CN109437326A - The preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture - Google Patents
The preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture Download PDFInfo
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- CN109437326A CN109437326A CN201811554532.4A CN201811554532A CN109437326A CN 109437326 A CN109437326 A CN 109437326A CN 201811554532 A CN201811554532 A CN 201811554532A CN 109437326 A CN109437326 A CN 109437326A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/70—Cobaltates containing rare earth, e.g. LaCoO3
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Abstract
The invention belongs to meso-porous nano field of material preparation, and in particular to a kind of preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture is implemented as follows: (i) weighs metal salt and adjuvant respectively, after grinding, the two is uniformly mixed, then is ground, mixture predecessor is obtained；(ii) by step, (i) the mixture predecessor is placed in high temperature furnace, under air or nitrogen atmosphere, temperature programming, and heating, then temperature programming, continue to heat, after natural cooling, obtains head product；(iii) by step, (ii) the head product is washed, and is dried to get target product.The present invention is low in cost, and process is simple, and easily operated, target product pore size distribution range is wide, large specific surface area.
Description
Technical field
The invention belongs to meso-porous nano field of material preparation, and in particular to a kind of adjustable mesoporous metal composite oxides in aperture
The preparation method of nano material.
Background technique
Material of the pore-size distribution between 2~50 nm belongs to mesoporous material, since the specific surface area of mesoporous material is larger,
Surface and body phase excellent, pore size distribution range is wide, has the characteristics that high absorption and diffusivity are strong, in separation, adsorbs, urges
The fields such as change, material and electrochemistry are with a wide range of applications.
The research of mesoporous metal composite oxides has obtained extensive concern, and cerium base mesoporous metal composite oxides are because of rare earth
The strong Oxygen storage capacity of cerium component can make the material be used in the fields such as oxidation removal volatile organic matter.As its shape of nanoparticle
Shape and specific surface area play critical influence to the application of particle.Currently, the preparation method of mesopore metal oxide mainly has
Hydro-thermal method, sol-gel method, template and micromeritics self-assembly method etc..Such as: Suhong Lu etc. is using citric acid auxiliary
Sol-gal process prepares series CeO2-Co3O4Composite oxides nanoparticle, specific surface area are 43~75 m2/ g, has rated it
Performance (Suhong Lu, Fan Wang, Canchang Chen, the Fenglin Huang, Kelun of catalytic elimination formaldehyde
Li. Journal of Rare Earths, 2017,35,867-874.)；Yu Wang etc. is prepared using KIT-6 template
Co-Mn series composite oxides nanoparticle, specific surface area are 92~150 m2/ g, the excellent performance for removing formaldehyde are situated between with it
Pore structure related (Yu Wang, Aimin Zhu, Bingbing Chen, Mark Crocker, Chuan with specific surface area
Shi. Catalysis Communications, 2013,36,52-57.).The preparation side of these mesoporous metal combined oxidations
Method is completed by processes such as hydro-thermal, gels, and process flow is more more complex, limits being widely used for these methods.
Summary of the invention
A kind of low in cost the present invention is directed to provide in place of overcome the deficiencies in the prior art, process is simple, easily operated,
Target product pore size distribution range is wide, the preparation of the adjustable mesoporous metal composite oxide nano-material in the aperture of large specific surface area
Method.
In order to solve the above technical problems, the present invention is implemented as follows:
The preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture, can implement as follows:
(i) metal salt and adjuvant are weighed respectively, after grinding, the two is uniformly mixed, then grinds, obtains mixture predecessor；
(ii) by step, (i) the mixture predecessor is placed in high temperature furnace, and under air or nitrogen atmosphere, temperature programming adds
Heat, then temperature programming continue to heat, and after natural cooling, obtain head product；
(iii) by step, (ii) the head product is washed, and is dried to get target product.
As a preferred embodiment, in step (i) of the present invention, the metal salt is nitrate or oxalates.
Further, nitrate of the present invention is one or more of cerous nitrate, cobalt nitrate and manganese nitrate
Mixture；The oxalates is the mixture of one or more of cerium oxalate, cobalt oxalate and manganese oxalate.
Further, nitrate of the present invention is cerous nitrate；The oxalates is cerium oxalate.
Further, in step (i) of the present invention, the adjuvant is one or both of glucose, citric acid, starch
Above mixture.
Further, in step (i) of the present invention, the molar ratio of the metal salt and adjuvant is 1: 0.5~4.
Further, in step (ii) of the present invention, high temperature furnace is placed in crucible by mixture predecessor is evenly laid out
It is interior, under air or nitrogen atmosphere, with 1 DEG C/min of heating rate, it is heated to 110~120 DEG C and is kept for 100~200 points
Clock, then continue to be heated to 450~850 DEG C with 1 DEG C/min of heating rate, and kept for 200~250 minutes, after natural cooling
Obtain head product.
Further, in step (iii) of the present invention, head product deionized water and dehydrated alcohol are washed three times respectively,
100 minutes are dried in 60 DEG C of baking ovens to get target product.
Further, in step (i) of the present invention, metal salt and adjuvant are weighed respectively, after being fully ground into powder, by two
Person is uniformly mixed, then grinds 30~60 minutes in superfine powdery or paste, obtains mixture predecessor.
Further, in step (ii) of the present invention, the flow of the air or nitrogen atmosphere is 15~30 ml/mins；
The average pore size of the target product is 4.1~14.2 nm；Specific surface area is 131~186 m2/g。
The method of the present invention can overcome the shortcomings of that the process of prior art is many and diverse, provide one by direct solid phase decomposition method
Kind is low in cost, and process is simple, easily operated, prepared convenient for the method for preparing mesoporous metal composite oxides of popularization
Target product pore size distribution range is wide.
The present invention is cheap and easy to get without basis materials, raw materials such as specific surfactants；Jie that this method is prepared
Mesoporous metal composite oxides have a large specific surface area, the features such as pore size distribution range is wide, can by adjusting metal salt and adjuvant,
Achieve the purpose that adjust nanoparticle aperture with conditions such as the chemical environments when thermally decomposed between different adjuvants.The material exists
The fields such as catalysis reaction, materials chemistry, environment absorption have a wide range of applications.
Present invention selection first grinds metal salt and adjuvant respectively, remixes and is ground to superfine powdery or paste, makes gold
Belong to salt and adjuvant sufficiently to react in the case where grinding environment with the free crystallization water, then divides two-step heating under air or nitrogen atmosphere
It decomposes, so that free water and volatile components is first volatilized evolution in 110~120 DEG C of temperature ranges, then in 450~850 DEG C of temperature
Resolving into remaining species in degree section, metal oxide is retained and gas escapes, and wherein air atmosphere facilitates decomposable process
In oxidizable component thermally decomposed, and nitrogen atmosphere can contribute to inhibit the thermal decomposition of oxidizable component, different points
Solution atmosphere helps to adjust the aperture of nanoparticle.Metal salt is also to influence from the proportion of the proportion of adjuvant, different adjuvants
One key factor in nanoparticle aperture.
Detailed description of the invention
The invention will be further described with specific embodiment with reference to the accompanying drawings of the specification.Protection scope of the present invention
It is not only limited to the statement of following content.
Fig. 1 is that meso-pore Ce CoO is prepared in the embodiment of the present invention 1, embodiment 2 and embodiment 3xXRD diagram.
Fig. 2 is that meso-pore Ce CoO is prepared in the embodiment of the present invention 4xSEM photograph.
Fig. 3 is that meso-pore Ce CoO is prepared in the embodiment of the present invention 5xTEM photo.
Fig. 4 is that meso-pore Ce MnO is prepared in the embodiment of the present invention 6 and embodiment 7xNitrogen adsorption desorption curve.
Fig. 5 is that meso-pore Ce MnO is prepared in the embodiment of the present invention 8xSEM photograph.
Fig. 6 is that meso-pore Ce MnO is prepared in the embodiment of the present invention 9xTEM photo.
Specific embodiment
Detailed description of the preferred embodiments below, and specific embodiment described herein is only limitted to solve
It releases and illustrates the present invention, be not intended to restrict the invention.
As shown, the preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture, it can be as follows
Implement:
(i) metal salt and adjuvant are weighed respectively, after being fully ground into powder, the two is uniformly mixed, then grind 30~60 points
Clock is in superfine powdery or paste, obtains mixture predecessor；The metal salt is nitrate or oxalates；The nitrate is nitre
Sour cerium；The oxalates is cerium oxalate；The adjuvant is the mixed of one or more of glucose, citric acid, starch
Close object；The molar ratio of the metal salt and adjuvant is 1:0.5~4；
(ii) it is placed in high temperature furnace in crucible by mixture predecessor is evenly laid out, under air or nitrogen atmosphere, with 1
DEG C/min heating rate, be heated to 110~120 DEG C and kept for 100~200 minutes, then with 1 DEG C/min of heating rate
Continue to be heated to 450~850 DEG C, and kept for 200~250 minutes, head product is obtained after natural cooling；The air or nitrogen
The flow of atmosphere is 15~30 ml/mins；The average pore size of the target product is 4.1~14.2 nm；Specific surface area is
131~186 m2/g；
(iii) head product deionized water and dehydrated alcohol are washed three times respectively, dry 100 minutes in 60 DEG C of baking ovens, i.e.,
Obtain target product.
Embodiment 1
First cerous nitrate, cobalt nitrate, citric acid are ground to fine-powdered respectively, then are mixed in a certain ratio grinding 30 minutes
To superfine powdery predecessor, predecessor is uniformly layered in crucible, is put into tube type high-temperature furnace, the sky of 15 ml/mins is passed through
Gas is warming up to 120 DEG C with the heating rate of 1 DEG C/min and is kept for 100 minutes, then continues to heat up with the heating rate of 1 DEG C/min
To 450 DEG C and 200 min are kept, sample deionized water is taken out after natural cooling and dehydrated alcohol washs 3 times respectively, then set
It is dried 100 minutes in 60 DEG C of baking ovens, obtains meso-pore Ce CoO x Composite oxides nanoparticle, is denoted as A2.Specific surface area peace
Equal aperture is respectively 145 m2/ g and 9.0 nm.Cerous nitrate used in it, cobalt nitrate, citric acid molar ratio be followed successively by 1:1:
2。
Embodiment 2
Meso-pore Ce CoO is prepared according to the method for embodiment 1 x Composite oxide nano-material is denoted as A4, specific surface area peace
Equal aperture is respectively 163 m2/ g and 8.4 nm.The difference is that the molar ratio of cerous nitrate used, cobalt nitrate, citric acid is followed successively by
1:1:8；Calcination temperature is 500 DEG C.
Embodiment 3
Meso-pore Ce CoO is prepared according to the method for embodiment 1 x Composite oxide nano-material is denoted as A5, specific surface area peace
Equal aperture is respectively 150 m2/ g and 7.7 nm.The difference is that the calcination atmosphere selected is nitrogen.
Embodiment 4
Meso-pore Ce CoO is prepared according to the method for embodiment 2 x Composite oxide nano-material is denoted as A6, specific surface area peace
Equal aperture is respectively 165 m2/ g and 5.2 nm.The difference is that using cerous nitrate, cobalt nitrate, citric acid and glucose as raw material,
Molar ratio is followed successively by 1:1:1:1.
Embodiment 5
Meso-pore Ce CoO is prepared according to the method for embodiment 1 x Composite oxide nano-material is denoted as A9, specific surface area peace
Equal aperture is respectively 166 m2/ g and 4.9 nm.Unlike using cerium oxalate, cobalt oxalate, glucose as raw material, molar ratio according to
Secondary is 1:1:2；And calcination temperature is 850 DEG C.
Embodiment 6
Cerous nitrate, manganese nitrate, glucose are ground to fine-powdered respectively, then obtained by certain molar ratio mixed grinding 60 minutes
Predecessor is uniformly layered in crucible, is put into tube type high-temperature furnace, the air of 20 ml/mins is passed through, with 1 by paste predecessor
DEG C/heating rate of min is warming up to 120 DEG C and kept for 200 minutes, then be continuously heating to 850 with the heating rate of 1 DEG C/min
DEG C and keep 250 min, take out sample deionized water after natural cooling and dehydrated alcohol wash 3 times respectively, then be placed in 60 DEG C
It is dried 100 minutes in baking oven, obtains meso-pore Ce MnO x Composite oxides nanoparticle, is denoted as B2.Specific surface area and average pore size
Respectively 149 m2/ g and 11.2 nm.Cerous nitrate used in it, manganese nitrate, glucose molar ratio be followed successively by 1:1:2.
Embodiment 7
Meso-pore Ce MnO is prepared according to the method for embodiment 6 x Composite oxide nano-material is denoted as B4, specific surface area peace
Equal aperture is respectively 171 m2/ g and 6.1 nm.The difference is that the molar ratio of cerous nitrate used, manganese nitrate, glucose is followed successively by
1:1:8, calcination temperature used are 550 DEG C.
Embodiment 8
Meso-pore Ce MnO is prepared according to the method for embodiment 6 x Composite oxide nano-material is denoted as B6, specific surface area peace
Equal aperture is respectively 139 m2/ g and 9.6 nm.The difference is that the molar ratio of cerous nitrate used, manganese nitrate, glucose is followed successively by
1:1:4, the nitrogen atmosphere that calcination condition used is 600 DEG C.
Embodiment 9
Meso-pore Ce MnO is prepared according to the method for embodiment 6 x Composite oxide nano-material is denoted as B8, specific surface area peace
Equal aperture is respectively 131 m2/ g and 14.2 nm.The difference is that raw material used is mole of cerium oxalate, manganese oxalate, glucose
Than being followed successively by 1:1:4, the air atmosphere that calcination condition used is 850 DEG C.
The main experimental conditions and result of 1 embodiment of table.
The above is only presently preferred embodiments of the present invention, not does limitation in any form to the present invention, it is all according to
According to any simple modification to the above embodiments in technical spirit of the invention, equivalent variations, guarantor of the invention is each fallen within
Within the scope of shield.
Claims (10)
1. a kind of preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture, which is characterized in that by following step
It is rapid to implement:
(i) metal salt and adjuvant are weighed respectively, after grinding, the two is uniformly mixed, then grinds, obtains mixture predecessor；
(ii) by step, (i) the mixture predecessor is placed in high temperature furnace, and under air or nitrogen atmosphere, temperature programming adds
Heat, then temperature programming continue to heat, and after natural cooling, obtain head product；
(iii) by step, (ii) the head product is washed, and is dried to get target product.
2. the preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture according to claim 1, special
Sign is: in step (i), the metal salt is nitrate or oxalates.
3. the preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture according to claim 2, special
Sign is: the nitrate is the mixture of one or more of cerous nitrate, cobalt nitrate and manganese nitrate；The oxalates
For the mixture of one or more of cerium oxalate, cobalt oxalate and manganese oxalate.
4. the preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture according to claim 3, special
Sign is: the nitrate is cerous nitrate；The oxalates is cerium oxalate.
5. the preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture according to claim 3, special
Sign is: in step (i), the adjuvant is the mixture of one or more of glucose, citric acid, starch.
6. the preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture according to claim 5, special
Sign is: in step (i), the molar ratio of the metal salt and adjuvant is 1: 0.5~4.
7. the preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture according to claim 6, special
Sign is: in step (ii), is placed in high temperature furnace in crucible by mixture predecessor is evenly laid out, in air or nitrogen gas
Under atmosphere, with 1 DEG C/min of heating rate, it is heated to 110~120 DEG C and is kept for 100~200 minutes, then with 1 DEG C/min
Heating rate continue to be heated to 450~850 DEG C, and kept for 200~250 minutes, head product obtained after natural cooling.
8. the preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture according to claim 7, special
Sign is: in step (iii), head product deionized water and dehydrated alcohol being washed three times respectively, dried in 60 DEG C of baking ovens
100 minutes to get target product.
9. the preparation side of any adjustable mesoporous metal composite oxide nano-material in aperture according to claim 1~8
Method, it is characterised in that: in step (i), weigh metal salt and adjuvant respectively, after being fully ground into powder, the two is mixed equal
It is even, then 30~60 minutes are ground in superfine powdery or paste, obtain mixture predecessor.
10. the preparation method of the adjustable mesoporous metal composite oxide nano-material in aperture according to claim 9, special
Sign is: in step (ii), the flow of the air or nitrogen atmosphere is 15~30 ml/mins；The target product is put down
Equal aperture is 4.1~14.2 nm；Specific surface area is 131~186 m2/g。
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| CN114177901A (en) * | 2020-09-14 | 2022-03-15 | 四川大学 | Preparation method of mesoporous metal oxide catalytic material |
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Application publication date: 20190308 |