CN110885240A - Process for preparing porous ceramic by adding pore-forming agent - Google Patents
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Abstract
The invention provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the steps of adding a pore-forming agent into ceramic powder, pressing and molding by using a mold, occupying a certain space in a blank by using the pore-forming agent, and then, heating and decomposing the pore-forming agent to form pores under high-temperature sintering to obtain the porous ceramic; the process can effectively control the porosity and mechanical property of the porous ceramic by adjusting the addition amount of the pore-forming agent and the sintering temperature, and the porous ceramic prepared by the process has higher mechanical strength.
Description
Technical Field
The invention relates to the field of ceramic preparation, in particular to a process for preparing porous ceramic by adding a pore-forming agent.
Background
The porous ceramic is an inorganic functional material taking pores as a main phase, and has the advantages of high porosity, large specific surface area, high temperature resistance, corrosion resistance, good heat insulation, uniform pore structure distribution, long service life and the like, so the porous ceramic is often used as materials for filtration, separation, sound absorption, heat insulation, carriers, sensitive elements and the like and is widely applied to the fields of environmental protection, chemical engineering, metallurgy, energy, bioengineering and the like. The advantages and applications of the porous ceramics are high attention of material scientists, and the workers actively explore the advantages and applications and hope to develop a green and environment-friendly preparation method of the porous ceramics with low cost.
Diatomite is a siliceous sedimentary rock formed by the deposition of ancient diatom biological remains in the water bottom, and is a very important nonmetallic mineral product. The proven diatomite reserves of China are the second in the world, and at present, China is 14The autonomous region of each province and city discovers more than 70 diatomite ores, the found resource reserves are about 4.84 hundred million tons, and the prospect reserves reach 20 hundred million tons. The chemical components of the diatomite are mainly amorphous SiO2And contains a small amount of Al2O3、Fe2O3、P2O5CaO, MgO and organic matters, and has wide sources and low price.
The preparation methods of the porous ceramic materials commonly used in the industry at present mainly comprise a foaming method, an injection molding method, a particle stacking method and the like. However, the preparation methods have limitations, the foaming method has higher requirements on raw materials, and the process conditions are not easy to control; the porosity of the product obtained by the particle packing method is low. Therefore, a porous ceramic material with high mechanical strength is a problem to be solved urgently.
Disclosure of Invention
The invention provides a process for preparing porous ceramic by adding a pore-forming agent, aiming at the problems in the preparation method of the conventional porous ceramic material.
The invention provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and pore-forming agent, and putting the diatomite, the calcium carbonate and the pore-forming agent on a planetary ball mill for ball milling to obtain ceramic powder;
(2) adding a certain amount of binder into the ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulating to ensure that the ceramic powder has certain cohesiveness, then pressing and molding the ceramic powder by using a metal mold, drying the ceramic powder for 24 hours at room temperature, and drying the ceramic powder for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a high-temperature furnace to obtain the porous ceramic.
Preferably, the pore-forming agent in step (1) is starch.
Preferably, the pore-forming agent is added in an amount of 0 wt% to 20 wt%.
Preferably, the calcium carbonate content in step (1) is from 20% to 60% by weight.
Preferably, the ball milling time in the step (1) is 2h-4h, and the ball milling speed is 200r/min-400 r/min.
Preferably, the binder in step (2) is a 5% strength polyvinyl alcohol (PVA) solution. When the polyvinyl alcohol (PVA) solution is used as a solvent to be mixed with the ceramic powder, a large amount of ceramic particles can be adsorbed by a polyvinyl alcohol (PVA) macromolecular chain in the solution, and the ceramic slurry and the organic foam can be firmly bonded together due to the good cohesiveness of the PVA, so that the phenomenon of hole blockage caused by slurry falling can not be generated. The polyvinyl alcohol (PVA) solution is directly used as the solvent, the link of organic foam surface modification is saved, the preparation process is simpler and more time-saving, and the slurry hanging effect after impregnation is better than that of impregnation with water as the solvent and then organic foam modification, and the invention is also the innovation point.
Preferably, the sintering temperature in step (3) is 1100 ℃ to 1300 ℃.
Compared with the prior art, the process for preparing the porous ceramic by adding the pore-forming agent comprises the steps of adding the pore-forming agent into ceramic powder, pressing and forming by using a die, occupying a certain space in a blank by using the pore-forming agent, and then, heating and decomposing the pore-forming agent to form pores under high-temperature sintering, thus obtaining the porous ceramic; the process can effectively control the porosity and mechanical property of the porous ceramic by adjusting the addition amount of the pore-forming agent and the sintering temperature, and the porous ceramic prepared by the process has higher mechanical strength.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
Example one
The embodiment provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and starch, and putting the diatomite, the calcium carbonate and the starch on a planetary ball mill for ball milling to obtain ceramic powder, wherein the content of calcium carbonate is 50 wt%, the ball milling time is 2 hours, and the ball milling speed is 200 r/min;
(2) adding a certain amount of 5% polyvinyl alcohol (PVA) solution into ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulation, then pressing and molding the mixture by using a metal mold, drying the mixture for 24 hours at room temperature, and drying the dried mixture for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a high-temperature furnace at 1200 ℃ to obtain the first porous ceramic.
Example two
The embodiment provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and starch, and putting the diatomite, the calcium carbonate and the starch on a planetary ball mill for ball milling to obtain ceramic powder, wherein the content of calcium carbonate is 50 wt%, the ball milling time is 2 hours, and the ball milling speed is 200 r/min;
(2) adding a certain amount of 5% polyvinyl alcohol (PVA) solution into ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulation, then pressing and molding the mixture by using a metal mold, drying the mixture for 24 hours at room temperature, and drying the dried mixture for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a high-temperature furnace at 1100 ℃ to obtain the second porous ceramic.
EXAMPLE III
The embodiment provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and starch, and putting the diatomite, the calcium carbonate and the starch on a planetary ball mill for ball milling to obtain ceramic powder, wherein the content of calcium carbonate is 50 wt%, the ball milling time is 2 hours, and the ball milling speed is 200 r/min;
(2) adding a certain amount of 5% polyvinyl alcohol (PVA) solution into ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulation, then pressing and molding the mixture by using a metal mold, drying the mixture for 24 hours at room temperature, and drying the dried mixture for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a high-temperature furnace at 1250 ℃ to obtain the third porous ceramic.
Example four
The embodiment provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and starch, and putting the diatomite, the calcium carbonate and the starch on a planetary ball mill for ball milling to obtain ceramic powder, wherein the content of calcium carbonate is 50 wt%, the ball milling time is 2 hours, and the ball milling speed is 200 r/min;
(2) adding a certain amount of 5% polyvinyl alcohol (PVA) solution into ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulation, then pressing and molding the mixture by using a metal mold, drying the mixture for 24 hours at room temperature, and drying the dried mixture for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a 1300 ℃ high-temperature furnace to obtain the fourth porous ceramic.
From the compressive strength of the first porous ceramic, the second porous ceramic, the third porous ceramic and the fourth porous ceramic, the compressive strength of the sample tends to increase with the increase of the sintering temperature. After sintering at 1100-1200 deg.c, the compression strength has no obvious change. This is because the solid-phase reaction is insufficient due to the low sintering temperature. The increase in compressive strength is evident in the two stages of sintering from 1200 c to 1250 c and then to 1300 c, because the increase in sintering temperature promotes solid phase diffusion and allows the particle surfaces to react with each other. And the sintering temperature is increased, the mobility of atoms is enhanced, the number of atoms for overcoming energy barriers is increased, the surface energy of the system is reduced, the sample is densified, the original solid-gas interface is gradually eliminated to form a new low-energy solid-solid interface, finally, the interface disappears, and particles are combined into a whole, so that the compressive strength of the sample is improved.
When the sample is sintered at a temperature lower than 1200 ℃ in the longitudinal direction, the compressive strength of the sample is reduced as the content of calcium carbonate is increased, because the calcium carbonate is decomposed into CaO and CO by heating2However, since calcium oxide has a high melting point and is difficult to sinter, and the sintering temperature is insufficient, the strength of calcium oxide is reduced when the calcium carbonate content is increased, i.e., the CaO content is increased.
EXAMPLE five
The embodiment provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and starch, and putting the diatomite, the calcium carbonate and the starch on a planetary ball mill for ball milling to obtain ceramic powder, wherein the content of the calcium carbonate is 20 wt%, the ball milling time is 2 hours, and the ball milling speed is 200 r/min;
(2) adding a certain amount of 5% polyvinyl alcohol (PVA) solution into ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulation, then pressing and molding the mixture by using a metal mold, drying the mixture for 24 hours at room temperature, and drying the dried mixture for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a high-temperature furnace at 1200 ℃ to obtain the fifth porous ceramic.
EXAMPLE six
The embodiment provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and starch, and putting the diatomite, the calcium carbonate and the starch on a planetary ball mill for ball milling to obtain ceramic powder, wherein the content of calcium carbonate is 30 wt%, the ball milling time is 2 hours, and the ball milling speed is 200 r/min;
(2) adding a certain amount of 5% polyvinyl alcohol (PVA) solution into ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulation, then pressing and molding the mixture by using a metal mold, drying the mixture for 24 hours at room temperature, and drying the dried mixture for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a high-temperature furnace at 1200 ℃ to obtain the No. six porous ceramic.
EXAMPLE seven
The embodiment provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and starch, and putting the diatomite, the calcium carbonate and the starch on a planetary ball mill for ball milling to obtain ceramic powder, wherein the content of the calcium carbonate is 40 wt%, the ball milling time is 2 hours, and the ball milling speed is 200 r/min;
(2) adding a certain amount of 5% polyvinyl alcohol (PVA) solution into ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulation, then pressing and molding the mixture by using a metal mold, drying the mixture for 24 hours at room temperature, and drying the dried mixture for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a high-temperature furnace at 1200 ℃ to obtain the No. seven porous ceramic.
Example eight
The embodiment provides a process for preparing porous ceramic by adding a pore-forming agent, which comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and starch, and putting the diatomite, the calcium carbonate and the starch on a planetary ball mill for ball milling to obtain ceramic powder, wherein the calcium carbonate content is 60 wt%, the ball milling time is 2 hours, and the ball milling speed is 200 r/min;
(2) adding a certain amount of 5% polyvinyl alcohol (PVA) solution into ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulation, then pressing and molding the mixture by using a metal mold, drying the mixture for 24 hours at room temperature, and drying the dried mixture for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a high-temperature furnace at 1200 ℃ to obtain the eighth porous ceramic.
When the content of calcium carbonate is low, the excessive amorphous SiO is analyzed by X-ray diffraction analysis of the first porous ceramic, the fifth porous ceramic, the sixth porous ceramic, the seventh porous ceramic and the eighth porous ceramic2Will be transformed into crystalline SiO2(α -cristobalite phase) As the calcium carbonate content increased, the calcium silicate (wollastonite phase) formed increased, and when the calcium carbonate content was 50%, SiO was present2And completely reacting with calcium carbonate to generate calcium silicate.
The foregoing has described preferred embodiments of the present invention and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary, and various changes made within the scope of the independent claims of the present invention are within the scope of the present invention.
Claims (7)
1. A process for preparing porous ceramic by adding a pore-forming agent method comprises the following steps:
(1) taking a certain amount of diatomite, calcium carbonate and pore-forming agent, and putting the diatomite, the calcium carbonate and the pore-forming agent on a planetary ball mill for ball milling to obtain ceramic powder;
(2) adding a certain amount of binder into the ceramic powder, putting the ceramic powder into an agate mortar for grinding and granulating, then pressing and molding by using a metal mold, drying for 24 hours at room temperature, and drying for 24 hours in a drying oven at 80 ℃ to obtain a ceramic blank;
(3) and sintering the ceramic blank in a high-temperature furnace to obtain the porous ceramic.
2. The process for preparing porous ceramic by adding pore-forming agent according to claim 1, wherein the pore-forming agent in step (1) is starch.
3. The process for preparing porous ceramic by adding the pore-forming agent according to claim 1 or 2, wherein the addition amount of the pore-forming agent is 0 wt% to 20 wt%.
4. The process for preparing porous ceramic by adding pore-forming agent according to claim 1, wherein the calcium carbonate content in step (1) is 20 wt% -60 wt%.
5. The process for preparing porous ceramic by adding the pore-forming agent according to claim 1, wherein the ball milling time in the step (1) is 2h to 4h, and the ball milling speed is 200r/min to 400 r/min.
6. The process for preparing porous ceramic by adding pore-forming agent according to claim 1, wherein the binder in step (2) is polyvinyl alcohol solution with concentration of 5%.
7. The process for preparing porous ceramic by adding pore-forming agent according to claim 1, wherein the sintering temperature in the step (3) is 1100-1300 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101397215A (en) * | 2008-06-23 | 2009-04-01 | 杜建耀 | Diatomaceous micropore ceramic filter cartridge and preparation method thereof |
| CN102391011A (en) * | 2011-08-10 | 2012-03-28 | 华南理工大学 | Preparation method of diatomite-based porous ceramic microspheres |
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- 2019-12-18 CN CN201911312316.3A patent/CN110885240A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101397215A (en) * | 2008-06-23 | 2009-04-01 | 杜建耀 | Diatomaceous micropore ceramic filter cartridge and preparation method thereof |
| CN102391011A (en) * | 2011-08-10 | 2012-03-28 | 华南理工大学 | Preparation method of diatomite-based porous ceramic microspheres |
Non-Patent Citations (1)
| Title |
|---|
| 袁国辉: "以硅藻土为硅源制备硅酸钙多孔陶瓷", 《现代技术陶瓷》 * |
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