CN100567160C - A kind of preparation method of high specific surface area meso-porous cerium dioxide micro-balloon - Google Patents
A kind of preparation method of high specific surface area meso-porous cerium dioxide micro-balloon Download PDFInfo
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- CN100567160C CN100567160C CNB2007101194019A CN200710119401A CN100567160C CN 100567160 C CN100567160 C CN 100567160C CN B2007101194019 A CNB2007101194019 A CN B2007101194019A CN 200710119401 A CN200710119401 A CN 200710119401A CN 100567160 C CN100567160 C CN 100567160C
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Abstract
A kind of preparation method of high specific surface area meso-porous cerium dioxide micro-balloon belongs to rare earth oxide material field.It is characterized in that utilizing spherical, the hemispherical mesoporous cerium oxide powder of Hydrothermal Preparation with height ratio than area and homogeneous exterior appearance; With (NH
4)
2Ce (NO
3)
4Be dissolved in stirring in the dehydrated alcohol as the cerium source and made its thorough mixing in 30～60 minutes, add N again after adding acid, dinethylformamide stirs after 5～30 minutes and puts into hydrothermal reaction kettle, 100～160 ℃ of temperature range internal reactions 40～140 hours, and gained sample Ce (COOH)
3Sintering is after 2～8 hours in 350～450 ℃ of temperature ranges for presoma, presoma, and cooled sample promptly obtains spherical, the hemispherical mesoporous cerium oxide of high-specific surface area.Material preparation method of the present invention is simple and easy, and equipment is simple, and synthesis temperature is low; Cost of material is cheap, need not expensive tensio-active agent and makes template; Good reproducibility.Advantages such as the mesoporous ceria that obtains has sphericity height, yardstick homogeneous, and pore diameter range is narrow, and specific surface area is big.
Description
Technical field:
The invention belongs to genus rare earth oxide material field, relate to a kind of mesoporous ceria preparation methods, particularly adopt micron, submicron order sphere, the semisphere of non-template agent preparation, specific surface area 150-280m
2/ g, the method for the meso-porous titanium dioxide cerium material of aperture 3-10nm.
Background technology:
CeO
2Be a kind of important compound in the rare earth family,, loaded metal dispersed high multinomial good characteristic good and getting most of the attention with its storage oxygen performance.Meso-pore Ce O
2Owing to its structural stability has CeO
2All character, comprise good chemical stability, store up oxygen oxygen release function, and the quick oxygen of high temperature room diffusibility by force.While meso-pore Ce O
2Have nano level duct structure, high-specific surface area again, can greatly widen CeO
2Application Areas.At present, meso-pore Ce O
2Preparation mainly contain surfactant templates method, sol-gel process, and hard template method etc.These methods mainly in shortcomings such as template or precursor material price height, complicated process of preparation, are unfavorable for large-scale production and application.Therefore the developing low-cost preparation has the long-pending CeO of meso-porous structural high specific surface
2Method significant.In addition, the external pattern of material also can produce the influence that can not be ignored to its performance and application, and the microspheroidal material has the significant application value of going out because of having advantages such as lower frictional coefficient, good flowability, close heap and dispersiveness in various fields.
Summary of the invention
The purpose of this invention is to provide a kind of with simple and easy process cheaply obtain height ratio than area, exterior appearance homogeneous, can handling strong micron, spherical, the hemispherical mesoporous ceria preparation methods of submicron order.
A kind of preparation method of high specific surface area meso-porous cerium dioxide micro-balloon utilizes that Hydrothermal Preparation is spherical, hemispherical to have high specific surface area and than the mesoporous cerium oxide powder of homogeneous exterior appearance.Presoma is Ce (COOH)
3With (NH
4)
2Ce (NO
3)
4Be dissolved in stirring in the dehydrated alcohol as the cerium source and made its thorough mixing in 30～60 minutes, add N again after adding a certain amount of acid, dinethylformamide (DMF) stirs after 5～30 minutes and puts into hydrothermal reaction kettle, 100～160 ℃ of temperature range internal reactions 40～140 hours, and gained sample Ce (COOH)
3Sintering is after 2～8 hours in 350～450 ℃ of temperature ranges for presoma, presoma, and cooled sample promptly obtains spherical, the hemispherical mesoporous cerium oxide of high-specific surface area.
Concrete processing condition are: (NH
4)
2Ce (NO
3)
4Strength of solution in reaction soln is 0.0685mol/L, (NH
4)
2Ce (NO
3)
4With the mol ratio of dehydrated alcohol 3: 103～1: 103, adding acid was solubility strong acid, its H
+Concentration in reaction liquid is between 0.04～0.1mol/L, (NH4)
2Ce (NO
3)
4With N, the mol ratio of dinethylformamide (DMF) 8: 303～1: 114.
Material preparation method of the present invention is simple and easy, and equipment is simple, and synthesis temperature is low; Cost of material is cheap, need not expensive tensio-active agent and makes template; Good reproducibility.Advantages such as the mesoporous ceria that obtains has sphericity height, yardstick homogeneous, and pore diameter range is narrow, and specific surface area is big.Specific surface area reaches 150-280m
2/ g, aperture 2-10nm., the cerium dioxide that the present invention obtains is micron, submicron order, makes this ball be easy to be controlled, and can effectively evade nano-scale particle is difficult for recovery in application shortcoming.
Description of drawings
Fig. 1 is the XRD figure spectrum of final product, illustrates that obtaining sample is CeO
2Single phase.
Fig. 2 is the absorption/desorption isotherm of this sample, from then among the figure as can be seen the reference area of this sample be 185.1m
2/ g has bigger specific surface area.
Fig. 3, Fig. 4 are the stereoscan photograph of sample, and sample has kept spherical preferably and hemispherical pattern.
Embodiment
Embodiment one
With 1g (NH
4)
2Ce (NO
3)
6Be dissolved in 9ml ethanol, drip the hydrochloric acid of 1ml 2mol/L, stirred 30 minutes, add 10ml DMF and stir after 10 minutes, put into reactor.100 degree reactions 140 hours, obtain black sphere and semisphere material.With the sample that obtains in air with 3 degree/minute speed be fired to 350 degree back insulations 3 hours.Cooled sample promptly obtains spherical, the hemispherical mesoporous cerium oxide of high-specific surface area.
Embodiment two
With 1g (NH
4)
2Ce (NO
3)
6Be dissolved in 5ml ethanol, drip the hydrochloric acid of 1ml 2mol/, stirred 40 minutes, add 10ml DMF and stir after 10 minutes, put into reactor.100 ℃ of reactions 160 hours, obtain black sphere and semisphere material.With the sample that obtains in air with 1 degree/minute speed be fired to 380 ℃ after insulation 2 hours.Cooled sample promptly obtains spherical, the hemispherical mesoporous cerium oxide of high-specific surface area, and the specific surface area of this sample is 196.2m
2/ g
Embodiment three
With 1g (NH
4)
2Ce (NO
3)
6Be dissolved in 5ml ethanol, drip the hydrochloric acid of 1.5ml 2mol/L, stirred 35 minutes, add 10ml DMF and stir after 10 minutes, put into reactor.After 60 hours, be cooled to the room temperature ageing 20 hours 140 ℃ of reactions, obtain black sphere and semisphere material in reaction under 140 ℃ of temperature after 25 hours again.With the sample that obtains in air with 1 degree/minute speed be fired to 400 ℃ after insulation 3 hours.Cooled sample promptly obtains spherical, the hemispherical mesoporous cerium oxide of high-specific surface area, and the specific surface area of this sample is 201.1m
2/ g
Claims (3)
1. the preparation method of a cerium oxide is characterized in that the (NH with 1g
4)
2Ce (NO
3)
6Be dissolved in 9ml ethanol, drip the hydrochloric acid of 1ml 2mol/L, stirred 30 minutes, add 10mlN, dinethylformamide stirred after 10 minutes, put into reactor; 100 degree reactions 140 hours, obtain black sphere and semisphere material, with the sample that obtains in air with 3 degree/minute speed be fired to 350 degree back insulations 3 hours, cooled sample promptly obtains spherical, the hemispherical mesoporous cerium oxide of high-specific surface area.
2. the preparation method of a cerium oxide is characterized in that: with 1g (NH
4)
2Ce (NO
3)
6Be dissolved in 5ml ethanol, drip the hydrochloric acid of 1ml 2mol/L, stirred 40 minutes, and added 10mlN, dinethylformamide stirred after 10 minutes, put into reactor, 100 ℃ of reactions 160 hours, obtain black sphere and semisphere material, with the sample that obtains in air with 1 degree/minute speed be fired to 380 ℃ after insulation 2 hours, cooled sample promptly obtains spherical, hemispherical mesoporous cerium oxide, and the specific surface area of this sample is 196.2m
2/ g.
3. the preparation method of a cerium oxide is characterized in that: with 1g (NH
4)
2Ce (NO
3)
6Be dissolved in 5ml ethanol, drip the hydrochloric acid of 1.5ml 2mol/L, stirred 35 minutes, add 10mlN, dinethylformamide stirred after 10 minutes, put into reactor, 140 ℃ the reaction 60 hours after, be cooled to the room temperature ageing 20 hours, obtain black sphere and semisphere material in reaction under 140 ℃ of temperature after 25 hours again, with the sample that obtains in air with 1 degree/minute speed be fired to 400 ℃ after insulation 3 hours, cooled sample promptly obtains spherical, hemispherical mesoporous cerium oxide, and the specific surface area of this sample is 201.1m
2/ g.
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| CN100567160C true CN100567160C (en) | 2009-12-09 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100586862C (en) * | 2008-03-13 | 2010-02-03 | 同济大学 | Method for manufacturing high purity nano-cerium dioxide |
| CN101584981B (en) * | 2009-06-12 | 2010-12-01 | 华中师范大学 | Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure |
| CN101825551B (en) * | 2009-07-23 | 2011-07-27 | 中国科学院过程工程研究所 | Cerium dioxide microsphere used as dimension standard material |
| CN101804318A (en) * | 2010-04-16 | 2010-08-18 | 北京科技大学 | Preparation of lanthanum doping cerium dioxide porous microspheres and application thereof to Cr<6+> removal |
| CN101857260A (en) * | 2010-06-29 | 2010-10-13 | 上海大学 | Method for preparing spherical cerium dioxide nano material with square-sheet surface structure by hydrothermal method |
| CN102757079B (en) * | 2012-05-16 | 2014-06-04 | 成都理工大学 | Hydrothermal synthesis process for preparing mesoporous CeO2 |
| CN102951940A (en) * | 2012-11-05 | 2013-03-06 | 昆明理工大学 | Mesoporous cerium dioxide material preparation method |
| CN103253695B (en) * | 2013-05-24 | 2014-11-12 | 成都理工大学 | Normal pressure heat treatment process for synthesizing mesoporous CeO2 from CeO2 hydrosol |
| CN103965036B (en) * | 2014-05-12 | 2015-09-16 | 青岛科技大学 | A kind of preparation method of taper cesium formate |
| CN105585043B (en) * | 2016-03-11 | 2017-04-12 | 九江学院 | Preparation method of flowerlike cerium oxide nano-material |
| CN109133144B (en) * | 2018-10-22 | 2021-04-02 | 九江学院 | Preparation method of monodisperse ultra-small particle size cerium dioxide nanocrystal |
| CN109467117B (en) * | 2018-11-08 | 2021-03-16 | 乐山师范学院 | Template-free CeO preparation method2Method for producing mesoporous material and CeO2Mesoporous material |
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2007
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