CN102020306A - Microwave rapid synthetic method of nanometer cerium oxide - Google Patents
Microwave rapid synthetic method of nanometer cerium oxide Download PDFInfo
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- CN102020306A CN102020306A CN2010105997102A CN201010599710A CN102020306A CN 102020306 A CN102020306 A CN 102020306A CN 2010105997102 A CN2010105997102 A CN 2010105997102A CN 201010599710 A CN201010599710 A CN 201010599710A CN 102020306 A CN102020306 A CN 102020306A
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Abstract
The invention provides a microwave rapid synthetic method of nanometer cerium oxide, which is characterized in that a household microwave oven with continuous adjustable power is taken as a heat source, a simple microwave assistance refluxing method is adopted, water is taken as a solvent, organic amine is as an alkali source, and nanometer cerium oxide is rapidly synthesized by triethylenetetramine, tetraethylenepentamine, diethanolamine and ethanolamine within 10-30min without the need of adding a surface activating agent, wherein, high temperature and high pressure are not required for the synthesis cerium oxide. By adopting microwave heating, not only the synthetic time of the cerium oxide is shortened, but also the particle size of the synthesized product is more uniform. The cerium oxide prepared by the method has the advantages that the grain size is 5nm, the dispersivity is good, the agglomeration is difficult to occur, the synthetic path is simple, the operation is convenient and the like.
Description
Technical field
The present invention relates to prepare the method for nano ceric oxide.
Background technology
The nano rare earth material is the main force of rare earth Industrial Revolution, it is an important directions of following rare-earth products research and development, its research is caused more and more research authors' concern, and many countries all drop into huge fund in this respect, capture the commanding elevation or the one seat of its research and development with it.CeO
2Be the extremely wide light rare earths oxide compound of a kind of cheapness, purposes, and enjoy the good reputation of " the industrial monosodium glutamate of 21st century ".Be widely used as rumbling compound, the glass decolouring finings of luminescent material, electronic ceramics, glass; It also is the important composition composition in superconductor, pottery, gas sensor, petroleum cracking catalyzer and the homogeneous catalyst.CeO
2Physicochemical property can directly influence the performance of material, as: add ultra-fine CeO
2Not only can reduce the sintering temperature of pottery, can also increase the density of pottery; Bigger serface can improve the catalytic activity of catalyzer; And cerium has and appraises at the current rate, and is also significant to luminescent material.Nano ceric oxide shows the excellent specific property that many body shape cerium dioxides do not have and becomes a main direction of the following research and development of current cerium dioxide, also is the focus of current research.Nano Ce O
2The particulate size is depended in the performance of excellent properties to a great extent, the nano Ce O that particle diameter is little, be evenly distributed
2The preparation of particulate material becomes a problem that presses for solution.The preparation method of nano ceric oxide mainly contains the precipitator method, sol-gel method, hydrothermal method, microemulsion method, spray reaction method etc.Wherein the precipitator method are methods that liquid phase chemical synthesis of high purity nanoparticle extensively adopts.It is precipitation agent (OH
One, CO
3 2 one, SO4
2-, C
2O
4 2-Deng) add and to carry out precipitation process in the metal salt solution, again with throw out filtration, drying, roasting, just make the nano-scale oxide powder, be typical liquid phase method.The precipitator method are mainly used in the preparation nanosize metal oxide powders.The precipitator method commonly used have direct precipitation method, coprecipitation method, hydrolytic precipitation method, homogeneous precipitation method, huge legendary turtle compound decomposition method etc.In the precipitin reaction process because intergranular direct contact or be subjected to " contact recrystallize " domination, particle can irreversibly stick together and condense.Experimentation can adopt electrostatic double layer, gel network and protection reagent to suppress.Document [Chinese rare-earth journal, 2001, l9 (1): 24] utilization adopts ethanol to be dispersion agent and protective material, is that precipitation agent is with Ce with ammoniacal liquor
3+Precipitation is also used H in the reaction process
2O
2For oxygenant promotes Ce (OH)
3To Ce (OH)
4Conversion, at last with the brown precipitate centrifugation that obtains, under different temperature, carry out roasting, obtain nano Ce O
2Experimental result shows that adopting organic solvent is solvent, and agglomeration traits makes moderate progress, and alcoholic acid coating effect has simultaneously also suppressed the growth of particle, the nano Ce O of acquisition
2Particle is little.Document [Materials Letters, 2002,56:610] is at preparation nano Ce O
2Process in Ce (OH)
4Filter, washing with alcohol, and then with oxalic acid ethylene glycol fat and ethanol circulating filtration redispersion, through roasting system median size be the CeO of 10-50 nm
2Particle.
Document [chemistry circular, 1998,12:51] successfully utilizes the W/O microemulsion method to prepare the CeO of particle diameter less than 40 nm
2Ultrafine particle.In this method preparation process, be difficult for coalescently between particle, the big I of particle is controlled by selecting different surfactant molecules.But this method in preparation process the tensio-active agent that consumes and quantity of solvent many, be difficult to remove these organism, and cost is higher from the particle surface of last acquisition.Therefore in reaction process, advocate the recycle of medium.At present this kind method is in research focus period, also need study microemulsion character, and it is low to seek cost, and the easy tensio-active agent that reclaims is set up and is fit to industrialized production system.
Prepare ultra-fine and nano Ce O
2Method also have scorification, spray reaction method, combustion method, electrochemical synthesis method etc., these prepare ultra-fine and nano Ce O
2Method, all be in the experimental study stage at present.Various preparation methods have its different characteristics from the aspects such as size of experimental raw, reaction conditions, used plant and instrument, last gained particle.
The eighties in 20th century, the emerging microwave that grows up was a kind of novel heating technique, have rapidly and efficiently (than fast 15～20 times of conventional high-temperature solid phase method), temperature of reaction also relatively low (lower 300～500 ℃ than conventional high-temperature solid phase), power and energy saving (50 %～80 %), environmental protection, product purity is high and advantage such as easy to operate.In addition, microwave synthetic product epigranular and tiny is a kind of effective means of nano materials.Particularly, be expected to realize in the near future suitability for industrialized production in today that the technology of microwave oven has become better and approaching perfection day by day.Once with successfully using half industrial microwave oven [02149755] to synthesize the 4A molecular sieve, volume production can reach 5 kilograms for we.The result shows that granularity is littler than conventional method with microwave synthetic product epigranular, and synthesis cycle is short, has advantages such as fast energy-saving.
Patent [200710118268] is mixed cerium ion solution with alkali lye, put into the microwave high pressure retort then, obtains cerium oxide nano particle through the microwave-assisted reaction.The advantage of this method is that preparation technology is simple, and the reaction times is short, saves the energy, and gained cerium oxide nano particle particle diameter is little, good dispersity, and pattern is regular.Document [inorganic chemicals industry, 2007,39:21] be reactant with four water ceric sulfates and sodium hydroxide, surfactant polyethylene plays the effect that disperses product, prepare nano ceric oxide under microwave action, the product grain diameter for preparing under the optimum process condition is 24. 9 nm.But above-mentioned reaction is all carried out in encloses container, and security is bad, and plant and instrument is had relatively high expectations, and is difficult for carrying out industrial amplification quantity and synthesizes.
Summary of the invention
CeO
2As a kind of important catalyst (or auxiliary agent) and support of the catalyst, all has unique character.Because the specific surface area of nanoparticle is big, chemically reactive is high and body shape CeO
2Compare, show the performance of many excellences.Purpose of the present invention just is to provide a kind of easy nano Ce O
2The method of particle.
The present invention's (first invention) provides a kind of simple and easy synthesis of nano CeO
2The preparation method of particle is characterized in that: adopt microwave method synthesizing superfine nano Ce O
2Particle, product have good dispersiveness, and particle size is little and even.By utilizing microwave heating, shortened CeO greatly
2Generated time, reduced energy consumption, reduced the synthetic cost.
The present invention prepares superfine nano CeO
2The method of particle is carried out as follows:
A. be the cerium source with cerous nitrate or ceric ammonium nitrate or cerous chlorate, triethylene tetramine or tetraethylene pentamine or diethanolamine or thanomin are alkali source, and solvent is a water;
B. cerium source and water are joined in the flask, stir 15 min, add organic bases then to above-mentioned solution, continue to stir 30min, microwave current is at 20～80 mA, 40 mA; Power 45～150 W, reaction times 15 min.
C. take out after question response is finished, centrifugation throw out, water and ethanol wash respectively three times, flush away surface alkali lye and impurity, oven dry.
The present invention prepares superfine nano CeO
2The more excellent method of particle is carried out as follows:
With cerous nitrate (Ce (NO
3)
36H
2O) and 30 mL water join in the round-bottomed flask of 100 mL, induction stirring 15 min add 150 μ L triethylene tetramines then to above-mentioned solution, continue to stir 30min, put up reaction unit, microwave power is transferred to 90 W, electric current 40 mA, the reaction times is set to 15 min.
The present invention adopts the microwave oven synthesis of nano cerium dioxide through repacking, need not high-pressure sealed synthesizing, and synthesizer is simple, good reproducibility, and it is synthetic to be beneficial to industrial amplification quantity.The present invention's reaction is medium with water, and need not adds tensio-active agent for opening wide system, is easy to carry out amplification quantity and synthesizes, and has than existing method to have good superiority.
The present invention adopts microwave heating, because rate of heating is fast, can form a large amount of CeO in the short period of time
2Nucleus, synthetic CeO
2Crystal grain is little and even, and the synthetic product is difficult for reuniting in microwave field.
The present invention is alkali source by the selection to composition of raw materials with the organic amine, both can play the effect of alkali, can play the effect of tensio-active agent again, has reduced CeO
2Particle diameter, the synthetic product be difficult for to be reunited, good dispersity.
Microwave heating power 90 ~ 150 W that the present invention adopts, electric current 40 ~ 80 mA.Top condition is power 90 W, and electric current 40 mA are reaction down, and the best reaction times is 15 min.
The preparation method of described nano ceric oxide carries out in the aqueous solution, has that solvent is easy to get, environmental protection and inexpensive characteristics.
Various raw materials are low to the material purity requirement among the present invention, and turndown ratio increases; The superfine nano CeO that synthesizes
2Average particle size 2～5 nm are evenly distributed.Be applicable to fields such as catalyzer, polishing powder, electrode materials fully.
Description of drawings
Fig. 1 superfine nano CeO
2XRD figure.
Fig. 2 triethylene tetramine is alkali source synthesis of nano CeO
2Transmission electron microscope picture.
Fig. 3 tetraethylene pentamine is alkali source synthesis of nano CeO
2Transmission electron microscope picture.
Fig. 4 thanomin is alkali source synthesis of nano CeO
2Transmission electron microscope picture.
Fig. 5 diethanolamine is alkali source synthesis of nano CeO
2Transmission electron microscope picture.
In order to further describe the present invention, provided several concrete case study on implementation below, but patent right is not limited to these examples.
Specific embodiment
Embodiment 1
Under continuously stirring, with the Ce (NO of 0.5 mmol
3)
36H
2O is dissolved in the 30 ml deionized waters; Then, the triethylene tetramine with 150 l is added drop-wise in the above-mentioned reaction solution under stirring condition; Continue to stir 30 min, finally form the purple suspension liquid; Suspension liquid is transferred in the 100 mL round-bottomed flasks then, places microwave oven (household microwave oven of repacking is taken back the stream device, and microwave power is adjustable), and controlled microwave power is 90 W, and the reaction times is 15 min; Reaction naturally cools to room temperature after finishing.With the product centrifugation, precipitate three times with deionized water and ethanol circulation cleaning.At last products therefrom is placed baking oven, dry by the fire 4 h down, promptly obtain final product at 80 ℃.
The XRD diffractogram uses Philips X ' Pert Pro Super X-ray diffraction instrument to measure (λ=1.541 78).The transmission photo is taken with Hitachi H-800 transmission electron microscope.
Fig. 1 is the XRD figure of synthetic sample, as we know from the figure, and the complete and CeO in the peak of sample
2The standard spectrogram coincide (JCPDS No. 81-0792), and assorted peak illustrates the synthetic fast higher cerium dioxide of purity of available microwave.In addition, the XRD diffraction peak broad of sample, the granularity that further specifies synthetic product is less.
Fig. 2 is the TEM figure of sample, and is very even from the size distribution of scheming synthetic cerium dioxide as can be known, and has dispersedly preferably, and particle diameter is between 3-5 nm.
Embodiment 2
Under continuously stirring, with the Ce (NO of 0.5 mmol
3)
36H
2O is dissolved in the 30 ml deionized waters; Then, the tetraethylene pentamine with 150 l is added drop-wise in the above-mentioned reaction solution under stirring condition; Continue to stir 30 min, finally form the purple suspension liquid; Suspension liquid is transferred in the 100 mL round-bottomed flasks then, places microwave oven (household microwave oven of repacking is taken back the stream device, and microwave power is adjustable), and controlled microwave power is 90 W, and the reaction times is 15 min; Reaction naturally cools to room temperature after finishing.With the product centrifugation, precipitate three times with deionized water and ethanol circulation cleaning.At last products therefrom is placed baking oven, dry by the fire 4 h down, promptly obtain final product at 80 ℃.Fig. 3 is the TEM figure of synthetic sample, and from figure as can be known, the crystallinity of sample is not fine, is very tiny particle, and the product particle diameter is less than 5 nm.
Embodiment 3
Under continuously stirring, with the Ce (NO of 0.5 mmol
3)
36H
2O is dissolved in the 30 ml deionized waters; Then, the thanomin with 150 l is added drop-wise in the above-mentioned reaction solution under stirring condition; Continue to stir 30 min, finally form the purple suspension liquid; Suspension liquid is transferred in the 100 mL round-bottomed flasks then, places microwave oven (household microwave oven of repacking is taken back the stream device, and microwave power is adjustable), and controlled microwave power is 90 W, and the reaction times is 15 min; Reaction naturally cools to room temperature after finishing.With the product centrifugation, precipitate three times with deionized water and ethanol circulation cleaning.At last products therefrom is placed baking oven, dry by the fire 4 h down, promptly obtain final product at 80 ℃.Fig. 4 is the TEM figure of sample, and the product granularity is comparatively even as can be known from scheming, and is the particle about 5 nm.
Embodiment 4
Under continuously stirring, with the Ce (NO of 0.5 mmol
3)
36H
2O is dissolved in the 30 ml deionized waters; Then, the diethanolamine with 150 l is added drop-wise in the above-mentioned reaction solution under stirring condition; Continue to stir 30 min, finally form the purple suspension liquid; Suspension liquid is transferred in the 100 mL round-bottomed flasks then, places microwave oven (household microwave oven of repacking is taken back the stream device, and microwave power is adjustable), and controlled microwave power is 90 W, and the reaction times is 15 min; Reaction naturally cools to room temperature after finishing.With the product centrifugation, precipitate three times with deionized water and ethanol circulation cleaning.At last products therefrom is placed baking oven, dry by the fire 4 h down, promptly obtain final product at 80 ℃.Fig. 5 is the TEM figure of sample, and the product granularity is comparatively even as can be known from scheming, and is the particle about 5 nm.
Claims (4)
1. the microwave fast synthesis method of nano ceric oxide is characterized in that under the microwave auxiliary reflux condition, its preparation process is as follows:
With cerous nitrate or ceric ammonium nitrate or cerous chlorate is the cerium source, and triethylene tetramine or tetraethylene pentamine or diethanolamine or thanomin are alkali source, and solvent is a water;
Cerium source and water are joined in the flask, stir 15 min, add organic bases then to above-mentioned solution, continue to stir 30min, microwave current is at 20～80 mA, 40 mA; Power 45～150 W, reaction times 15 min;
Question response takes out after finishing, and centrifugation throw out, water and ethanol wash respectively three times, flush away surface alkali lye and impurity, oven dry.
2. the preparation method of nano ceric oxide according to claim 1, it is characterized in that cerium source and 30 mL water are joined in the round-bottomed flask of 100 mL, induction stirring 15 min, add 150 μ L triethylene tetramines then to above-mentioned solution, continue to stir 30min, put up reaction unit, microwave power is transferred to 90 W, electric current 40 mA, the reaction times is set to 15 min.
3. the preparation method of nano ceric oxide according to claim 1 is characterized in that the cerium source selects cerous nitrate (Ce (NO for use
3)
36H
2O).
4. the preparation method of nano ceric oxide according to claim 1 is characterized in that alkali source is a triethylene tetramine.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942204A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer powder |
| CN103011235A (en) * | 2012-11-28 | 2013-04-03 | 江西师范大学 | Industrial microwave rapid synthesis method of ultra-large specific surface area nano cerium dioxide |
| CN104445339A (en) * | 2014-10-30 | 2015-03-25 | 东北大学 | Preparation method of highly-catalytic type nanometer cerium oxide |
| CN106622227A (en) * | 2016-12-29 | 2017-05-10 | 天津大学 | Preparation method of monoatomic catalyst for indoor air purification |
| CN107879349A (en) * | 2017-12-01 | 2018-04-06 | 江西师范大学 | A kind of monodisperse mesoporous silica microballoon powder and preparation method thereof |
| CN109133140A (en) * | 2018-08-27 | 2019-01-04 | 江西师范大学 | A method of preparing cerium oxide nanoparticles |
| CN109534383A (en) * | 2019-01-18 | 2019-03-29 | 江西师范大学 | A kind of synthetic method of cerium dioxide nano piece |
| US10639621B2 (en) | 2018-03-05 | 2020-05-05 | Qatar University | Nanoporous cerium oxide with interconnected pores for catalysis and a cost-effective method of preparing thereof |
| CN112266730A (en) * | 2020-12-04 | 2021-01-26 | 内蒙古科技大学 | Preparation method of fluorinated cerium dioxide polishing powder under microwave condition |
| WO2021072641A1 (en) * | 2019-10-15 | 2021-04-22 | 诸暨易联众创企业管理服务有限公司 | Method for preparing ceric dioxide-based nanomaterial |
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| CN102942204A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer powder |
| CN103011235A (en) * | 2012-11-28 | 2013-04-03 | 江西师范大学 | Industrial microwave rapid synthesis method of ultra-large specific surface area nano cerium dioxide |
| CN104445339A (en) * | 2014-10-30 | 2015-03-25 | 东北大学 | Preparation method of highly-catalytic type nanometer cerium oxide |
| CN104445339B (en) * | 2014-10-30 | 2016-07-06 | 东北大学 | A kind of preparation method of high catalytic type nano ceric oxide |
| CN106622227A (en) * | 2016-12-29 | 2017-05-10 | 天津大学 | Preparation method of monoatomic catalyst for indoor air purification |
| CN106622227B (en) * | 2016-12-29 | 2019-03-08 | 天津大学 | A kind of preparation method of the monatomic catalyst of indoor air purification |
| CN107879349A (en) * | 2017-12-01 | 2018-04-06 | 江西师范大学 | A kind of monodisperse mesoporous silica microballoon powder and preparation method thereof |
| CN107879349B (en) * | 2017-12-01 | 2020-06-19 | 江西师范大学 | Monodisperse mesoporous silica microsphere powder and preparation method thereof |
| US10639621B2 (en) | 2018-03-05 | 2020-05-05 | Qatar University | Nanoporous cerium oxide with interconnected pores for catalysis and a cost-effective method of preparing thereof |
| CN109133140A (en) * | 2018-08-27 | 2019-01-04 | 江西师范大学 | A method of preparing cerium oxide nanoparticles |
| CN109534383A (en) * | 2019-01-18 | 2019-03-29 | 江西师范大学 | A kind of synthetic method of cerium dioxide nano piece |
| WO2021072641A1 (en) * | 2019-10-15 | 2021-04-22 | 诸暨易联众创企业管理服务有限公司 | Method for preparing ceric dioxide-based nanomaterial |
| CN112266730A (en) * | 2020-12-04 | 2021-01-26 | 内蒙古科技大学 | Preparation method of fluorinated cerium dioxide polishing powder under microwave condition |
| CN112266730B (en) * | 2020-12-04 | 2021-08-31 | 内蒙古科技大学 | Preparation method of fluorinated cerium dioxide polishing powder under microwave condition |
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Application publication date: 20110420 |