CN107572573A - A kind of preparation method of the nano ceric oxide particle of polyhedral structure - Google Patents
A kind of preparation method of the nano ceric oxide particle of polyhedral structure Download PDFInfo
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- CN107572573A CN107572573A CN201711013466.5A CN201711013466A CN107572573A CN 107572573 A CN107572573 A CN 107572573A CN 201711013466 A CN201711013466 A CN 201711013466A CN 107572573 A CN107572573 A CN 107572573A
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Abstract
The invention discloses a kind of preparation method of the nano ceric oxide particle of polyhedral structure, comprise the following steps:1)By Ce2(CO3)3·xH2O is pre-processed, and its particle diameter is less than 20 μm, is obtained A product;2)LiCl and KCl are taken, grinds and crushes after being well mixed, is sufficiently mixed it fragment heating, obtains B product;3)It is put into after A product and B product are mixed in reaction vessel, 320 350 DEG C is heated under normal pressure, atmospheric environment, is preheated 13 hours, temperature is then increased to 370 700 DEG C again, be incubated at least 3 hours, obtain C product;4)C product are cooled to after room temperature and is cleaned and is filtered with water, filtrate is dried, obtain the nano ceric oxide particle of polyhedral structure.The present invention had both had the characteristics of industrial production difficulty is small, and synthetic quantity is big, and operating procedure is simply controllable, and production cost is low, had the characteristics of green, to meet social development demand again.
Description
Technical field
The present invention relates to a kind of preparation method of nano ceric oxide particle, the nanometer two of particularly a kind of polyhedral structure
The preparation method of cerium oxide particle.
Background technology
Ceria is due to excellent redox ability, being widely used as using in functional material, titanium dioxide
Cerium has obtained widely using in fields such as catalytic industries, polishing industry, energy conversions.The eighties in last century, ceria quilt
For preparing the three-way catalyst (Three Way Catalysis (TWCs)) of purifying vehicle exhaust, turn into rare earth material at that time
One of widest application.In addition, early in the sixties in last century, ceria just instead of the materials such as ferriferous oxide as polishing
Agent, the chemically mechanical polishing to optical element and the chemical-mechanical planarization to semiconductor wafer.With development in science and technology, the energy
Utilization also as one of new application of ceria, such as changing dielectric material of the solar energy into fuel, conduct
Electrolyte of Solid-state fuel cell etc..
And it is well known that the nano-structured performance to material of material has extraordinary facilitation.Nano material, i.e.,
The material that size is 0.1-100 nm nanometers is often referred to, has that specific surface area is big, the advantages that active sites are more, can effectively strengthening material
The physical and chemical performance of material.And CeO2Nano-structured enable the shape that Lacking oxygen is more prone in ceria lattice
Into can also strengthen redox ability, electric charge/electronic conduction ability and specific surface area of ceria etc..Therefore, people is studied
Substantial amounts of research work has been carried out in synthesis and preparation of the member for nano ceric oxide.
The ceria of nanostructured mainly includes, one-dimensional nano ceric oxide, nano ceric oxide film and receives
Rice cerium oxide particles, nano ceric oxide particle is then to apply most nanostructured cerias at present.Prepare nanometer two
Method, the technology of cerium oxide particle have many, such as conventional means such as hydro-thermal Hydrolyze method, coprecipitation, gel method, combustion methods.Its
Middle most of method carries out the synthesis of nano ceric oxide using wet method, but is that synthesis is complicated the problem of wet method, control strip
Part is more, and cost is higher, and synthetic quantity is relatively low, causes the cost of nano ceric oxide higher.And combustion method, compare surface although can prepare
The larger nano ceric oxide particle of product and also have preferably to produce in enormous quantities and prepare potentiality, but it is uncontrollable due to process
Property processed, limit its further application.In the application industry of nano ceric oxide industry nanometer two is prepared to inexpensive, simple
The technology of cerium oxide is expected for a long time.
Meanwhile with social economy, the development of technology, the problem of people are to environmental protection growing interest, such as greenhouse effects, energy-conservation
The problem of environmental protection is paid close attention to jointly as the whole mankind.And the pollutant of current technique discharge is more serious, environment can be caused
Larger destruction, it is impossible to meet the needs of social development.
The content of the invention
It is an object of the present invention to provide a kind of preparation method of the nano ceric oxide particle of polyhedral structure.This hair
It is bright that both there is the characteristics of industrial production difficulty is small, and synthetic quantity is big, and operating procedure is simply controllable, and production cost is low, there is green again
Environmental protection, the characteristics of social development demand can be met.
Technical scheme:A kind of preparation method of the nano ceric oxide particle of polyhedral structure, including it is as follows
Step:
1)By Ce2(CO3)3·xH2O is pre-processed, and its particle diameter is less than 20 μm, is obtained A product;
2)LiCl and KCl are taken, grinds and crushes after being well mixed, is sufficiently mixed it fragment heating, obtains B product;
3)It is put into after A product and B product are mixed in reaction vessel, 320-350 DEG C is heated under normal pressure, atmospheric environment, preheating
1-3 hours, temperature is then increased to 370-700 DEG C again, is incubated at least 3 hours, obtains C product;
4)C product are cooled to after room temperature and is cleaned and is filtered with water, filtrate is dried, obtain the nanometer of polyhedral structure
Cerium oxide particles.
The preparation method of the nano ceric oxide particle of foregoing polyhedral structure, the step 1)In, pretreatment be by
Ce2(CO3)3·xH2Heated after O grindings at 100-140 DEG C at least 12 hours.
The preparation method of the nano ceric oxide particle of foregoing polyhedral structure, the step 2)In, LiCl and KCl's
Mixing mol ratio is 0.66-0.72.
The preparation method of the nano ceric oxide particle of foregoing polyhedral structure, the step 2)In, fragment heating
Temperature is 350-360 DEG C, and the heat time is 0.5-1 hours.
The preparation method of the nano ceric oxide particle of foregoing polyhedral structure, the step 3)In, A product and B product
Mix mol ratio and be less than 1.
The preparation method of the nano ceric oxide particle of foregoing polyhedral structure, the mixing mol ratio of the A product and B product
For 0.2-0.3.
The preparation method of the nano ceric oxide particle of foregoing polyhedral structure, the step 3)In, A product mix with B product
After closing preheating, temperature is increased to 550-650 DEG C, is incubated 3-5 hours.
The preparation method of the nano ceric oxide particle of foregoing polyhedral structure, the step 4)In, nanometer titanium dioxide
The particle diameter of cerium particle is less than 80nm.
The preparation method of the nano ceric oxide particle of foregoing polyhedral structure, the step 4)In drying be by mistake
Screening dries 4-6 hours at 80-120 DEG C.
The preparation method of the nano ceric oxide particle of foregoing polyhedral structure, by the step 4)Obtained by middle filtering
Filtrate is distilled, and obtains LiCl-KCl crystallizations and distilled water, and LiCl-KCl crystallizes the conjunction for continuing on for nano ceric oxide
Into distilled water is used for the cleaning of C product.
Beneficial effects of the present invention
1st, simple production process of the present invention, preparation temperature is low, it is workable, can largely be produced, there is preferably industry
Productive potentialities, there is preferable replicability., can be to nanometer titanium dioxide such as because process of the present invention control, preparation technology are simple
Cerium carries out large batch of production and preparation, can by the synthetic quantity of current synthesis technique by current kg/day improve to several tons/
My god, there is extraordinary application prospect.
2nd, the present invention is by using reaction vessel, and is reacted under normal pressure, atmospheric environment, avoids using autoclave, reactor
Etc. a series of restrictive condition, the complexity of production is greatly reduced, operation is simpler, meanwhile, synthesis cycle is short, synthesis
The step of it is few, can effectively reduce the cost of nano ceric oxide particle.Prime cost such as the present invention is presoma cost, added
Thermal energy consumption and fused salt distillation energy consumption, compared to current synthesis technique, do not produce the consumption of other synthesis materials, effectively reduce and be produced into
This.
3rd, the band gap of the nano ceric oxide with polyhedral structure prepared by the present invention is 2.7 eV, more current city
The 3.2eV of business nano ceric oxide have it is larger narrow, be advantageous to its photoelectric field application.
4th, KCl-LiCl used in the present invention can be recycled, and distilled water can also reuse, and process does not produce waste liquid
Deng pollutant, there is good environment protecting, be fully able to meet social development to environmentally friendly proposed requirement.
Experimental example
Nano ceric oxide and present analysis prepared by the present invention carries out UV-Visible absorption with nano ceric oxide reagent
The contrast of spectrum, as shown in Figure 3, it is seen then that the longer spectrum of the energy absorbing wavelength of nano ceric oxide prepared by the present invention, it is right
The photocatalytic application of nano ceric oxide has facilitation.
Brief description of the drawings
XRD the and TEM collection of illustrative plates for the nano ceric oxide that accompanying drawing 1 is prepared for the present invention;
The TEM secondary electron images for the nano ceric oxide that accompanying drawing 2 is prepared for the present invention;
The nano ceric oxide and existing nano ceric oxide at present on the market that accompanying drawing 3 is prepared for the present invention are to ultraviolet-visible light
The comparison diagram of absorption spectrum.
The particle diameter that nano ceric oxide prepared by the present invention is can be seen that from Fig. 1 and Fig. 2 is about 30nm.
From figure 3, it can be seen that the band gap of the nano ceric oxide with polyhedral structure prepared by the present invention is
2.7 eV, compared with existing market business nano ceric oxide 3.2eV have it is larger narrow, be advantageous to its photoelectric field application.
Embodiment
With reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
Embodiments of the invention
Embodiment 1:A kind of preparation method of the nano ceric oxide particle of polyhedral structure, step are as follows:
1)By Ce2(CO3)3·xH2Its particle diameter is less than 20 μm after O grindings, heated 12 hours at 120 DEG C, obtain A product;
2)Take LiCl and KCl, in molar ratio 0.69 it is well mixed after grind it is broken, fragment is sufficiently mixed and at 353 DEG C plus
Heat is 0.8 hour, obtains B product;
3)It will be put into after A product and B product in molar ratio 0.25 mixing in reaction vessel, 340 be heated under normal pressure, atmospheric environment
DEG C, preheat 2 hours, temperature is then increased to 600 DEG C again, be incubated 4 hours, obtain C product;
4)C product are cooled to after room temperature and is cleaned and is filtered with water, filtrate is dried 5 hours at 100 DEG C, particle diameter is obtained and is less than
The nano ceric oxide particle of 80nm polyhedral structure;
5)Step 4)Filtrate obtained by middle filtering is distilled, and obtains LiCl-KCl crystallizations and distilled water, LiCl-KCl crystallizations
Continue on for the synthesis of nano ceric oxide, distilled water is used for the cleaning of C product.
Embodiment 2:A kind of preparation method of the nano ceric oxide particle of polyhedral structure, step are as follows:
1)By Ce2(CO3)3·xH2Its particle diameter is less than 20 μm after O grindings, heated at 100 DEG C at least 15 hours, obtain A product;
2)Take LiCl and KCl, in molar ratio 0.66 it is well mixed after grind it is broken, fragment is sufficiently mixed and at 350 DEG C plus
Heat is 1 hour, obtains B product;
3)It will be put into after A product and B product in molar ratio 0.2 mixing in reaction vessel, 320 DEG C be heated under normal pressure, atmospheric environment,
Preheating 3 hours, temperature is then increased to 370 DEG C again, is incubated 5 hours, obtains C product;
4)C product are cooled to after room temperature and is cleaned and is filtered with water, filtrate is dried 6 hours at 80 DEG C, particle diameter is obtained and is less than
The nano ceric oxide particle of 80nm polyhedral structure;
5)Step 4)Filtrate obtained by middle filtering is distilled, and obtains LiCl-KCl crystallizations and distilled water, LiCl-KCl crystallizations
Continue on for the synthesis of nano ceric oxide, distilled water is used for the cleaning of C product.
Embodiment 3:A kind of preparation method of the nano ceric oxide particle of polyhedral structure, step are as follows:
1)By Ce2(CO3)3·xH2Its particle diameter is less than 20 μm after O grindings, heated 12 hours at 140 DEG C, obtain A product;
2)Take LiCl and KCl, in molar ratio 0.72 it is well mixed after grind it is broken, fragment is sufficiently mixed and at 360 DEG C plus
Heat is 0.5 hour, obtains B product;
3)It will be put into after A product and B product in molar ratio 0.3 mixing in reaction vessel, 350 DEG C be heated under normal pressure, atmospheric environment,
Preheating 1 hour, temperature is then increased to 700 DEG C again, is incubated 3 hours, obtains C product;
4)C product are cooled to after room temperature and is cleaned and is filtered with water, filtrate is dried 4 hours at 120 DEG C, particle diameter is obtained and is less than
The nano ceric oxide particle of 80nm polyhedral structure;
5)Step 4)Filtrate obtained by middle filtering is distilled, and obtains LiCl-KCl crystallizations and distilled water, LiCl-KCl crystallizations
Continue on for the synthesis of nano ceric oxide, distilled water is used for the cleaning of C product.
Embodiment 4:A kind of preparation method of the nano ceric oxide particle of polyhedral structure, step are as follows:
1)By Ce2(CO3)3·xH2O is ground to less than 20 μm, then 12 hours of drying and dewatering in 100 DEG C of drying box,
Then toasted 4 hours at 500 DEG C, obtain A product;
2)Grind broken after 11.16 gLiCl are mixed with 8.84 g KCl, fragment is then preheated 1 hour at 350 DEG C, so
Heated 2 hours at 500 DEG C afterwards, obtain B product;
3)B product and A product are pressed into A again:B=1:4 ratio mixing, mixture is put into alumina crucible, crucible is placed on Muffle furnace
In be warming up to 350 DEG C be incubated 1 hour, then heat to 500 DEG C be incubated 2 hours, obtain C product;
4)Power supply is then shut off, allows alumina crucible to be cooled to room temperature in Muffle furnace, C product are cleaned several times with deionized water,
Filtering, then the solid powder on filter paper is dried 4 hours in 100 DEG C of drying baker;
5)Remaining filtrate carries out distillation processing at 80 DEG C, obtains LiCl-KCl and distilled water.
Claims (10)
1. the preparation method of the nano ceric oxide particle of a kind of polyhedral structure, it is characterised in that comprise the following steps:
1)By Ce2(CO3)3·xH2O is pre-processed, and its particle diameter is less than 20 μm, is obtained A product;
2)LiCl and KCl are taken, grinds and crushes after being well mixed, is sufficiently mixed it fragment heating, obtains B product;
3)It is put into after A product and B product are mixed in reaction vessel, 320-350 DEG C is heated under normal pressure, atmospheric environment, preheating
1-3 hours, temperature is then increased to 370-700 DEG C again, is incubated at least 3 hours, obtains C product;
4)C product are cooled to after room temperature and is cleaned and is filtered with water, filtrate is dried, obtain the nanometer of polyhedral structure
Cerium oxide particles.
2. the preparation method of the nano ceric oxide particle of polyhedral structure as claimed in claim 1, it is characterised in that:It is described
Step 1)In, pretreatment is by Ce2(CO3)3·xH2Heated after O grindings at 100-140 DEG C at least 12 hours.
3. the preparation method of the nano ceric oxide particle of polyhedral structure as claimed in claim 1, it is characterised in that:It is described
Step 2)In, LiCl and KCl mixing mol ratio are 0.66-0.72.
4. the preparation method of the nano ceric oxide particle of polyhedral structure as claimed in claim 1, it is characterised in that:It is described
Step 2)In, fragment heating-up temperature is 350-360 DEG C, and the heat time is 0.5-1 hours.
5. the preparation method of the nano ceric oxide particle of polyhedral structure as claimed in claim 1, it is characterised in that:It is described
Step 3)In, the mixing mol ratio of A product and B product is less than 1.
6. the preparation method of the nano ceric oxide particle of polyhedral structure as claimed in claim 5, it is characterised in that:It is described
The mixing mol ratio of A product and B product is 0.2-0.3.
7. the preparation method of the nano ceric oxide particle of polyhedral structure as claimed in claim 1, it is characterised in that:It is described
Step 3)In, after A product mix preheating with B product, temperature is increased to 550-650 DEG C, is incubated 3-5 hours.
8. the preparation method of the nano ceric oxide particle of polyhedral structure as claimed in claim 1, it is characterised in that:It is described
Step 4)In, the particle diameter of nano ceric oxide particle is less than 80nm.
9. the preparation method of the nano ceric oxide particle of polyhedral structure as claimed in claim 1, it is characterised in that:It is described
Step 4)In drying be by filtrate 80-120 DEG C dry 4-6 hours.
10. the preparation method of the nano ceric oxide particle of polyhedral structure as claimed in claim 1, it is characterised in that:Will
The step 4)Filtrate obtained by middle filtering is distilled, obtain LiCl-KCl crystallization and distilled water, LiCl-KCl crystallization after
Continue the synthesis for nano ceric oxide, distilled water is used for the cleaning of C product.
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Cited By (3)
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CN111378386A (en) * | 2018-12-28 | 2020-07-07 | 安集微电子(上海)有限公司 | Application of cerium oxide abrasive in polishing of PI dielectric material |
CN113332976A (en) * | 2021-05-18 | 2021-09-03 | 贵州大学 | CeCO3OH nanosphere wrapped MnCO3Preparation method and application of microsphere composite material |
CN113769752A (en) * | 2021-09-23 | 2021-12-10 | 淮阴师范学院 | Preparation method of dodecahedron doped cerium dioxide composite photocatalyst |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111378386A (en) * | 2018-12-28 | 2020-07-07 | 安集微电子(上海)有限公司 | Application of cerium oxide abrasive in polishing of PI dielectric material |
CN111378386B (en) * | 2018-12-28 | 2022-04-01 | 安集微电子(上海)有限公司 | Application of cerium oxide abrasive in polishing of PI dielectric material |
CN113332976A (en) * | 2021-05-18 | 2021-09-03 | 贵州大学 | CeCO3OH nanosphere wrapped MnCO3Preparation method and application of microsphere composite material |
CN113332976B (en) * | 2021-05-18 | 2022-06-07 | 贵州大学 | CeCO3OH nanosphere wrapped MnCO3Preparation method and application of microsphere composite material |
CN113769752A (en) * | 2021-09-23 | 2021-12-10 | 淮阴师范学院 | Preparation method of dodecahedron doped cerium dioxide composite photocatalyst |
CN113769752B (en) * | 2021-09-23 | 2023-08-22 | 淮阴师范学院 | Preparation method of dodecahedron iron doped cerium dioxide composite photocatalyst |
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