CN107381615A - A kind of method and its application of Effective Regulation ceria Mesoporous Spheres particle diameter - Google Patents
A kind of method and its application of Effective Regulation ceria Mesoporous Spheres particle diameter Download PDFInfo
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- CN107381615A CN107381615A CN201710803847.7A CN201710803847A CN107381615A CN 107381615 A CN107381615 A CN 107381615A CN 201710803847 A CN201710803847 A CN 201710803847A CN 107381615 A CN107381615 A CN 107381615A
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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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- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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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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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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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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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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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- 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
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
Application the present invention relates to a kind of method of Effective Regulation ceria Mesoporous Spheres particle diameter and its in the preparation of different scale ceria Mesoporous Spheres, it is characterized in that preparation process is in addition to cerium salt and reaction dissolvent, any other surfactant, derivant, stabilizer or template need not be added, and its yardstick can carry out Effective Regulation by water content in presoma, preparation process includes：（1）Under stirring condition, deionized water, cerous nitrate are added in ethylene glycol successively, acquisition prepares the presoma of ceria Mesoporous Spheres；（2）Reaction precursor liquid solution is reacted 0.5 to 6 hour in 180 degree oil bath, yellow ceria Mesoporous Spheres colloidal solution is made；（3）After ceria Mesoporous Spheres colloidal solution is first centrifuged with supercentrifuge, then it is cleaned by ultrasonic the ceria Mesoporous Spheres of 35 acquisition different scales.The ceria Mesoporous Spheres that the present invention obtains can be applied to purifying vehicle exhaust, catalyzing carbon monoxide oxidation, mechanical polishing etc..
Description
Technical field
The present invention relates to a kind of method of Effective Regulation ceria Mesoporous Spheres particle diameter and its in different scale ceria
Application in Mesoporous Spheres preparation, belongs to nano material controllable preparation field.
Background technology
Ceria is that a kind of stability is good, hardness is high and puts the dilute of oxygen ability with the reduction of very excellent oxidative and storage oxygen
Native oxide, it is now widely used for purifying vehicle exhaust, catalyzing carbon monoxide oxidation, mechanical polishing, fuel cell, waste gas give up
The numerous areas such as water process.Therefore, control synthesis, structure-activity relationship, the application study of cerium dioxide nano material enjoy in recent years
Concern.The methods of people are using hydro-thermal, solvent heat, sol-gel, microemulsion, precipitation calcining, template auxiliary, electrochemical deposition
It is prepared for the cerium dioxide nano material of the different-shape structure such as spherical, bar-shaped, wire, tubulose, sheet, flower-shaped.Research shows,
In numerous ceria materials, ceria mesoporous material has that specific surface area is big, porosity is high, density is low, good penetrability
The advantages that, in catalysis, separation, absorption, sensing, light material such as constructs at many fields has very wide application prospect.It is aobvious
So, preparing ceria mesoporous material has highly important scientific meaning and practical value.At present, scientific research personnel is based on template
The synthesis strategies such as auxiliary, sol-gel, hydro-thermal solvent heat, precipitation calcining, with nitric acid in the solution such as ethanol, water, polyalcohol
The cerium salt such as cerium, cerium chloride, ammonium ceric nitrate, cerous acetate, cerium acid N-butyl make presoma, with polyvinylpyrrolidone, cetyl
It is trimethylammonium bromide, alkylamine, acrylic acid, acetic acid, amino acid, block copolymer, mesoporous carbon, mesoporous silicon oxide, carbon containing more
Glycan ball etc. makees surfactant, derivant, stabilizer or template and is successfully prepared a series of ceria mesoporous materials.So
And in actual applications, the above method obtain ceria mesoporous material usually require subsequent high temperature calcining, strong acid and strong base it is molten
The methods of solution processing, makes a return journey removing template, to obtain the performances such as excellent catalysis, absorption, infiltration.That is, using side at present
Method not only needs expensive surfactant, derivant, stabilizer or the template of addition, and subsequent treatment work in building-up process
Skill very complicated, it is clear that be unfavorable for large-scale production and application.Meanwhile using current synthesis technique in same reaction system
Also it is difficult to effectively regulate and control the yardstick of ceria mesoporous material.
The content of the invention
The technical problem to be solved in the present invention regulates and controls skill to overcome existing ceria mesoporous material to prepare especially yardstick
The weak point of art, there is provided it is a kind of easy, quick, without template, without preparing ceria Jie under conditions of stabilizer and derivant
Porous materials simultaneously realize the method to its particle diameter yardstick Effective Regulation.It is another object of the present invention to application mesoscale of the present invention to regulate and control
Method prepares that specific surface area is big, porosity is high, size is homogeneous, the ceria Mesoporous Spheres of different scale, is that vehicle exhaust is net
It is basic that the application of change, catalyzing carbon monoxide oxidation, mechanical polishing etc. provides important substance.
In the present invention ceria Mesoporous Spheres be using cerous nitrate as cerium source, do not add any surfactant, derivant,
Under conditions of stabilizer or template, obtained using solvent-thermal method in aqueous ethylene glycol solution, the regulation and control of its yardstick are to pass through
What precursors reclaimed water content volume percentage was realized, its preparation process includes step in detail below：
（1）A certain amount of deionized water is added in ethylene glycol solution, is uniformly mixing to obtain aqueous ethylene glycol solution, its reclaimed water contains
The percent by volume of amount is the % of 2 %- 6；
（2）Under agitation, to step（1）Cerous nitrate is added in the aqueous ethylene glycol solution obtained, obtains and prepares titanium dioxide
The precursor solution of cerium Mesoporous Spheres reaction, wherein, the concentration of cerous nitrate is 0.01-0.20 mol/Ls；
（3）By step（2）In reaction precursor liquid solution reacted 0.5 to 6 hour in 180 degree oil bath, reaction system is by colourless
It is changed into yellow, ceria Mesoporous Spheres colloidal solution is made；
（4）After question response terminates, ceria Mesoporous Spheres colloidal solution is centrifuged with supercentrifuge, in rotating speed 8000-
After 14000 revs/min of centrifugation 10-30 minutes, colorless supernatant liquid in centrifuge tube is removed, obtains yellow mercury oxide product；
（5）With deionized water or EtOH Sonicate cleaning step（4）The precipitated product of acquisition, and 60 points are dried in 100 degree of baking ovens
Clock, obtain ceria Mesoporous Spheres powder.
Beneficial effects of the present invention：
The invention provides a kind of method of Effective Regulation ceria Mesoporous Spheres particle diameter, it is characterised in that yardstick regulation and control are to pass through
The percent by volume of water content is realized in precursors；
The ceria Mesoporous Spheres that the present invention obtains are by small scale nanometer particle（2-3 nanometers）Assembling accumulation is formed, its chi
Degree can Effective Regulation, pore size be 2-4 nanometers in 30-200 nanometer ranges, and specific surface area is 120-200 meters squared per grams,
And have the characteristics that yield is high, monodispersity is good, stability is good；
The present invention is in addition to cerium salt and reaction dissolvent, without adding any other surfactant, derivant, stabilizer or template
Agent, prepare the only conventional equipment that need to commonly use, without the special equipment of costliness, therefore, no matter its preparation condition, technique or after
Continuous processing procedure is all very simple and easy to do, is adapted to magnanimity, low cost, large-scale production, and the following commercial applications that are content with very little need
Ask.
Brief description of the drawings
Fig. 1 is with multiple transmission electron microscopes shot after JEOL-1400 transmission electron microscope observings to the ceria Mesoporous Spheres of acquisition
（TEM）One of photo, wherein, Fig. 1 a are ceria Mesoporous Spheres low power TEM image, and Fig. 1 b are ceria Mesoporous Spheres high power
TEM image, TEM results show that product is by small scale nanometer particle（2-3 nanometers）50 nanometers of single dispersings that assembling accumulation is formed
Ceria Mesoporous Spheres.
Fig. 2 is the ceria Mesoporous Spheres Zeiss, Germany FE-Sigma300 type field emission microscopy observations to acquisition
Multiple stereoscan photographs shot afterwards（SEM image）One of, SEM results are shown, primer size is homogeneous, good dispersion, with TEM
Observed result is consistent.
Fig. 3 is after obtained ceria Mesoporous Spheres are evenly spread on slide, with Bruker D8-Advance types
X-ray diffractometer carries out testing the X-ray diffraction of acquisition to it（XRD）Collection of illustrative plates, wherein, ordinate is relative intensity, horizontal seat
It is designated as the angle of diffraction, XRD data and ceria standard spectrogram（JCPDS cards No.34-0394）It coincide, titanium dioxide made from explanation
Cerium Mesoporous Spheres have fluorite type face-centred cubic structure.
Fig. 4 is with Japanese Shimadzu UV-3101PC types ultraviolet-visible-near infrared spectrometer（UV-Vis-NIR）
The light absorbs spectrogram obtained after testing ceria Mesoporous Spheres, wherein, ordinate is absorption intensity, and abscissa is light wave
Wavelength.It can be seen that ceria Mesoporous Spheres have significant exciton absorption peak in 310 nanometers.
Fig. 5 is the titanium dioxide automatically tested with TriStar II 3020 than surface and lacunarity analysis instrument under 77 K
Isothermal nitrogen adsorption-desorption curve of cerium Mesoporous Spheres, wherein, ceria Mesoporous Spheres are in 200 degrees Celsius of vacuum conditions before measurement
4 hours degassing process of lower progress, wherein, Fig. 5 a are N2Adsorption/desorption curve, Fig. 5 b are pore size distribution curve, are as a result shown, chi
The specific surface area for spending the ceria Mesoporous Spheres for 50 nanometers is 124 meters squared per grams, and pore size is 2-4 nanometers.
Fig. 6 is the transmission electricity that ceria Mesoporous Spheres are obtained under precursors reclaimed water content volume percentage different condition
Nitric acid cerium concentration is 0.05 mol/L in mirror photo, wherein reaction system, and reaction temperature is 180 degree, water content in Fig. 6 a-6d
Percent by volume is followed successively by 3 %, 4 %, 5 % and 6 %, and all scales are 50 nanometers in figure.
Embodiment
First from market, purchase prepares six water cerous nitrates, the ethylene glycol that ceria Mesoporous Spheres are used, 18 needed for experiment
Megaohm deionized water is as made from vertical pure LCT-I-10T tests professional water purifier.
Present disclosure is described in further detail with reference to specific embodiment, but the invention is not restricted to following
The specific examples of act.
Embodiment 1
The preparation of 30 nano ceric oxide Mesoporous Spheres
Under agitation, 2.1 ml deionized waters are added in 67.9 milliliters of ethylene glycol solutions, be uniformly mixing to obtain aqueous
Ethylene glycol solution, the water cerous nitrates of 1.52 g six are then added, being stirred 30 minutes under the conditions of 500 revs/min makes cerous nitrate complete
Dissolving, acquisition prepares the reaction precursor liquid solution of ceria Mesoporous Spheres, wherein, the concentration of cerous nitrate is respectively 0.05 mole/
Rise, the percent by volume of water content is 3 %.And then the reaction precursor liquid solution prepared is reacted to 1 in 180 degree oil bath small
When, obtain ceria Mesoporous Spheres colloidal solution；It is after reaction end naturally cools to room temperature, the mesoporous spherocolloid of ceria is molten
Liquid is centrifuged with supercentrifuge, after the centrifugation 30 minutes of 14000 revs/min of rotating speed, is removed colourless solution in centrifuge tube, is obtained
To yellow mercury oxide product；The precipitated product of acquisition is cleaned by ultrasonic 5-6 times with deionized water or absolute alcohol, and in 100 degree of bakings
Dry 60 minutes, be made as shown in Figure 6 a, yardstick is 30 nano ceric oxide Mesoporous Spheres in case.
Embodiment 2
The preparation of 50 nano ceric oxide Mesoporous Spheres
Under agitation, 2.8 ml deionized waters are added in 67.2 milliliters of ethylene glycol solutions, be uniformly mixing to obtain aqueous
Ethylene glycol solution, the water cerous nitrates of 1.52 g six are then added, being stirred 30 minutes under the conditions of 500 revs/min makes cerous nitrate complete
Dissolving, acquisition prepares the reaction precursor liquid solution of ceria Mesoporous Spheres, wherein, the concentration of cerous nitrate is respectively 0.05 mole/
Rise, the percent by volume of water content is 4 %.And then the reaction precursor liquid solution prepared is reacted to 2 in 180 degree oil bath small
When, obtain ceria Mesoporous Spheres colloidal solution；It is after reaction end naturally cools to room temperature, the mesoporous spherocolloid of ceria is molten
Liquid is centrifuged with supercentrifuge, after the centrifugation 30 minutes of 12000 revs/min of rotating speed, is removed colourless solution in centrifuge tube, is obtained
To yellow mercury oxide product；The precipitated product of acquisition is cleaned by ultrasonic 5-6 times with deionized water or absolute alcohol, and in 100 degree of bakings
Dry 60 minutes, be made as shown in Figure 6 b, yardstick is 50 nano ceric oxide Mesoporous Spheres in case.
Embodiment 3
The preparation of 100 nano ceric oxide Mesoporous Spheres
Under agitation, 3.5 ml deionized waters are added in 66.5 milliliters of ethylene glycol solutions, be uniformly mixing to obtain aqueous
Ethylene glycol solution, the water cerous nitrates of 1.52 g six are then added, being stirred 30 minutes under the conditions of 500 revs/min makes cerous nitrate complete
Dissolving, acquisition prepares the reaction precursor liquid solution of ceria Mesoporous Spheres, wherein, the concentration of cerous nitrate is respectively 0.05 mole/
Rise, the percent by volume of water content is 5 %.And then the reaction precursor liquid solution prepared is reacted to 4 in 180 degree oil bath small
When, obtain ceria Mesoporous Spheres colloidal solution；It is after reaction end naturally cools to room temperature, the mesoporous spherocolloid of ceria is molten
Liquid is centrifuged with supercentrifuge, after the centrifugation 30 minutes of 10000 revs/min of rotating speed, is removed colourless solution in centrifuge tube, is obtained
To yellow mercury oxide product；The precipitated product of acquisition is cleaned by ultrasonic 5-6 times with deionized water or absolute alcohol, and in 100 degree of bakings
Dry 60 minutes, be made as fig. 6 c, yardstick is 100 nano ceric oxide Mesoporous Spheres in case.
Embodiment 4
The preparation of 200 nano ceric oxide Mesoporous Spheres
Under agitation, 4.2 ml deionized waters are added in 65.8 milliliters of ethylene glycol solutions, be uniformly mixing to obtain aqueous
Ethylene glycol solution, the water cerous nitrates of 1.52 g six are then added, being stirred 30 minutes under the conditions of 500 revs/min makes cerous nitrate complete
Dissolving, acquisition prepares the reaction precursor liquid solution of ceria Mesoporous Spheres, wherein, the concentration of cerous nitrate is respectively 0.05 mole/
Rise, the percent by volume of water content is 6 %.And then the reaction precursor liquid solution prepared is reacted to 6 in 180 degree oil bath small
When, obtain ceria Mesoporous Spheres colloidal solution；It is after reaction end naturally cools to room temperature, the mesoporous spherocolloid of ceria is molten
Liquid is centrifuged with supercentrifuge, after the centrifugation 30 minutes of 8000 revs/min of rotating speed, is removed colourless solution in centrifuge tube, is obtained
To yellow mercury oxide product；The precipitated product of acquisition is cleaned by ultrasonic 5-6 times with deionized water or absolute alcohol, and in 100 degree of bakings
Dry 60 minutes, be made as shown in fig 6d, yardstick is 200 nano ceric oxide Mesoporous Spheres in case.
Obviously, those skilled in the art can have ceria Mesoporous Spheres and preparation method thereof to of the present invention
Carry out various changes and modification without departing from the spirit and scope of the present invention.So, if these modifications and variations of the present invention
Belong within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to exist comprising these changes and modification
It is interior.
Claims (3)
- A kind of 1. method of Effective Regulation ceria Mesoporous Spheres particle diameter, it is characterised in that the yardstick of ceria Mesoporous Spheres is logical Cross the percent by volume regulation and control of water content in precursors.
- 2. ceria Mesoporous Spheres are using cerous nitrate as cerium source in the present invention, any surfactant, derivant, steady is not being added Under the conditions of determining agent or template, obtained in aqueous ethylene glycol solution, ceria Mesoporous Spheres are by small scale nanometer particle （2-3 nanometers）Assembling accumulation is formed, and its yardstick Effective Regulation, pore size can be received in 30-200 nanometer ranges for 2-4 Rice, specific surface area is 120-200 meters squared per grams.
- 3. the preparation method of the ceria Mesoporous Spheres described in claim 2, it is characterized in that comprising the following steps：（1）A certain amount of deionized water is added in ethylene glycol solution, is uniformly mixing to obtain aqueous ethylene glycol solution, its reclaimed water contains The percent by volume of amount is the % of 2 %- 6；（2）Under agitation, to step（1）Cerous nitrate is added in the aqueous ethylene glycol solution obtained, obtains and prepares titanium dioxide The precursor solution of cerium Mesoporous Spheres reaction, wherein, the concentration of cerous nitrate is 0.01-0.20 mol/Ls；（3）By step（2）In reaction precursor liquid solution reacted 0.5 to 6 hour in 180 degree oil bath, be made ceria be situated between Hole spherocolloid solution；（4）After question response terminates, by ceria Mesoporous Spheres colloidal solution supercentrifuge in 8000-14000 revs/min of rotating speed After Zhongli's heart 10-30 minutes, colorless supernatant liquid in centrifuge tube is removed, obtains yellow mercury oxide product；（5）With deionized water or EtOH Sonicate cleaning step（4）The precipitated product of acquisition, and 60 points are dried in 100 degree of baking ovens Clock, obtain ceria Mesoporous Spheres.
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Cited By (5)
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| CN108722391A (en) * | 2018-06-04 | 2018-11-02 | 中国科学院海洋研究所 | A kind of 3D C/CeO2Hollow nanostructured frame material and the preparation method and application thereof |
| CN109467117A (en) * | 2018-11-08 | 2019-03-15 | 乐山师范学院 | A kind of no template preparation CeO2The method and CeO of mesoporous material2Mesoporous material |
| CN110354799A (en) * | 2019-07-24 | 2019-10-22 | 济南大学 | A kind of cerium dioxide nano material possessing good low temperature NOx storage capacity |
| CN112850776A (en) * | 2021-01-27 | 2021-05-28 | 苏州大学 | Ultra-light three-dimensional hierarchical-pore cerium dioxide material and preparation method thereof |
| CN115637043A (en) * | 2022-10-28 | 2023-01-24 | 江苏宏盛尼龙有限公司 | High-strength super-wear-resistant MC nylon composite material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108722391A (en) * | 2018-06-04 | 2018-11-02 | 中国科学院海洋研究所 | A kind of 3D C/CeO2Hollow nanostructured frame material and the preparation method and application thereof |
| CN109467117A (en) * | 2018-11-08 | 2019-03-15 | 乐山师范学院 | A kind of no template preparation CeO2The method and CeO of mesoporous material2Mesoporous material |
| 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 |
| CN110354799A (en) * | 2019-07-24 | 2019-10-22 | 济南大学 | A kind of cerium dioxide nano material possessing good low temperature NOx storage capacity |
| CN112850776A (en) * | 2021-01-27 | 2021-05-28 | 苏州大学 | Ultra-light three-dimensional hierarchical-pore cerium dioxide material and preparation method thereof |
| CN112850776B (en) * | 2021-01-27 | 2022-02-01 | 苏州大学 | Three-dimensional hierarchical-pore cerium dioxide material and preparation method thereof |
| CN115637043A (en) * | 2022-10-28 | 2023-01-24 | 江苏宏盛尼龙有限公司 | High-strength super-wear-resistant MC nylon composite material and preparation method thereof |
| CN115637043B (en) * | 2022-10-28 | 2023-10-27 | 江苏宏盛尼龙有限公司 | High-strength super-wear-resistant MC nylon composite material and preparation method thereof |
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