CN109678193B - Preparation method of nano cerium oxide particles - Google Patents
Preparation method of nano cerium oxide particles Download PDFInfo
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- CN109678193B CN109678193B CN201811587542.8A CN201811587542A CN109678193B CN 109678193 B CN109678193 B CN 109678193B CN 201811587542 A CN201811587542 A CN 201811587542A CN 109678193 B CN109678193 B CN 109678193B
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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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a preparation method of nano cerium oxide particles, belonging to the field of nano powder materials, and the method comprises the following steps: (1) preparing a cerous nitrate-complexing agent aqueous solution, adjusting the pH value, and stirring to form sol; (2) dispersing the sol serving as a water phase in a mixed solution of a surfactant, a cosurfactant and cyclohexane to form stable reverse microemulsion, and reacting to prepare gel particles; (3) and cooling, freezing, filtering, drying and calcining the gel particles to obtain the nano cerium oxide particles. The nano cerium oxide prepared by the method has the advantages of tiny and controllable particle size, uniform appearance, lower agglomeration and high surface activity. The invention solves the problem that the colloidal particles are hard to agglomerate in the drying and heat treatment of the traditional sol-gel method, and has simple preparation process, reusable solvent and easy realization of industrial production.
Description
Technical Field
The invention belongs to the field of nano powder materials, and particularly relates to a preparation method of nano cerium oxide particles.
Technical Field
At present, the research on the nano metal oxide particles in various countries around the world mainly comprises preparation, microstructure, macro physical properties and application, wherein the preparation technology of the nano particles is key, because the preparation process and process control have important influence on the microstructure and macro properties of the nano particles. The preparation method of the nanometer metal oxide particles mainly comprises a chemical method and a physical method. The chemical methods are classified into impregnation, coprecipitation, homogeneous deposition, sol-gel, and microemulsion. The sol-gel method and the reverse microemulsion method have mild reaction conditions, easy control, small equipment investment and uniform and controllable particle size dispersion of the prepared particles, thereby being favored in the industry.
Cerium oxide (CeO)2) Is a light rare earth oxide with low cost and wide application, and is used for high-performance nickel-hydrogen power batteries, silver leaching agents, rare earth ore clean utilization, methane catalysts and the like. Compared with the current domestic commonly used vehicle new energy power battery, the high-performance nickel-hydrogen power battery has the advantages of high safety, attenuation resistance, low temperature resistance, recoverability, high charging speed and the like, and has the advantages of high charging speedThe application of the method to the field of pure electric buses opens the way for the high-end application of the light rare earth in China to enter large-scale industry. The Shanghai science and technology university researches a high-efficiency catalyst combination, namely a cerium-based catalyst and an alcohol catalyst. Under the condition of room temperature, the conversion of methane is completed under the concerted catalysis of trichloroethanol and rare earth metal cerium. The method solves a great problem in organic chemistry, finds a conversion method with low cost, high conversion efficiency and mild reaction conditions, provides a new scheme for converting methane into high-added-value chemical products such as rocket propellant fuel and the like, and provides a new idea for efficiently utilizing special rare earth metal resources in China.
The performance of the rare earth powder material is in important correlation with the granularity and the size of the rare earth powder material when CeO is used2The size of the powder reaches the nano level, and the powder has the surface effect, the volume effect, the size effect and the macroscopic tunnel effect of nano particles and has excellent application performance of nano materials, so the nano CeO2Has very wide application and development prospect. In recent years, the material research workers have conducted on the CeO nanoparticles2The preparation method and the application of the CeO nanoparticles are researched in a large quantity2Has become one of the research hotspots of nano powder material. But the nanometer CeO prepared by the traditional sol-gel method2Easy to agglomerate, poor in dispersibility and poor in application performance of the product. So as to research the nano CeO with accurate and controllable grain diameter and good dispersibility2The preparation method of the powder is necessary.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of nano cerium oxide particles, which is used for solving the problem of nano CeO in the prior art2Agglomeration is easy to occur in the preparation, and the dispersibility is poor, so that the application performance is poor.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a method for preparing nano cerium oxide particles is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing Ce (NO)3)3﹒6H2Dissolving O in deionized water to prepare an aqueous solution; weighing complexing agent and dissolvingDissolving in deionized water to prepare an aqueous solution, and mixing the two solutions to obtain a system Ce3+The concentration of the mixed solution is 1mol/L, the pH value is adjusted to 1-8 by 25 percent ammonia water, and the mixed solution is stirred for 1 hour at the temperature of 30 ℃ to form sol;
(2) adding cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, and sequentially dropwise adding a surfactant, a cosurfactant and the sol prepared in the step (1) into the reactor, wherein the sol is wrapped by the surfactant to form a stable sol-reverse microemulsion system; keeping the temperature of the water bath unchanged, and continuously stirring for 3-6 h to form gel particles;
(3) cooling and freezing the gel particles obtained in the step (2), performing suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at the temperature of minus 20 ℃;
(4) drying the gel particles washed in the step (3) in vacuum to remove moisture, thus obtaining a precursor;
(5) and (4) calcining the precursor in the step (4) at high temperature to obtain the nano cerium oxide particles.
The complexing agent is any one of citric acid, tartaric acid, malic acid or polyethylene glycol, and the complexing agent is preferably citric acid or tartaric acid.
The complexing agent and Ce (NO)3)3﹒6H2The mass ratio of O is 3 to 3.2: 1.
the surfactant is Cetyl Trimethyl Ammonium Bromide (CTAB), and the cosurfactant is n-butyl alcohol.
The mass ratio of the surfactant to the cyclohexane is 1: 50, the mass ratio of the cosurfactant to the cyclohexane is 1: 45.
the volume ratio of the sol to cyclohexane is 3: 100.
the temperature for freezing the gel in the step 3) is 0 to-30 ℃.
The vacuum drying in the step 4) is vacuum freeze drying, the drying temperature is-60 to-30 ℃, and the drying time is 24 to 48 hours.
The calcination temperature in the step 5) is 400-600 ℃, and the time is 2-4 h.
The preparation method of the nano cerium oxide particles has the following beneficial effects:
the invention utilizes the combination of the sol-gel method and the reverse microemulsion method to lead cerium to form a sol precursor under the action of a complexing agent and then to be dispersed in the reverse microemulsion, and the sol precursor is gelled in a water core wrapped by a surfactant, so the particle size of the formed gel is tiny and controllable, and the gel is wrapped by the surfactant, thereby solving the problem that colloidal particles are hard agglomerated during drying and heat treatment by the traditional sol-gel method, and the prepared nano cerium oxide has the advantages of uniform shape, controllable particle size, good dispersibility and high surface activity.
Drawings
FIG. 1 is an SEM photograph of nano-cerium oxide prepared in example 1 of the present invention
FIG. 2 is a flow chart of the preparation method of nano cerium oxide of the present invention
Detailed Description
The flow chart of the preparation method of the nano cerium oxide of the embodiments 1 to 10 of the present invention is shown in fig. 2.
Example 1
1.085g Ce (NO) was weighed out3)3﹒6H2Dissolving O in 1ml of deionized water; weighing 1.44g of citric acid, dissolving in 1.5ml of deionized water, mixing the two solutions, stirring for 1h at 30 ℃ without adjusting the pH value to form sol; adding 50ml of cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, sequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into the reactor, wrapping the sol by a surfactant to form a stable sol-reversed phase microemulsion system, keeping the temperature of a water bath unchanged, and continuously stirring for 3 hours to form gel particles; cooling the gel particles to 0-30 ℃, freezing, carrying out suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at-20 ℃; then, carrying out vacuum freeze drying for 24h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 500 ℃ for 3h to obtain the nano cerium oxide. The measured SEM image is shown in FIG. 1. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 90% at 52-82 nm.
Example 2
1.085g Ce (NO) was weighed out3)3﹒6H2Dissolving O in 1ml of deionized water; then weighing 1.41g of tartaric acid, dissolving in 1.5ml of deionized water, mixing the two solutions, stirring for 1h at 30 ℃ without adjusting the pH value to form sol; adding 50ml of cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, sequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into the reactor, wrapping the sol by a surfactant to form a stable sol-reversed phase microemulsion system, keeping the temperature of a water bath unchanged, and continuously stirring for 3 hours to form gel particles; cooling the gel particles to 0-30 ℃, freezing, carrying out suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at-20 ℃; then, carrying out vacuum freeze drying for 24h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 500 ℃ for 3h to obtain the nano cerium oxide. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 90% between 62 and 98 nm.
Example 3
1.085g Ce (NO) was weighed out3)3﹒6H2Dissolving O in 1ml of deionized water; weighing 1.44g of citric acid, dissolving in 1.5ml of deionized water, mixing the two solutions, adjusting the pH to 5 by using 25% ammonia water, and stirring for 1h at 30 ℃ to form sol; adding 50ml of cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, sequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into the reactor, wrapping the sol by a surfactant to form a stable sol-reversed phase microemulsion system, keeping the temperature of a water bath unchanged, and continuously stirring for 3 hours to form gel particles; cooling the gel particles to 0-30 ℃, freezing, carrying out suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at-20 ℃; then, carrying out vacuum freeze drying for 24h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 500 ℃ for 3h to obtain the nano cerium oxide. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 90% between 45 and 70 nm.
Example 4
1.085g Ce (NO) was weighed out3)3﹒6H2Dissolving O in 1ml of deionized water; weighing 1.44g of citric acid, dissolving in 1.5ml of deionized water, and mixingAfter the solutions are mixed, adjusting the pH value to 8 by using 25% ammonia water, and stirring for 1h at 30 ℃ to form sol; adding 50ml of cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, sequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into the reactor, wrapping the sol by a surfactant to form a stable sol-reversed phase microemulsion system, keeping the temperature of a water bath unchanged, and continuously stirring for 3 hours to form gel particles; cooling the gel particles to 0-30 ℃, freezing, carrying out suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at-20 ℃; then, carrying out vacuum freeze drying for 24h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 500 ℃ for 3h to obtain the nano cerium oxide. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 90% between 40 and 70 nm.
Example 5
1.085g Ce (NO) was weighed out3)3﹒6H2Dissolving O in 1ml of deionized water; weighing 1.44g of citric acid, dissolving in 1.5ml of deionized water, mixing the two solutions, adjusting the pH to 8 by using 25% ammonia water, and stirring for 1h at 30 ℃ to form sol; adding 50ml of cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, sequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into the reactor, wrapping the sol by a surfactant to form a stable sol-reversed phase microemulsion system, keeping the temperature of a water bath unchanged, and continuously stirring for 4.5 hours to form gel particles; cooling the gel particles to 0-30 ℃, freezing, carrying out suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at-20 ℃; then, carrying out vacuum freeze drying for 24h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 500 ℃ for 3h to obtain the nano cerium oxide. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 90% between 25 and 45 nm.
Example 6
1.085g Ce (NO) was weighed out3)3﹒6H2Dissolving O in 1ml of deionized water; weighing 1.44g of citric acid, dissolving in 1.5ml of deionized water, mixing the two solutions, adjusting the pH to 8 by using 25% ammonia water, and stirring for 1h at 30 ℃ to form sol; adding 50ml of cyclohexane into the reactor, starting stirring, and controlling the reaction systemSequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into a reactor at the temperature of 60 +/-2 ℃, wrapping the sol by a surfactant to form a stable sol-reverse microemulsion system, keeping the temperature of a water bath unchanged, and continuously stirring for 6 hours to form gel particles; cooling the gel particles to 0-30 ℃, freezing, carrying out suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at-20 ℃; then, carrying out vacuum freeze drying for 24h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 500 ℃ for 3h to obtain the nano cerium oxide. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 82% between 35 and 57 nm.
Example 7
Weighing 1.085gCe (NO)3)3﹒6H2Dissolving O in 1ml of deionized water; weighing 1.54g of citric acid, dissolving in 1.5ml of deionized water, mixing the two solutions, adjusting the pH to 8 by using 25% ammonia water, and stirring for 1h at 30 ℃ to form sol; adding 50ml of cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, sequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into the reactor, wrapping the sol by a surfactant to form a stable sol-reversed phase microemulsion system, keeping the temperature of a water bath unchanged, and continuously stirring for 4.5 hours to form gel particles; cooling the gel particles to 0-30 ℃, freezing, carrying out suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at-20 ℃; then, carrying out vacuum freeze drying for 36h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 400 ℃ for 4h to obtain the nano cerium oxide. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 90% between 25 and 45 nm.
Example 8
1.085g Ce (NO) was weighed out3)3﹒6H2Dissolving O in 1ml of deionized water; weighing 1.49g of citric acid, dissolving in 1.5ml of deionized water, mixing the two solutions, adjusting the pH to 8 by using 25% ammonia water, and stirring for 1h at 30 ℃ to form sol; adding 50ml cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, and sequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into the reactor, wherein the sol is coated by a surfactantWrapping to form a stable sol-reversed microemulsion system, keeping the temperature of the water bath unchanged, and continuously stirring for 4.5 hours to form gel particles; cooling the gel particles to 0-30 ℃, freezing, carrying out suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at-20 ℃; then, carrying out vacuum freeze drying for 48h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 600 ℃ for 2h to obtain the nano cerium oxide. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 90% between 25 and 45 nm.
Example 9
1.085g Ce (NO) was weighed out3)3﹒6H2Dissolving O in 1ml of deionized water; weighing 1.44g of citric acid, dissolving in 1.5ml of deionized water, mixing the two solutions, adjusting the pH to 8 by using 25% ammonia water, and stirring for 1h at 30 ℃ to form sol; adding 50ml of cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, sequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into the reactor, wrapping the sol by a surfactant to form a stable sol-reversed phase microemulsion system, keeping the temperature of a water bath unchanged, and continuously stirring for 4.5 hours to form gel particles; cooling the gel particles to 0-30 ℃, freezing, carrying out suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at-20 ℃; then, carrying out vacuum freeze drying for 24h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 400 ℃ for 3h to obtain the nano cerium oxide. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 90% between 17 and 45 nm.
Example 10
Weighing 1.085gCe (NO)3)3﹒6H2Dissolving O in 1ml of deionized water; weighing 1.44g of citric acid, dissolving in 1.5ml of deionized water, mixing the two solutions, adjusting the pH to 8 by using 25% ammonia water, and stirring for 1h at 30 ℃ to form sol; adding 50ml of cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, sequentially adding 0.87g of hexadecyl trimethyl ammonium bromide, 1.0ml of n-butyl alcohol and 1.5ml of prepared sol into the reactor, wrapping the sol by a surfactant to form a stable sol-reversed phase microemulsion system, keeping the temperature of a water bath unchanged, and continuously stirring for 4.5 hours to form gel particles; cooling the gel particles to 0 ℃Freezing at-30 deg.C, filtering at low temperature, and repeatedly washing with-20 deg.C anhydrous alcohol; then, carrying out vacuum freeze drying for 24h at the temperature of minus 60 ℃ to obtain a precursor; and calcining the precursor at 600 ℃ for 3h to obtain the nano cerium oxide. The distribution of the particle size of the cerium oxide was measured as shown in Table 1, and the particle size was 90% between 42 and 70 nm.
TABLE 1
As can be seen from the test results shown in Table 1, the nano cerium oxide particles prepared by the method have the advantages of average particle size of 31.84-77.16nm, narrow particle size distribution, no agglomeration phenomenon and good dispersibility. Through the adjustment of experimental parameters, the nano cerium oxide particles prepared by the method can be accurately controlled between 30 nm and 80nm, and the controllability of the particle size interval is realized.
The above description is only a preferred example of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like of the present invention shall be included in the protection scope of the present invention.
Claims (7)
1. A method for preparing nano cerium oxide particles is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing Ce (NO3)3, and dissolving in deionized water to obtain an aqueous solution, wherein the pH is 6H 2O; weighing a complexing agent, dissolving the complexing agent in deionized water to prepare an aqueous solution, mixing the two solutions to ensure that the concentration of Ce3+ in the system is 1mol/L, adjusting the pH to 1-8 with 25% ammonia water or not, and stirring for 1h at 30 ℃ to form sol;
(2) adding cyclohexane into a reactor, starting stirring, controlling the temperature of a reaction system to be 60 +/-2 ℃, sequentially adding a surfactant, a cosurfactant and the sol prepared in the step (1) into the reactor, and wrapping the sol by the surfactant to form a stable sol-reverse microemulsion system; keeping the temperature of the water bath unchanged, and continuously stirring for 3-6 h to form gel particles;
(3) cooling and freezing the gel particles obtained in the step (2), performing suction filtration at low temperature, and repeatedly washing with absolute ethyl alcohol at the temperature of minus 20 ℃;
(4) drying the gel particles washed in the step (3) in vacuum to remove moisture, thus obtaining a precursor;
(5) calcining the precursor in the step (4) at high temperature to obtain nano cerium oxide particles,
the surfactant is cetyl trimethyl ammonium bromide, the cosurfactant is n-butyl alcohol,
the vacuum drying in the step 4) is vacuum freeze drying, the drying temperature is-60 to-30 ℃, and the drying time is 24 to 48 hours.
2. The method for preparing nano cerium oxide particles according to claim 1, wherein: the complexing agent is any one of citric acid, tartaric acid, malic acid and polyethylene glycol.
3. The method for preparing nano cerium oxide particles according to claim 1, wherein: the complexing agent is citric acid or tartaric acid.
4. The method for preparing nano cerium oxide particles according to claim 1, wherein: the complexing agent and Ce (NO)3)3﹒6H2The mass ratio of O is 3 to 3.2: 1.
5. the method for preparing nano cerium oxide particles according to claim 1, wherein: the mass ratio of the surfactant to the cyclohexane is 1: 50; the mass ratio of the cosurfactant to the cyclohexane is 1: 45, wherein the volume ratio of the sol to the cyclohexane is 3: 100.
6. the method for preparing nano cerium oxide particles according to claim 1, wherein: the temperature for freezing the gel in the step 3) is 0 to-30 ℃.
7. The method for preparing nano cerium oxide particles according to claim 1, wherein: the calcination temperature in the step 5) is 400-600 ℃, and the time is 2-4 h.
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