CN100364662C - Process for preparing rare-earth composite porous aluminium oxide loaded Pd catalyst - Google Patents
Process for preparing rare-earth composite porous aluminium oxide loaded Pd catalyst Download PDFInfo
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- CN100364662C CN100364662C CNB2005100605429A CN200510060542A CN100364662C CN 100364662 C CN100364662 C CN 100364662C CN B2005100605429 A CNB2005100605429 A CN B2005100605429A CN 200510060542 A CN200510060542 A CN 200510060542A CN 100364662 C CN100364662 C CN 100364662C
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Abstract
The present invention relates to a method for preparing a load Pd catalyst of rare earth composite porous aluminum oxide, which uses a cordierite ceramic honeycomb as a carrier and comprises the following steps: a sol dip coating method is adopted for coating hydrated alumina oxide; a heat adsorption method is adopted for the load compounding of the active constituents of a cerium-zirconium oxide and load metal Pd. Every liter of the catalyst comprises 0.2 to 0.8 g of Pd and 3.0 to 5.0 g of CeO2 and ZrO2. Under the condition of an airspeed of 10000 to 30000 h<-1>, the catalyst completely oxidizes toluene and ethyl acetate at respective temperatures of 180 to 200 DEG C and 260 to 280 DEG C. After being treated for 4 hours in the air at a temperature of 1000 DEG C, the complete oxidation temperatures can be only increased by 20 to 40 DEG C. The present invention has the characteristics of simple process, low production cost, and high low-temperature activation and good high-temperature resistance of the catalyst.
Description
Technical field
The present invention relates to the preparation of environmental catalysis materials chemistry, particularly a kind of CO and volatile organic contaminant (VOCs) catalyzing oxidizing degrading Preparation of catalysts method of being used for.
Background technology
Develop rapidly along with China is industrialized, the volatile organic matter of industrial discharge (VOCs) waste gas has become one of primary pollution source that influences China's urban air-quality because its amount is big, composition complexity etc. is all multifactor.The VOCs pollution problem of industrial discharge be always countries in the world one of the environmental problem paid attention to the most, and have rules of strict relevant discharging, classify 189 kinds of air organic pollutions in the industry as toxic pollutant as the U.S., and China present discharge standard of air pollutants (GB16297-1996) has stipulated the emission limit of 14 class volatile organic matters, further strict day by day along with environmental regulation has more urgent demand and market to efficient, the energy-conserving control technology of industrial discharge VOCs.
To the improvement of VOCs waste gas, adopt both at home and abroad usually absorption, absorption or condensation to reclaim, catalytic combustion or direct processing method such as burning.Yet, for some uncontrollable discharges in the production process or low concentration (hundreds of milligram～several grams/cubic meter), plurality of organic pollutants waste gas that some discharge in a organized way, if utilize processing means such as processing such as direct burning, absorption or condensation recovery,, be difficult to use because of energy consumption is big; Although utilize absorption such as active carbon can reach the purpose of purification treatment, there is very big potential safety hazard in its last handling process (particularly desorption process).At present, catalyzed conversion and absorption-catalytic integration technology has been brought into play bigger effect to the improvement of this class VOCs waste gas, and the catalyst that is adopted mainly contains three classes: 1. carried noble metal (Pd, Pt) catalyst; 2. supported transitional metal oxide catalyst; 3. rare earth metal composite oxide type catalyst (as composite oxides such as perovskite, hexa-aluminate, spinelle, monazite types).These catalyst usually with traditional micropore, low mesopore material (as gama-alumina, natural mordenite zeolite etc.) for supporting material, to organic compound such as the alkane of most low-carbon (LC)s, aromatic hydrocarbons and contain oxygen, nitrogen and sulfur derivatives and under higher temperature conditions, can both obtain catalytic oxidation and eliminate, but the organic pollution of most of industrial source dischargings, all have bigger molecular dimension as polycyclic aromatic hydrocarbon, ester class and amine etc., and concentration is low and the component complexity.Because sterically hindered, the organic pollution that the catalysis material that traditional micropore, low mesopore material support does not allow these big molecular dimensions near with absorption; Along with the supporting of active constituent, its carrier aperture can further descend in addition.Therefore the catalytic oxidation treatment to these low concentrations, plurality of organic pollutants needs higher catalytic bed temperature, and the raising greatly that this just means energy consumption and operating cost is unfavorable for applying of catalysis technique.Aluminium oxide has bigger specific surface, is the common carrier of catalyst.Because hydrated alumina can utilize the synthetic method of hydro-thermal, carry out reaming by introducing some inorganic or organic pore-forming agents, introduce metal cation such as rare earth, transition metal and carry out surface modification, the modulation alumina material is to the adsorption desorption performance of big molecule organic reactant, the decentralization of catalytic active component Pd and the heat-resistant stability of catalyst, thereby improve catalysis material to the absorption of low concentration, plurality of organic pollutants and the service life of low-temperature catalytic oxidation performance and catalyst, this means and to reduce operation energy consumption and cost.Therefore, the exploitation of this class high-performance new catalytic material will greatly improve existing problem in the present catalytic purifier, widens the scope of application of catalysis material, and the development that promotes the Environmental Protection in China cause is had epochmaking meaning.
Summary of the invention
The technology of preparing that the purpose of this invention is to provide a kind of rare-earth composite porous aluminium oxide loaded Pd catalyst.
The invention provides the method for preparing rare-earth composite porous aluminium oxide loaded Pd catalyst.With the cordierite ceramic honeycomb is carrier, the steps include: at first to adopt the colloidal sol dip coating to apply hydrated alumina, makes hydrated alumina/ceramic honeycomb carrier; On hydrated alumina/ceramic honeycomb carrier, adopt hot absorption method load cerium-zirconium mixed oxide then, make rare-earth composite porous aluminium oxide/ceramic honeycomb carrier; On rare-earth composite porous aluminium oxide/ceramic honeycomb carrier, adopt hot absorption method carried metal Pd active constituent at last, make rare-earth composite porous aluminium oxide loaded Pd catalyst.
Adopt the colloidal sol dip coating to apply hydrated alumina, earlier with quantitative hydrated alumina (Al
2O
3H
2O) powder and organic pore-forming agents are mixed with water, transfer to pH value to 1.5～2.5 with rare nitric acid, grind with high-speed grinder again and made the aluminium oxide slurries in 5～10 minutes, soak with the cordierite ceramic honeycomb carrier then and inhale these slurries, and blow away the slurries that are blocked in the duct with compressed air, leave standstill after 3～6 hours in the air atmosphere through 120 ℃ of dryings and 350 ℃ and handled 1～2 hour.
Hot absorption method load cerium-zirconium mixed oxide, earlier quantitative cerium and zirconium nitrate are dissolved in the water, the back rare nitric acid of dropping that stirs transfers to pH value to 1.5～2.5, immerse hydrated alumina/ceramic honeycomb carrier then, leave standstill after 0.5～1.0 hour and be heated to boiling, continue heating and take out carrier after 1.0～3.0 hours, in precipitating reagent, soaked 0.5 hour again, then with distilled water washing for several times to neutral, in air atmosphere, handled 0.5～2.0 hour through 120 ℃ of dryings and 450～700 ℃.
Hot absorption method carried metal Pd active constituent is immersed in rare-earth composite porous aluminium oxide/ceramic honeycomb carrier earlier and contains quantitative H
2PdCl
4The aqueous solution in, be heated to boiling back and continue heating 1.0～2.0 hours, take out carrier, be cooled to room temperature, handled 1.0～2.0 hours with the reducing agent electronation again, then with the distilled water washing for several times to there not being Cl
-In air atmosphere, handled 1.0～2.0 hours, make rare-earth composite porous aluminium oxide loaded Pd catalyst through 120 ℃ of dryings and 500 ℃.
Contain Pd 0.2～0.8 gram/every liter of catalyst in this catalyst, CeO
2+ ZrO
25.0～15.0 gram/every liter of catalyst, the coating quality of hydrated alumina are 50～150 gram/every liter of carriers.
Above-mentioned cordierite ceramic honeycomb carrier is a kind of of square 100 * 100 * 40～100mm, 50 * 50 * 40～50mm and 47 * 47 * 47mm, 200～300 sides of its number of aperture (or circle) hole/in
2, the thick 0.1 5～0.3mm of hole wall and water absorption rate 18～28%wt.
The mass ratio that contains hydration aluminium oxide, organic pore-forming agents and water in the above-mentioned aluminium oxide slurries is 1: 0～0.05: 2～4.5.
Described organic pore-forming agents is PEG (polyethylene glycol), and molecular weight is 1000～10000.
Ce: Zr=5 in above-mentioned cerium and the zirconium nitrate aqueous solution: 1～1: 5 (mol ratios), CeO
2And ZrO
2Total content be 30～15.0 gram/every liter of carriers.
Above-mentioned precipitating reagent is KOH, NaOH and NH
3H
2A kind of among the O, this aqueous solution weight percent concentration is 0.5～2.0%.
Above-mentioned H
2PdCl
4The content of Pd is 0.2～0.8 gram/every liter of carrier in the aqueous solution.
Above-mentioned reducing agent is a kind of in formaldehyde, potassium borohydride and the hydrazine hydrate, and this concentration of aqueous solution is 0.5～3%.
The technology of preparation rare-earth composite porous aluminium oxide loaded Pd catalyst provided by the present invention, its advantage is: the employing cordierite ceramic honeycomb is a carrier, and gas-flow resistance is low; Adopt the technology of hot absorption method load cerium-zirconium mixed oxide and metal Pd active constituent simple, course of reaction is controlled easily, realizes industrialized production easily; The catalyst activity height, the resistance to elevated temperatures that make are good, as at 10000～30000h
-1Complete oxidation temperature to toluene or ethyl acetate under the air speed condition is respectively 180～200 ℃ and 260～280 ℃, in 1000 ℃ of air atmospheres, handle 4h, its complete oxidation temperature only improves 20～40 ℃, and rare-earth composite porous aluminium oxide loaded Pd catalyst of the present invention will have broad application prospects aspect the VOCs waste gas pollution control and treatment of industrial source discharging.
The specific embodiment
Embodiment 1
With the cordierite ceramic honeycomb is carrier (square 100 * 100 * 40mm, 250 square hole/in
2, the thick 0.25mm of hole wall, water absorption rate 22～24%wt), the ratio Al of dip-coating aluminium oxide slurries (pH=1.5～2.0)
2O
3H
2O: PEG-1000: H
2O=1: 0.03: 3 (mass ratio), handled 1 hour through 120 ℃ of dryings and 350 ℃, obtain hydrated alumina/ceramic honeycomb carrier that the hydrated alumina load capacity is 120 gram/every liter of carriers.Get an above-mentioned carrier, be immersed in and contain Ce: Zr is 3: 1 (mol ratio), CeO
2And ZrO
2Total content be 6 the gram ceriums and zirconium nitrate aqueous solution (pH=2.0) in, leave standstill after 0.5 hour and be heated to boiling, continue heating and take out carrier after 2.0 hours, in containing the aqueous solution of 1%KOH, soaked 0.5 hour again, then with distilled water washing for several times to neutral, in air atmosphere, handled 2.0 hours through 120 ℃ of dryings and 500 ℃.This carrier is immersed in the H that contains 0.15 gram Pd then
2PdCl
4In the aqueous solution, be heated to the back continuation heating 1.0 hours of seething with excitement, take out carrier, be cooled to room temperature, be immersed in again to reduce in the aqueous solution that contains 1% hydrazine hydrate and handled 1.0 hours, wash for several times to there not being Cl with distilled water then
-In air atmosphere, handled 2.0 hours, make rare-earth composite porous aluminium oxide loaded Pd catalyst through 120 ℃ of dryings and 500 ℃.Contain 0.15g Pd in the catalyst, 6.0g CeO
2+ ZrO
2This catalyst is at 10000～30000h
-1Air speed, 3～5g/m
3Under the condition of organic concentration, the complete oxidation temperature of toluene or ethyl acetate is respectively 180 ℃ and 260 ℃, handles 4h in 1000 ℃ of air atmospheres, its complete oxidation temperature is respectively 200 ℃ (toluene) and 280 ℃ (ethyl acetate).
Embodiment 2
With embodiment 1 identical operations, difference is: with the CeO in cerium and the zirconium nitrate aqueous solution
2And ZrO
2Total content changes 3.0 grams into; Contain 0.15g Pd in the resulting catalyst, 3.0g CeO
2+ ZrO
2Organic pore-forming agents is PEG-10000, and the mass ratio of hydrated alumina, organic pore-forming agents and water is 1: 0.05: 4.5; The precipitating reagent weight percent concentration is 2% NH
3H
2O; The reducing agent concentration that is weight percentage is 0.5% potassium borohydride.At 10000～30000h
-1Air speed, 3～5g/m
3Under the condition of organic concentration, this catalyst is respectively 180 ℃ and 280 ℃ to the complete oxidation temperature of toluene or ethyl acetate, handles 4h in 1000 ℃ of air atmospheres, and its complete oxidation temperature is respectively 220 ℃ (toluene) and 320 ℃ (ethyl acetate).
Embodiment 3
With embodiment 1 identical operations, difference is: with H
2PdCl
4Pd content in the aqueous solution changes 0.2 gram into; Contain 0.2gPd in the resulting catalyst, 6.0g CeO
2+ ZrO
2The precipitating reagent weight percent concentration is 0.5% NaOH; The reducing agent concentration that is weight percentage is 1.5% formaldehyde.At 10000～30000h
-1Air speed, 3～5g/m
3Under the condition of organic concentration, this catalyst is respectively 180 ℃ and 260 ℃ to the complete oxidation temperature of toluene or ethyl acetate, handles 4h in 1000 ℃ of air atmospheres, and its complete oxidation temperature is respectively 200 ℃ (toluene) and 260 ℃ (ethyl acetate).
Embodiment 4
With embodiment 1 identical operations, difference is: the size of cordierite ceramic honeycomb carrier is changed into: square 47 * 47 * 47mm (250 circumference hole/in
2, the thick 0.2～0.3mm of hole wall, water absorption rate 22～24%wt).Contain 0.15gPd in the resulting catalyst agent, 6.0g CeO
2+ ZrO
2At 10000～30000h
-1Air speed, 3～5g/m
3Under the condition of organic concentration, this catalyst is respectively 200 ℃ and 280 ℃ to the complete oxidation temperature of toluene or ethyl acetate, handles 4h in 1000 ℃ of air atmospheres, and its complete oxidation temperature is respectively 220 ℃ (toluene) and 310 ℃ (ethyl acetate).
Claims (7)
1. the preparation method of a rare-earth composite porous aluminium oxide loaded Pd catalyst is a carrier with the cordierite ceramic honeycomb, the steps include: at first to adopt the colloidal sol dip coating to apply hydrated alumina, makes hydrated alumina/ceramic honeycomb carrier; On hydrated alumina/ceramic honeycomb carrier, adopt hot absorption method load cerium-zirconium mixed oxide then, make rare-earth composite porous aluminium oxide/ceramic honeycomb carrier; On rare-earth composite porous aluminium oxide/ceramic honeycomb carrier, adopt hot absorption method carried metal Pd active constituent at last, make rare-earth composite porous aluminium oxide loaded Pd catalyst, it is characterized in that:
Described coating hydrated alumina method is: earlier quantitative alumina hydrate powder and organic pore-forming agents are mixed with water, transfer to pH value to 1.5～2.5 with rare nitric acid, grind with high-speed grinder again and made the aluminium oxide slurries in 5～10 minutes, soak with the cordierite ceramic honeycomb carrier then and inhale these slurries, and blow away the slurries that are blocked in the duct with compressed air, leave standstill after 3～6 hours in the air atmosphere through 120 ℃ of dryings and 350 ℃ and handled 1～2 hour, make hydrated alumina/ceramic honeycomb carrier, the coated weight of hydrated alumina is: 50～150 gram/every liter of carriers;
The compound cerium of described load-Zirconium oxide method is: the nitrate with quantitative cerium and zirconium is dissolved in the water earlier, the back rare nitric acid of dropping that stirs transfers to pH value to 1.5～2.5, immerse hydrated alumina/ceramic honeycomb carrier then, leave standstill after 0.5～1.0 hour and be heated to boiling, continue heating and take out carrier after 1.0～3.0 hours, in precipitating reagent, soaked 0.5 hour again, extremely neutral for several times with the distilled water washing then, in air atmosphere, handled 0.5～2.0 hour through 120 ℃ of dryings and 450～700 ℃, make rare-earth composite porous aluminium oxide/ceramic honeycomb carrier, CeO
2And ZrO
2Content be 5.0～15.0 gram/every liter of catalyst;
Described carried metal Pd active constituent method is: rare-earth composite porous aluminium oxide/ceramic honeycomb carrier is immersed in contains quantitative H earlier
2PdCl
4The aqueous solution in, be heated to boiling back and continue heating 1.0～2.0 hours, take out carrier, be cooled to room temperature, handled 1.0～2.0 hours with the reducing agent electronation again, then with the distilled water washing for several times to there not being Cl
-, in air atmosphere, handled 1.0～2.0 hours through 120 ℃ of dryings and 500 ℃, make rare-earth composite porous aluminium oxide loaded Pd catalyst, the content of Pd is 0.2～0.8 gram/every liter of catalyst.
2. the preparation method of rare-earth composite porous aluminium oxide loaded Pd catalyst according to claim 1, it is characterized in that described cordierite ceramic honeycomb carrier dimensions: square 100mm * 100mm * 40～100mm, 50mm * 50mm * 40～50mm or 47mm * 47mm * 47mm, 200～300 hole/in of number of aperture
2, the thick 0.15～0.3mm of hole wall, water absorption rate 18～28%wt.
3. the preparation method of rare-earth composite porous aluminium oxide loaded Pd catalyst according to claim 1, the mass ratio that it is characterized in that described hydrated alumina, organic pore-forming agents and water is 1: 0.03: 3 or 1: 0.05: 4.5.
4. the preparation method of rare-earth composite porous aluminium oxide loaded Pd catalyst according to claim 1 is characterized in that described organic pore-forming agents is a polyethylene glycol, and molecular weight is 1000～10000.
5. the preparation method of rare-earth composite porous aluminium oxide loaded Pd catalyst according to claim 1, it is characterized in that cerium in the nitrate aqueous solution of described cerium and zirconium: the zirconium mol ratio is: Ce: Zr=5: 1～1: 5.
6. the preparation method of rare-earth composite porous aluminium oxide loaded Pd catalyst according to claim 1 is characterized in that described precipitating reagent be weight percentage KOH, NaOH and the NH of concentration 0.5～2.0%
3H
2The aqueous solution of O a kind of.
7. the preparation method of rare-earth composite porous aluminium oxide loaded Pd catalyst according to claim 1 is characterized in that: the be weight percentage aqueous solution a kind of of formaldehyde, potassium borohydride and hydrazine hydrate of concentration 0.5～3% of described reducing agent.
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| CN101734946B (en) * | 2009-12-18 | 2012-05-23 | 广东工业大学 | Method for applying coating on cordierite honeycomb ceramics and applications thereof |
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| CN109046345B (en) * | 2018-08-01 | 2021-04-30 | 中国科学院城市环境研究所 | Supported catalyst and preparation method and application thereof |
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Assignee: Hangzhou Kaiming Catalysts Co., Ltd. Assignor: Zhejiang University Contract fulfillment period: 2008.10.6 to 2013.10.5 contract change Contract record no.: 2008330001153 Denomination of invention: Process for preparing rare-earth composite porous aluminium oxide loaded Pd catalyst Granted publication date: 20080130 License type: Exclusive license Record date: 20081017 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.10.6 TO 2013.10.5; CHANGE OF CONTRACT Name of requester: HANGZHOU KAIMING CATALYST CO., LTD. Effective date: 20081017 |
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