CN112679225A - Porous ceramic material pore-forming agent and preparation method thereof - Google Patents
Porous ceramic material pore-forming agent and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
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- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 28
- 235000009566 rice Nutrition 0.000 claims abstract description 28
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 22
- 239000011148 porous material Substances 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- 239000010903 husk Substances 0.000 claims abstract description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000001110 calcium chloride Substances 0.000 claims abstract description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 11
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 11
- 239000001103 potassium chloride Substances 0.000 claims abstract description 11
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000000919 ceramic Substances 0.000 claims description 38
- 239000000463 material Substances 0.000 claims description 37
- 238000007873 sieving Methods 0.000 claims description 24
- 238000005469 granulation Methods 0.000 claims description 21
- 230000003179 granulation Effects 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 238000001694 spray drying Methods 0.000 claims description 20
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- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
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- 238000000498 ball milling Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims 1
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- 239000005445 natural material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 16
- 239000007767 bonding agent Substances 0.000 description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 229910052681 coesite Inorganic materials 0.000 description 8
- 229910052593 corundum Inorganic materials 0.000 description 8
- 229910052906 cristobalite Inorganic materials 0.000 description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 8
- 229910052682 stishovite Inorganic materials 0.000 description 8
- 229910052905 tridymite Inorganic materials 0.000 description 8
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- 239000004615 ingredient Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention discloses a porous ceramic material pore-forming agent and a preparation method thereof, wherein the raw material is rice husk, which comprises 27-28.5 wt% of carbon, 65.9-67.5 wt% of silicon dioxide, 2.1-2.3 wt% of calcium chloride, 0.1-0.15 wt% of ferric trichloride and 3.2-3.4 wt% of potassium chloride. The natural material rice husk is treated at high temperature to form carbide, which is crushed and sieved to form pore forming agent grains. Compared with organic pore-forming additives and inorganic pore-forming additives, the pore-forming additive has the characteristics of controllable shape, no undesirable residue after sintering and the like.
Description
Technical Field
The invention belongs to the technical field of organic materials, and particularly relates to a porous ceramic material pore-forming agent and a preparation method thereof.
Background
The porous ceramic has the advantages of high porosity, good strength, stable physical and chemical properties, high filtration precision, good regeneration performance and the like. The open porous ceramic has good functions of adsorption, filtration, echo elimination and the like, and the closed porous ceramic has good barrier function on heat, sound and transmission of solid and liquid particles. Porous ceramics have been widely used in the fields of carriers, filtration and separation, sound absorption, heat insulation, bioengineering, and new energy materials, and the shape, size, distribution, and porosity of pores in porous ceramic materials seriously affect the performance of porous materials.
In the prior art, porous ceramics have various pore-forming modes, including a foaming process, a pore-forming agent adding process, an organic foam impregnation process, a gel process, freeze drying and the like. Wherein the addition of pore formers is one of the most common ways of making porous ceramics porous. The shape, size and porosity of the pores can be well controlled by using the method.
The pore-forming agent of the existing porous ceramic mainly comprises an organic additive and an inorganic additive, the organic pore-forming additive has the advantages of no residue after sintering and the like, but has obvious problems that the gasification temperature is low in the sintering process, the shape of pores is difficult to maintain in the sintering process, the inorganic pore-forming agent is just opposite and can maintain the shape of the pores, but the residue of the inorganic pore-forming agent is difficult to remove, and the ceramic main body is greatly influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a porous ceramic material pore-forming agent.
The invention also aims to provide a preparation method of the pore-forming agent for porous ceramic materials.
The technical scheme of the invention is as follows:
a porous ceramic material pore-forming agent is characterized in that: the raw material is rice husk containing 27-28.5 wt% of carbon, 65.9-67.5 wt% of silicon dioxide, 2.1-2.3 wt% of calcium chloride, 0.1-0.15 wt% of ferric trichloride and 3.2-3.4 wt% of potassium chloride.
In a preferred embodiment of the invention, it contains 27 to 28.5 wt% of carbon, 65.9 to 67.4 wt% of silicon dioxide, 2.18 to 2.2 wt% of calcium chloride, 0.1 to 0.12 wt% of ferric trichloride and 3.3 wt% of potassium chloride.
In a preferred embodiment of the invention, the particle size is 20 to 100. mu.m.
More preferably, the particle size is 40 to 50 μm.
The preparation method of the porous ceramic material pore-forming agent comprises the following steps:
(1) carrying out heat treatment on the rice hull at 590-610 ℃ for 1-4h in the air atmosphere, and cooling to room temperature along with the furnace to obtain a first product;
(2) crushing the first product and then sieving the crushed first product with a 5000-mesh sieve to obtain a second product;
(3) and (3) performing spray drying granulation on the second product, sieving the second product by using a 300-mesh sieve, and sieving the material which passes through the second product by using a 325-mesh sieve to obtain the material which does not pass through the second product, namely the porous ceramic material pore-forming agent.
In a preferred embodiment of the present invention, the step (1) is: the rice husk is heat treated at 600 ℃ for 1-4h in the air atmosphere, and cooled to room temperature along with the furnace to obtain a first product.
In a preferred embodiment of the present invention, the crushing in step (2) is performed by using a planetary ball mill, and the planetary ball mill has the following process parameters: the ball is 6mm ceramic ball, and the rotation speed ratio is as follows: the rotation and revolution are 2: 1, the revolution speed is 200rpm, and the ball milling time is 12 h.
In a preferred embodiment of the present invention, the specific process of the spray drying granulation is as follows: the air inlet temperature is 195-205 ℃, the feeding speed is 45-55rpm, a centrifugal atomization mode is adopted, and the feed rate is 275-285m3Flow, pressure of 1.8-2.2 MPa.
Further preferably, the specific process of spray drying granulation comprises the following steps: the inlet air temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the feed rate is 280m3Flow,/h, 2MPa pressure.
Further preferably, the step (1) is: putting the rice hull into a vacuum atmosphere furnace, carrying out heat treatment at 600 ℃ for 4h, and cooling to room temperature along with the furnace to obtain a first product; the crushing mode in the step (2) is that a planetary ball mill is used for crushing, and the technological parameters of the planetary ball mill are as follows: the ball is 6mm ceramic ball, and the rotation speed ratio is as follows: the rotation and revolution are 2: 1, the revolution speed is 200rpm, and the ball milling time is 12 h; the specific process of spray drying granulation comprises the following steps: the inlet air temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the feed rate is 280m3Flow,/h, 2MPa pressure.
The invention has the beneficial effects that:
1. the natural material rice husk is treated at high temperature to form carbide, which is crushed and sieved to form pore forming agent grains.
2. Compared with organic pore-forming additives and inorganic pore-forming additives, the invention has the characteristics of controllable shape, no undesirable residue after sintering and the like.
3. The preparation process is simple and the cost is extremely low.
Drawings
FIG. 1 is a scanning electron microscope photograph of a porous ceramic material prepared from a pore-forming agent for a porous ceramic material prepared in example 1 of the present invention.
FIG. 2 is a scanning electron microscope photograph of a porous ceramic material prepared from the pore-forming agent for porous ceramic materials prepared in example 2 of the present invention.
FIG. 3 is a scanning electron micrograph of a porous ceramic material prepared from the pore-forming agent for porous ceramic materials prepared in comparative example 2 according to the present invention.
FIG. 4 is a scanning electron micrograph of a porous ceramic material prepared from the pore-forming agent for porous ceramic material prepared in comparative example 4 of the present invention.
FIG. 5 is a scanning electron micrograph of a porous ceramic material according to comparative example 5 of the present invention in which starch was used as a pore-forming agent.
FIG. 6 is a scanning electron micrograph of a porous ceramic material in comparative example 5 of the present invention, in which alumina ceramic hollow spheres are used as pore-forming agents.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Example 1
(1) Carrying out heat treatment on rice hulls at 600 ℃ for 4h in an air atmosphere, and cooling the rice hulls to room temperature along with a furnace to obtain a first product;
(2) putting the first product into a planetary ball mill for crushing treatment, and then sieving the crushed first product with a 5000-mesh sieve to obtain a second product;
(3) spray drying the second product, granulating, sieving with 300 mesh sieve, and sieving with 325 mesh sieve to obtain the final productThe material which does not penetrate through is the porous ceramic material pore-forming agent with the particle size of 40-50 mu m, and the composition of the porous ceramic material pore-forming agent is detected by adopting an X-ray photoelectron spectroscopy: 27 wt% of carbon, 67.4 wt% of silicon dioxide, 2.2 wt% of calcium chloride, 0.1 wt% of ferric trichloride and 3.3 wt% of potassium chloride; the parameters of the planetary ball mill are as follows: the ball is 6mm ceramic ball, and the rotation speed ratio is as follows: the rotation and revolution are 2: 1, the revolution speed is 200rpm, and the ball milling time is 12 h; the technological parameters of the spray drying granulation are as follows: the inlet air temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the feed rate is 280m3Flow,/h, 2MPa pressure.
(4) Mixing the porous ceramic material pore-forming agent prepared by the embodiment with a ceramic bonding agent for 4h, wherein the component of the ceramic bonding agent is SiO2：60.32wt％，Al2O3：36.35wt％，CaO：0.31wt％，MgO：0.23wt％，Fe2O3：0.32wt％，TiO2：0.07wt％，K2O: 2.40 wt%, the granularity of the ingredients is 8000 meshes, the pore-forming agent of the porous ceramic material accounts for 30 wt%, the materials are pressed by 3Mpa, the pressure maintaining time is 1min, the materials are sintered for 2h in the air atmosphere at 830 ℃, the materials are cooled to room temperature along with the furnace, the porous ceramic material shown in the figure 1 can be obtained, and finally the prepared porous ceramic material has regular pores and uniform size. Tests show that the porous ceramic material has the compressive strength of 42MPa, the breaking strength of 35MPa, the hardness of 32.4HRB and the porosity of 28.9 percent.
Example 2
(1) Carrying out heat treatment on the rice hulls at 600 ℃ for 2.5h in the air atmosphere, and cooling the rice hulls to room temperature along with a furnace to obtain a first product;
(2) putting the first product into a planetary ball mill for crushing treatment, and then sieving the crushed first product with a 5000-mesh sieve to obtain a second product;
(3) and (3) carrying out spray drying granulation on the second product, sieving the second product by using a 300-mesh sieve, sieving the material which passes through the second product by using a 325-mesh sieve, and detecting the composition of the material which does not pass through the second product by adopting an X-ray photoelectron spectroscopy, wherein the obtained material is the porous ceramic material pore-forming agent with the particle size of 40-50 mu m: 28 wt% of carbon, 66.4 wt% of silicon dioxide, 2.18 wt% of calcium chloride, 0.12 wt% of ferric trichloride and 3.3 wt% of potassium chloride; (ii) a The parameters of the planetary ball mill are as follows: fitting for mixingThe ball is a 6mm ceramic ball, and the rotating speed ratio is as follows: the rotation and revolution are 2: 1, the revolution speed is 200rpm, and the ball milling time is 12 h; the technological parameters of the spray drying granulation are as follows: the inlet air temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the feed rate is 280m3Flow,/h, 2MPa pressure.
(4) Mixing the porous ceramic material pore-forming agent prepared by the embodiment with a ceramic bonding agent for 4h, wherein the component of the ceramic bonding agent is SiO2：60.32wt％，Al2O3：36.35wt％，CaO：0.31wt％，MgO：0.23wt％，Fe2O3：0.32wt％，TiO2：0.07wt％，K2O: 2.40 wt%, the granularity of the ingredients is 8000 meshes, the pore-forming agent of the porous ceramic material accounts for 30 wt%, the materials are pressed by 3Mpa, the pressure maintaining time is 1min, the materials are sintered for 2h in the air atmosphere at 830 ℃, the materials are cooled to room temperature along with the furnace, the porous ceramic material shown in the figure 2 can be obtained, and finally the prepared porous ceramic material has regular pores and uniform size. Tests show that the porous ceramic material has the compressive strength of 41.4MPa, the breaking strength of 32MPa, the hardness of 29.2HRB and the porosity of 29.3 percent.
Example 3
(1) Carrying out heat treatment on rice hulls at 600 ℃ for 1h in an air atmosphere, and cooling the rice hulls to room temperature along with a furnace to obtain a first product;
(2) putting the first product into a planetary ball mill for crushing treatment, and then sieving the crushed first product with a 5000-mesh sieve to obtain a second product;
(3) and (3) carrying out spray drying granulation on the second product, sieving the second product by using a 300-mesh sieve, sieving the material which passes through the second product by using a 325-mesh sieve, and detecting the composition of the material which does not pass through the second product by adopting an X-ray photoelectron spectroscopy, wherein the obtained material is the porous ceramic material pore-forming agent with the particle size of 40-50 mu m: 28.5 wt% of carbon, 65.9 wt% of silicon dioxide, 2.18 wt% of calcium chloride, 0.12 wt% of ferric trichloride and 3.3 wt% of potassium chloride; the parameters of the planetary ball mill are as follows: the ball is 6mm ceramic ball, and the rotation speed ratio is as follows: the rotation and revolution are 2: 1, the revolution speed is 200rpm, and the ball milling time is 12 h; the technological parameters of the spray drying granulation are as follows: the inlet air temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the feed rate is 280m3Flow,/h, 2MPa pressure.
(4) Mixing the porous ceramic material pore-forming agent prepared by the embodiment with a ceramic bonding agent for 4h, wherein the component of the ceramic bonding agent is SiO2：60.32wt％，Al2O3：36.35wt％，CaO：0.31wt％，MgO：0.23wt％，Fe2O3：0.32wt％，TiO2：0.07wt％，K2O: 2.40 wt%, the granularity of the ingredients is 8000 meshes, the pore-forming agent of the porous ceramic material accounts for 30 wt%, the materials are pressed by 3Mpa, the pressure maintaining time is 1min, the materials are sintered for 2h in the air atmosphere at 830 ℃, the materials are cooled to room temperature along with the furnace, the porous ceramic material is obtained, and finally the prepared porous ceramic material has regular pores and uniform size. Tests show that the porous ceramic material has the compressive strength of 44.4MPa, the breaking strength of 36MPa, the hardness of 31.1HRB and the porosity of 30.5 percent.
Comparative example 1
The rice husk is subjected to heat treatment at 600 ℃ for 0.5h in the air atmosphere, and is cooled to room temperature along with the furnace to obtain a first product. The first product was examined to find that the rice husk was not completely carbonized, and the rice husk contained fibers, and further crushing and granulation could not be carried out.
Comparative example 2
(1) Carrying out heat treatment on rice hulls at 600 ℃ for 4.5h in an air atmosphere, and cooling to room temperature along with a furnace to obtain a first product;
(2) putting the first product into a planetary ball mill for crushing treatment, and then sieving the crushed first product with a 5000-mesh sieve to obtain a second product;
(3) and (3) carrying out spray drying granulation on the second product, sieving the second product by using a 300-mesh sieve, and sieving the material which passes through the second product by using a 325-mesh sieve to obtain the material which does not pass through, namely the porous ceramic material pore-forming agent with the particle size of 40-50 mu m, wherein the porous ceramic material pore-forming agent comprises the following components: 8.6 wt% of carbon, 85.54 wt% of silicon dioxide, 2.5 wt% of calcium chloride, 0.16 wt% of ferric trichloride and 3.2 wt% of potassium chloride; the parameters of the planetary ball mill are as follows: the ball is 6mm ceramic ball, and the rotation speed ratio is as follows: the rotation and revolution are 2: 1, the revolution speed is 200rpm, and the ball milling time is 12 h; the technological parameters of the spray drying granulation are as follows: the inlet air temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the feed rate is 280m3Flow,/h, 2MPa pressure.
(4) Mixing the porous ceramic material pore-forming agent prepared by the comparative example with a ceramic bonding agent for 4 hours, wherein the component of the ceramic bonding agent is SiO2：60.32wt％，Al2O3：36.35wt％，CaO：0.31wt％，MgO：0.23wt％，Fe2O3：0.32wt％，TiO2：0.07wt％，K2O: 2.40 wt%, the granularity of the ingredients is 8000 meshes, the pore-forming agent of the porous ceramic material accounts for 30 wt%, the porous ceramic material is pressed under 3Mpa, the pressure maintaining time is 1min, the porous ceramic material is sintered for 2h in the air atmosphere at 830 ℃, and the porous ceramic material is cooled to room temperature along with the furnace, so that the porous ceramic material shown in the figure 2 is obtained.
As can be seen from FIG. 3, the porous ceramic material prepared by this comparative example has a carbon content of less than 10 wt% and a silicon content of more than 80 wt%, and therefore, an unremovable residue is formed at the pore-forming site, which affects the parameters of the ceramic body. Compared with the embodiment 1, the compressive strength of the prepared porous ceramic material is improved by 10Mpa, the flexural strength is improved by 12Mpa, and the porosity is reduced by 15%.
Comparative example 3
Respectively carrying out heat treatment on the rice hulls at 580 ℃ for 4h and 5h in an air atmosphere, and cooling to room temperature along with a furnace to obtain a first product. The first product was examined to find that the rice husk was not completely carbonized, and the rice husk contained fibers, and further crushing and granulation could not be carried out.
Comparative example 4
(1) Carrying out heat treatment on rice hulls at 620 ℃ for 4h in an air atmosphere, and cooling the rice hulls to room temperature along with a furnace to obtain a first product;
(2) putting the first product into a planetary ball mill for crushing treatment, and then sieving the crushed first product with a 5000-mesh sieve to obtain a second product;
(3) and (3) carrying out spray drying granulation on the second product, sieving the second product by using a 300-mesh sieve, and sieving the material which passes through the second product by using a 325-mesh sieve to obtain the material which does not pass through, namely the porous ceramic material pore-forming agent with the particle size of 40-50 mu m, wherein the porous ceramic material pore-forming agent comprises the following components: 5.4 wt% of carbon, 88.46 wt% of silicon dioxide, 2.6 wt% of calcium chloride, 0.15 wt% of ferric trichloride and 3.3 wt% of potassium chloride; the parameters of the planetary ball mill are as follows: the ball is 6mm ceramic ball, and the rotation speed ratio is as follows: the rotation and revolution ratio is 2: 1The revolution speed is 200rpm, and the ball milling time is 12 h; the technological parameters of the spray drying granulation are as follows: the inlet air temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the feed rate is 280m3Flow,/h, 2MPa pressure.
(4) Mixing the porous ceramic material pore-forming agent prepared by the comparative example with a ceramic bonding agent for 4 hours, wherein the component of the ceramic bonding agent is SiO2：60.32wt％，Al2O3：36.35wt％，CaO：0.31wt％，MgO：0.23wt％，Fe2O3：0.32wt％，TiO2：0.07wt％，K2O: 2.40 wt%, the granularity of the ingredients is 8000 meshes, the pore-forming agent of the porous ceramic material accounts for 30 wt%, the porous ceramic material is pressed under 3Mpa, the pressure maintaining time is 1min, the porous ceramic material is sintered for 2h in the air atmosphere at 830 ℃, and the porous ceramic material is cooled to the room temperature along with the furnace, so that the porous ceramic material shown in the figure 3 can be obtained.
As can be seen from FIG. 4, the porous ceramic material prepared by this comparative example has a carbon content of less than 10 wt% and a silicon content of more than 80 wt%, and therefore, an unremovable residue is formed at the pore-forming site, which affects the parameters of the ceramic body. Compared with the embodiment 1, the compressive strength of the prepared porous ceramic material is improved by 12Mpa, the flexural strength is improved by 15Mpa, and the porosity is reduced by 20%.
Comparative example 5
(1) Performing heat treatment on the rice hulls at 620 ℃ for 0.5h in an air atmosphere, and cooling the rice hulls to room temperature along with a furnace to obtain a first product;
(2) putting the first product into a planetary ball mill for crushing treatment, and then sieving the crushed first product with a 5000-mesh sieve to obtain a second product;
(3) and (3) carrying out spray drying granulation on the second product, sieving the second product by using a 300-mesh sieve, and sieving the material which passes through the second product by using a 325-mesh sieve to obtain the material which does not pass through, namely the porous ceramic material pore-forming agent with the particle size of 40-50 mu m, wherein the porous ceramic material pore-forming agent comprises the following components: 6.2 wt% of carbon, 87.56 wt% of silicon dioxide, 2.7 wt% of calcium chloride, 0.14 wt% of ferric trichloride and 3.4 wt% of potassium chloride; the parameters of the planetary ball mill are as follows: the ball is 6mm ceramic ball, and the rotation speed ratio is as follows: the rotation and revolution are 2: 1, the revolution speed is 200rpm, and the ball milling time is 12 h; the technological parameters of the spray drying granulation are as follows: intoThe wind temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the rotating speed is 280m3Flow,/h, 2MPa pressure.
(4) Mixing the porous ceramic material pore-forming agent prepared by the comparative example with a ceramic bonding agent for 4 hours, wherein the component of the ceramic bonding agent is SiO2：60.32wt％，Al2O3：36.35wt％，CaO：0.31wt％，MgO：0.23wt％，Fe2O3：0.32wt％，TiO2：0.07wt％，K2O: 2.40 wt%, the granularity of the ingredients is 8000 meshes, the pore-forming agent of the porous ceramic material accounts for 30 wt%, the porous ceramic material is pressed under 3Mpa, the pressure maintaining time is 1min, the porous ceramic material is sintered for 2h in the air atmosphere at 830 ℃, and the porous ceramic material is cooled to the room temperature along with the furnace, so that the porous ceramic material shown in the figure 3 can be obtained.
As can be seen from FIG. 4, the porous ceramic material prepared by this comparative example has a carbon content of less than 10 wt% and a silicon content of more than 80 wt%, and therefore, an unremovable residue is formed at the pore-forming site, which affects the parameters of the ceramic body. Compared with the embodiment 1, the compressive strength of the prepared porous ceramic material is improved by 11MPa, the flexural strength is improved by 14MPa, and the porosity is reduced by 19%.
Comparative example 6
The organic pore-forming agent mainly comprises natural fibers, high-molecular polymers, organic acids and the like, such as sawdust, naphthalene, starch, polyvinyl alcohol, urea, methyl methacrylate, polyvinyl chloride, polystyrene and the like, the starch is used as the organic pore-forming agent in the comparative example, the materials are mixed for 4 hours, and the ceramic bonding agent is made of SiO2：60.32wt％，Al2O3：36.35wt％，CaO：0.31wt％，MgO：0.23wt％，Fe2O3：0.32wt％，TiO2：0.07wt％，K2O: 2.40 wt%, the material granularity is 8000 meshes, the pore-forming agent of the porous ceramic material accounts for 30 wt%, the material is pressed under 3Mpa, the pressure maintaining time is 1min, the material is treated for 2h in the air atmosphere at 830 ℃, and the material is cooled to the room temperature along with the furnace, and the porous material is obtained as shown in figure 5. Since the ceramic body is decomposed or volatilized at a temperature far lower than the firing temperature of the ceramic body, pores are easily deformed, and the sizes and shapes of the pores are not uniform.
The inorganic pore-forming agent comprises high-temperature decomposable salts such as ammonium carbonate, ammonium bicarbonate, ammonium chloride and the like, the pore-forming agent is not removed at the temperature of a ceramic matrix, the comparative example uses an alumina ceramic hollow sphere as the inorganic pore-forming agent, and the materials are mixed for 4 hours, wherein the component of the ceramic bonding agent is SiO2：60.32wt％，Al2O3：36.35wt％，CaO：0.31wt％，MgO：0.23wt％，Fe2O3：0.32wt％，TiO2：0.07wt％，K2O: 2.40 wt%, the material granularity is 8000 meshes, the pore-forming agent of the porous ceramic material accounts for 30 wt%, the material is pressed under 3Mpa, the pressure maintaining time is 1min, the material is treated for 2h in the air atmosphere at 830 ℃, and the material is cooled to the room temperature along with the furnace, and the porous ceramic material is obtained as shown in figure 6. The pores formed by the pore-forming agent are mostly closed pores, which is the advantage of a porous ceramic material severely limited.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. A porous ceramic material pore-forming agent is characterized in that: the raw material is rice husk containing 27-28.5 wt% of carbon, 65.9-67.5 wt% of silicon dioxide, 2.1-2.3 wt% of calcium chloride, 0.1-0.15 wt% of ferric trichloride and 3.2-3.4 wt% of potassium chloride.
2. The pore former for porous ceramic materials as claimed in claim 1, wherein: wherein the carbon content is 27-28.5 wt%, the silicon dioxide content is 65.9-67.4 wt%, the calcium chloride content is 2.18-2.2 wt%, the ferric trichloride content is 0.1-0.12 wt% and the potassium chloride content is 3.3 wt%.
3. The pore former for porous ceramic materials according to claim 1 or 2, wherein: the particle size is 20-100 μm.
4. The pore former for porous ceramic materials as claimed in claim 3, wherein: the particle size is 40-50 μm.
5. The method for preparing the pore-forming agent for porous ceramic materials as claimed in any one of claims 1 to 4, wherein: the method comprises the following steps:
(1) carrying out heat treatment on the rice hull at 590-610 ℃ for 1-4h in the air atmosphere, and cooling to room temperature along with the furnace to obtain a first product;
(2) crushing the first product and then sieving the crushed first product with a 5000-mesh sieve to obtain a second product;
(3) and (3) performing spray drying granulation on the second product, sieving the second product by using a 300-mesh sieve, and sieving the material which passes through the second product by using a 325-mesh sieve to obtain the material which does not pass through the second product, namely the porous ceramic material pore-forming agent.
6. The method of claim 5, wherein: the step (1) is as follows: the rice husk is heat treated at 600 ℃ for 1-4h in the air atmosphere, and cooled to room temperature along with the furnace to obtain a first product.
7. The method of claim 5, wherein: the crushing mode in the step (2) is that a planetary ball mill is used for crushing, and the technological parameters of the planetary ball mill are as follows: the ball is 6mm ceramic ball, and the rotation speed ratio is as follows: autorotation: the conversion is 2: 1, the revolution speed is 200rpm, and the ball milling time is 12 h.
8. The method of claim 5, wherein: the specific process of spray drying granulation comprises the following steps: the air inlet temperature is 195-205 ℃, the feeding speed is 45-55rpm, a centrifugal atomization mode is adopted, and the feed rate is 275-285m3Flow, pressure of 1.8-2.2 MPa.
9. The method of claim 8, wherein: the specific process of spray drying granulation comprises the following steps: the inlet air temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the feed rate is 280m3Flow,/h, 2MPa pressure.
10. As claimed in claim 5The preparation method is characterized by comprising the following steps: the step (1) is as follows: putting the rice hull into a vacuum atmosphere furnace, carrying out heat treatment at 600 ℃ for 4h, and cooling to room temperature along with the furnace to obtain a first product; the crushing mode in the step (2) is that a planetary ball mill is used for crushing, and the technological parameters of the planetary ball mill are as follows: the ball is 6mm ceramic ball, and the rotation speed ratio is as follows: autorotation: the revolution speed is 2: 1, the revolution speed is 200rpm, and the ball milling time is 12 h; the specific process of spray drying granulation comprises the following steps: the inlet air temperature is 200 ℃, the feeding speed is 50rpm, a centrifugal atomization mode is adopted, and the feed rate is 280m3Flow,/h, 2MPa pressure.
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