CN108585798B - Nano porous alumina aerogel ceramic pellet and preparation method thereof - Google Patents
Nano porous alumina aerogel ceramic pellet and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a nano porous alumina aerogel ceramic pellet, wherein the diameter of the pellet is 0.2-2mm, the pore diameter is 5-15nm, and the specific surface area is 200-500 m2(iv)/g, white or translucent color, prepared as follows: (1): preparing aluminum sol containing polyvinyl alcohol; (2): preparing an oil ammonia column solution; (3): balling; (4): aging; (5): supercritical drying; (6): and (6) heat treatment. The method improves the balling property by adding polyvinyl alcohol to improve the surface tension, simultaneously combines the sol-gel technology and the aerogel drying technology to ensure the nano-pore structure of the pellet, and finally obtains the alumina aerogel ceramic pellet with certain strength, and simultaneously reserves the nano-pore structure and high specific surface area through thermal sintering. The method has the advantages of simple process, low cost and high sphericity, and is favorable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of nano-porous aerogel ceramics, and particularly relates to a nano-porous alumina aerogel ceramic pellet and a preparation method thereof.
Background
The aerogel is a solid material with a porous structure formed by mutually aggregating nano particles, and has a plurality of excellent performances such as high porosity, low density, large specific surface area, low thermal conductivity, low sound velocity, low refractive index and the like. These excellent properties have led to the wide use of aerogels in a variety of applications, such as high efficiency thermal insulation materials, sound insulation materials, catalysts and catalyst supports, aerospace materials, and rechargeable battery supports. At present, most applied silica aerogel is sintered when used at a high temperature, the structural characteristics of the nano-porous silica aerogel can not be maintained, the long-term use temperature of the silica aerogel is generally not higher than 650 ℃, and meanwhile, the structural strength of the aerogel is low and the silica aerogel is difficult to use in some environments. In order to adapt to the conditions of higher use temperature and certain requirement on strength in some special fields (such as aerospace, high-temperature catalysis and the like), the search for a nano-porous aerogel ceramic material which is resistant to higher temperature and has a nano-porous structure and a certain strength has become one of important development directions.
In a plurality of material systems, the alumina has higher use temperature (the melting point is as high as 2054 ℃ and the boiling point is 2980 ℃), and is an ideal choice for preparing the high-temperature resistant aerogel ceramic material. Meanwhile, if the macroscopic structure of the nano porous aerogel ceramic is made into a spherical shape, the application range and the efficiency of the nano porous aerogel ceramic in the fields of heat insulation, catalysis, chromatographic filling and the like can be greatly expanded. And the aerogel ceramic beads are convenient to use and easy to recover, are easier to exchange solvents and quickly dry, shorten the production period and are beneficial to industrial production. At present, no relevant patent literature is found to prepare alumina aerogel ceramic beads, and more silica aerogel beads and alumina ceramic beads are used, so that the nano porous alumina aerogel ceramic beads have wide application prospects.
Disclosure of Invention
The invention aims to provide a porous alumina aerogel ceramic pellet with high sphericity, high specific surface area, high strength and the like, and also provides a method for quickly preparing the alumina aerogel ceramic pellet with simple process and low preparation cost. In order to achieve the above objects, the present invention discloses a preparation method for obtaining alumina aerogel ceramic beads by a smart and fast process.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a nano porous alumina aerogel ceramic pellet, the diameter of the pellet is 0.2-2mm, the aperture is 5-15nm, and the specific surface area is 200-500 m 2/g; the beads are white or translucent in color.
Further, the preparation method of the nano porous alumina aerogel ceramic beads comprises the following steps:
SS01 preparation of polyvinyl alcohol-containing aluminum sol:
mixing an aluminum source: solvent: chelating agent: acid: water = 1: 3-12: 0.1-0.4: 0.3-0.5: sequentially adding 20-40 into a container, and stirring for 30-60min under the water bath condition at the temperature of 65-85 ℃; forming clear and transparent aluminum sol; then adding polyvinyl alcohol with the mass fraction of 0.2-2% (the mass fraction of the polyvinyl alcohol to the aluminum source) and continuing stirring for 30-60 min; after the polyvinyl alcohol is completely melted into the transparent sol; cooling to room temperature; namely, the aluminum sol containing polyvinyl alcohol is prepared.
SSO2 preparation of oil ammonia column solution:
preparing an ammonia water solution (water is a solvent) with the concentration of 5-15% in a container; adding a certain amount of paraffin oil or n-hexane into a container; controlling the height of the paraffin oil to be 2-5 cm; due to differences in density and compatibility; thus, paraffin oil or n-hexane is formed on the upper layer; the ammonia water solution is in the lower layer of the oil ammonia column solution.
SS03 balling:
dripping the prepared polyvinyl alcohol-containing aluminum sol into the oil ammonia column solution at the speed of 60-100 drops/min by using an injector with the inner diameter of a pipe of 0.4-2.2 mm; thus obtaining the alumina gel beads.
Aging in SS04, supercritical drying:
aging and replacing in ethanol for 12-24 h; replacing the ethanol every 6 hours; finally, the alumina aerogel pellet can be prepared by supercritical drying.
SS05 heat treatment:
the prepared alumina aerogel pellet is firstly insulated for 1-2h at the temperature of 300-400 ℃; then heating to 1000-1200 ℃ for heat treatment for 2-4 h; thus obtaining the alumina aerogel ceramic pellet.
Further, the aluminum source is any one of aluminum isopropoxide, aluminum nitrate, aluminum chloride and boehmite powder; aluminum isopropoxide is preferred.
Further, the alcohol solvent is any one of ethanol or methanol; ethanol is preferred.
Further, the chelating agent is any one of ethyl acetoacetate or acetylacetone; ethylacetoacetate is preferred.
Further, the acid is any one of hydrochloric acid, nitric acid, acetic acid or oxalic acid; nitric acid is preferred.
Further, the alcoholysis degree of the polyvinyl alcohol is 86-90%; the molecular weight of the polyvinyl alcohol is 100000-170000.
Further, the supercritical fluid drying is to take ethanol as a drying medium; pre-charging 2-3 MPa nitrogen; then heating to 260-270 ℃ at the speed of 1-2 ℃/min; preserving the heat for 1 to 3 hours; releasing the pressure to normal pressure at the speed of 200 and 300 kPa/min; the pressure release process keeps the temperature constant; finally flushing nitrogen for 20-30 min; cooling to room temperature and taking out.
The invention has the following beneficial effects:
the alumina aerogel ceramic beads with high sphericity, high specific surface area and high strength can be rapidly and continuously prepared in a large scale by blending the aluminum sol containing the polyvinyl alcohol and utilizing the cross-linking and shaping effects of the polyvinyl alcohol, so that the spherical shape is better, the later removal is convenient, and the requirements of various aspects are met.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a graph showing the pore size distribution of alumina aerogel ceramic beads after heat treatment in example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
As shown in fig. 1, SS01 was formulated with an aluminum sol containing polyvinyl alcohol:
aluminum isopropoxide: ethanol: ethyl acetoacetate: nitric acid: water = 1: 8: 0.2: 0.2: 30 are sequentially added into a container and stirred for 30min under the condition of water bath with the temperature of 80 ℃ to form clear and transparent aluminum sol. Then adding 0.5 percent of polyvinyl alcohol by mass fraction, continuing stirring for 30min, cooling to room temperature after the polyvinyl alcohol is completely dissolved in the transparent sol, and preparing the aluminum sol containing polyvinyl alcohol.
SSO2 preparation of oil ammonia column solution:
the ammonia water solution with the concentration of 10% is prepared in a container, a certain amount of paraffin oil is added in the container, the height of the paraffin oil is controlled to be 5cm, and due to the difference of density and compatibility, the oil ammonia column solution with the paraffin oil at the upper layer and the ammonia water solution at the lower layer is formed.
SS03 balling:
dropping the prepared polyvinyl alcohol-containing aluminum sol into the oil ammonia column solution at the rate of 60 drops/min by using an injector with the inner diameter of a pipe being 1.0 mm to prepare the alumina gel beads.
Aging in SS04, supercritical drying:
and then aging and replacing the mixture in ethanol for 24 hours, replacing the ethanol every 6 hours, and finally performing supercritical drying to obtain the alumina aerogel beads, wherein the supercritical fluid drying is to use the ethanol as a drying medium, pre-flush 2 MPa of nitrogen, heat the mixture to 260 ℃ at the speed of 1 ℃/min, preserve the heat for 1 hour, release the pressure to the normal pressure at the speed of 200 kPa/min, keep the temperature constant in the pressure release process, flush 30 minutes of nitrogen, cool the mixture to the room temperature and take the mixture out.
SS05 heat treatment:
and (3) firstly preserving the temperature of the prepared alumina aerogel spheres for 1h at 400 ℃, and then heating the alumina aerogel spheres to 1100 ℃ for heat treatment for 2h to obtain the alumina aerogel ceramic spheres.
The diameter of the aerogel ceramic bead is 5-15nm, and the specific surface area is 200-500 m 2/g.
Example two
SS01 preparation of polyvinyl alcohol-containing aluminum sol:
aluminum nitrate: ethanol: ethyl acetoacetate: nitric acid: water = 1: 8: 0.2: 0.1: 30 are sequentially added into a container and stirred for 30min under the condition of water bath with the temperature of 80 ℃ to form clear and transparent aluminum sol. And then adding 1% polyvinyl alcohol by mass, continuing stirring for 30min, cooling to room temperature after the polyvinyl alcohol is completely dissolved in the transparent sol, and configuring to obtain the polyvinyl alcohol-containing aluminum sol.
SSO2 preparation of oil ammonia column solution:
the ammonia water solution with the concentration of 10% is prepared in a container, a certain amount of paraffin oil is added in the container, the height of the paraffin oil is controlled to be 5cm, and due to the difference of density and compatibility, the oil ammonia column solution with the paraffin oil at the upper layer and the ammonia water solution at the lower layer is formed.
SS03 balling:
dropping the prepared polyvinyl alcohol-containing aluminum sol into the oil ammonia column solution at the rate of 60 drops/min by using an injector with the inner diameter of a pipe being 1.0 mm to prepare the alumina gel beads.
Aging in SS04, supercritical drying:
and then aging and replacing the mixture in ethanol for 24 hours, replacing the ethanol every 6 hours, and finally performing supercritical drying to obtain the alumina aerogel beads, wherein the supercritical fluid drying is to use the ethanol as a drying medium, pre-flush 2 MPa of nitrogen, heat the mixture to 260 ℃ at the speed of 1 ℃/min, preserve the heat for 1 hour, release the pressure to the normal pressure at the speed of 200 kPa/min, keep the temperature constant in the pressure release process, flush 30 minutes of nitrogen, cool the mixture to the room temperature and take the mixture out.
SS05 heat treatment:
and (3) firstly preserving the temperature of the prepared alumina aerogel spheres for 1h at 400 ℃, and then heating the alumina aerogel spheres to 1100 ℃ for heat treatment for 2h to obtain the alumina aerogel ceramic spheres.
EXAMPLE III
SS01 preparation of polyvinyl alcohol-containing aluminum sol:
mixing aluminum chloride: ethanol: ethyl acetoacetate: nitric acid: water = 1: 8: 0.2: 0.1: 30 are sequentially added into a container and stirred for 30min under the condition of water bath with the temperature of 80 ℃ to form clear and transparent aluminum sol. And then adding 1% polyvinyl alcohol by mass, continuing stirring for 60min, cooling to room temperature after the polyvinyl alcohol is completely dissolved in the transparent sol, and configuring to obtain the polyvinyl alcohol-containing aluminum sol.
SSO2 preparation of oil ammonia column solution:
preparing an ammonia water solution with the concentration of 10% in a container, adding a certain amount of paraffin oil into the container, controlling the height of normal hexane to be 5cm, and forming an oil ammonia column solution with the paraffin oil at the upper layer and the ammonia water solution at the lower layer due to different densities and compatibilities.
SS03 balling:
dropping the prepared polyvinyl alcohol-containing aluminum sol into the oil ammonia column solution at the rate of 60 drops/min by using an injector with the inner diameter of a pipe being 1.0 mm to prepare the alumina gel beads.
Aging in SS04, supercritical drying:
and then aging and replacing the mixture in ethanol for 24 hours, replacing the ethanol every 6 hours, and finally performing supercritical drying to obtain the alumina aerogel beads, wherein the supercritical fluid drying is to use the ethanol as a drying medium, pre-flush 2 MPa of nitrogen, heat the mixture to 260 ℃ at the speed of 1 ℃/min, preserve the heat for 1 hour, release the pressure to the normal pressure at the speed of 200 kPa/min, keep the temperature constant in the pressure release process, flush 30 minutes of nitrogen, cool the mixture to the room temperature and take the mixture out.
SS05 heat treatment:
and (3) firstly preserving the temperature of the prepared alumina aerogel spheres for 1h at 400 ℃, and then heating the alumina aerogel spheres to 1100 ℃ for heat treatment for 2h to obtain the alumina aerogel ceramic spheres.
Example four
SS01 preparation of polyvinyl alcohol-containing aluminum sol:
aluminum isopropoxide: ethanol: ethyl acetoacetate: nitric acid: water = 1: 8: 0.2: 0.1: 30 are sequentially added into a container and stirred for 30min under the condition of water bath with the temperature of 80 ℃ to form clear and transparent aluminum sol. And then adding 1% polyvinyl alcohol by mass, continuing stirring for 60min, cooling to room temperature after the polyvinyl alcohol is completely dissolved in the transparent sol, and configuring to obtain the polyvinyl alcohol-containing aluminum sol.
SSO2 preparation of oil ammonia column solution:
preparing an ammonia water solution with the concentration of 10% in a container, adding a certain amount of n-hexane into the container, controlling the height of the n-hexane to be 5cm, and forming an oil ammonia column solution with the n-hexane on the upper layer and the ammonia water solution on the lower layer due to different densities and compatibilities.
SS03 balling:
dropping the prepared polyvinyl alcohol-containing aluminum sol into the oil ammonia column solution at the rate of 60 drops/min by using an injector with the inner diameter of a pipe being 1.0 mm to prepare the alumina gel beads.
Aging in SS04, supercritical drying:
and then aging and replacing the mixture in ethanol for 24 hours, replacing the ethanol every 6 hours, and finally performing supercritical drying to obtain the alumina aerogel beads, wherein the supercritical fluid drying is to use the ethanol as a drying medium, pre-flush 2 MPa of nitrogen, heat the mixture to 260 ℃ at the speed of 1 ℃/min, preserve the heat for 1 hour, release the pressure to the normal pressure at the speed of 200 kPa/min, keep the temperature constant in the pressure release process, flush 30 minutes of nitrogen, cool the mixture to the room temperature and take the mixture out.
SS05 heat treatment:
and (3) firstly preserving the temperature of the prepared alumina aerogel spheres for 1h at 400 ℃, and then heating the alumina aerogel spheres to 1100 ℃ for heat treatment for 2h to obtain the alumina aerogel ceramic spheres.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (5)
1. The preparation method of the nano porous alumina aerogel ceramic beads is characterized in that the diameter of each bead is 0.2-2mm, the pore diameter is 5-15nm, and the specific surface area is 200-500 m2(iv)/g, white or translucent color, prepared as follows:
(1): mixing an aluminum source: solvent: chelating agent: acid: water = 1: 3-12: 0.1-0.4: 0.3-0.5: 20-40, sequentially adding the mixture into a container, stirring the mixture for 30-60min under a water bath condition at the temperature of 65-85 ℃ to form clear and transparent aluminum sol, then adding 0.2-2% by mass of polyvinyl alcohol, and continuously stirring the mixture for 30-60min, wherein the alcoholysis degree of the polyvinyl alcohol is 86-90%, the molecular weight of the polyvinyl alcohol is 100000-170000, and after the polyvinyl alcohol is completely melted into the transparent sol, cooling the transparent sol to room temperature, and configuring the mixture to obtain the polyvinyl alcohol-containing aluminum sol;
(2): preparing an ammonia water solution with the concentration of 5-15% in a container, adding a certain amount of paraffin oil or n-hexane in the container, and controlling the paraffin oil height to be 2-5cm, wherein due to different densities and compatibility, an oily ammonia column solution with the paraffin oil or n-hexane on the upper layer and the ammonia water solution on the lower layer is formed;
(3): dripping the prepared polyvinyl alcohol-containing aluminum sol into the oil ammonia column solution by using an injector with the inner diameter of a pipe being 0.4-2.2mm at the speed of 60-100 drops/min to prepare the alumina gel beads;
(4): aging and replacing in ethanol for 12-24h, replacing the ethanol every 6 h, and finally performing supercritical drying to obtain alumina aerogel spheres;
the supercritical fluid drying is carried out by taking ethanol as a drying medium, pre-charging 2-3 MPa of nitrogen, heating to 260-270 ℃ at the speed of 1-2 ℃/min, preserving heat for 1-3 hours, releasing pressure to normal pressure at the speed of 200-300 kPa/min, keeping the temperature constant in the pressure releasing process, finally purging the nitrogen for 20-30min, cooling to room temperature and taking out;
(5): and (3) firstly preserving the heat of the prepared alumina aerogel pellets for 1-2h at 300-400 ℃, and then heating the alumina aerogel pellets to 1000-1200 ℃ for heat treatment for 2-4h to obtain the alumina aerogel ceramic pellets.
2. The method for preparing nanoporous alumina aerogel ceramic beads according to claim 1, wherein the aluminum source in (1) is any one of aluminum isopropoxide, aluminum nitrate and boehmite powder.
3. The method for preparing nanoporous alumina aerogel ceramic beads according to claim 1, wherein the solvent in (1) is ethanol or methanol.
4. The method for preparing nano porous alumina aerogel ceramic beads as claimed in claim 1, wherein the chelating agent in (1) is ethyl acetoacetate or acetylacetone.
5. The method for preparing nanoporous alumina aerogel ceramic beads according to claim 1, wherein the acid in (1) is any one of hydrochloric acid, nitric acid, acetic acid or oxalic acid.
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