ceramic after the roasting is weighed.With catalyst V
2O
5/ WO
3/ TiO
2After the grinding, get 6.4 grams and be dispersed in 8 gram water, the solution made of 8 grams, 20% silica gel, stirred 1.5 hours, make catalyst content and be 28.6% slurry.The carrier cordierite honeycomb ceramic is dipped in the above-mentioned slurry, slowly take out after 5 minutes, dry up raffinate with ear washing bulb, wore out 8 hours under the room temperature, 110 ℃ of dryings 4 hours, then in Muffle furnace with 2 ℃ of/minute temperature programmings to 550 ℃ calcining 2 hours, make denitrating integral catalyst, and it weighed to determine coated weight.
Embodiment 4
Cordierite honeycomb ceramic after the roasting is weighed.With catalyst V
2O
5/ WO
3/ TiO
2After the grinding, get 2 grams and be dispersed in 4 gram water, the solution made of 6 grams, 20% silica gel, stirred 2 hours, make catalyst content and be 16.7% slurry.The carrier cordierite honeycomb ceramic is dipped in the above-mentioned slurry, slowly take out after 5 minutes, dry up raffinate with ear washing bulb, wore out 8 hours under the room temperature, 110 ℃ of dryings 4 hours, then in Muffle furnace with 2 ℃ of/minute temperature programmings to 550 ℃ calcining 2 hours, make denitrating integral catalyst, and it weighed to determine coated weight.
Embodiment 5
Cordierite honeycomb ceramic after the roasting is weighed.With catalyst V
2O
5/ WO
3/ TiO
2After the grinding, get 2 grams and be dispersed in 6 gram water, the solution made of 6 grams, 20% silica gel, stirred 2 hours, make catalyst content and be 14.3% slurry.The carrier cordierite honeycomb ceramic is dipped in the above-mentioned slurry, slowly take out after 5 minutes, dry up raffinate with ear washing bulb, wore out 8 hours under the room temperature, 110 ℃ of dryings 4 hours, then in Muffle furnace with 2 ℃ of/minute temperature programmings to 550 ℃ calcining 2 hours, make denitrating integral catalyst, and it weighed to determine coated weight.
In order to verify beneficial effect of the present invention, experimentize at laboratory simulation diesel vehicle vehicle exhaust, process is as follows: it is that 9mm, length are the fixed bed reactors of 40mm that the integral catalyzer that embodiment 1 to 5 and prior art are made is put into diameter, feed simulated automotive tail gas, concrete composition is 500ppm for NO content, NH
3Content is 533ppm, O
2Content is 10%, H
2O content is 4%, and all the other are balance gas, and the control air speed is 30000h
-1, NO
xRemoval efficiency as depicted in figs. 1 and 2.As seen, 200-460 ℃ temperature range, the present invention makes denitrating integral catalyst to NO
xRemoval efficiency more than 90%, and the removal efficiency of the catalyst that makes a little more than prior art.
In sum, slurry of the present invention is not for containing the pure green formula of any organic solvent, not only simple, environmental protection, and can reduce production costs, and also its integral catalyzer of preparing still has the higher denitration activity and the temperature window of broad, to NO
xRemoval efficiency a little more than prior art.In addition, from in appearance, the integral catalyzer coating that the present invention prepares is even, coated weight can be realized by catalyst concentration in the modulation slurries especially, therefore only need primary coating just can obtain the target coated weight, thereby shorten preparation process greatly, significantly reduce production costs, also just be more suitable for large-scale production.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change and revise above-mentioned embodiment.Therefore, the specific embodiment that discloses and describe above the present invention is not limited to also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although used some specific terms in this specification, these terms do not constitute any restriction to the present invention just for convenience of description.
Claims (10)
1. a slurry for preparing denitrating integral catalyst is characterized in that: comprise catalyst, silica gel and water.
2. slurry according to claim 1 is characterized in that: the mass percent of each composition is in the described slurry: silica gel is with SiO
2Count 5-10%, catalyst 10-50%, water 40-85%.
3. slurry according to claim 1 is characterized in that: the better quality percentage of each composition is in the described slurry: silica gel is with SiO
2Count 6-7%, catalyst 30-35%, water 58-65%.
4. slurry according to claim 1 is characterized in that: described water is deionized water, and silica gel is 20% silica gel.
5. slurry according to claim 1 is characterized in that: described catalyst is the catalytic component based on vanadium of titania supported.
6. slurry according to claim 5 is characterized in that: the content of vanadium in the described catalyst is with V
2O
5Quality is counted 0.5-10%, and contains with WO
3The tungsten auxiliary agent of quality meter 0.5-10%.
7. a method for preparing denitrating integral catalyst is characterized in that: utilize each described slurry in the claim 1 to 5, adopt the immersion process for preparing denitrating integral catalyst.
8. method according to claim 7 is characterized in that, preparation process is: after catalyst is ground, be dispersed in the aqueous solution of silica gel, solid content is determined by the final coated weight of catalyst, stirs 0.5-2 hour, makes slurry; Carrier is dipped in the slurry, slowly takes out after 5 minutes, dry up raffinate with ear washing bulb, wore out 6-10 hour under the room temperature, at 80-110 ℃ of dry 3-5 hour, then in Muffle furnace with 1-5 ℃ of/minute temperature programming to 450-600 ℃ the calcining 1-5 hour, make denitrating integral catalyst.
9. method according to claim 8 is characterized in that: described carrier is a cellular structure ceramic carrier.
10. method according to claim 9 is characterized in that: also comprise to before applying and the cellular structure ceramic carrier after applying weigh, to determine the step of coated weight.
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Cited By (5)
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CN105457627A (en) * | 2015-12-09 | 2016-04-06 | 武汉理工大学 | Manganese-based low-temperature SCR (selective catalytic reduction) denitration catalyst supported on glass fiber cloth and preparation method of catalyst |
CN105536879A (en) * | 2015-12-09 | 2016-05-04 | 武汉理工大学 | Low-temperature glue for low-temperature denitration manganese catalyst loading and preparation method of low-temperature glue |
US10071369B2 (en) * | 2014-07-07 | 2018-09-11 | Toyota Jidosha Kabushiki Kaisha | Method of making a particulate filter carry a catalyst |
CN109482226A (en) * | 2018-10-29 | 2019-03-19 | 昆明贵研催化剂有限责任公司 | One-step method prepares transition metal modified molecular sieve integral type catalyst and method |
CN116422384A (en) * | 2023-06-12 | 2023-07-14 | 中国汽车技术研究中心有限公司 | Method for coating monolithic catalyst and monolithic catalyst |
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CN101347722A (en) * | 2008-09-05 | 2009-01-21 | 江苏中科节能环保技术有限公司 | Catalyst for denitration by SCR method with low cost and preparation method thereof |
CN101371970A (en) * | 2008-09-15 | 2009-02-25 | 江苏中科节能环保技术有限公司 | Catalyst and preparation method thereof suitable for denitration of flue gas containing alkali metal oxide |
CN101676019A (en) * | 2008-09-17 | 2010-03-24 | 晶锐瓷业(北京)有限公司 | Catalyst for low-temperature denitration of power-plant flue gas by selective catalytic reduction (SCR) and preparation method thereof |
CN101912775A (en) * | 2010-09-03 | 2010-12-15 | 中国汽车技术研究中心 | Selective catalyst for removing oxynitrides from tail gases of diesel vehicles and preparation method thereof |
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2011
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Patent Citations (5)
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JP2006223959A (en) * | 2005-02-16 | 2006-08-31 | Babcock Hitachi Kk | Method of producing exhaust gas denitrification catalyst |
CN101347722A (en) * | 2008-09-05 | 2009-01-21 | 江苏中科节能环保技术有限公司 | Catalyst for denitration by SCR method with low cost and preparation method thereof |
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Cited By (8)
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---|---|---|---|---|
US10071369B2 (en) * | 2014-07-07 | 2018-09-11 | Toyota Jidosha Kabushiki Kaisha | Method of making a particulate filter carry a catalyst |
CN105457627A (en) * | 2015-12-09 | 2016-04-06 | 武汉理工大学 | Manganese-based low-temperature SCR (selective catalytic reduction) denitration catalyst supported on glass fiber cloth and preparation method of catalyst |
CN105536879A (en) * | 2015-12-09 | 2016-05-04 | 武汉理工大学 | Low-temperature glue for low-temperature denitration manganese catalyst loading and preparation method of low-temperature glue |
CN105457627B (en) * | 2015-12-09 | 2018-01-12 | 武汉理工大学 | A kind of glass fabric Supported Manganese base low temperature SCR denitration catalyst and preparation method thereof |
CN105536879B (en) * | 2015-12-09 | 2018-03-16 | 武汉理工大学 | A kind of low-temperature denitration manganese series catalyzer load low temperature glue and preparation method thereof |
CN109482226A (en) * | 2018-10-29 | 2019-03-19 | 昆明贵研催化剂有限责任公司 | One-step method prepares transition metal modified molecular sieve integral type catalyst and method |
CN116422384A (en) * | 2023-06-12 | 2023-07-14 | 中国汽车技术研究中心有限公司 | Method for coating monolithic catalyst and monolithic catalyst |
CN116422384B (en) * | 2023-06-12 | 2023-10-10 | 中国汽车技术研究中心有限公司 | Method for coating monolithic catalyst and monolithic catalyst |
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Address after: Lotus Road 511441 Guangdong city of Guangzhou province Panyu District town No. 368 block stone Patentee after: WAYGREEN TECHNOLOGIES, Inc. Address before: 510006 Guangdong city of Guangzhou province Panyu District Xiaoguwei Street Outer Ring Road No. 232 Building 5 floor B District 13 Patentee before: Waygreen Technologies, Inc. |
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