CN100391599C - Carried by CeO2 based composite oxides coated carrier Pd catalyst, its prepn. method - Google Patents
Carried by CeO2 based composite oxides coated carrier Pd catalyst, its prepn. method Download PDFInfo
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- CN100391599C CN100391599C CNB2005100602651A CN200510060265A CN100391599C CN 100391599 C CN100391599 C CN 100391599C CN B2005100602651 A CNB2005100602651 A CN B2005100602651A CN 200510060265 A CN200510060265 A CN 200510060265A CN 100391599 C CN100391599 C CN 100391599C
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Abstract
A catalyst for catalytic combustion features that a coated composite oxide layer based on CeO2 is carried by cellular ceramic carrier. It contains the cellular cordierite ceramic matrix, coated composite oxide layer based on CeO2, and Pd. Its preparing process is also disclosed.
Description
Technical field
The present invention relates to a kind of CeO
2Based composite oxides coated Pt-supported catalyst and preparation method thereof, particularly a kind of organic waste gas catalytic combustion cleaning catalyst and manufacture method thereof of being used for.
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.Catalytic combustion is as the effective technology of cleaning organic waste gas, and its core is a catalyst for catalytic combustion.Therefore, the catalyst for catalytic combustion of exploitation function admirable becomes the key of this technical development.
Existing catalyst for catalytic combustion 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.If carrier and Bond Strength of Coating are low, coating chaps, comes off, and will directly influence catalytic activity.Existing catalyst generally adopts Al
2O
3Coating is second carrier, because Al
2O
3Higher specific surface can be provided, can other metal oxide of load and noble metal.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.For example, in the open method by Chinese patent literature patent No. 01133374.X, coating is by Al
2O
3, TiO
2, CeO
2And ZrO
2Form; In the open method by Chinese patent literature number of patent application 02133123.5, 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 catalyst preparation process complexity, and high temperature simultaneously solid phase reaction takes place down easily generates spinels (AB
2O
4) compound, reduce catalytic performance.
Summary of the invention
The objective of the invention is at existing Al
2O
3The coating poor heat stability, easily with carrier or auxiliary agent reaction generation catalytic removal of nox, Al
2O
3Defectives such as coating easily comes off are utilized CeO
2Storage oxygen performance and high temperature sintering resistant that base composite oxidate is high, provide a kind of on honeycomb ceramic carrier load C eO
2Based composite oxides coated Catalysts and its preparation method, catalyst of the present invention has coating and combines firmly with the honeycomb ceramic carrier skeleton, use floating coat difficult drop-off, and advantage such as noble metal effective rate of utilization height, catalytic performance and resistance to elevated temperatures be good.
Catalyst for catalytic combustion of the present invention is a kind of honeycomb ceramic type catalyst for catalytic combustion, and there is a coating on the ceramic honey comb surface, and coating comprises CeO
2, in the 3rd subgroup metal oxide one or more, wherein CeO
2Based composite oxides coated mass percent is 5%～30% of a honeycomb ceramic carrier, CeO in the mixed oxide coatings
2With the ratio (in metal) of the amount of substance of the 3rd subgroup metal oxide be 9: 1～1: 9, the 3rd subgroup metal oxide adopts La
2O
3, Sm
2O
3And Y
2O
3In one or more mixture; Catalyst is an active component with the Pd that loads on the coating, and its loading is that every liter of catalyst contains 0.1～2.0gPd.
The preparation method of catalyst for catalytic combustion of the present invention is:
(1) preparation of coating liquid and being coated with is carried
1. in a certain amount of the 3rd subgroup metal oxide, add HNO
3, with Ce (NO
3)
3With organic acid or ethylene glycol or the mixture of the two mixing, add an amount of water, stir, get coating liquid.Wherein, used organic acid or ethylene glycol or the total amount of substance of the mixture of the two are CeO
2In the composite oxide coating 0.2～4 of the total amount of substance of metal ion times;
2. take out after honeycomb ceramic carrier being immersed coating liquid, remove the coating liquid that residues in the honeycomb ceramic carrier duct;
3. the ceramic honey comb in will be is 2. placed and was dried in 0.5～24 hour, again in 80～120 ℃ of dryings 0.5～12 hour;
4. the ceramic honey comb in inciting somebody to action 3. was 400～1000 ℃ of roastings 0.5～2 hour;
5. repeat 2.～4. step 2～four time, to the absorption of coating liquid dipping fully, 400～1000 ℃ of roastings 1～5 hour, promptly make the honeycomb ceramic carrier that contains coating at last.
(2) active metal component dipping, by an amount of noble metal component Pd of infusion process load, then in 80～120 ℃ of dryings 0.5～12 hour, 400～1000 ℃ of roastings 1～5 hour finally make catalyst finished product of the present invention.
The CeO of the present invention's preparation
2Based composite oxides coated Pt-supported catalyst has coating and combines firmly the characteristics of difficult drop-off in the use with the honeycomb ceramic carrier surface.Catalyst of the present invention has high catalytic activity, heat endurance and anti-sintering, anti-poisoning performance simultaneously, adopts infusion process to support the noble metal active component, noble metal active component strong adhesion, decentralization height, effective rate of utilization advantages of higher.
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.
Embodiment 1
Take by weighing 10.67g Ce (NO
3)
36H
2O and 7.98g 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 taken out for after the 31.41g cordierite honeycomb ceramic immerses coating liquid, blow out residual solution in the honeycomb channel, this moment, coating liquid also had the part residue, and cordierite honeycomb ceramic ℃ is dried in the air to dry tack free in room temperature to 50, again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 1 hour in Muffle furnace then.Repeat said process 2～3 times, to the absorption of coating liquid dipping fully, 500 ℃ of roastings 4 hours in Muffle furnace at last promptly make CeO
2Coating.
Compound concentration is the H of 8.9g Pd (1g/L)/L solution
2PdCl
4Aqueous solution 100mL is as noble metal active component maceration extract.Measure 5.6mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution after the water bath with thermostatic control vibration 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 (1g/L)/CeO
2Catalyst for catalytic combustion.
Embodiment 2
Take by weighing 0.57g Y
2O
3Add HNO
3, with 9.16g Ce (NO
3)
36H
2O and 5.35g citric acid mix and add proper amount of deionized water, stir, and get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is taken out for after the 31.40g cordierite honeycomb ceramic immerses coating liquid, blows out residual solution in the honeycomb channel, cordierite honeycomb ceramic ℃ is dried in the air to dry tack free in room temperature to 50, and again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 1 hour in Muffle furnace then.Repeat said process 2～3 times, to the absorption of coating liquid dipping fully, 500 ℃ of roastings 4 hours in Muffle furnace at last promptly make Ce
0.8Y
0.2O
1.9Coating.
Measure 5.6mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution after the water bath with thermostatic control vibration 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 (1g/L)/Ce
0.8Y
0.2O
1.9Catalyst.
Embodiment 3
Take by weighing 0.98g Sm
2O
3Add HNO
3, with 9.73g Ce (NO
3)
36H
2O and 4.93g citric acid mix and add proper amount of deionized water, stir, and get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is taken out for after the 31.23g cordierite honeycomb ceramic immerses coating liquid, blows out residual solution in the honeycomb channel, cordierite honeycomb ceramic ℃ is dried in the air to dry tack free in room temperature to 50, and again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 1 hour in Muffle furnace then.Repeat said process 2～3 times, to the absorption of coating liquid dipping fully, Ce is promptly made in 500 ℃ of roastings 4 hours in Muffle furnace at last
0.8Sm
0.2O
1.9Coating.
Measure 5.6mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution after the water bath with thermostatic control vibration 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 (1g/L)/Ce
0.8Sm
0.2O
1.9Catalyst.
Embodiment 4
Take by weighing 0.91g La
2O
3Add HNO
3, with 9.73g Ce (NO
3)
36H
2O and 5.88g citric acid mix and add proper amount of deionized water, stir, and get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is taken out for after the 33.46g cordierite honeycomb ceramic immerses coating liquid, blows out residual solution in the honeycomb channel, cordierite honeycomb ceramic ℃ is dried in the air to dry tack free in room temperature to 50, and again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 1 hour in Muffle furnace then.Repeat said process 2～3 times, to the absorption of coating liquid dipping fully, 500 ℃ of roastings 4 hours in Muffle furnace at last promptly make Ce
0.8La
0.2O
1.9Catalyst coat.
Measure 5.6mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution after the water bath with thermostatic control vibration 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 (1g/L)/Ce
0.8La
0.2O
1.9Catalyst.
Embodiment 5
Take by weighing 0.89g La
2O
3Add HNO
3, with 9.44g Ce (NO
3)
36H
2O and 1.69g ethylene glycol mix and add proper amount of deionized water, stir, and get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is taken out for after the 32.58g cordierite honeycomb ceramic immerses coating liquid, blows out residual solution in the honeycomb channel, cordierite honeycomb ceramic ℃ is dried in the air to dry tack free in room temperature to 50, and again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 1 hour in Muffle furnace then.Repeat said process 2～3 times, to the absorption of coating liquid dipping fully, 500 ℃ of roastings 4 hours in Muffle furnace at last promptly make Ce
0.8La
0.2O
1.9Coating.
Measure 5.6mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution after the water bath with thermostatic control vibration 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 (1g/L)/Ce
0.8La
0.2O
1.9Catalyst.
Embodiment 6
Take by weighing 0.83g La
2O
3Add HNO
3, with 9.17g Ce (NO
3)
36H
2O and 5.36g citric acid mix and add proper amount of deionized water, stir, and get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is taken out for after the 32.56g cordierite honeycomb ceramic immerses coating liquid, blows out residual solution in the honeycomb channel, cordierite honeycomb ceramic ℃ is dried in the air to dry tack free in room temperature to 50, and again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 1 hour in Muffle furnace then.Repeat said process 2～3 times, to the absorption of coating liquid dipping fully, 500 ℃ of roastings 4 hours in Muffle furnace at last promptly make Ce
0.8La
0.2O
1.9Coating.
Measure 5.6mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution after the water bath with thermostatic control vibration applying cated honeycomb ceramic carrier again, take out, blow away residual solution in the hole, 120 ℃ of dryings 1 hour in air then, 900 ℃ of roastings are 4 hours in the air, promptly make Pd (1g/L)/Ce
0.8La
0.2O
1.9Catalyst.
Embodiment 7
Take by weighing 0.83g La
2O
3Add HNO
3, with 9.16g Ce (NO
3)
36H
2O and 5.35g citric acid mix and add proper amount of deionized water, stir, and get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is taken out for after the 31.46g cordierite honeycomb ceramic immerses coating liquid, blows out residual solution in the honeycomb channel, cordierite honeycomb ceramic ℃ is dried in the air to dry tack free in room temperature to 50, and again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 1 hour in Muffle furnace then.Repeat said process 2～3 times, to the absorption of coating liquid dipping fully, 500 ℃ of roastings 4 hours in Muffle furnace at last promptly make Ce
0.8La
0.2O
1.9Coating.
Measure 5.6mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution after the water bath with thermostatic control vibration applying cated honeycomb ceramic carrier again, take out, blow away residual solution in the hole, 120 ℃ of dryings 1 hour in air then, 1050 ℃ of roastings are 4 hours in the air, promptly make Pd (1g/L)/Ce
0.8La
0.2O
1.9Catalyst.
Embodiment 8
Take by weighing 0.84g La
2O
3Add HNO
3, with 9.30g Ce (NO
3)
36H
2O and 5.44g citric acid mix and add proper amount of deionized water, stir, and get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is taken out for after the 31.96g cordierite honeycomb ceramic immerses coating liquid, blows out residual solution in the honeycomb channel, cordierite honeycomb ceramic ℃ is dried in the air to dry tack free in room temperature to 50, and again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 1 hour in Muffle furnace then.Repeat said process 2～3 times, to the absorption of coating liquid dipping fully, 500 ℃ of roastings 4 hours in Muffle furnace at last promptly make Ce
0.8La
0.2O
1.9Coating.
Measure 5.6mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution after the water bath with thermostatic control vibration applying cated honeycomb ceramic carrier again, take out, blow away residual solution in the hole, 120 ℃ of dryings 1 hour in air then, 1200 ℃ of roastings are 4 hours in the air, promptly make Pd (1g/L)/Ce
0.8La
0.2O
1.9Catalyst.
Embodiment 9
Take by weighing 0.42g La
2O
3, 0.29g Y
2O
3In add HNO respectively
3, with 9.19g Ce (NO
3)
36H
2O and 5.37g citric acid mix and add proper amount of deionized water, stir, and get coating liquid.To be of a size of 50mm * 25mm * 40mm, percent opening is 195cell/in
2, quality is taken out for after the 31.76g cordierite honeycomb ceramic immerses coating liquid, blows out residual solution in the honeycomb channel, cordierite honeycomb ceramic ℃ is dried in the air to dry tack free in room temperature to 50, and again in 120 ℃ of dryings 1 hour, 500 ℃ of roastings 1 hour in Muffle furnace then.Repeat said process 2～3 times, to the absorption of coating liquid dipping fully, 500 ℃ of roastings 4 hours in Muffle furnace at last promptly make Ce
0.8La
0.1Y
0.1O
1.9Coating.
Measure 5.6mL H
2PdCl
4The aqueous solution adds deionized water and is diluted to just with the honeycomb ceramic carrier submergence, be impregnated in this dilution after the water bath with thermostatic control vibration 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 (1g/L)/Ce
0.8La
0.1Y
0.1O
1.9Catalyst.
Make organic waste gas catalytic combustion catalyst prepared in the above embodiment of the present invention 1～9 cylindrical, fill in the fixed-bed catalytic combustion reactor, 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 40mm, by the air carrying band toluene reactor of flowing through, the aerial content 4～6gm of toluene
-3, air speed 13000h
-1The results are shown in Table 1.
The toluene catalytically combustion efficiency of each catalyst for catalytic combustion of table 1
Data from table 1 as can be known, catalyst of the present invention has higher organic waste-gas purification and handles active, the organic waste gas catalytic combustion purified treatment had lower initiation temperature, catalyst also has good heat endurance, as example 7,8, behind the high temperature sintering, its active decline slowly, the lower limit temperature of 1200 ℃ of calcined catalyst toluene oxidations only improves 40 ℃.Simultaneously catalyst coat combine with the honeycomb ceramic carrier surface firm, flood and use in there is no coating and have and come off.
Claims (6)
1. CeO
2Based composite oxides coated Pt-supported catalyst, it comprises honeycomb support skeleton, coating and precious metals pd, it is characterized in that described coating is by CeO
2, one or more compositions in the 3rd subgroup metal oxide, wherein CeO
2Based composite oxides coated mass percent is 5%～30% of a honeycomb ceramic carrier, CeO in the mixed oxide coatings
2With the ratio (in metal) of the amount of substance of the 3rd subgroup metal oxide be 9: 1～1: 9, its loading of active metal component Pd is that every liter of catalyst contains 0.1～2.0gPd.
2. organic waste gas catalytic combustion catalyst according to claim 1 is characterized in that described the 3rd subgroup metal oxide adopts La
2O
3, Sm
2O
3And Y
2O
3In one or more.
3. organic waste gas catalytic combustion catalyst according to claim 1 and 2 is characterized in that described cellular structure ceramic carrier skeleton is the cordierite-quality honeycombed ceramics skeleton.
4. CeO
2Based composite oxides coated Pt-supported catalyst preparation method is characterized in that this method for preparing catalyst may further comprise the steps:
(1) preparation of applying coating liquid adds HNO in a certain amount of the 3rd subgroup metal oxide
3, with Ce (NO
3)
3With organic acid or ethylene glycol or the mixture of the two mixing, add an amount of water, stir, make applying coating liquid;
(2) coating of honeycomb ceramic carrier skeleton coating is taken out after 1. honeycomb ceramic carrier being immersed applying coating liquid, removes the coating liquid that residues in the honeycomb ceramic carrier duct; 2. the ceramic honey comb in will be is 1. placed and was dried in 0.5～24 hour, again in 80～120 ℃ of dryings 0.5～12 hour; 3. the ceramic honey comb in inciting somebody to action 2. was 400～1000 ℃ of roastings 0.5～2 hour; 4. repeat 1.～3. step 2～four time, to the absorption of applying coating liquid dipping fully, 400～1000 ℃ of roastings 1～5 hour, promptly make the honeycomb ceramic carrier that contains coating at last;
(3) certain density H is prepared in the load of active metal component
2PdCl
4Solution is as the maceration extract that supports the noble metal active component.To apply cated honeycomb ceramic carrier and be impregnated into H
2PdCl
4Behind the solution, take out, remove the aqueous solution that residues in the honeycomb ceramic carrier duct, 80～120 ℃ of dryings 0.5～12 hour, 400～1000 ℃ of roastings are 1～5 hour in the final high temperature stove, promptly make the catalyst finished product.
5. CeO according to claim 4
2Based composite oxides coated Pt-supported catalyst preparation method is characterized in that organic acid is one or more in citric acid, malic acid and the tartaric acid.
6. CeO according to claim 4
2Based composite oxides coated Pt-supported catalyst preparation method is characterized in that used organic acid or ethylene glycol or the total amount of substance of the mixture of the two are CeO
2In the base composite oxidate 0.2～4 times of the total amount of substance of metal ion.
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|---|---|---|---|
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|---|---|---|---|
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| JP6709652B2 (en) * | 2016-03-24 | 2020-06-17 | 日本碍子株式会社 | Porous ceramic structure |
| CN107754866A (en) * | 2017-10-27 | 2018-03-06 | 宇星科技发展(深圳)有限公司 | It is catalyzed catalyst of burning and its preparation method and application |
| CN109126762B (en) * | 2018-09-10 | 2021-08-24 | 郑州科技学院 | CeO (CeO)2/TiO2Method for preparing nanotube composite material |
| CN110124689B (en) * | 2019-05-31 | 2021-12-24 | 金华铂锐催化科技有限公司 | Catalyst for purifying kitchen waste fermentation tail gas and preparation method thereof |
| JP2021070004A (en) * | 2019-11-01 | 2021-05-06 | トヨタ自動車株式会社 | Method for producing coating layer for exhaust gas purification catalyst device |
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