CN111484053A - Preparation method of aluminum trioxide microspheres - Google Patents
Preparation method of aluminum trioxide microspheres Download PDFInfo
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- CN111484053A CN111484053A CN202010351405.5A CN202010351405A CN111484053A CN 111484053 A CN111484053 A CN 111484053A CN 202010351405 A CN202010351405 A CN 202010351405A CN 111484053 A CN111484053 A CN 111484053A
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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
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J20/282—Porous sorbents
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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
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
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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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
-
- 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
Abstract
The invention discloses a preparation method of aluminum trioxide microspheres, which comprises the following steps: adding the seed microspheres into an aqueous solution containing a dispersing agent, and fully mixing to form a uniformly dispersed seed suspension, wherein the seed microspheres account for less than 60% of the weight of the seed suspension; adding an initiator into an aqueous solution containing a dispersant, and fully mixing to obtain an initiator suspension; uniformly mixing a mixed solution of aluminum isopropoxide, an alcohol solvent and ammonia water to obtain a precursor mixed solution; at the polymerization temperature, dropwise adding an initiator suspension into the seed suspension, performing ultrasonic treatment, and then dropwise adding a precursor mixed solution; obtaining polymer/aluminum trioxide composite microspheres; and separating, drying and calcining the polymer/aluminum trioxide composite microspheres to finally obtain the aluminum trioxide microspheres. According to the method, the initiator suspension and the precursor mixed solution are sequentially added into the seed suspension, so that the raw materials are favorably dispersed, and the aluminum trioxide microspheres with uniform dispersion, uniform particle size and controllable particle size can be obtained.
Description
Technical Field
The invention relates to a preparation method of microspheres, and belongs to the technical field of preparation of aluminum trioxide microspheres.
Background
The aluminum trioxide microspheres have excellent physical and chemical properties such as high mechanical strength, good chemical stability, acid and alkali resistance, high melting point, boiling point, high specific surface area and the like, and are widely applied to the fields of solid fuel cells, chemical sensors, adsorption, separation, chromatographic packing, catalysis and the like. Taking porous aluminum trioxide as an example, in recent years, porous aluminum trioxide microspheres have prominent functions in the field of catalysis, such as hydrogenation, Friedel-crafts alkylation, esterification and isomerization of alkane of carbon monoxide. The porous aluminum trioxide microspheres have wide application prospect in the fields of catalysis, adsorption separation and the like due to the excellent characteristics of spherical morphology, high specific surface area, easiness in modification and the like. At present, the aluminum trioxide microspheres prepared by the prior art have uniform particle size and poor size controllability, and how to obtain the aluminum trioxide microspheres with uniform particle size and controllable size is a difficult point.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of aluminum trioxide microspheres.
In order to achieve the purpose, the invention adopts the following technical scheme:
the embodiment of the invention provides a preparation method of aluminum trioxide microspheres, which comprises the following steps:
adding the seed microspheres into an aqueous solution containing a dispersing agent, and fully mixing to form a uniformly dispersed seed suspension, wherein the seed microspheres account for less than 60% of the weight of the seed suspension;
adding an initiator into an aqueous solution containing a dispersant, and fully mixing to obtain an initiator suspension;
uniformly mixing a mixed solution of aluminum isopropoxide, an alcohol solvent and ammonia water to obtain a precursor mixed solution;
at the polymerization temperature, dropwise adding an initiator suspension into the seed suspension, performing ultrasonic treatment, and then dropwise adding a precursor mixed solution; obtaining polymer/aluminum trioxide composite microspheres;
and separating, drying and calcining the polymer/aluminum trioxide composite microspheres to finally obtain the aluminum trioxide microspheres.
Further, the seed microspheres are polystyrene seeds or styrene-divinylbenzene seeds, and the monomer is selected from one or more of styrene, divinylbenzene, 2, 4-dichlorostyrene, acrylic acid, methyl methacrylate, methyl acrylate, ethyl acrylate, vinyl acetate, glycidyl methacrylate or derivatives thereof.
Further, the initiator is an azo initiator or a peroxide initiator.
Further, the dispersing agent is at least one of polyethylene glycol, dextrin and polyvinylpyrrolidone.
Further, the calcination is a temperature rise section by section, and comprises the following steps: firstly heating to 300-350 ℃, keeping for at least 1.0h, then heating to 400-600 ℃, and keeping for at least 1.0 h.
Further, after the polymer/aluminum trioxide composite microspheres are obtained, the temperature is raised to 600 ℃ section by section, the temperature is maintained, and the firing is carried out for 6-12h, so that the porous aluminum trioxide microspheres are obtained.
The porous oxide microspheres can be applied to a high performance liquid chromatography stationary phase matrix, and have the advantages that: (1) the high-performance liquid chromatography has high mechanical strength and rigidity, and can realize the purpose of high-performance liquid chromatography; (2) the particle size is controllable, and particles with small and uniform particle size can be obtained; (3) the aperture is controllable; (4) easy bonding and can be widely used for preparing various types of chromatographic stationary phases.
Further, after obtaining the porous aluminum trioxide microspheres, the preparation method further comprises: and continuously heating to 700 ℃ and 1500 ℃, and burning for 2-10h at the temperature to obtain the solid aluminum trioxide microspheres.
The invention achieves the following beneficial effects: according to the method, the initiator suspension and the precursor mixed solution are sequentially added into the seed suspension, so that the raw materials are favorably dispersed, and the aluminum trioxide microspheres with uniform dispersion, uniform particle size and controllable particle size can be obtained.
Detailed Description
The invention is further described with reference to specific examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1:
adding styrene-divinylbenzene copolymer seed microspheres (the particle size is 5 mu m, and CV is 3%) into an aqueous solution containing dextrin, fully stirring to form a uniformly dispersed seed suspension, wherein the styrene-divinylbenzene copolymer seeds account for 45% of the weight of the seed suspension, the dextrin accounts for 8% of the weight of the seed microspheres, adding benzoyl peroxide into the aqueous solution containing polyvinylpyrrolidone, emulsifying to form an initiator suspension for later use, mixing 10% of aluminum isopropoxide, 40m L deionized water, 400m L isopropanol and 5m L28% of ammonia water, performing ultrasonic treatment for 2 hours, and uniformly mixing to obtain a precursor mixed solution.
Adding an initiator suspension into the seed suspension within 60 minutes at 70 ℃ to enable seeds to grow, stopping adding the initiator suspension after the particle size of the preset microspheres is reached, then dropwise adding 50m L precursor mixed solution into a reaction system of the solution within 2 hours under an ultrasonic environment, reacting for 24 hours at room temperature, then placing the polymer/aluminum trioxide composite microspheres into a 50 ℃ vacuum drying oven for drying, placing the dried polymer/aluminum trioxide composite microspheres into a muffle furnace, heating to 310 ℃, keeping at the temperature for 2 hours, heating to 450 ℃ for the second time, keeping at the temperature of 450 ℃ for 3 hours, finally heating to 600 ℃, keeping at the temperature for 6 hours, and finally obtaining the porous aluminum trioxide microspheres.
Example 2:
adding polystyrene seed microspheres (the particle size is 0.5 mu m, CV is 3%) into an aqueous solution containing polyethylene glycol, fully stirring to form a uniformly dispersed seed suspension, adding styrene-divinylbenzene copolymer seeds accounting for 45% of the weight of the seed suspension, the weight of the polyethylene glycol accounting for 8% of the weight of the seed microspheres, adding benzoyl peroxide into the aqueous solution containing polyvinylpyrrolidone, emulsifying to form an initiator suspension for later use, adding 10% of aluminum isopropoxide, 40m L deionized water, 400m L isopropanol and 5m L28% of ammonia water, performing ultrasonic treatment for 2 hours, and uniformly mixing to obtain a precursor mixed solution.
Adding an initiator suspension into the seed suspension within 60 minutes at 70 ℃ to enable seeds to grow, stopping adding the initiator suspension after the particle size of preset microspheres is reached, then dropwise adding 50m L precursor mixed solution into the reaction system containing the polymer microsphere solution within 2 hours under an ultrasonic environment, reacting for 24 hours at room temperature to obtain polymer/aluminum trioxide composite microspheres, then placing the polymer/aluminum trioxide composite microspheres into a 50 ℃ vacuum drying oven for drying, placing the dried polymer/aluminum trioxide composite microspheres in a muffle furnace, heating to 330 ℃, keeping for 1 hour, heating to 400 ℃ for the second time, keeping for 2 hours at 400 ℃, finally heating to 600 ℃, keeping the temperature for 6 hours of ignition, and finally obtaining the porous aluminum trioxide microspheres.
Example 3
Adding polystyrene seed microspheres (the particle size is 0.5 mu m, and CV is 2.8%) into an aqueous solution containing dextrin, fully stirring to form a uniformly dispersed seed suspension, adding styrene-divinylbenzene copolymer seeds which account for 55% of the weight of the seed suspension, and the dextrin which accounts for 9% of the weight of the seed microspheres, adding benzoyl peroxide into the aqueous solution containing polyvinylpyrrolidone, emulsifying to form an initiator suspension for later use, performing ultrasonic treatment for 2 hours after adding the initiator suspension containing 12% of aluminum isopropoxide, 40m L deionized water, 400m L isopropanol and 8m L28% of ammonia water, and uniformly mixing to obtain a precursor mixed solution.
Adding an initiator suspension into the seed suspension within 60 minutes at 70 ℃ to enable seeds to grow, stopping adding the initiator suspension after the particle size of the preset microspheres is reached, then dropwise adding 150m L precursor mixed solution into the reaction system containing the polymer microsphere solution within 2 hours under an ultrasonic environment, reacting for 24 hours at room temperature to obtain polymer/aluminum trioxide composite microspheres, then placing the polymer/aluminum trioxide composite microspheres into a 50 ℃ vacuum drying oven for drying, placing the dried polymer/aluminum trioxide composite microspheres into a muffle furnace, gradually heating to 600 ℃, maintaining the temperature, and burning for 6 hours to finally obtain the porous aluminum trioxide microspheres.
Example 4
Adding polystyrene seed microspheres (the particle size is 650 mu m, CV is 3%) into an aqueous solution containing dextrin, fully stirring to form a uniformly dispersed seed suspension, adding styrene-divinylbenzene copolymer seeds which account for 58% of the weight of the seed suspension, wherein the weight of the dextrin is 10% of the weight of the seed microspheres, adding benzoyl peroxide into the aqueous solution containing polyvinylpyrrolidone, emulsifying to form an initiator suspension for later use, mixing 10% of aluminum isopropoxide, 85m L deionized water, 420m L isopropanol and 7m L28% of ammonia water, and performing ultrasonic treatment for 2 hours to obtain a precursor mixed solution.
Adding an initiator suspension into the seed suspension within 60 minutes at 70 ℃ to enable seeds to grow, stopping adding the initiator suspension after the particle size of the microspheres reaches a preset value, then dropwise adding 110m L precursor mixed solution into a reaction system of the solution within 2 hours under an ultrasonic environment, reacting for 24 hours at room temperature to obtain polymer/aluminum trioxide composite microspheres, washing, drying in a 50 ℃ vacuum drying oven, heating to 350 ℃, keeping for 2 hours, heating to 600 ℃, maintaining the temperature, and burning for 6 hours to obtain the porous aluminum trioxide microspheres.
Example 5
Adding polystyrene seed microspheres (the particle size is 45 mu m, CV is 3%) into an aqueous solution containing dextrin, fully stirring to form a uniformly dispersed seed suspension, adding styrene-divinylbenzene copolymer seeds which account for 58% of the weight of the seed suspension, adding 10% of the weight of the dextrin which accounts for 10% of the weight of the seed microspheres, adding benzoyl peroxide into the aqueous solution containing polyvinylpyrrolidone, emulsifying to form an initiator suspension for later use, mixing 10% of aluminum isopropoxide, 85m L deionized water, 420m L isopropanol and 7m L28% of ammonia water, and performing ultrasonic treatment for 2 hours to obtain a precursor mixed solution.
Adding an initiator suspension into the seed suspension within 60 minutes at 70 ℃ to enable seeds to grow, stopping adding the initiator suspension after the particle size of the preset microspheres is reached, then dropwise adding 110m L precursor mixed liquor into the reaction system within 2 hours in an ultrasonic environment, reacting for 24 hours at room temperature to obtain polymer/aluminum trioxide composite microspheres, washing, drying in a 50 ℃ vacuum drying oven, gradually heating to 600 ℃ in a muffle furnace, maintaining the temperature for 6 hours, continuously heating to 950 ℃, and burning for 7 hours to obtain the solid aluminum trioxide microspheres.
Comparative example 1
The porogen cyclohexane was added and the remaining conditions were the same as in example 1.
Comparative example 2
The same conditions as in example 1 were followed without sonication and with direct addition of aluminium chloride.
Taking example 1 as an example, the results of comparison with comparative examples 1 and 2 are as follows:
wherein, the particle size and the particle size distribution are measured by a Beckman Counter, and the average pore diameter and the specific surface area in the porous zirconium dioxide microspheres are measured by a BET instrument.
From the above table, it is understood that porous aluminum trioxide microspheres having a large specific surface area can be obtained without adding a porogen, and from examples 2 and 3, porous aluminum trioxide microspheres having different particle diameters can be obtained by controlling the reaction conditions using seed microspheres having the same size.
In the embodiment of the invention, the seed microspheres are used for swelling, aluminum isopropoxide enters the inside of the swollen seed microspheres, the particle size of the generated microspheres can be effectively controlled by controlling the adding sequence and the adding amount of the seed suspension, the initiator suspension, the precursor mixed solution and the like, and the uniformity of the generated microspheres is improved. Furthermore, porous or solid aluminum trioxide microspheres can be obtained by controlling the calcination conditions.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of aluminum trioxide microspheres is characterized by comprising the following steps:
adding the seed microspheres into an aqueous solution containing a dispersing agent, and fully mixing to form a uniformly dispersed seed suspension, wherein the seed microspheres account for less than 60% of the weight of the seed suspension;
adding an initiator into an aqueous solution containing a dispersant, and fully mixing to obtain an initiator suspension;
uniformly mixing a mixed solution of aluminum isopropoxide, an alcohol solvent and ammonia water to obtain a precursor mixed solution;
at the polymerization temperature, dropwise adding an initiator suspension into the seed suspension, performing ultrasonic treatment, and then dropwise adding a precursor mixed solution; obtaining polymer/aluminum trioxide composite microspheres;
and separating, drying and calcining the polymer/aluminum trioxide composite microspheres to finally obtain the aluminum trioxide microspheres.
2. The method for preparing aluminum trioxide microspheres according to claim 1, wherein the seed microspheres are polystyrene seeds or styrene-divinylbenzene seeds, and the monomer is selected from one or more of styrene, divinylbenzene, 2, 4-dichlorostyrene, acrylic acid, methyl methacrylate, methyl acrylate, ethyl acrylate, vinyl acetate, glycidyl methacrylate or derivatives thereof.
3. The method for preparing aluminum trioxide microspheres according to claim 1 or 2, wherein the initiator is an azo initiator or a peroxide initiator.
4. The method for preparing microspheres of aluminum trioxide according to claim 1, wherein the dispersant is at least one of polyethylene glycol, dextrin and polyvinylpyrrolidone.
5. The method for preparing the aluminum trioxide microspheres according to claim 1, wherein the calcining is carried out at an elevated temperature section by section, and comprises the following steps: firstly heating to 300-350 ℃, keeping for at least 1.0h, then heating to 400-600 ℃, and keeping for at least 1.0 h.
6. The method for preparing aluminum trioxide microspheres according to claim 1, wherein after the polymer/aluminum trioxide composite microspheres are obtained, the temperature is raised to 600 ℃ section by section, and the temperature is maintained and the firing is carried out for 6-12h, so as to obtain the porous aluminum trioxide microspheres.
7. The method of claim 6, wherein after obtaining the porous aluminum trioxide microspheres, the method further comprises: and continuously heating to 700 ℃ and 1500 ℃, and burning for 2-10h at the temperature to obtain the solid aluminum trioxide microspheres.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112403032A (en) * | 2020-11-18 | 2021-02-26 | 中国核动力研究设计院 | In homogeneous water solution nuclear reactor fuel solution99Mo、131I co-extraction method |
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