CN108706623A - A kind of preparation method of cerium oxide nanoparticles - Google Patents
A kind of preparation method of cerium oxide nanoparticles Download PDFInfo
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- CN108706623A CN108706623A CN201810675446.2A CN201810675446A CN108706623A CN 108706623 A CN108706623 A CN 108706623A CN 201810675446 A CN201810675446 A CN 201810675446A CN 108706623 A CN108706623 A CN 108706623A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation methods of cerium oxide nanoparticles it is characterized in that, it includes the following steps：A. six nitric hydrate cerium solution, dilute alkaline soln are made respectively；B. six nitric hydrate cerium solution are added rapidly in dilute alkaline soln, are vigorously stirred at room temperature；Then this solution is transferred in stainless steel cauldron, 150~180 DEG C of baking oven is placed in and carries out hydro-thermal reactions 18~for 24 hours；C. it is cooled to room temperature, centrifuges, washing disperses 1h, dry 12h for several times, using ultrasonication machine；D. 3~4h is calcined, cerium oxide nanoparticles are obtained.The advantages that present invention has good crystallinity, and pattern is uniform, and good dispersion, grain size is easy to control, and preparation process is succinct can effectively solve the problems such as nano material preparation process is complicated, and environmental pollution is serious, and abundant residues waste.
Description
Technical field
The present invention relates to a kind of preparation methods of cerium oxide nanoparticles, belong to nano-oxide fabricating technology neck
Domain.
Background technology
The performance of nano material and the size of its nano material have it is critically important contact, the often nano material tool of small size
There are preferable physics and chemical property, therefore, the nano material for preparing small size has become the research heat of nm regime in recent years
Point.Wherein, cerium oxide nanoparticles are because it is with larger specific surface area and higher oxygen mobility, auto-emission control,
The fields such as catalyst carrier, coating material and electrode material are all widely used.
Six nitric hydrate ceriums are also referred to as cerous nitrate (III) hexahydrate, are the chemical substances that molecular weight is 434.22, combustion-supporting,
Has irritation, industrial goods are in blush, there is hygroscopy.The substance may be harmful to environment, there is cumulative effect in underground water.
It is the raw material for producing cerium salt as fan tail additive, petrochemical catalyst.It is used as analytical reagent in analytical chemistry,
For pharmaceuticals industry.
Currently, the method for preparing cerium oxide nanoparticles has very much, including reactive deposition method, sol-gel method, microemulsion
Method etc., but that there are still processes is complicated, environmental pollution is serious, material waste is serious in preparation process, system for most of preparation method
At the shortcomings of granule-morphology is inhomogenous, size disunity, therefore, find a kind of low cost, environmentally protective method prepares shape
Looks are uniform, good dispersion cerium oxide nanoparticles, just become a challenging job.In existing literature, it is not yet found that one
The preparation method of kind cerium oxide nanoparticles, when can solve to prepare cerium oxide nanoparticles, the particle size disunity of appearance,
The problem of pattern is inhomogenous and poor dispersion.
Invention content
The present invention be directed to particle size disunity, the pattern of the appearance of existing preparation method of nano material it is inhomogenous and
The deficiencies of poor dispersion, it is proposed that the preparation method of nano particle is prepared using hydro-thermal method, the nano particle prepared has
The advantages that good crystallinity, pattern is uniform, and good dispersion, grain size is easy to control, and preparation process is succinct.
In order to achieve the above objectives, technical solution provided by the invention is：
A kind of preparation method of cerium oxide nanoparticles, which is characterized in that it includes the following steps that (each component is according to weight
Measure part meter)：
A. it by 8~9 parts of six nitric hydrate ceriums, is dissolved in 35~45 parts of deionized waters, it is molten that six nitric hydrate ceriums is made
Liquid；It is dissolved in 3~3.5 parts of sodium hydroxides in 35~45 parts of deionized waters, dilute alkaline soln is made；
B. above-mentioned six nitric hydrates cerium solution is added rapidly in dilute alkaline soln, is vigorously stirred 30min at room temperature；Then
This solution is transferred in the stainless steel cauldron that 100ml has polytetrafluoroethyllining lining, is placed in 150~180 DEG C of progress water of baking oven
Thermal response 18~for 24 hours；
C. it waits for that temperature of reaction kettle is cooled to room temperature, centrifuges, washed for several times with water and absolute ethyl alcohol respectively, utilize ultrasonication
Machine disperses 1h, 60~80 DEG C of dry 12h；
D. powder obtained above is being warming up to 400~500 DEG C with the rate of 5~10 DEG C/min, is calcining 3~4h, obtains
To cerium oxide nanoparticles.
Further, the step a, specially：
It is dissolved in 8.5~8.8 parts of six nitric hydrate ceriums in 38~42 parts of deionized waters, six nitric hydrate ceriums are made
Solution；It is dissolved in 3.2~3.4 parts of sodium hydroxides in 38~42 parts of deionized waters, dilute alkaline soln is made.
Further, the step a, specially：
It is dissolved in 8.48 parts of six nitric hydrate ceriums in 40 parts of deionized waters, six nitric hydrate cerium solution are made；It will
3.2 parts of sodium hydroxides are dissolved in 40 parts of deionized waters, and dilute alkaline soln is made.
The preparation method of the cerium oxide nanoparticles, which is characterized in that the ultrasonication time is 20~60min.
The preparation method of cerium oxide nanoparticles provided by the invention, the core using hydro-thermal reaction as this method walk
Suddenly, compared with other methods, hydro-thermal method has many advantages, such as that good dispersion, grain size are easy to control, preparation process is succinct, and can effectively solve
The problems such as certainly nano material preparation process is complicated, and environmental pollution is serious, and abundant residues waste；And manufactured nano particle has knot
The features such as crystalline substance is good, pattern is uniform.
The method of the present invention makes cerium oxide nanoparticles using dilute alkaline soln and cerous nitrate precursor salt solution, in high temperature item
Hydro-thermal reaction is carried out under part, ultrasonication crusher machine is used in combination, and finally obtains that pattern is uniform, the cerium oxide nano of better crystallinity degree
Grain.Whole manufacturing cost is low, is easy to industrialization, and secondary pollution, the preparation of the cerium oxide nanoparticles will not be caused to environment
Method solves the problems, such as to prepare that particle size disunity, pattern in cerium oxide nanoparticles be inhomogenous and poor dispersion.
Description of the drawings
Fig. 1 is the SEM photograph of the cerium oxide nanoparticles obtained by the embodiment of the present invention.
Specific implementation mode
Specific embodiments of the present invention are described in detail below in conjunction with technical solution and attached drawing.
Embodiment 1
A kind of preparation method of cerium oxide nanoparticles provided in an embodiment of the present invention comprising following steps (each component
In parts by weight)：
A. it by 8~9 parts of six nitric hydrate ceriums, is dissolved in 35~45 parts of deionized waters, it is molten that six nitric hydrate ceriums is made
Liquid；It is dissolved in 3~3.5 parts of sodium hydroxides in 35~45 parts of deionized waters, dilute alkaline soln is made；
B. above-mentioned six nitric hydrates cerium solution is added rapidly in dilute alkaline soln, is vigorously stirred 30min at room temperature；Then
This solution is transferred in the stainless steel cauldron that 100ml has polytetrafluoroethyllining lining, is placed in 150~180 DEG C of progress water of baking oven
Thermal response 18~for 24 hours；
C. it waits for that temperature of reaction kettle is cooled to room temperature, centrifuges, washed for several times with water and absolute ethyl alcohol respectively, utilize ultrasonication
Machine disperses 1h, 60~80 DEG C of dry 12h；
D. powder obtained above is being warming up to 400~500 DEG C with the rate of 5~10 DEG C/min, is calcining 3~4h, obtains
To cerium oxide nanoparticles.
The ultrasonication time in the step c is 20~60min.
The amount of above-mentioned sodium hydroxide should not be excessive or very few, and amount wants moderate, otherwise so that the pattern of cerium oxide nanoparticles
It is inhomogenous, size is uncontrollable.
Above-mentioned hydrothermal temperature is unsuitable too low or excessively high, and reaction temperature can influence the crystallinity of cerium oxide nanoparticles.
Above-mentioned the hydro-thermal reaction time is unsuitable too short or long, the reaction time can influence cerium oxide nanoparticles crystallinity and
Nano-scale.
Above-mentioned hydro-thermal reaction must be washed to neutrality after being down to room temperature.The cerium oxide nanoparticles of different sizes,
Its physico-chemical property is different, and there are difference in terms of oxygen mobility.
Unsuitable long with the ultrasonic crusher machine time after above-mentioned centrifuge washing, broken overlong time can influence cerium oxide nano
The pattern of grain.
The above-mentioned calcination process heating rate being related to is 5~10 DEG C/min, and calcination temperature is 400~500 DEG C, calcining 3~
4h.Cerium oxide nanoparticles can be caused to reunite the broken of sintering and appearance structure as calcination temperature is excessively high or calcination time is long
It is bad.
Embodiment 2：
A kind of preparation method of cerium oxide nanoparticles provided in an embodiment of the present invention, it is substantially the same manner as Example 1,
The difference is that：
The step a, specially：
It is dissolved in 8.5~8.8 parts of six nitric hydrate ceriums in 38~42 parts of deionized waters, six nitric hydrate ceriums are made
Solution；It is dissolved in 3.2~3.4 parts of sodium hydroxides in 38~42 parts of deionized waters, dilute alkaline soln is made.
Embodiment 3：
The preparation method of a kind of cerium oxide nanoparticles provided in an embodiment of the present invention, with embodiment 1 and 2 basic phases
Together, the difference is that：
The step a, specially：
It is dissolved in 8.48 parts of six nitric hydrate ceriums in 40 parts of deionized waters, six nitric hydrate cerium solution are made；It will
3.2 parts of sodium hydroxides are dissolved in 40 parts of deionized waters, and dilute alkaline soln is made.
Embodiment 4：
A kind of preparation method of cerium oxide nanoparticles provided in an embodiment of the present invention, it is essentially identical with embodiment 1-3,
The difference is that：
It weighs six nitric hydrate ceriums of 0.848g and 0.32g NaOH is dissolved separately in 40ml deionized waters.Quickly stirring
Under, cerous nitrate solution is added rapidly in dilute alkaline soln, after being vigorously stirred 30min, is transferred in 100ml tool polytetrafluoroethylene (PTFE)
In the stainless steel cauldron of lining, 150 DEG C are placed in baking oven, reacts 18h.After being cooled to room temperature, water and anhydrous second are used in centrifugation respectively
Alcohol washs three times, 80 DEG C of dry 12h, and heating rate is 5 DEG C/min under air atmosphere, and 400 DEG C of calcining 3h obtain cerium oxide nano
Particle.
Embodiment 5
The preparation method of a kind of cerium oxide nanoparticles provided in an embodiment of the present invention, with the basic phases of embodiment 1-4
Together, the difference is that：
It weighs six nitric hydrate ceriums of 0.848g and 0.32g NaOH is dissolved separately in 40ml deionized waters.Quickly stirring
Under, cerous nitrate solution is added rapidly in dilute alkaline soln, after being vigorously stirred 30min, is transferred in 100ml tool polytetrafluoroethylene (PTFE)
In the stainless steel cauldron of lining, 170 DEG C are placed in baking oven, reacts 20h.After being cooled to room temperature, water and anhydrous second are used in centrifugation respectively
Alcohol washs three times, 80 DEG C of dry 12h, and heating rate is 5 DEG C/min under air atmosphere, and 400 DEG C of calcining 4h obtain cerium oxide nano
Particle.
A kind of preparation method of cerium oxide nanoparticles provided in an embodiment of the present invention of embodiment 6, with embodiment 1-5 bases
This is identical, the difference is that：
It weighs six nitric hydrate ceriums of 0.848g and 0.32g NaOH is dissolved separately in 40ml deionized waters.Quickly stirring
Under, cerous nitrate solution is added rapidly in dilute alkaline soln, after being vigorously stirred 30min, is transferred in 100ml tool polytetrafluoroethylene (PTFE)
In the stainless steel cauldron of lining, 180 DEG C are placed in baking oven, reaction is for 24 hours.After being cooled to room temperature, water and anhydrous second are used in centrifugation respectively
Alcohol washs three times, 80 DEG C of dry 12h, and heating rate is 10 DEG C/min under air atmosphere, and 400 DEG C of calcining 3h obtain cerium oxide and receive
Rice grain.
The preparation method of cerium oxide nanoparticles provided by the invention, this method have good crystallinity, and pattern is uniform, dispersion
Property good, the features such as grain size is easy to control, and preparation process is succinct, can effectively solve that nano material preparation process is complicated, and environmental pollution is tight
The problems such as weight, abundant residues waste.
The SEM photograph of cerium oxide nanoparticles obtained by 1 embodiment of the present invention of attached drawing is observed it is found that using the method for the present invention system
Standby cerium oxide nanoparticles, particle size is unified, pattern is uniform, and favorable dispersibility.
Above-described two embodiments, are only presently preferred embodiments of the present invention, not make any shape to the present invention
Limitation in formula.Any technical person familiar with the field, it is without departing from the scope of the technical proposal of the invention, all available
The methods and technical content of the disclosure above makes many possible changes and modifications to technical solution of the present invention, or is revised as equivalent
The equivalent embodiment of variation.Therefore every content without departing from technical solution of the present invention, shape, construction and principle according to the present invention
Made by equivalence changes, should all be covered by protection scope of the present invention.
Claims (4)
1. a kind of preparation method of cerium oxide nanoparticles, which is characterized in that it includes the following steps that (each component is according to parts by weight
Meter)：
A. it by 8~9 parts of six nitric hydrate ceriums, is dissolved in 35~45 parts of deionized waters, six nitric hydrate cerium solution is made；It will
3~3.5 parts of sodium hydroxides are dissolved in 35~45 parts of deionized waters, and dilute alkaline soln is made；
B. above-mentioned six nitric hydrates cerium solution is added rapidly in dilute alkaline soln, is vigorously stirred 30min at room temperature；Then by this
Solution is transferred in the stainless steel cauldron of 100ml tool polytetrafluoroethyllining linings, and it is anti-to be placed in 150~180 DEG C of progress hydro-thermals of baking oven
Answer 18~for 24 hours；
C. it waits for that temperature of reaction kettle is cooled to room temperature, centrifuges, washed for several times with water and absolute ethyl alcohol respectively, utilize ultrasonication machine point
Dissipate 1h, 60~80 DEG C of dry 12h；
D. powder obtained above is being warming up to 400~500 DEG C with the rate of 5~10 DEG C/min, is calcining 3~4h, obtains oxygen
Change cerium nano particle.
2. according to the preparation method of cerium oxide nanoparticles described in claim 1, which is characterized in that the step a, specifically
For：
It is dissolved in 8.5~8.8 parts of six nitric hydrate ceriums in 38~42 parts of deionized waters, six nitric hydrate cerium solution are made；
It is dissolved in 3.2~3.4 parts of sodium hydroxides in 38~42 parts of deionized waters, dilute alkaline soln is made.
3. according to the preparation method of cerium oxide nanoparticles described in claim 1, which is characterized in that the step a, specifically
For：
It is dissolved in 8.48 parts of six nitric hydrate ceriums in 40 parts of deionized waters, six nitric hydrate cerium solution are made；By 3.2 parts
Sodium hydroxide is dissolved in 40 parts of deionized waters, and dilute alkaline soln is made.
4. according to the preparation method of one of claims 1 to 3 cerium oxide nanoparticles, which is characterized in that the ultrasound is broken
The broken time is 20~60min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109999810A (en) * | 2019-04-10 | 2019-07-12 | 天津理工大学 | Using spherical nanometer alpha-ferric oxide as the preparation method of the catalyst for phenylethylene dehydrogenation of source of iron |
| CN115353639A (en) * | 2022-07-12 | 2022-11-18 | 昆明理工大学 | Method for preparing potassium humate by using corn straws and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109999810A (en) * | 2019-04-10 | 2019-07-12 | 天津理工大学 | Using spherical nanometer alpha-ferric oxide as the preparation method of the catalyst for phenylethylene dehydrogenation of source of iron |
| CN109999810B (en) * | 2019-04-10 | 2022-05-03 | 天津理工大学 | Preparation method of ethylbenzene dehydrogenation catalyst by taking spherical nano alpha-iron oxide as iron source |
| CN115353639A (en) * | 2022-07-12 | 2022-11-18 | 昆明理工大学 | Method for preparing potassium humate by using corn straws and application |
| CN115353639B (en) * | 2022-07-12 | 2023-08-08 | 昆明理工大学 | Method for preparing potassium humate by using corn straw and application |
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Application publication date: 20181026 |