CN107855127A - Preparation and product and application based on metal Yu the loaded cobaltosic oxide of high-temperature stable of carrier strong interaction - Google Patents
Preparation and product and application based on metal Yu the loaded cobaltosic oxide of high-temperature stable of carrier strong interaction Download PDFInfo
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- CN107855127A CN107855127A CN201711098478.2A CN201711098478A CN107855127A CN 107855127 A CN107855127 A CN 107855127A CN 201711098478 A CN201711098478 A CN 201711098478A CN 107855127 A CN107855127 A CN 107855127A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/035—Precipitation on carriers
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- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
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- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
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- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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Abstract
The present invention discloses a kind of preparation and product and application based on metal Yu the loaded cobaltosic oxide of high-temperature stable of carrier strong interaction, and using cobalt nitrate as cobalt source, sodium carbonate is precipitating reagent, and cerium zirconium aluminium solid solution is carrier, and loaded Co is prepared using deposition-precipitation method3O4；Cobalt nitrate and cerium zirconium aluminium solid solution are in beaker, add deionized water solution, stirring makes cobalt nitrate dissolving complete, sodium carbonate liquor is slowly added in above-mentioned suspension, pH is adjusted to 9, stirs supersonic oscillations, products therefrom is filtered, wash, is freeze-dried, 3h is calcined at 800 DEG C, obtains powdered Co3O4/ CeZrAlO materials.The catalyst, applied to propane catalyst combustion reaction, still has activity well after 800 DEG C of high-temperature process.Catalyst raw material of the present invention is easy to get, and technique is simple, and catalyst high-temperature stability is good, has fabulous application prospect.
Description
Technical field
The present invention relates to the preparation field of nano material, is specifically related to a kind of based on metal and carrier strong interaction
The preparation method of the loaded cobaltosic oxide of high-temperature stable and product and application.
Background technology
Hydrocarbon（HC）It is one of primary pollution source of urban air, most HC are virose, and some HC are very
To being potential carcinogen, environment and human health are seriously endangered.In addition, photochemical reaction occurs for HC and NOx, it is possible to leads
Photochemical pollution is caused, more serious influence is caused to human health and ecological environment.Catalysis burning, product is carbon dioxide
And water, non-secondary pollution, it is a kind of Perfected process of improvement HC pollutions.
Low chain HC has the characteristics that nonpolar and chemical stability, and catalyst combustion reaction could often occur at high temperature.
Therefore, it is urgent and tool challenge a problem to develop high activity and high-temperature stability catalyst.Cobalt/cobalt oxide has most
Weak M-O keys, show the activity comparable with noble metal catalyst in alkane catalyst combustion reaction, cause increasing
Concern.
Nanometer, sub- nano-cobaltic-cobaltous oxide（Co3O4）, there is higher specific surface area and more avtive spots, selectivity
Exposed high miller index surface, possess more highdensity step positions, kink position atom etc., Co can be effectively improved3O4Catalyst
Activity.But under the high temperature conditions, above-mentioned Co3O4Reunion and structural rearrangement etc. easily occur for catalyst, cause stability to decline.Cause
This, there is an urgent need to develop the Co of high-temperature stable3O4Catalyst.
Activated alumina（γ-Al2O3）It is application with abundant pore structure, high-specific surface area, lower-price characteristic
One of widest catalyst carrier.It can effectively improve the decentralization of active component, improve catalyst activity and stability.But
It is γ-Al2O3With Co3O4Inertia aluminic acid cobalt compound is generated under hot conditions, the activity of catalyst can be reduced on the contrary.For a long time
Under hot conditions, inertia cobalt aluminate or inertia cobalt aluminate can be all generated by Co3O4Cladding completely, and make catalyst thorough
Inactivation.
Cerium zirconium aluminium solid solution（CeZrAlO）At high temperature, it is existing preferably to store oxygen ability, have high-specific surface area concurrently again.
By the ratio between modulation cerium zirconium aluminium, using rational preparation method by Co3O4Orientation supports aluminium, cerium zirconium in the carrier and had a common boundary
Place.It is expected under the high temperature conditions, interface forms a small amount of cobalt aluminate by Co3O4It is secured firmly to carrier surface, while interface cerium
Zirconium provides active oxygen, further improves Co3O4Activity.
The content of the invention
For prior art shortcoming and deficiency, present invention aims at：One kind is provided and is based on metal and the strong phase interaction of carrier
The preparation method of the loaded cobaltosic oxide of high-temperature stable.
Still a further object of the present invention is：Product prepared by a kind of above method is provided.
Another object of the present invention is：A kind of application of the said goods is provided.
The object of the invention is realized by following proposal：
To achieve the above object, the present invention uses following technical scheme：A kind of high temperature based on metal Yu carrier strong interaction
Stablize the preparation method of loaded cobaltosic oxide, using cobalt nitrate as cobalt source, sodium carbonate is precipitating reagent, and cerium zirconium aluminium solid solution is load
Body, loaded Co is prepared using deposition-precipitation method3O4, comprise the steps：
The deposition-precipitation method is specially：Appropriate cobalt nitrate and 1.5g cerium zirconium aluminium solid solution is weighed in beaker, 100ml is added and goes
Deionized water solution, stirring make cobalt nitrate dissolving complete, are slowly added to 1mol/L sodium carbonate liquor in above-mentioned suspension, pH is adjusted
To 9, during be stirred continuously at least 15min, supersonic oscillations 15-30min, it is uniformly dispersed, products therefrom filtered, washed
Wash, be freeze-dried, 3h is calcined at 800 DEG C, obtain powdered Co3O4/ CeZrAlO materials；Wherein, the loaded Co3O4In
Co3O4Loading be 5-25%.
The present invention is using cobalt nitrate as cobalt source, and sodium carbonate is precipitating reagent, and CeZrAlO is carrier, is prepared using deposition-precipitation method
Loaded Co3O4.Under the high temperature conditions, on the one hand, aluminium and Co3O4Cobalt aluminate is generated by Co3O4Carrier surface is secured firmly to, is tieed up
Hold Co3O4Higher decentralization；On the other hand, cerium zirconium provides active oxygen, maintains Co3O4High activity.Catalyst raw material of the present invention
It is easy to get, technique is simple.
The mol ratio of cerium zirconium aluminium is 1 in described cerium zirconium aluminium solid solution:1:0.5–1:1:2.
The present invention provides a kind of loaded cobaltosic oxide of high-temperature stable based on metal Yu carrier strong interaction, according to
Method described above is prepared.As catalyst, high-temperature stability is good, has fabulous application prospect.
The present invention provides a kind of answering for loaded cobaltosic oxide of high-temperature stable based on metal and carrier strong interaction
With the catalyst, applied to propane catalyst combustion reaction, still has activity well after 800 DEG C of high-temperature process.
The preparation of carrier cerium zirconium aluminium solid solution：Weigh appropriate cerous nitrate, zirconium nitrate and aluminum nitrate to be placed in beaker, add
100ml deionized water solutions, stirring make its dissolving complete.1mol/L sodium carbonate liquor is slowly added in above-mentioned solution, pH
Be adjusted to 9, during be stirred continuously at least 15min.In supersonic oscillations 15-30min after solution mixing, it is set to be uniformly dispersed.Will
Products therefrom filtering, washing, freeze-drying, are calcined 3h at 800 DEG C, obtain pale yellow powder shape cerium zirconium aluminium solid solution.
Compared with prior art, the present invention has the advantage that：
（1）Prepared Co3O4/ CeZrAlO catalyst, a small amount of cobalt aluminate is formed in interface by Co3O4It is secured firmly to carrier
Surface, improve Co3O4Decentralization；Meanwhile the aluminium of interface can not consume Co completely3O4, the cobalt aluminate of generation be also not enough to by
Co3O4Cladding completely.Therefore, prepared Co3O4/ CeZrAlO catalyst has good high-temperature stability.
（2）Prepared Co3O4/ CeZrAlO catalyst, CeZrAlO has at high temperature stores oxygen ability, boundary well
Face cerium zirconium can provide active oxygen for reaction, further improve Co3O4Activity.
（3）The inventive method has the characteristics that raw material is easy to get, technique is simple, catalyst activity is high, has application well
Prospect.
Embodiment
Embodiment 1
S1, the cerous nitrate for weighing 4.341g, 4.293g zirconium nitrate, 1.875g aluminum nitrate are placed in beaker, are added 100ml and are gone
Deionized water solution, stirring make its dissolving complete.
S2, be slowly added to 1mol/L sodium carbonate liquor in above-mentioned solution, pH is adjusted to 9, during be stirred continuously at least
15min.In supersonic oscillations 15-30min after solution mixing, it is set to be uniformly dispersed.
S3, products therefrom filtered, washs, be freeze-dried, be calcined 3h at 800 DEG C, obtain pale yellow powder shape cerium zirconium aluminium
Solid solution.
S4,0.5455g cobalt nitrates and 1.5g cerium zirconium aluminium solid solution are weighed in beaker, add 100ml deionized water solutions,
Stirring makes cobalt nitrate dissolving complete.
S5, be slowly added to 1mol/L sodium carbonate liquor in above-mentioned suspension, pH is adjusted to 9, during be stirred continuously to
Few 15min.Supersonic oscillations 15-30min, makes it be uniformly dispersed.
S6, products therefrom filtered, washs, be freeze-dried, be calcined 3h at 800 DEG C, it is powdered to obtain dark gray solid
Co3O4/ CeZrAlO-1 materials.
Embodiment 2
S1, the cerous nitrate for weighing 4.341g, 4.293g zirconium nitrate, 3.75g aluminum nitrate are placed in beaker, are added 100ml and are gone
Deionized water solution, stirring make its dissolving complete.
S2, be slowly added to 1mol/L sodium carbonate liquor in above-mentioned solution, pH is adjusted to 9, during be stirred continuously at least
15min.In supersonic oscillations 15-30min after solution mixing, it is set to be uniformly dispersed.
S3, products therefrom filtered, washs, be freeze-dried, be calcined 3h at 800 DEG C, obtain pale yellow powder shape cerium zirconium aluminium
Solid solution.
S4,0.5455g cobalt nitrates and 1.5g cerium zirconium aluminium solid solution are weighed in beaker, add 100ml deionized water solutions,
Stirring makes cobalt nitrate dissolving complete.
S5, be slowly added to 1mol/L sodium carbonate liquor in above-mentioned suspension, pH is adjusted to 9, during be stirred continuously to
Few 15min.Supersonic oscillations 15-30min, makes it be uniformly dispersed.
S6, products therefrom filtered, washs, be freeze-dried, be calcined 3h at 800 DEG C, it is powdered to obtain dark gray solid
Co3O4/ CeZrAlO-2 materials.
Embodiment 3
S1, the cerous nitrate for weighing 4.341g, 4.293g zirconium nitrate, 5.625g aluminum nitrate are placed in beaker, are added 100ml and are gone
Deionized water solution, stirring make its dissolving complete.
S2, be slowly added to 1mol/L sodium carbonate liquor in above-mentioned solution, pH is adjusted to 9, during be stirred continuously at least
15min.In supersonic oscillations 15-30min after solution mixing, it is set to be uniformly dispersed.
S3, products therefrom filtered, washs, be freeze-dried, be calcined 3h at 800 DEG C, obtain pale yellow powder shape cerium zirconium aluminium
Solid solution.
S4,0.5455g cobalt nitrates and 1.5g cerium zirconium aluminium solid solution are weighed in beaker, add 100ml deionized water solutions,
Stirring makes cobalt nitrate dissolving complete.
S5, be slowly added to 1mol/L sodium carbonate liquor in above-mentioned suspension, pH is adjusted to 9, during be stirred continuously to
Few 15min.Supersonic oscillations 15-30min, makes it be uniformly dispersed.
S6, products therefrom filtered, washs, be freeze-dried, be calcined 3h at 800 DEG C, it is powdered to obtain dark gray solid
Co3O4/ CeZrAlO-3 materials.
Embodiment 4
S1, the cerous nitrate for weighing 4.341g, 4.293g zirconium nitrate, 7.5g aluminum nitrate are placed in beaker, add 100ml go from
The sub- aqueous solution, stirring make its dissolving complete.
S2, be slowly added to 1mol/L sodium carbonate liquor in above-mentioned solution, pH is adjusted to 9, during be stirred continuously at least
15min.In supersonic oscillations 15-30min after solution mixing, it is set to be uniformly dispersed.
S3, products therefrom filtered, washs, be freeze-dried, be calcined 3h at 800 DEG C, obtain pale yellow powder shape cerium zirconium aluminium
Solid solution.
S4,0.5455g cobalt nitrates and 1.5g cerium zirconium aluminium solid solution are weighed in beaker, add 100ml deionized water solutions,
Stirring makes cobalt nitrate dissolving complete.
S5, be slowly added to 1mol/L sodium carbonate liquor in above-mentioned suspension, pH is adjusted to 9, during be stirred continuously to
Few 15min.Supersonic oscillations 15-30min, makes it be uniformly dispersed.
S6, products therefrom filtered, washs, be freeze-dried, be calcined 3h at 800 DEG C, it is powdered to obtain dark gray solid
Co3O4/ CeZrAlO-4 materials.
Comparative example 1
S1, weigh 0.5455g cobalt nitrates and 1.5gAl2O3In beaker, 100ml deionized water solutions are added, stirring makes nitric acid
Cobalt dissolving is complete.
S2, be slowly added to 1mol/L sodium carbonate liquor in above-mentioned suspension, pH is adjusted to 9, during be stirred continuously to
Few 15min.Supersonic oscillations 15-30min, makes it be uniformly dispersed.
S3, products therefrom filtered, washs, be freeze-dried, be calcined 3h at 800 DEG C, obtain the powdered Co of blue solid3O4/
Al2O3Material.
Application examples 1
Catalyst catalytic performance evaluation is carried out in internal diameter 8mm, long 250mm quartz tube reactor.Unstripped gas air speed is
30000mLg-1 cat h-1, propane concentration 1000ppm, Balance Air is air.Catalytic performance test the results are shown in Table 1.
The specific embodiment of the present invention is described above.It should be pointed out that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (5)
1. a kind of preparation method based on metal Yu the loaded cobaltosic oxide of high-temperature stable of carrier strong interaction, its feature
It is：Using cobalt nitrate as cobalt source, sodium carbonate is precipitating reagent, and cerium zirconium aluminium solid solution is carrier, is prepared and supported using deposition-precipitation method
Type Co3O4, comprise the following steps：
Appropriate cobalt nitrate and 1.5g cerium zirconium aluminium solid solution is weighed in beaker, adds 100ml deionized water solutions, stirring makes nitric acid
Cobalt dissolving is complete, is slowly added to 1mol/L sodium carbonate liquor in above-mentioned suspension, and pH is adjusted to 9, during be stirred continuously to
Few 15min, supersonic oscillations 15-30min, makes it be uniformly dispersed, products therefrom is filtered, wash, is freeze-dried, at 800 DEG C
Lower roasting 3h, obtains powdered Co3O4/ CeZrAlO materials；Wherein, the loaded Co3O4Middle Co3O4Loading be 5-25%.
2. the high-temperature stable loaded cobaltosic oxide according to claim 1 based on metal and carrier strong interaction
Preparation method, it is characterised in that：The mol ratio of cerium zirconium aluminium is 1 in the cerium zirconium aluminium solid solution:1:0.5–2.
3. loaded four oxidation three of the high-temperature stable according to claim 1 or 2 based on metal and carrier strong interaction
The preparation method of cobalt, it is characterised in that：The preparation of carrier cerium zirconium aluminium solid solution：Weigh appropriate cerous nitrate, zirconium nitrate and nitric acid
Aluminium is placed in beaker, adds 100ml deionized water solutions, and stirring makes its dissolving complete；The sodium carbonate for being slowly added to 1mol/L is molten
For liquid in above-mentioned solution, pH is adjusted to 9, during be stirred continuously at least 15min.In supersonic oscillations 15- after solution mixing
30min, it is set to be uniformly dispersed.Products therefrom is filtered, wash, is freeze-dried, 3h is calcined at 800 DEG C, obtains pale yellow powder
Shape cerium zirconium aluminium solid solution.
A kind of 4. loaded cobaltosic oxide of high-temperature stable based on metal Yu carrier strong interaction, it is characterised in that according to
Claims 1 to 3 either method is prepared.
5. the high-temperature stable loaded cobaltosic oxide according to claim 4 based on metal and carrier strong interaction
Using, it is characterised in that：The catalyst, applied to propane catalyst combustion reaction, still has very after 800 DEG C of high-temperature process
Good activity.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111111656A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | High-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of VOCs self-sustaining combustion and preparation method and application thereof |
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| CN104014340A (en) * | 2014-05-28 | 2014-09-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Supported cobaltosic oxide catalyst, and preparation method and application thereof |
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| CN105817229A (en) * | 2016-04-25 | 2016-08-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Rare earth element modified load type cobaltosic oxide catalyst and preparation method thereof |
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| JP2013505996A (en) * | 2010-07-10 | 2013-02-21 | 住友化学株式会社 | Process for producing olefin oxide |
| CN103846089A (en) * | 2014-01-14 | 2014-06-11 | 台州欧信环保净化器有限公司 | Homogeneous solid-solution cerium-zirconium-cobalt-aluminum composite material and preparation method thereof |
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| CN111111656A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | High-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of VOCs self-sustaining combustion and preparation method and application thereof |
| CN111111656B (en) * | 2018-10-30 | 2023-07-21 | 中国石油化工股份有限公司 | High-temperature-resistant catalytic combustion catalyst capable of catalyzing and igniting VOCs (volatile organic compounds) to perform self-sustaining combustion at normal temperature and preparation method and application thereof |
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