CN106064829B - A kind of preparation method of the flower-shaped magnesia of carrying tin oxide - Google Patents
A kind of preparation method of the flower-shaped magnesia of carrying tin oxide Download PDFInfo
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- CN106064829B CN106064829B CN201610399685.0A CN201610399685A CN106064829B CN 106064829 B CN106064829 B CN 106064829B CN 201610399685 A CN201610399685 A CN 201610399685A CN 106064829 B CN106064829 B CN 106064829B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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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
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
- C01P2004/88—Thick layer coatings
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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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Abstract
A kind of preparation method of the flower-shaped magnesia of carrying tin oxide, comprises the following steps：According to the preparation amount and its stoichiometric proportion of the flower-shaped magnesia of carrying tin oxide, prepare appropriate flower-shaped magnesium hydroxide template, and prepare the tin-salt solution that the concentration of proper volume is 0.01 ~ 0.2 mol/L and pH value is 5 ~ 7, then the flower-shaped magnesium hydroxide of preparation is added in the tin-salt solution prepared, under the conditions of 10 ~ 90 DEG C, stirring 20 ~ 120 minutes, filtering, washing, at 60 ~ 100 DEG C, dry 60 ~ 240 minutes, finally by desciccate at 400 ~ 1000 DEG C, calcine 30 ~ 240 minutes, produce final product.Generated time of the present invention is short, implements simply, with low cost, and product has high-specific surface area, the three-dimensional flower-shaped structure of the nanometer sheet composition of high porosity, and particularly load oxide particle energy is uniform, firm, be controllably attached on flower-shaped bitter earth nano piece.
Description
The applying date of divisional application original application：2015-09-17, application number：201510592272X
Invention and created name：A kind of preparation method of the flower-shaped magnesia of carrying transition metal oxide.
Technical field
The invention belongs to the preparation field of loaded nano oxide material.
Background technology
In recent years, it is a focus of materials synthesis by self assembly multidimensional structure material, pattern control is current
One key issue of functional material synthesis.Flower-like structure has high-specific surface area, good light absorbs and refractive index, and multistage
The micro-flowers of structure, because it integrates nano particle, three kinds of structures of nanometer sheet and micro-flowers so that its in write head, receive
There is good application prospect in the fields such as meter Cui Hua, biology sensor, nanosecond medical science.Support type multidimensional structure metal oxide（Such as
Core shell structure oxide）Because having many unique physics and chemical characteristic, in super-hydrophobic surface coating, material, chemistry, magnetic
The fields such as, electricity, optics, biomedicine all have potential application value, are particularly opened in the research of catalyst new material
Originating party face has been obtained for the great attention of domestic and international relevant technical worker.Although the support type flower including core shell structure
Shape magnesia is expected have important application in terms of catalysis, biology sensor, battery electrode material, but has no oxidation at present
The report of the flower-shaped magnesium oxide material synthesis of tin cladding.
Preparing the topmost method of Core-shell structure material at present has sol-gal process and homogeneous precipitation method.Both approaches exist
Preparing Core-shell structure material has equipment simple, the features such as product homogeneity is good.Can not be complete in preparation process but can not solve
Full cladding causes cladding not fine and close, has the problems such as part is not coated up as the particle of shell, there is poor controllability, limits
Its application.The present invention based on spontaneous precipitation convert from template is sacrificed, not only have that solution system method has concurrently sets
It is standby simple, the advantage such as product homogeneity is good；And the magnesium hydroxide template that the present invention is used is without surface-functionalized, in nucleocapsid knot
During being configured to, partly consume, the release magnesium ion hydroxide ion into required with hull shape, due to hydrogen-oxygen near template
Radical ion is high so that transition metal ions is preferentially completely deposited at the surface of template, and template pattern is kept well, is overcome molten
The deficiency of sol-gel and homogeneous precipitation method, can efficiently control the thickness of shell, form the close shell caused, be a kind of letter
New method and approach single, that efficiently, fast prepare Core-shell structure material, with important application value.
The content of the invention
It is an object of the invention to provide a kind of simple, flower-shaped magnesia that is efficiently, fast preparing carrying tin oxide system
Preparation Method.
The present invention is achieved by the following technical solutions.
Preparation method of the present invention, comprises the following steps.
（1）According to the preparation amount and its stoichiometric proportion of the flower-shaped magnesia of carrying tin oxide, the magnesium of respective quality is weighed
Salt is dissolved in the magnesium salt solution that 2mol/L is obtained in deionized water, under the conditions of 20 ~ 60 DEG C, side stirring, while toward in magnesium salt solution
The ammoniacal liquor that mass concentration is 30% is added dropwise, when solution ph is 10.5, that is, stops that ammoniacal liquor and stirring, obtained suspension is added dropwise
It is aged 30 ~ 120 minutes at room temperature, after filtering, washing, drying, produces the flower-shaped magnesium hydroxide as template.
（2）According to the stoichiometric proportion of the preparation amount of flower-shaped magnesia of carrying tin oxide and its tin of load and magnesium, claim
The pink salt of respective amount is taken, the solution that concentration is 0.01 ~ 0.2 mol/L and pH value is 5 ~ 7 is configured to.
（3）By step（1）The flower-shaped magnesium hydroxide prepared adds step（2）In the solution of preparation, in 10 ~ 90 DEG C of conditions
Under, stir 20 ~ 120 minutes, filtering, washing then at 60 ~ 100 DEG C, are dried 60 ~ 240 minutes.
（4）By step（3）Obtained product is calcined 30 ~ 240 minutes at 400 ~ 1000 DEG C, produces final product.
Step of the present invention（1）Described in magnesium salts be one or more in magnesium sulfate, magnesium nitrate or magnesium chloride.
Step of the present invention（2）Described in pink salt be tin nitrate, chlorate and sulfate in one kind or many
Kind.
The flower-shaped method of magnesium oxide that the present invention prepares carrying tin oxide is that flower-shaped magnesium hydroxide is added into load pink salt
In solution, spontaneous precipitation conversion reaction occurs for stirring at a proper temperature, after being filtered, washed and dried, and obtains surface and bears
The flower-shaped magnesium hydroxide presoma of stannic hydroxide has been carried, after being heat-treated at a proper temperature, has just obtained loading oxide
Flower-shaped magnesia.This method generated time is short, it is simple, with low cost to implement, be easy to industrialization, and load oxide particle is completely firm
Admittedly be attached on flower-shaped bitter earth nano piece that dispersiveness is uniform, thickness is controllable, overcome homogeneous precipitation method and sol-sol method
Prepare the scattered problem for leading to not control the thickness of shell in the solution of the particle considerable part to be coated during core shell structure particle.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of magnesium hydroxide obtained by embodiment 1, as illustrated, magnesium hydroxide has micro-meter scale
Flower-like nanostructure.
Fig. 2 is prepared by the analysis shows of XRD spectrum in the X-ray diffractogram of flower-shaped magnesium hydroxide obtained by embodiment 1, figure
Obtained flower-like nanometer material is magnesium hydroxide, and its JCPDF card number is 07-0239.
Fig. 3 is the scanning electron microscope (SEM) photograph of the magnesia of carrying tin oxide obtained by embodiment 1, as illustrated, carrying tin oxide
Magnesia there is flower-like nanostructure, periphery has no any small particles, and tin oxide nano crystal grain is adhering completely to flower-shaped oxidation
Magnesium surface.
Fig. 4 is XRD spectrum in the X-ray diffractogram of the magnesia of carrying tin oxide obtained by embodiment 1, figure
On there is the feature diffraction that JCPDF card numbers are 65-0476 magnesia and JCPDF card numbers are 41-1445 tin oxide
Peak, the characteristic diffraction peak for any composite oxides do not occur shows that tin oxide nano crystal grain is attached on flower-shaped magnesia.
Embodiment
The present invention will be described further by following examples.
Embodiment 1.
4.8144g anhydrous magnesium sulfates accurately are weighed, the solution that 2mol/L is configured in 20ml deionized waters are dissolved in, then
While stirring, while toward dropwise addition mass concentration 30% in magnesium salt solution, when solution ph is 10.5, that is, stopping that ammoniacal liquor is added dropwise
And stirring, obtained suspension obtains white precipitate after being aged 120 minutes at room temperature, to white precipitate filtering, washing, 75
Obtain being used as the flower-shaped magnesium hydroxide of template after drying 180 minutes at DEG C；The 2.6050g butters of tin accurately weighed are stirred molten
In 200ml deionized waters and regulate and control pH value for 5, then flower-shaped magnesium hydroxide prepared above added in butter of tin solution,
At room temperature stirring 60min after, filtering, washing, at 75 DEG C dry 150 minutes after, then 800 DEG C be incubated 150 minutes, born
The flower-shaped magnesia of tin oxide is carried, its specific surface area is 73m2/g。
Claims (3)
1. the preparation method of the flower-shaped magnesia of a kind of carrying tin oxide, it is characterized in that comprising the following steps：
（1）According to the preparation amount and its stoichiometric proportion of the flower-shaped magnesia of carrying tin oxide, the magnesium salts for weighing respective quality is molten
Solution obtains 2mol/L magnesium salt solution in deionized water, under the conditions of 20 ~ 60 DEG C, side stirring, while being added dropwise toward in magnesium salt solution
Mass concentration is 30% ammoniacal liquor, when solution ph is 10.5, that is, stops that ammoniacal liquor and stirring is added dropwise, obtained suspension is in room
The lower ageing of temperature 30 ~ 120 minutes, filtering, washing, dry after, produce the flower-shaped magnesium hydroxide as template；
（2）According to the stoichiometric proportion of the preparation amount of flower-shaped magnesia of carrying tin oxide and its tin of load and magnesium, phase is weighed
The pink salt that should be measured, is configured to the solution that concentration is 0.01 ~ 0.2 mol/L and pH value is 5 ~ 7；
（3）By step（1）The flower-shaped magnesium hydroxide prepared adds step（2）In the solution of preparation, under the conditions of 10 ~ 90 DEG C, stir
Mix 20 ~ 120 minutes, filtering, washing then at 60 ~ 100 DEG C, are dried 60 ~ 240 minutes；
（4）By step（3）Obtained product is calcined 30 ~ 240 minutes at 400 ~ 1000 DEG C, produces final product.
2. preparation method according to claim 1, it is characterized in that step（1）Described in magnesium salts be magnesium sulfate, magnesium nitrate
Or the one or more in magnesium chloride.
3. preparation method according to claim 1, it is characterized in that step（2）Described in pink salt be the nitrate of tin, chlorine
One or more in salt dissolving and sulfate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610399685.0A CN106064829B (en) | 2015-09-17 | 2015-09-17 | A kind of preparation method of the flower-shaped magnesia of carrying tin oxide |
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| CN201610399685.0A CN106064829B (en) | 2015-09-17 | 2015-09-17 | A kind of preparation method of the flower-shaped magnesia of carrying tin oxide |
| CN201510592272.XA CN105197967B (en) | 2015-09-17 | 2015-09-17 | A kind of preparation method of the flower-shaped magnesium oxide of carrying transition metal oxide |
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| CN201510592272.XA Division CN105197967B (en) | 2015-09-17 | 2015-09-17 | A kind of preparation method of the flower-shaped magnesium oxide of carrying transition metal oxide |
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| CN106757247A (en) * | 2016-12-02 | 2017-05-31 | 北京工业大学 | A kind of method of the immobilized flower-shaped magnesium hydroxide of Nano tube array of titanium dioxide |
| CN108314067B (en) * | 2018-04-11 | 2019-12-20 | 南昌大学 | Preparation method of magnesium oxide nanorod |
| CN111392780B (en) * | 2020-03-26 | 2023-04-25 | 陈宛莎 | Composite oxide nano particle capable of emitting THz frequency and preparation method thereof |
| CN113697832B (en) * | 2021-09-16 | 2023-07-14 | 安徽建筑大学 | Preparation method of basic magnesium carbonate nanosheet-loaded activated carbon sponge |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103803593A (en) * | 2012-11-15 | 2014-05-21 | 朱振明 | Preparation method of flower-like magnesium oxide |
| CN103922368A (en) * | 2014-04-23 | 2014-07-16 | 中北大学 | Preparation method of nano-sheet-based flower-shaped level substructure magnesium hydroxide powder body |
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| JPH0788271B2 (en) * | 1988-03-14 | 1995-09-27 | 松下電器産業株式会社 | Method of manufacturing oxide thin film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103803593A (en) * | 2012-11-15 | 2014-05-21 | 朱振明 | Preparation method of flower-like magnesium oxide |
| CN103922368A (en) * | 2014-04-23 | 2014-07-16 | 中北大学 | Preparation method of nano-sheet-based flower-shaped level substructure magnesium hydroxide powder body |
Non-Patent Citations (1)
| Title |
|---|
| 高活性MgO/SnO2复合金属氧化物催化剂的合成及其在双氧水选择氧化环己酮制ε-己内酯反应中的应用;李静霞 等;《化学学报》;20081231;第66卷(第1期);5-9 * |
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| CN105197967A (en) | 2015-12-30 |
| CN106064829A (en) | 2016-11-02 |
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