CN111138174A - Preparation method of alumina-based foamed ceramic spherical shell for civil air defense engineering - Google Patents
Preparation method of alumina-based foamed ceramic spherical shell for civil air defense engineering Download PDFInfo
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Abstract
The invention relates to a preparation method of an alumina-based foam ceramic spherical shell for civil air defense engineering. The technical scheme is as follows: 67-80 wt% of bauxite powder, 15-18 wt% of Guangxi white mud and 5-13 wt% of kaolin are used as raw materials, 10-15 wt% of a bonding agent, 10-40 wt% of water and 40-80 wt% of a pore-forming agent are added, and the raw materials are uniformly mixed to obtain the pug. Filling the pug into a hemispherical shell mold with the outer diameter of 8-12 cm and the inner diameter of 4-6 cm, pressing under 1-4 Mpa to prepare a hemispherical shell green body, butting the side openings of the hemispherical shells under the same pressure to combine into a hollow sphere, and demolding. Curing at 25 ℃ for 2-5 h, drying at 60-110 ℃ for 6-12 h, placing in an air atmosphere, heating to 1100-1300 ℃ at 1-5 ℃/min, preserving heat for 1-2 h, sintering and sealing to obtain the alumina-based foamed ceramic spherical shell. The method has the advantages of cheap and easily-obtained raw materials, high production efficiency, no by-product in the production process, safety and environmental protection, and capability of realizing automatic production.
Description
Technical Field
The invention belongs to the technical field of foam ceramic spherical shells. In particular to a preparation method of an alumina-based foam ceramic spherical shell for civil air defense engineering.
Background
The foamed ceramic spherical shell is a novel protective material emerging in the field of protective engineering, and has the dual characteristics of high energy absorption of a porous material and high strength of a shell structure; in the aspect of energy absorption, the porous material and the shell structure can also generate an interaction effect, and the energy absorption effect is greater than the energy absorption effect superposition of the independent porous material and the independent shell structure under the same loading condition, so that the porous material and the shell structure have wide application space in the fields of impact dynamics, civil air defense engineering and the like.
Xuxing star et al (Xuxing star, Qifei, Wang Xianhui, etc. hollow sphere coating treatment for preparing alumina porous ceramic [ J ] silicate science, 2014, 42 (9): 1134) 1139) presintering the alumina hollow sphere at 1200 ℃ by adopting a slurry impregnation method, adding kaolin, talcum powder, water and a dispersing agent into a ball-milling tank according to a certain proportion, and carrying out ball milling for 8 hours to prepare slurry; adding a certain amount of presintered alumina hollow spheres into the slurry for dipping and coating, uniformly stirring for 10min, heating and evaporating water in the slurry to dryness under the stirring condition, and completely drying the alumina hollow spheres to obtain the alumina hollow spheres coated with kaolin and talcum powder; and finally, preserving the heat at 1500 ℃ for 2h to prepare the alumina porous hollow sphere. The technology is complex in process, and only the alumina porous hollow spheres with the sphere body of less than 20mm and the sphere shell thickness of less than 5mm can be prepared, and the thicknesses of the prepared alumina porous hollow sphere shells are not uniform.
The Chinese invention patent 'foamed ceramic microsphere with core-shell structure and preparation method and application thereof, 201610319091.4' discloses the following technology: firstly, preparing silica sol with sol particles of 35-100 nm, and then adding electrolyte and ammonia water to gelatinize the silica sol to obtain silica gel; adding the silica gel into heat-conducting oil containing 6-10% dilute sulfuric acid, and stirring for 5-7 h at the temperature of 300-360 ℃ to obtain silicic acid xerogel microspheres; and finally, washing, drying and foaming at 1300-1400 ℃ to obtain the foamed ceramic microspheres with the core-shell structure. The particle size of the foamed ceramic microspheres prepared by the technology is only 0.3-5 mm, the process is complex, byproducts in the production process are harmful to the environment, and the energy consumption is high.
The parameter indexes corresponding to the national standard (GB/T3995-2014) of the high-alumina heat-insulating refractory brick which is also a foam ceramic material show that when the volume density of the material is 0.8 g/cm3In the process, the static strength at normal temperature is 2.5MPa, and the low density and the high strength of the foamed ceramic material are in contradiction, so that the technical requirements of the civil air defense engineering on the low density and the high strength of the foamed ceramic spherical shell cannot be met.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the alumina-based foamed ceramic spherical shell for civil air defense engineering and the preparation method thereof.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
step one, taking 67-80 wt% of bauxite powder, 15-18 wt% of Guangxi white mud and 5-13 wt% of kaolin as raw materials, adding 10-15 wt% of a bonding agent, 10-40 wt% of water and 40-80 wt% of a pore-forming agent, and uniformly mixing to obtain a pug;
and step two, filling the pug into a hemispherical shell mold with the outer diameter of 8-12 cm and the inner diameter of 4-6 cm, pressing under 1-4 Mpa to prepare a hemispherical shell green body, butting and combining the side openings of the hemispherical shells into a hollow sphere under the same pressure, and demolding. Curing at 25 ℃ for 2-5 h, and drying at 60-110 ℃ for 6-12 h to obtain an alumina-based foamed ceramic spherical shell blank;
and step three, placing the alumina-based foamed ceramic spherical shell blank in an air atmosphere, heating to 1100-1300 ℃ at the speed of 1-5 ℃/min, preserving the heat for 1-2 hours, and cooling to room temperature to obtain the alumina-based foamed ceramic spherical shell.
The particle size of the bauxite powder is 10-90 mu m.
The particle size of the Guangxi white mud is 10-90 mu m.
The particle size of the kaolin is 10-90 mu m.
The pore-forming agent is at least one of carbon powder, fly ash floating beads and sawdust.
The binding agent is at least one of sodium carboxymethyl cellulose, ethyl cellulose and hydroxyethyl cellulose.
The molding mode is compression molding, and the molding pressure is between 1 and 4 Mpa.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
the invention relates to a preparation method of an alumina-based foamed ceramic spherical shell for civil air defense engineering, which uses natural mineral powder as main raw materials, and has the advantages of cheap and easily obtained raw materials, low cost and excellent normal-temperature mechanical property; the invention adopts a compression molding process, has simple operation, can realize automatic production and high production efficiency, and can further control the sphere size and the wall thickness of the alumina-based foamed ceramic spherical shell by controlling the cavity of the mold. The invention adopts the method of adding the pore-forming agent to prepare the alumina-based foam ceramic spherical shell, and can further control the porosity, density and aperture size of the alumina-based foam ceramic spherical shell and the corresponding normal-temperature mechanical property thereof by controlling the addition amount of the pore-forming agent and the particle size of the pore-forming agent. The pore-forming agent used in the invention is at least one of carbon powder, fly ash floating beads and saw dust, and the pore-forming agent does not generate toxic gas in the sintering process, thereby being safe and environment-friendly.
Therefore, the invention has the characteristics of simple process, low cost, high production efficiency, easy product forming and easy process control, and the size of the sphere, the wall thickness of the spherical shell, the porosity, the density, the pore size and the normal-temperature mechanical property of the alumina-based foamed ceramic spherical shell prepared by the method are controllable.
Drawings
FIG. 1 is a semi-spherical alumina-based foamed ceramic shell blank for civil air defense engineering;
FIG. 2 is a diagram of a bauxite-based foamed ceramic spherical shell for civil air defense engineering prepared by the present invention.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope. The starting materials and reagents required in the embodiments are commercially available.
In order to avoid repetition, the raw materials of the present specific embodiment are described as follows, and are not described in the embodiments again:
the particle size of the bauxite powder is 10-90 mu m.
The particle size of the Guangxi white mud is 10-90 mu m.
The particle size of the kaolin is 10-90 mu m.
The pore-forming agent is at least one of carbon powder, fly ash floating beads and sawdust.
The binding agent is at least one of sodium carboxymethyl cellulose, ethyl cellulose and hydroxyethyl cellulose.
Example 1
An alumina-based foamed ceramic spherical shell for civil air defense engineering and a preparation method thereof are provided, and the preparation method comprises the following steps:
step one, taking 67-75 wt% of bauxite powder, 15-16 wt% of Guangxi white mud and 5-10 wt% of kaolin as raw materials, adding 10-12 wt% of a bonding agent, 10-20 wt% of water and 40-80 wt% of a pore-forming agent, and uniformly mixing to obtain the pug.
Filling the pug into a hemispherical shell mold with the outer diameter of 8-12 cm and the inner diameter of 4-6 cm, pressing under 1-2 Mpa to prepare a hemispherical shell green body 1, wherein the middle part of the hemispherical shell green body 1 is a hollow hemisphere 3, and the cross section of the hemispherical shell green body 1 is of an annular structure 2;
and (3) butting the edge openings of the two semi-spherical shell green bodies 1 under the same pressure to combine into a hollow sphere 4, and demolding. Curing at 25 ℃ for 2-3 h, and drying at 60-80 ℃ for 6-12 h to obtain an alumina-based foamed ceramic spherical shell blank.
And step three, placing the alumina-based foamed ceramic spherical shell blank in an air atmosphere, heating to 1100-1200 ℃ at the speed of 1-2 ℃/min, preserving the heat for 1-2 hours, and cooling to room temperature to obtain the alumina-based foamed ceramic spherical shell.
The pore-forming agent is carbon powder; the binding agent is sodium carboxymethyl cellulose. The volume density of the obtained alumina-based foamed ceramic spherical shell matrix material is 0.7-1.2 g/cm3And the normal-temperature compressive strength is 5-8 MPa.
Example 2
An alumina-based foam ceramic spherical shell for civil air defense engineering and a preparation method thereof. In this example, the procedure is the same as in example 1 except for step three:
and step three, placing the alumina-based foamed ceramic spherical shell blank in an air atmosphere, heating to 1200-1300 ℃ at the speed of 1-2 ℃/min, preserving the heat for 1-2 h, and cooling to room temperature to obtain the alumina-based foamed ceramic spherical shell.
The pore-forming agent is carbon powder; the binding agent is sodium carboxymethyl cellulose. The volume density of the obtained alumina-based foamed ceramic spherical shell matrix material is 1.0-1.5 g/cm3And the normal-temperature compressive strength is 6-10 MPa.
Example 3
An alumina-based foam ceramic spherical shell for civil air defense engineering and a preparation method thereof. The preparation method in this example is:
step one, taking 67-75 wt% of bauxite powder, 16-18 wt% of Guangxi white mud and 10-13 wt% of kaolin as raw materials, adding 12-14 wt% of a bonding agent, 20-30 wt% of water and 40-80 wt% of a pore-forming agent, and uniformly mixing to obtain the pug.
And step two, filling the pug into a hemispherical shell mold with the outer diameter of 8-12 cm and the inner diameter of 4-6 cm, pressing the mixture into a hemispherical shell green body under 2-3 Mpa, butting and combining the side openings of the hemispherical shells into a hollow sphere under the same pressure, and demolding. Curing at 25 ℃ for 3-4 h, and drying at 80-100 ℃ for 6-12 h to obtain an alumina-based foamed ceramic spherical shell blank.
And step three, placing the alumina-based foamed ceramic spherical shell blank in an air atmosphere, heating to 1100-1200 ℃ at the speed of 2-5 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain the alumina-based foamed ceramic spherical shell.
The pore-forming agent is fly ash floating beads; the binder is ethyl cellulose. The volume density of the obtained alumina-based foamed ceramic spherical shell matrix material is 0.6-1.1 g/cm3And the normal-temperature compressive strength is 4-8 MPa.
Example 4
An alumina-based foam ceramic spherical shell for civil air defense engineering and a preparation method thereof. This example is the same as example 3 except for the third step:
and step three, placing the alumina-based foamed ceramic spherical shell blank in an air atmosphere, heating to 1200-1300 ℃ at the speed of 2-5 ℃/min, preserving the heat for 1-2 hours, and cooling to room temperature to obtain the alumina-based foamed ceramic spherical shell.
The pore-forming agent is fly ash floating beads; the binder is ethyl cellulose. The volume density of the obtained alumina-based foamed ceramic spherical shell matrix material is 0.8-1.2 g/cm3And the normal-temperature compressive strength is 6-10 MPa.
Example 5
An alumina-based foam ceramic spherical shell for civil air defense engineering and a preparation method thereof. The preparation method in this example is:
step one, taking 75-80 wt% of bauxite powder, 16-18 wt% of Guangxi white mud and 10-13 wt% of kaolin as raw materials, adding 14-15 wt% of a bonding agent, 30-40 wt% of water and 40-80 wt% of a pore-forming agent, and uniformly mixing to obtain the pug.
And step two, filling the pug into a hemispherical shell mold with the outer diameter of 8-12 cm and the inner diameter of 4-6 cm, pressing the mixture into a hemispherical shell green body under the pressure of 3-4 Mpa, butting and combining the side openings of the hemispherical shells into a hollow sphere under the same pressure, and demolding. Curing at 25 ℃ for 4-5 h, and drying at 100-110 ℃ for 6-12 h to obtain the alumina-based foamed ceramic spherical shell blank.
And step three, placing the alumina-based foamed ceramic spherical shell blank in an air atmosphere, heating to 1100-1200 ℃ at the speed of 2-5 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain the alumina-based foamed ceramic spherical shell.
The pore-forming agent is sawdust; the binder is hydroxyethyl cellulose. The volume density of the obtained alumina-based foamed ceramic spherical shell matrix material is 1.0-1.5 g/cm3And the normal-temperature compressive strength is 10-15 MPa.
Example 6
An alumina-based foam ceramic spherical shell for civil air defense engineering and a preparation method thereof. This example is the same as example 5 except for step three:
and step three, placing the alumina-based foamed ceramic spherical shell blank in an air atmosphere, heating to 1200-1300 ℃ at the speed of 2-5 ℃/min, preserving the heat for 1-2 hours, and cooling to room temperature to obtain the alumina-based foamed ceramic spherical shell.
The pore-forming agent is sawdust; the binder is hydroxyethyl cellulose. The volume density of the obtained alumina-based foamed ceramic spherical shell matrix material is 1.2-1.8 g/cm3And the normal-temperature compressive strength is 11-18 MPa.
The main raw materials used by the invention are natural minerals such as bauxite powder, Guangxi white mud, kaolin and the like, and the raw materials are cheap and easy to obtain and have low cost. Adding a bonding agent, water and a certain amount of pore-forming agent into the raw materials, and uniformly mixing to obtain the pug. Pressing the pug into a semi-spherical shell green body, then butting and combining the side openings of the semi-spherical shells into a hollow sphere under the same pressure, and demoulding. Firing the alumina-based foamed ceramic spherical shell blank at 1100-1300 ℃ to obtain the alumina-based foamed ceramic spherical shell.
The invention adopts a compression molding process, has simple operation, can realize automatic production and high production efficiency, and can further control the sphere size and the wall thickness of the alumina-based foamed ceramic spherical shell by controlling the cavity of the mold. The invention adopts the method of adding the pore-forming agent to prepare the alumina-based foam ceramic spherical shell, and can further control the porosity, density and aperture size of the alumina-based foam ceramic spherical shell and the corresponding normal-temperature mechanical property thereof by controlling the addition amount of the pore-forming agent and the particle size of the pore-forming agent.
The pore-forming agent used in the invention is at least one of carbon powder, fly ash floating beads and saw dust, and the pore-forming agent does not generate toxic gas in the sintering process, thereby being safe and environment-friendly. The invention adopts the method of adding the pore-forming agent to prepare the alumina-based foam ceramic spherical shell, and can further control the porosity, density and aperture size of the alumina-based foam ceramic spherical shell and the corresponding normal-temperature mechanical property thereof by controlling the addition amount of the pore-forming agent and the particle size of the pore-forming agent.
Therefore, the invention has the characteristics of simple process, low cost, high production efficiency, easy product forming and easy process control. The alumina-based foamed ceramic spherical shell prepared by the method has uniform wall thickness and controllable density, wall thickness and sphere size.
Claims (8)
1. A preparation method of an alumina-based foamed ceramic spherical shell for civil air defense engineering is characterized by comprising the following steps: the preparation method comprises the following steps:
step one, taking 67-80 wt% of bauxite powder, 15-18 wt% of Guangxi white mud and 5-13 wt% of kaolin as raw materials, adding 10-15 wt% of a bonding agent, 10-40 wt% of water and 40-80 wt% of a pore-forming agent, and uniformly mixing to obtain a pug;
filling the pug into a hemispherical shell mold with the outer diameter of 8-12 cm and the inner diameter of 4-6 cm, pressing under 1-4 Mpa to prepare a hemispherical shell green body 1, wherein the middle part of the hemispherical shell green body 1 is a hollow hemisphere 3, and the cross section of the hemispherical shell green body 1 is of an annular structure 2;
the side openings of the hemispherical shells are butted and combined into a hollow sphere 4 under the same pressure, and demoulding is carried out; curing at 25 ℃ for 2-5 h, and drying at 60-110 ℃ for 6-12 h to obtain an alumina-based foamed ceramic spherical shell blank;
thirdly, placing the alumina-based foamed ceramic spherical shell blank in an air atmosphere, heating to 1100-1300 ℃ at the speed of 1-5 ℃/min, preserving heat for 1-2 h, and cooling to room temperature to obtain an alumina-based foamed ceramic spherical shell;
the pore-forming agent is carbon powder; the binding agent is sodium carboxymethyl cellulose; the volume density of the obtained alumina-based foamed ceramic spherical shell matrix material is 0.7-1.2 g/cm3And the normal-temperature compressive strength is 5-8 MPa.
2. The method for preparing the alumine-based foamed ceramic spherical shell for civil air defense engineering according to claim 1, which is characterized in that: the particle size of the bauxite powder is 10-90 mu m.
3. The method for preparing the alumine-based foamed ceramic spherical shell for civil air defense engineering according to claim 1, which is characterized in that: the particle size of the Guangxi white mud is 10-90 mu m.
4. The method for preparing the alumine-based foamed ceramic spherical shell for civil air defense engineering according to claim 1, which is characterized in that: the particle size of the kaolin is 10-90 mu m.
5. The method for preparing the alumine-based foamed ceramic spherical shell for civil air defense engineering according to claim 1, which is characterized in that: the pore-forming agent is at least one of carbon powder, fly ash floating beads and sawdust.
6. The method for preparing the alumine-based foamed ceramic spherical shell for civil air defense engineering according to claim 1, which is characterized in that: the binding agent is at least one of sodium carboxymethyl cellulose, ethyl cellulose and hydroxyethyl cellulose.
7. The alumina-based foamed ceramic spherical shell for civil air defense engineering as claimed in claim 1, wherein: the molding mode is compression molding, and the molding pressure is between 1 and 4 Mpa.
8. An alumina-based foam ceramic spherical shell for civil air defense engineering and a preparation method thereof are characterized in that: the alumyte-based foamed ceramic spherical shell for civil air defense engineering is prepared by the method for preparing the alumyte-based foamed ceramic spherical shell for civil air defense engineering according to any one of claims 1 to 7.
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