CN101007274A - Preparation method of rare earth composite oxides coating Pt-supported catalyst - Google Patents
Preparation method of rare earth composite oxides coating Pt-supported catalyst Download PDFInfo
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- CN101007274A CN101007274A CN 200610049232 CN200610049232A CN101007274A CN 101007274 A CN101007274 A CN 101007274A CN 200610049232 CN200610049232 CN 200610049232 CN 200610049232 A CN200610049232 A CN 200610049232A CN 101007274 A CN101007274 A CN 101007274A
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Abstract
The invention involves environmental protect technology field, particularly a rare earth compound oxide covering load Pd catalyst preparation method used for organic waste gas treatment. The invention aims at: because the covering of the existing honeycomb ceramics carrier catalyst is easy to reacting with carrier or adjuvant and generating spinel compounds and the covering is easy to drop, the method provides a preparation method which preparation art is simple, does not generate harmful substances in the preparation process, covering has strong adsorption capacity to Pd and is combine with honeycomb ceramics carrier firmly. The preparation method is: adding organic acid or ethandiol or mixture of said both into certain amount of the third and fourth subgroup metal oxide or hydroxide and mixing uniformly and preparing the covering liquid, immersing the honeycomb ceramics carrier into covering liquid and getting it out, then airing, drying and roasting it to preparing the carrier with covering; then immersing the carrier with covering into prepared H2PdCl4 solution, preparing the accelerant after drying and roasting.
Description
Technical field
The present invention relates to environmental protection technical field, the preparation method of a kind of rare earth composite oxides coating Pt-supported catalyst of handling especially for organic exhaust gas.
Background technology
In the organic waste-gas purification processing method, catalytic combustion technology more and more comes into one's own as a kind of easy, practical organic waste-gas purification technology.And the core of catalytic combustion technology is a catalyst, and therefore, the catalyst of exploitation function admirable becomes the key of this technical development.
Existing catalyst adopts the honeycomb type structure mostly, promptly is matrix with the cordierite honeycomb ceramic, and applying coating is as carrier thereon, and then load active component.Its floating coat is the key component of catalyst, if carrier and Bond Strength of Coating are low, coating chaps, comes off, and will directly influence catalytic activity.Because Al
2O
3Higher specific surface can be provided, easy other metal oxide of load and noble metal, existing catalyst generally adopts Al
2O
3Coating is second carrier.But, Al
2O
3Poor heat stability influences the catalytic performance of catalyst, stablizes Al so generally add other auxiliary agents
2O
3Coating is as ZrO
2, MgO, La
2O
3, CeO
2Deng.In the CN1132682C disclosed method, coating is by Al
2O
3, TiO
2, CeO
2And ZrO
2Form; The CN1488435A coating is by Al
2O
3, SiO
2Form with alkaline-earth metal, all improved the resistance to elevated temperatures of catalyst.But, the oxides additive powder and the Al of interpolation
2O
3The adhesive strength of thin layer is not high, comes off easily, and solid phase reaction generation spinels takes place down catalyst preparation process complexity, and high temperature simultaneously easily is AB
2O
4Compound reduces catalytic performance.
Summary of the invention
The objective of the invention is at above-mentioned traditional Al
2O
3The coating poor heat stability, easily with carrier or auxiliary agent reaction generation catalytic removal of nox, Al
2O
3The caducous weak point of coating, provide a kind of on honeycomb ceramic carrier the direct composite oxides coating Pt-supported Preparation of catalysts method of supported rare earth.Catalyst preparation process of the present invention is simple, and its maximum characteristics are not generate harmful waste gas and waste liquid in preparation process, and have coating to the high adsorption capacity of Pd, combine firmly with honeycomb ceramic carrier, advantage such as catalytic performance is good.
Catalyst for catalytic combustion of the present invention is a kind of honeycomb ceramic type catalyst, there is a coating on the ceramic honey comb surface, coating comprises in the periodic table of elements the 3rd, in the fourth officer family metal oxide one or both, wherein the mass percent of rare earth composite oxides coating is 3%～5% of a honeycomb ceramic carrier, the ratio of the amount of substance of two kinds of metal oxides with metal count 8: 2～2: 8, catalyst is an active component with the Pd that loads on the coating, and its loading is that every liter of catalyst contains 0.1～0.5gPd.
Rare earth composite oxides coating of the present invention and Preparation of catalysts method are:
(1) preparation of rare earth composite oxides coating
A. in a certain amount of the 3rd, fourth officer family metal oxide or hydroxide, add organic acid or ethylene glycol or the mixture of the two and mix, add an amount of water, stir, make coating liquid.Wherein, used organic acid or ethylene glycol or the total amount of substance of the mixture of the two are 0.5～3 times of the total amount of substance of metal ion in the composite oxides;
B. take out after honeycomb ceramic carrier being immersed coating liquid, remove the coating liquid that residues in the honeycomb ceramic carrier duct;
C. the b ceramic honey comb is placed and dried in 0.5～24 hour, again in 80～120 ℃ of dryings 0.5～12 hour;
D. with the c ceramic honey comb 400～600 ℃ of roastings 2～5 hours, promptly make the honeycomb ceramic carrier that contains coating.
(2) load of noble metal active component Pd
Prepare certain density H
2PdCl
4Solution is as the maceration extract that supports the noble metal active component.By absorption method the noble metal active component is loaded to carrier surface, take out, remove the aqueous solution that residues in the honeycomb ceramic carrier duct, 80～120 ℃ of dryings 0.5～12 hour, 400～700 ℃ of roastings are 1～5 hour in the final high temperature stove, finally make catalyst of the present invention.
Compared with the prior art, Preparation of Catalyst environmental protection of the present invention, technology is simple, catalytic performance is good, coating is firm and to noble metal active component high adsorption capacity, characteristics that effective rate of utilization is high.
Description of drawings
Fig. 1 is that coating in the embodiment of the invention 4,5,7 is to the evaluation test figure of Pd adsorption capacity.
The specific embodiment
Below in conjunction with embodiment the present invention is made further and to specify, but the present invention is not limited to these embodiment.
The preparation of coating: take by weighing homemade 1.08g Ce (OH)
3, 0.32g Y
2O
3With the 1.78g citric acid, mix the back and add the proper amount of deionized water dissolving, get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is after the cordierite honeycomb ceramic of 25.81g immerses coating liquid, to take out, and blows out residual solution in the honeycomb channel, and cordierite honeycomb ceramic is dried in the air to dry tack free in room temperature, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 4 hours in Muffle furnace then promptly make Ce
0.8Y
0.2O
1.9Coating.
The load of Pd: compound concentration is the H of 8.9gPd/L solution
2PdCl
4Aqueous solution 100mL is as noble metal active component maceration extract.Measure 1.5mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution water bath with thermostatic control absorption after 1.5 hours applying cated honeycomb ceramic carrier again, take out, blow away residual solution in the hole, 120 ℃ of dryings 1 hour in air then, 500 ℃ of roastings are 4 hours in the air, promptly make Pd/Ce
0.8Y
0.2O
1.9Catalyst for catalytic combustion.
The performance evaluation of catalyst: the catalyst that this example is prepared is made cylindrical, fill in the fixed-bed catalytic combustion reactor, under different temperatures, with the catalytic combustion of toluene as probe reaction, carry out the evaluation of organic waste-gas purification catalytic combustion properties, ceramic honeycomb catalyst filling specification is diameter 20mm, long 80mm, by the air carrying band toluene reactor of flowing through, the aerial content 3～5gm of toluene
-3, air speed 15000h
-1Catalyst activity is T with toluene conversion greater than 95% minimum response temperature
95Represent the T of this catalyst
95It is 230 ℃.
Embodiment 2
The preparation of coating: take by weighing 1.30g Ce (OH)
4, 0.36g Y
2O
3With the 1.97g citric acid, mix the back and add proper amount of deionized water, stir, get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is after the cordierite honeycomb ceramic of 28.66g immerses coating liquid, to take out, and blows out residual solution in the honeycomb channel, and cordierite honeycomb ceramic is dried in the air to dry tack free in room temperature, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 4 hours in Muffle furnace then promptly make Ce
0.8Y
0.2O
1.9Coating.
The load of Pd: measure 1.6mL H by the method for implementing 1
2PdCl
4The aqueous solution, absorption, dry, roasting promptly make Pd/Ce
0.8Y
0.2O
1.9Catalyst.
The performance evaluation of catalyst: by the method for implementing 1, the T of this catalyst
95It is 250 ℃
Embodiment 3
The preparation of coating: take by weighing 1.47g La (OH)
3, 0.17g CeO
2With the 1.83g citric acid, mix the back and add the proper amount of deionized water dissolving, get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is after the cordierite honeycomb ceramic of 28.54g immerses coating liquid, to take out, and blows out residual solution in the honeycomb channel, and cordierite honeycomb ceramic is dried in the air to dry tack free in room temperature, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 4 hours in Muffle furnace then promptly make Ce
0.2La
0.8O
1.6Coating.
The load of Pd: measure 1.6mL H by the method for implementing 1
2PdCl
4The aqueous solution, absorption, dry, roasting promptly make Pd/Ce
0.2La
0.8O
1.6Catalyst.
The performance evaluation of catalyst: by the method for implementing 1, the T of this catalyst
95It is 280 ℃.
Embodiment 4
The preparation of coating: take by weighing 1.10g La (OH)
3, 0.50g CeO
2With 0.78g acetic acid, mix the back and add the proper amount of deionized water dissolving, get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is after the cordierite honeycomb ceramic of 28.74g immerses coating liquid, to take out, and blows out residual solution in the honeycomb channel, and cordierite honeycomb ceramic is dried in the air to dry tack free in room temperature, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 4 hours in Muffle furnace then promptly make Ce
0.5La
0.5O
1.75Coating.
The load of Pd: measure 1.6mL H by the method for implementing 1
2PdCl
4The aqueous solution, absorption, in dry, roasting, promptly make Pd/Ce
0.5La
0.5O
1.75Catalyst.
The performance evaluation of catalyst: by the method for implementing 1, the T of this catalyst
95It is 260 ℃.
The preparation of coating: take by weighing 0.67g La (OH)
3, 0.31g CeO
2With 0.47g acetic acid, mix the back and add the proper amount of deionized water dissolving, get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is after the cordierite honeycomb ceramic of 29.01g immerses coating liquid, to take out, and blows out residual solution in the honeycomb channel, and cordierite honeycomb ceramic is dried in the air to dry tack free in room temperature, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 4 hours in Muffle furnace then promptly make Ce
0.5La
0.5O
1.75Coating.
The load of Pd: measure 1.6mL H by the method for implementing 1
2PdCl
4The aqueous solution, absorption, dry, roasting promptly make Pd/Ce
0.5La
0.5O
1.75Catalyst.
The performance evaluation of catalyst: by the method for implementing 1, the T of this catalyst
95It is 260 ℃.
Embodiment 6
The preparation of coating: take by weighing 0.97g Y (OH)
3, 0.15g CeO
2With the 1.64g citric acid, mix the back and add the proper amount of deionized water dissolving, get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is after the cordierite honeycomb ceramic of 31.17g immerses coating liquid, to take out, and blows out residual solution in the honeycomb channel, and cordierite honeycomb ceramic is dried in the air to dry tack free in room temperature, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 4 hours in Muffle furnace then promptly make Ce
0.2Y
0.8O
1.6Coating.
The load of Pd: measure 1.8mL H by the method for implementing 1
2PdCl
4The aqueous solution, absorption, dry, roasting promptly make Pd/Ce
0.2Y
0.8O
1.6Catalyst.
The performance evaluation of catalyst: by the method for implementing 1, the T of this catalyst
95It is 210 ℃.
The preparation of coating: take by weighing 0.68g Y (OH)
3, 0.42g CeO
2With the 1.54g citric acid, mix the back and add the proper amount of deionized water dissolving, get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is after the cordierite honeycomb ceramic of 32.44g immerses coating liquid, to take out, and blows out residual solution in the honeycomb channel, and cordierite honeycomb ceramic is dried in the air to dry tack free in room temperature, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 4 hours in Muffle furnace then promptly make Ce
0.5Y
0.5O
1.75Coating.
The load of Pd: measure 1.8mL H by the method for implementing 1
2PdCl
4The aqueous solution, absorption, dry, roasting promptly make Pd/Ce
0.5Y
0.5O
1.75Catalyst.
The performance evaluation of catalyst: by the method for implementing 1, the T of this catalyst
95It is 220 ℃.
Embodiment 8
The preparation of coating: take by weighing 0.61g Y (OH)
3, 0.38g CeO
2With the 1.38g citric acid, mix the back and add the proper amount of deionized water dissolving, get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is after the cordierite honeycomb ceramic of 28.97g immerses coating liquid, to take out, and blows out residual solution in the honeycomb channel, and cordierite honeycomb ceramic is dried in the air to dry tack free in room temperature, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 4 hours in Muffle furnace then promptly make Ce
0.5Y
0.5O
1.75Coating.
The load of Pd: measure 1.6mL H by the method for implementing 1
2PdCl
4The aqueous solution, absorption, dry, roasting promptly make Pd/Ce
0.5Y
0.5O
1.75Catalyst, wherein sintering temperature adopts 700 ℃.
The performance evaluation of catalyst: by the method for implementing 1, the T of this catalyst
95It is 260 ℃.
Embodiment 9
The preparation of coating: take by weighing 0.30g Zr (OH)
4, 1.29g CeO
2, 0.32g ethylene glycol mixes the back and adds the proper amount of deionized water dissolving, coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is after the cordierite honeycomb ceramic of 30.20g immerses coating liquid, to take out, and blows out residual solution in the honeycomb channel, and cordierite honeycomb ceramic is dried in the air to dry tack free in room temperature, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 4 hours in Muffle furnace then promptly make Zr
0.2Ce
0.8O
2Coating.
The load of Pd: measure 1.7mL H by the method for implementing 1
2PdCl
4The aqueous solution, absorption, dry, roasting promptly make Pd/Zr
0.2Ce
0.8O
2Catalyst.
The performance evaluation of catalyst: by the method for implementing 1, the T of this catalyst
95It is 280 ℃.
Claims (7)
1, a kind of rare earth composite oxides coating Pt-supported catalyst, it comprises honeycomb support, coating and precious metals pd, it is characterized in that described coating is by one or both complex rare-earth oxidate containing valuable metals formed in the periodic table of elements the 3rd, in the fourth officer family metal oxide, its mass percent is 3%～5% of a honeycomb ceramic carrier, in the composite oxide coating ratio of the amount of substance of two kinds of metal oxides with metal count 8: 2～2: 8, the loading of active metal component Pd is that every liter of catalyst contains 0.1～0.5g Pd.
2, a kind of rare earth composite oxides coating Pt-supported catalyst according to claim 1 is characterized in that described the 3rd, fourth officer family metal oxide is CeO
2, La
2O
3, ZrO
2, Y
2O
3And Sm
2O
3
3, a kind of rare earth composite oxides coating Pt-supported catalyst according to claim 1 and 2 is characterized in that described cellular structure ceramic carrier is a cordierite-quality honeycombed ceramics.
4, a kind of preparation method of rare earth composite oxides coating Pt-supported catalyst, the preparation method who it is characterized in that rare earth composite oxides coating Pt-supported catalyst is: mix with adding organic acid or ethylene glycol or the mixture of the two in a certain amount of the 3rd, fourth officer family metal oxide or the hydroxide, add an amount of water, stir, make coating liquid, take out after honeycomb ceramic carrier immersed coating liquid, remove the coating liquid that residues in the honeycomb ceramic carrier duct, then it is dried, dry, roasting makes the honeycomb ceramic carrier that contains coating; Preparation H
2PdCl
4Solution is at the H that is prepared
2PdCl
4Dipping contains the honeycomb ceramic carrier of coating in the solution, and dry then, roasting makes catalyst.
5, the preparation method of a kind of rare earth composite oxides coating Pt-supported catalyst according to claim 4 is characterized in that organic acid is one or more in citric acid, malic acid, the acetic acid.
6, the preparation method of a kind of rare earth composite oxides coating Pt-supported catalyst according to claim 4 is characterized in that used organic acid or ethylene glycol or the total amount of substance of the mixture of the two are 0.5～3 times of the total amount of substance of metal ion in the composite oxides.
7, the preparation method of a kind of rare earth composite oxides coating Pt-supported catalyst according to claim 4 is characterized in that the preparation process of rare earth composite oxides coating Pt-supported catalyst is as follows:
(1) preparation of applying coating liquid
In a certain amount of the 3rd, fourth officer family metal oxide or hydroxide, add organic acid or ethylene glycol or the mixture of the two and mix, add an amount of water, stir, make coating liquid;
(2) coating of honeycomb ceramic carrier coating
A. take out after honeycomb ceramic carrier being immersed coating liquid, remove the coating liquid that residues in the honeycomb ceramic carrier duct;
B. a ceramic honey comb is placed and dried in 0.5～24 hour, again in 80～120 ℃ of dryings 0.5～24 hour;
C. with the b ceramic honey comb 400～600 ℃ of roastings 1～6 hour;
(3) load of active metal component
Compound concentration is the H of 8.5～9.0g Pd/L
2PdCl
4Solution is as the maceration extract that supports the noble metal active component, then the noble metal active component is loaded to carrier surface, take out, remove the solution that residues in the honeycomb ceramic carrier duct, 80～120 ℃ of dryings 0.5～24 hour, 400～700 ℃ of roastings are 1～6 hour in the final high temperature stove, promptly make catalyst of the present invention.
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