CN1415410A - Catalyzer for catalyzing combustion and its preparing method - Google Patents
Catalyzer for catalyzing combustion and its preparing method Download PDFInfo
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- CN1415410A CN1415410A CN 01133374 CN01133374A CN1415410A CN 1415410 A CN1415410 A CN 1415410A CN 01133374 CN01133374 CN 01133374 CN 01133374 A CN01133374 A CN 01133374A CN 1415410 A CN1415410 A CN 1415410A
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Abstract
A catalyst for the catalytic combustion of combustible waste gas is prepared by dipping the Pt as active component on the coated layer of cellular ceramics as carrier. The said coated layer contains Al2O3 (20-80 wt.%), TiO2 (10-40 wt.%), CeO2 (5-30 wt.%) and ZrO2 (5-20 wt.%). Its advantages are high utilization rate of Pt, and high distribution uniformity.
Description
1, technical field
The present invention relates to a kind of catalyst for catalytic combustion and preparation method thereof, more particularly, the present invention relates to a kind ofly be used for the purified treatment organic exhaust gas and other contain honeycombed catalyst for catalytic combustion of combustible component waste gas and preparation method thereof.
2, technical background
A lot of industrial enterprises discharge organic exhaust gas in a large number, and this problem is particularly outstanding in petroleum refining and chemical industry and industries such as electronics, printing, coating, shoemaking, enamel-covered wire processing and food and feed processing.The discharging severe contamination of organic exhaust gas atmospheric environment, and human body caused very big harm, therefore cause people's common concern.In the organic waste-gas purification processing method, catalytic combustion technology is particularly noticeable.Catalytic combustion is as the effective technology of cleaning organic waste gas, and its core is a catalyst for catalytic combustion.Therefore develop the key that function admirable and catalyst for catalytic combustion with low cost become this technical development.
Practical catalyst for catalytic combustion mostly is the honeycombed structure greatly, promptly is matrix with the honeycomb ceramic body, and applying coating is as carrier thereon, and then supports active component.Chinese patent CN1013245B discloses a kind of catalyst and production method thereof of purifying exhaust air, wherein said catalyst is made up of the honeycomb support of en-block construction and the coating that applies on it, and this coating is made up of zirconia, refractory inorganic oxide and the rare-earth oxide of load platinum group metal.This Preparation of catalysts method is: with the zirconia that has supported noble metal and the washcoated honeycomb ceramic body of making after other oxides mix of moisture thin pulp, drying and calcination process then.This preparation method has determined the noble metal active component of this catalyst to have very most of other oxides in coated to cover, thereby has influenced making full use of and effectively playing a role of noble metal.The method that supports noble metal active component rhodium and platinum in this patent is: with the aqueous solution dipping inorganic oxide, the drying and the calcination process then of radium chloride and platinum chloride.This existing problem of noble metal method that supports is that the noble metal active component can not evenly support in catalyst surface by effective competitive Adsorption, thereby has reduced the performance of noble metal active component.
3, summary of the invention
Noble metal component utilization rate at catalyst for catalytic combustion in the prior art is low, disperse uneven problem, the invention provides the catalyst for catalytic combustion that the effect of a kind of fully effectively performance noble metal, noble metal are uniformly distributed in catalyst surface, another object of the present invention is to provide this Preparation of catalysts method.
Catalyst for catalytic combustion of the present invention is a kind of honeycombed noble metal catalyst, is made up of with the noble metal active component Pt that supports on it honeycomb ceramic carrier with coating.Wherein the coating of honeycomb ceramic carrier composition is by weight percentage: active A l
2O
320%～80%, TiO
210%～40%, CeO
25%～30%, ZrO
25%～20%.Active component Pt supports in the honeycomb ceramic carrier coating surface by containing organic acid platiniferous solution impregnation, and its loading is that every liter of catalyst contains 0.5～4.0gPt.
Honeycomb ceramic body generally is that raw material is made with the cordierite, also can select other materials for use.The active A l that coating is used
2O
3Can use various crystal formations, but with γ-Al
2O
3Effect is best.TiO
2Common crystal formation has the rutile-type Detitanium-ore-type, for catalyst of the present invention, uses Detitanium-ore-type TiO
2Effect is better.
The preparation method of catalyst for catalytic combustion of the present invention is: with platiniferous 0.001～0.100g/ml, the mixed solution that contains organic acid 0.01～1.5mol/l floods the honeycomb ceramic carrier with coating, and dry then, roasting makes catalyst.
By the honeycombed catalyst for catalytic combustion of the inventive method preparation, the noble metal active component is loaded on the catalyst by infusion process, has avoided noble metal other oxides in coated to cover, and has given full play to the useful effect of noble metal; In addition, owing in dipping solution, added organic acid as competitive adsorbate, can make noble metal be distributed in the coating outer surface more equably, can reduce noble metal dosage, and owing to be uniformly dispersed, even under higher temperature, also difficult gathering of noble metal cause active the reduction.These characteristics make this catalyst when purified treatment organic exhaust gas and other contain the waste gas of combustible component, even also show higher oxidation activity when the noble metal active constituent content is low, and have good activity stability.
4, the specific embodiment
The concrete preparation process of catalyst for catalytic combustion of the present invention is:
(1) takes by weighing active A l by constant weight percentage
2O
3, TiO
2, CeO
2, ZrO
2Powder adds an amount of distilled water and mixes, and is modulated into moisture thin pulp.The percentage by weight of four kinds of oxide powders is: active A l
2O
320%～80%, TiO
210%～40%, CeO
25%～30%, ZrO
25%～20%.The distilled water and the Al that add
2O
3, TiO
2, CeO
2, ZrO
2The ratio of the gross weight of four kinds of oxides is 10～50: 1.
(2) take out honeycomb ceramic body is flooded 20～60 minutes in above-mentioned moisture thin pulp after, blow residual slurries in the most honeycomb body opening with compressed air, drying and calcination process are promptly made and are had the honeycomb ceramic carrier that mixes inorganic oxide coating.The drying and the roasting condition of preparation honeycomb ceramic carrier are: 100～120 ℃ of air dryings 3～20 hours, and roasting 1～10 hour in 450～650 ℃ of air then.
(3) preparation contains the solution of organic acid and platinum, is 0.001～0.100g/ml in the concentration of platinum in the platinum mixed solution, is preferably 0.008～0.015g/ml, and the concentration of organic acid in mixed solution is 0.01～1.5mol/l, is preferably 0.05～0.30mol/l.Platinum in the mixed solution is from H
2PtCl
6, PtCl
2, simple substance platinum is dissolved in solution of chloroazotic acid etc.With this add organic acid as the platiniferous solution of competitive adsorbate as the maceration extract that supports active component Pt.Above-mentioned organic acid is monocarboxylic acid or the polybasic carboxylic acid that is selected from C1～C6, as formic acid, acetate, oxalic acid, citric acid, tartaric acid etc., also can be that wherein two or more use simultaneously.
(4) honeycomb ceramic carrier behind the applying coating is immersed in the above-mentioned maceration extract that supports active component Pt, flood taking-up after 20～180 minutes, drying and calcination process are promptly made the honeycombed catalyst for catalytic combustion.Dry and roasting condition is: 100～120 ℃ of air dryings 3～25 hours, and roasting 1～5 hour in 400～600 ℃ of air then.
Catalyst of the present invention can have in the purified treatment of various low-concentration organic exhaust gas and other combustible component waste gas, as industrial tail gas, gas tail gas etc.
Below in conjunction with embodiment the present invention is made further specifying, but the present invention is not limited to these
Embodiment.
Embodiment 1
Take by weighing the active γ-Al of 70g
2O
3Powder, the 20g rutile TiO
2Powder, 5gCeO
2Powder, 5gZrO
2Powder mixes the back and adds 4.0L distilled water, carefully grinds to form moisture thin pulp.The submergence in above-mentioned moisture thin pulp of cordierite honeycomb ceramic body was taken out after 20 minutes, blow residual slurries in the most hole with compressed air, 120 ℃ of air dryings 10 hours, roasting was 3 hours in 550 ℃ of air, promptly makes the honeycomb ceramic carrier with coating.Compound concentration is the H that contains 0.008gPt in every ml water solution then
2PtCl
6The aqueous solution adds the 30w% aqueous citric acid solution, makes the concentration 0.5mol/l of the citric acid in the mixed solution, with this mixed solution as the maceration extract that supports active component Pt.The honeycomb ceramic carrier with coating of preparation flood taking-up after 120 minutes in above-mentioned Pt maceration extract, 100～120 ℃ of air dryings 10 hours, roasting was 5 hours in 550 ℃ of air, promptly makes catalyst for catalytic combustion.The content of this activity of such catalysts component Pt is: every liter of catalyst contains 2.24gPt.The coating of this catalyst is formed: active A l
2O
37O%, TiO
220%, CeO
25%, ZrO
25%.
Embodiment 2
Take by weighing 50g active A l
2O
3Powder, 30g Detitanium-ore-type TiO
2Powder, 15gCeO
2Powder, 5gZrO
2Powder mixes the back and adds 2.0L distilled water, carefully grinds to form moisture thin pulp.The submergence in above-mentioned moisture thin pulp of cordierite honeycomb ceramic body was taken out after 40 minutes, blow residual slurries in the most hole with compressed air, 120 ℃ of air dryings 20 hours, roasting was 5 hours in 500 ℃ of air, promptly makes the honeycomb ceramic carrier with coating.Compound concentration is the H that contains 0.004gPt in every ml water solution then
2PtCl
6The aqueous solution adds the 30w% oxalic acid aqueous solution, and making the concentration of oxalic acid in the mixed solution is 0.85mol/l, with this mixed solution as the maceration extract that supports active component Pt.The honeycomb ceramic carrier with coating of preparation flood taking-up after 30 minutes in above-mentioned Pt maceration extract, 120 ℃ of air dryings 15 hours, roasting was 2 hours in 500 ℃ of air, promptly makes catalyst for catalytic combustion.The content of this activity of such catalysts component Pt is: every liter of catalyst contains 1.22gPt.The coating of this catalyst is formed: active A l
2O
350%, TiO
230%, CeO
215%, ZrO
25%.
Embodiment 3
Take by weighing 70g γ-Al
2O
3Powder, 14g Detitanium-ore-type TiO
2Powder, 10gCeO
2Powder, 6gZrO
2Powder mixes the back and adds 1.4L distilled water, carefully grinds to form moisture thin pulp.The submergence in above-mentioned moisture thin pulp of cordierite honeycomb ceramic body was taken out after 30 minutes, blow residual slurries in the most hole with compressed air, 120 ℃ of air dryings 12 hours, roasting was 3 hours in 550 ℃ of air, promptly makes the honeycomb ceramic carrier with coating.Compound concentration is the H that contains 0.008gPt in every ml water solution then
2PtCl
6The aqueous solution adds acetate, and the concentration that makes the acetate in the mixed solution is 0.05mol/l, with this mixed solution as the maceration extract that supports active component Pt.The honeycomb ceramic carrier with coating of preparation flood taking-up after 60 minutes in above-mentioned Pt maceration extract, 120 ℃ of air dryings 20 hours, roasting was 3 hours in 550 ℃ of air, promptly makes catalyst for catalytic combustion.The content of this activity of such catalysts component Pt is: every liter of catalyst contains 1.83gPt.The coating of this catalyst is formed: active A l
2O
370%, TiO
214%, CeO
210%, ZrO
26%.
Embodiment 4
Take by weighing 30g active A l
2O
3Powder, the 40g rutile TiO
2Powder, 20gCeO
2Powder, 10gZrO
2Powder mixes the back and adds 3.0L distilled water, carefully grinds to form moisture thin pulp.The submergence in above-mentioned moisture thin pulp of cordierite honeycomb ceramic body was taken out after 50 minutes, blow residual slurries in the most hole with compressed air, 100 ℃ of air dryings 12 hours, roasting was 9 hours in 450 ℃ of air, promptly makes the honeycomb ceramic carrier with coating.Compound concentration is the H that contains 0.100gPt in every ml water solution then
2PtCl
6The aqueous solution adds formic acid, and the concentration that makes formic acid in the mixed solution is 0.17mol/l, with this mixed solution as the maceration extract that supports active component Pt.The honeycomb ceramic carrier with coating of preparation flood taking-up after 90 minutes in above-mentioned Pt maceration extract, 120 ℃ of air dryings 6 hours, roasting was 1 hour in 600 ℃ of air, promptly makes catalyst for catalytic combustion.The content of this activity of such catalysts component Pt is: every liter of catalyst contains 3.43gPt.The coating of this catalyst is formed: active A l
2O
330%, TiO
240%, CeO
220%, ZrO
210%.
Embodiment 5
Take by weighing 40g γ-Al
2O
3Powder, 15g Detitanium-ore-type TiO
2Powder, 30gCeO
2Powder, 15gZrO
2Powder mixes the back and adds 1.0L distilled water, carefully grinds to form moisture thin pulp.The submergence in above-mentioned moisture thin pulp of cordierite honeycomb ceramic body was taken out after 30 minutes, blow residual slurries in the most hole with compressed air, 120 ℃ of air dryings 15 hours, roasting was 2 hours in 600 ℃ of air, promptly makes the honeycomb ceramic carrier with coating.Compound concentration is the H that contains 0.002gPt in every ml water solution then
2PtCl
6The aqueous solution adds the mixed liquor of 30w% aqueous citric acid solution and acetate, and mixed volume ratio 1: 3 makes that the organic acid total concentration is 1.2mol/l in the mixed liquor, with this mixed solution as the maceration extract that supports active component Pt.The honeycomb ceramic carrier with coating of preparation flood taking-up after 60 minutes in above-mentioned Pt maceration extract, 100 ℃ of air dryings 25 hours, roasting was 4 hours in 400 ℃ of air, promptly makes catalyst for catalytic combustion.The content of this activity of such catalysts component Pt is: every liter of catalyst contains 0.63gPt.The coating of this catalyst is formed: active A l
2O
340%, TiO
215%, CeO
230%, ZrO
215%.
Embodiment 6
The mixed liquor that adds acetate and 30w% oxalic acid aqueous solution, mixed volume ratio 1: 2 makes that total organic acids concentration is 1.50mol/l in the mixed liquor, and all the other steps are with embodiment 3.
Embodiment 7
The mixed liquor that adds 30w% aqueous citric acid solution, 30w% oxalic acid aqueous solution, mixed volume ratio 1: 1 makes that the organic acid total concentration is 1.30mol/l in the mixed liquor, and all the other steps are with embodiment 3.
Embodiment 8
The mixed liquor that adds 30w% aqueous citric acid solution, 30w% aqueous tartaric acid solution, mixed volume ratio 3: 1 makes that the organic acid total concentration is 1.00mol/l in the mixed liquor, and all the other steps are with embodiment 3.
Embodiment 9
The mixed liquor that adds 30w% aqueous citric acid solution, 30w% oxalic acid aqueous solution, acetate, mixed volume ratio 1: 1: 2 makes that the organic acid total concentration is 0.15mol/l in the mixed liquor, and all the other steps are with embodiment 3.
Comparative Examples 1
With the radium chloride aqueous solution dipping 10g zirconia that contains the 0.3g rhodium, the zirconia of dipping was 120 ℃ of air dryings 12 hours, and roasting is 1 hour in 500 ℃ of air, generates the Zirconium oxide powder that contains the 2.9wt% rhodium.With the platinum chloride aqueous solution dipping 150g activated alumina that contains 1.5g platinum, 150 ℃ of air dryings 12 hours, roasting was 1 hour in 500 ℃ air, so that the alumina powder of platiniferous to be provided with impregnated activated alumina.Two kinds of powder of as above gained and 75g ceria oxide powder are added water grind 20 hours to prepare moisture thin pulp.The cordierite honeycomb ceramic matrix is soaked as in the above-mentioned moisture thin pulp,, blow superfluous thin pulp in the most micropore,, promptly make the contrast catalyst for catalytic combustion 140 ℃ of air dryings 3 hours with compressed air then with its taking-up.
Each catalyst is used for organic waste-gas purification handles to estimate its performance, the actual conditions of evaluation is: handling a total hydrocarbon concentration of discharging with sewage from oil refinery is that 3000 μ L/L organic exhaust gas serve as to handle object, and reaction velocity is 40000h
-1, the catalytic bed inlet temperature is 300 ℃.That estimates the results are shown in table 1.Data from table 1 as can be known, catalyst of the present invention has higher organic waste-gas purification and handles actively, catalyst also has durability preferably.
The organic waste-gas purification of table 1 catalyst is handled active
| Catalyst | The purifying rate of start of run (%) | Purifying rate (%) after 1000 hours turns round |
| Embodiment 1 | ????94.8 | ????92.2 |
| Embodiment 2 | ????95.3 | ????94.6 |
| Embodiment 3 | ????97.2 | ????96.8 |
| Embodiment 4 | ????95.5 | ????93.3 |
| Embodiment 5 | ????94.8 | ????93.9 |
| Embodiment 6 | ????96.3 | ????95.5 |
| Embodiment 7 | ????96.6 | ????96.1 |
| Embodiment 8 | ????96.4 | ????95.8 |
| Embodiment 9 | ????95.6 | ????95.2 |
| Comparative Examples 1 | ????86.5 | ????80.2 |
Claims (10)
1, a kind of catalyst for catalytic combustion is formed with honeycomb ceramic carrier with coating and the noble metal active component platinum that supports on it, and wherein the coating of honeycomb ceramic carrier composition is by weight percentage: active al2o3 20%～80%, TiO
210%～40%, CeO
25%～30%, ZrO
25%～20%, it is characterized in that described noble metal active component platinum by containing organic acid platiniferous solution impregnation on the honeycomb ceramic carrier coating surface, its loading is that every liter of catalyst contains 0.5～4.0gPt.
2,, it is characterized in that described honeycomb ceramic body is that raw material is made with the cordierite, the active A l that coating is used according to the described catalyst for catalytic combustion of claim 1
2O
3Be γ-Al
2O
3, TiO
2Be rutile-type or Detitanium-ore-type.
3, the preparation method of the described catalyst for catalytic combustion of a kind of claim 1, it is characterized in that with platiniferous 0.001～0.100g/ml, contain the honeycomb ceramic carrier that the mixed solution dipping of organic acid 0.01～1.5mol/l has coating, dry then, roasting makes catalyst.
4, according to the preparation method of the described catalyst for catalytic combustion of claim 3, it is characterized in that described preparation process with honeycomb ceramic carrier of coating is: forming content by coating weight is active A l
2O
320%～80%, TiO
210%～40%, CeO
25%～30%, ZrO
25%～20% takes by weighing various raw materials, adding distilled water mixes, be modulated into moisture thin pulp, the distilled water that adds is 10～50: 1 with the ratio of total weight of solids, honeycomb ceramic body is flooded in this thin pulp, blow residual slurries in the most honeycomb body opening with compressed air then, drying, roasting make.
5,, it is characterized in that described honeycomb ceramic body dip time in moisture thin pulp is 20～60 minutes according to the preparation method of the described catalyst for catalytic combustion of claim 4; Described drying and roasting condition are: 100～120 ℃ of air dryings 3～20 hours, and roasting 1～10 hour in 450～650 ℃ of air then.
6, according to the preparation method of the described catalyst for catalytic combustion of claim 3, the platinum content that it is characterized in that described mixed solution is 0.008～0.15g/ml, and organic acid content is 0.05～0.30mol/l.
7, according to the preparation method of the described catalyst for catalytic combustion of claim 3, the platinum that it is characterized in that described mixed solution is from H
2PtCl
6, PtCl
2, simple substance platinum is dissolved in the solution of chloroazotic acid.
8,, it is characterized in that described organic acid is to be selected from the monocarboxylic acid of C1～C6 or in the polybasic carboxylic acid one or more according to the preparation method of the described catalyst for catalytic combustion of claim 3.
9,, it is characterized in that described organic acid is selected from one or more in formic acid, acetate, oxalic acid, citric acid, the tartaric acid according to the preparation method of claim 3 or 8 described catalyst for catalytic combustion.
10, according to the preparation method of the described catalyst for catalytic combustion of claim 3, it is characterized in that described dip time is 20～180 minutes, dry and roasting condition is: 100～120 ℃ of air dryings 3～25 hours, and roasting 1～5 hour in 400～600 ℃ of air then.
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|---|---|---|---|
| CN 01133374 CN1132682C (en) | 2001-10-30 | 2001-10-30 | Catalyzer for catalyzing combustion and its preparing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01133374 CN1132682C (en) | 2001-10-30 | 2001-10-30 | Catalyzer for catalyzing combustion and its preparing method |
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| Publication Number | Publication Date |
|---|---|
| CN1415410A true CN1415410A (en) | 2003-05-07 |
| CN1132682C CN1132682C (en) | 2003-12-31 |
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| CN100427208C (en) * | 2006-01-19 | 2008-10-22 | 清华大学 | Method for preparing catalyst to purify automobile tail gas |
| CN100430131C (en) * | 2005-12-26 | 2008-11-05 | 浙江师范大学 | Catalytic combustion catalyst |
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| CN101475405B (en) * | 2009-01-21 | 2012-01-04 | 景德镇陶瓷学院 | Method for improving honeycomb ceramic antifouling property |
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| CN100427208C (en) * | 2006-01-19 | 2008-10-22 | 清华大学 | Method for preparing catalyst to purify automobile tail gas |
| CN101475405B (en) * | 2009-01-21 | 2012-01-04 | 景德镇陶瓷学院 | Method for improving honeycomb ceramic antifouling property |
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| CN101961653A (en) * | 2010-09-30 | 2011-02-02 | 浙江工业大学 | Composite oxide catalytic combustion catalyst as well as preparation method and application thereof |
| CN101961653B (en) * | 2010-09-30 | 2012-06-27 | 浙江工业大学 | Composite oxide catalytic combustion catalyst as well as preparation method and application thereof |
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| CN112403490A (en) * | 2020-10-27 | 2021-02-26 | 福建龙新三维阵列科技有限公司 | Sulfur-resistant catalyst, preparation method and application |
| CN114082417A (en) * | 2021-11-22 | 2022-02-25 | 复旦大学 | Supported noble metal honeycomb catalyst and preparation method and application thereof |
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