CN117160143A - Foam ceramic filter and preparation method thereof - Google Patents
Foam ceramic filter and preparation method thereof Download PDFInfo
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- CN117160143A CN117160143A CN202311063174.8A CN202311063174A CN117160143A CN 117160143 A CN117160143 A CN 117160143A CN 202311063174 A CN202311063174 A CN 202311063174A CN 117160143 A CN117160143 A CN 117160143A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 202
- 239000006260 foam Substances 0.000 title claims abstract description 147
- 238000002360 preparation method Methods 0.000 title claims description 21
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 81
- 239000002245 particle Substances 0.000 claims abstract description 48
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims description 56
- 238000003756 stirring Methods 0.000 claims description 55
- 239000000758 substrate Substances 0.000 claims description 33
- 238000005245 sintering Methods 0.000 claims description 32
- 239000000835 fiber Substances 0.000 claims description 30
- 239000012528 membrane Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 25
- 239000004927 clay Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 22
- 229920002401 polyacrylamide Polymers 0.000 claims description 22
- 229920001451 polypropylene glycol Polymers 0.000 claims description 22
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 22
- 229920002635 polyurethane Polymers 0.000 claims description 21
- 239000004814 polyurethane Substances 0.000 claims description 21
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000009987 spinning Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 11
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 238000010030 laminating Methods 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000010000 carbonizing Methods 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 88
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 54
- 239000011148 porous material Substances 0.000 abstract description 22
- 230000007423 decrease Effects 0.000 abstract description 18
- 230000008569 process Effects 0.000 abstract description 6
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- 229910052761 rare earth metal Inorganic materials 0.000 description 2
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Abstract
The invention provides a foam ceramic filter, which comprises a multi-layer filtering structure, wherein the filtering structure comprises a foam structure layer and a wavy electrostatic spinning layer, the pores of the electrostatic spinning layer gradually decrease from top to bottom, the porosity of the foam layer is unchanged along the flowing direction, the porosity of the wavy electrostatic spinning layer gradually increases from top to bottom along the flowing direction, and the pore diameter gradually decreases from top to bottom. The filter has complete filtering structure, can prevent impurities in castings through the composite design of the two structures, and can improve the mechanical property of the silicon carbide ceramic filter by adopting a novel process to prepare ceramic particles.
Description
Technical Field
The invention relates to the field of metal ceramic filtration, in particular to a foam ceramic filter and a preparation method thereof.
Background
Ceramic filters for soaking have been known for many years, and the ceramic filter technology can effectively reduce or eliminate nonmetallic inclusions in castings, purify liquid casting alloys, and has good economic and social benefits. The foamed ceramic is a porous ceramic which is foamed in shape and is a third-generation porous ceramic product developed after common porous ceramic and honeycomb porous ceramic. The high-technology ceramic has three-dimensional communicating pore passages, and the shape, pore size, permeability, surface area and chemical property of the ceramic can be properly adjusted and changed, so that the product is like a toughened foam plastic or a porcelain sponge. As a novel inorganic nonmetallic filter material, the foamed ceramic has the advantages of light weight, high strength, high temperature resistance, corrosion resistance, simple regeneration, long service life, good filter adsorptivity and the like. Compared with the traditional filter such as ceramic particle sintered body and glass fiber cloth, the preparation process is simple, the energy is saved, the cost is low, and the filtering effect is good. The foamed ceramic can be widely applied to the fields of metallurgy, chemical industry, light industry, food, environmental protection, energy conservation and the like. In recent years, the application field of the foamed ceramics is expanded to the fields of aviation, electronics, medical materials, biochemistry and the like. The most common method for preparing foamed ceramics at present is an organic foam impregnating process. The ceramic body takes organic foam plastic as a framework, is dried after slurry dipping, and is sintered at high temperature, and organic matters are burnt and volatilized in the sintering process, so that the ceramic body with a network structure is left.
The best molten metal filters include sintered ceramic foam filters, but the particular construction of the foam filter means that this form of filter also has its limitations. During the ceramic coating and sintering process, tiny particles may form inside the filter structure, which only slightly sinter together with the matrix material. The passage of the metal stream through the filter causes these particles to separate from the filter into the melt, which can impair the purity of the melt, leading to inclusions in the casting.
Disclosure of Invention
The technical problems to be solved are as follows: the invention aims to provide a foam ceramic filter with complete filtering structure, impurities in castings can be prevented by the composite design of the two structures, and meanwhile, the mechanical property of the silicon carbide ceramic filter can be improved by adopting a novel process to prepare ceramic particles.
The technical scheme is as follows: the utility model provides a foam ceramic filter, includes multilayer filtration, filtration is including foam structural layer and wave formula electrostatic spinning layer, and the aperture from the top down of electrostatic spinning layer diminishes gradually, foam layer is unchangeable along flow direction porosity, wave formula electrostatic spinning layer increases gradually from top to bottom along flow direction porosity, and the aperture diminishes gradually from top to bottom.
The preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a wavy structure by using polyurethane sponge, laminating a polyurethane electrostatic spinning film into a wavy shape, and compounding the foam structure layer and the electrostatic spinning film layer in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Adding water after clay is uniformly mixed, stirring and uniformly mixing, sequentially adding polypropylene glycol and polyacrylamide, stirring and uniformly mixing, adding silica sol, stirring and uniformly mixing, adding modified SiC ceramic flaky particles, and stirring and uniformly mixing to obtain ceramic slurry;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, and naturally cooling to obtain the SiC foam ceramic.
Preferably, the preparation method of the modified SiC ceramic platelet particles comprises the following steps:
s11, adding ethyl orthosilicate into an ethanol solution, then adding polyvinylpyrrolidone and N, N-dimethylformamide, uniformly stirring to obtain a spinning solution, carrying out electrostatic spinning on the spinning solution, and carrying out presintering to obtain a SiC fiber membrane;
s12, weighing a certain amount of cerium nitrate, yttrium nitrate, sodium dodecyl sulfate and urea to be dissolved in deionized water together, stirring at 30-40 ℃ to be fully dissolved, immersing the SiC fiber membrane prepared in the step S11 into the mixed solution, raising the temperature of the solution to 70-80 ℃ to react and precipitate, and then taking out the SiC fiber membrane to be sintered to obtain the modified SiC fiber membrane;
s13, crushing the modified SiC fiber membrane prepared in the step 12 to obtain modified SiC ceramic flaky particles.
Preferably, the height from the crest to the trough of the foam structure layer and the electrostatic spinning layer in the step S1 is 10mm-15mm, and the crest-to-crest interval is 10mm-20mm.
PreferablyIn the step S1, al 2 O 3 The mass ratio of clay, polypropylene glycol, polyacrylamide, silica sol, modified SiC ceramic flaky particles and water is 1-2:0.5-1.2:0.05-0.1:0.05-0.12:2-6:55-65:20-30.
Preferably, the sintering parameter in the step S3 is that the temperature is raised to 890-1080 ℃, and the temperature is kept for 2-4 hours.
Preferably, the temperature of the pre-sintering in the step S11 is 180-200 ℃ and the time is 2-4h.
Preferably, in the step S12, the molar ratio of cerium nitrate, yttrium nitrate, sodium dodecyl sulfate and urea is 2:3-8:20:22.
Preferably, the sintering parameters in the step S12 are pre-sintering 2.5-3.5 h at 360-400 ℃ in Ar atmosphere, heating up at 3 ℃/min, and then carbonizing and reducing 2h at 1480-1500 ℃ at 2-3 ℃/min.
Preferably, the particle size of the modified SiC ceramic platelet particles in the step S13 is 20-50um.
The beneficial effects are that: the preparation method of the invention has the following advantages:
the high structural integrity of the filter of the present invention ensures that loose particles are not present, thereby preventing contamination of the molten metal by the resulting filter debris and time consuming reworking;
the product obtained by the filter has a complex pore canal structure, and on one hand, the foam layer can improve the flux of metal liquid flow; on the other hand, the pore canal structure of the electrostatic spinning layer is in a network through shape, so that the contact area of molten steel and products can be increased, the contact time is prolonged, more nonmetallic inclusions can be adsorbed, and the filtering efficiency of the products on the molten steel is improved;
the filter is designed to be wavy, and the wavy structure increases the contact area with the filter in the flowing process of the molten metal, so that the filtering effect is further improved;
the SiC of the invention adopts rare earth modified electrostatic spinning to grind into sheet material, and then sintered into ceramic material, and the effect of rare earth elements can increase the mechanical property of the ceramic filter.
Description of the embodiments
The invention is further described below with reference to the following examples, which are illustrative of the invention and are not intended to limit the invention thereto:
example 1
The preparation method of the modified SiC ceramic flaky particles comprises the following steps:
s11, adding ethyl orthosilicate into an ethanol solution, then adding polyvinylpyrrolidone and N, N-dimethylformamide, uniformly stirring to obtain a spinning solution, carrying out electrostatic spinning on the spinning solution, and carrying out presintering at 180 ℃ for 4 hours to obtain a SiC fiber membrane;
s12, weighing cerium nitrate, yttrium nitrate, sodium dodecyl sulfate and urea which are mixed according to a molar ratio of 2:3:20:22, dissolving the cerium nitrate, the yttrium nitrate, the sodium dodecyl sulfate and the urea in deionized water together, stirring the mixture at 30 ℃, fully dissolving the mixture, immersing the SiC fiber membrane prepared in the step S11 in the mixed solution, raising the temperature of the solution to 70 ℃, reacting and precipitating the solution, then taking out the SiC fiber membrane for sintering, presintering the SiC fiber membrane in Ar atmosphere at 360 ℃ for 2.5 hours, and carrying out carbonization reduction at 1480 ℃ for 2h at a heating rate of 3 ℃/min to obtain the modified SiC fiber membrane;
s13, crushing the modified SiC fiber membrane prepared in the step 12 to obtain modified SiC ceramic flaky particles.
Example 2
The preparation method of the modified SiC ceramic flaky particles comprises the following steps:
s11, adding ethyl orthosilicate into an ethanol solution, then adding polyvinylpyrrolidone and N, N-dimethylformamide, uniformly stirring to obtain a spinning solution, carrying out electrostatic spinning on the spinning solution, and carrying out presintering at 200 ℃ for 2 hours to obtain a SiC fiber membrane;
s12, weighing cerium nitrate, yttrium nitrate, sodium dodecyl sulfate and urea which are mixed according to a molar ratio of 1:4:10:11, dissolving the cerium nitrate, the yttrium nitrate, the sodium dodecyl sulfate and the urea in deionized water, stirring the mixture at 40 ℃, fully dissolving the mixture, immersing the SiC fiber membrane prepared in the step S11 in the mixed solution, raising the temperature of the solution to 80 ℃ for reaction and sedimentation, taking out the SiC fiber membrane for sintering, presintering the SiC fiber membrane at 400 ℃ in Ar atmosphere for 3.5 h, and carrying out carbonization reduction at 1500 ℃ for 2h at a heating rate of 2 ℃/min to obtain the modified SiC fiber membrane;
s13, crushing the modified SiC fiber membrane prepared in the step 12 to obtain modified SiC ceramic flaky particles.
Example 3
The preparation method of the modified SiC ceramic flaky particles comprises the following steps:
s11, adding ethyl orthosilicate into an ethanol solution, then adding polyvinylpyrrolidone and N, N-dimethylformamide, uniformly stirring to obtain a spinning solution, carrying out electrostatic spinning on the spinning solution, and carrying out presintering at 200 ℃ for 3 hours to obtain a SiC fiber membrane;
s12, weighing cerium nitrate, yttrium nitrate, sodium dodecyl sulfate and urea which are mixed according to a molar ratio of 1:3:10:11, dissolving the cerium nitrate, the yttrium nitrate, the sodium dodecyl sulfate and the urea in deionized water, stirring the mixture at 35 ℃, fully dissolving the mixture, immersing the SiC fiber membrane prepared in the step S11 in the mixed solution, raising the temperature of the solution to 75 ℃, reacting and precipitating the solution, then taking out the SiC fiber membrane for sintering, presintering the SiC fiber membrane in Ar atmosphere at 380 ℃ for 3 hours, and carrying out carbonization reduction at 1500 ℃ for 2h at a heating rate of 2.5 ℃/min to obtain a modified SiC fiber membrane;
s13, crushing the modified SiC fiber membrane prepared in the step 12 to obtain modified SiC ceramic flaky particles.
Particle diameter of modified SiC ceramic flake particles
| Average particle diameter of flaky particles (um) | |
| Example 1 | 44.8 |
| Example 2 | 46.9 |
| Example 3 | 45.3 |
Example 4
The foam ceramic filter comprises a multi-layer filter structure, wherein the filter structure comprises a foam structure layer and a wavy electrostatic spinning layer, the pores of the electrostatic spinning layer gradually decrease from top to bottom, the porosity of the foam layer is unchanged along the flowing direction, the porosity of the wavy electrostatic spinning layer gradually increases from top to bottom along the flowing direction, and the pore diameter gradually decreases from top to bottom;
the preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a wavy structure by using polyurethane sponge, laminating a polyurethane electrostatic spinning film into a wavy shape, wherein the height from the crest to the trough of the foam structure layer and the electrostatic spinning layer is 10mm, the distance from the crest to the crest is 20mm, the thickness of the foam structure layer is 10mm, the porosity of the foam structure layer is 80%, the electrostatic spinning layer is 10mm, the porosity of the foam structure layer is changed from 80% to 90% along the flowing direction, and the foam structure layer and the electrostatic spinning film layer are compounded in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Mixing clay uniformly, adding water, stirring and mixing uniformly, sequentially adding polypropylene glycol and polyacrylamide, stirring uniformly, adding silica sol, stirring uniformly, adding the modified SiC ceramic flake particles prepared in the embodiment 1, stirring uniformly to obtain ceramic slurry, wherein Al 2 O 3 Clay, polypropylene glycol, polyacrylamide, silica sol, and the mass ratio of the modified SiC ceramic flaky particles to water is 1:0.5:0.05:0.05:2:55:20;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, wherein the sintering parameters are that the temperature is raised to 890 ℃, the temperature is kept for 4 hours, and the SiC foam ceramic is obtained after natural cooling.
Example 5
The foam ceramic filter comprises a multi-layer filter structure, wherein the filter structure comprises a foam structure layer and a wavy electrostatic spinning layer, the pores of the electrostatic spinning layer gradually decrease from top to bottom, the porosity of the foam layer is unchanged along the flowing direction, the porosity of the wavy electrostatic spinning layer gradually increases from top to bottom along the flowing direction, and the pore diameter gradually decreases from top to bottom;
the preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a wavy structure by using polyurethane sponge, laminating a polyurethane electrostatic spinning film into a wavy shape, wherein the height from the crest to the trough of the foam structure layer and the electrostatic spinning layer is 20mm, the distance from the crest to the crest is 20mm, the thickness of the foam structure layer is 15mm, the porosity of the foam structure layer is 90%, the electrostatic spinning layer is 5mm, the porosity of the foam structure layer is changed from 90% to 95% along the flowing direction, and the foam structure layer and the electrostatic spinning film layer are compounded in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Mixing clay uniformly, adding water, stirring and mixing uniformly, sequentially adding polypropylene glycol and polyacrylamide, stirring uniformly, adding silica sol, stirring uniformly, adding the modified SiC ceramic flake particles prepared in the embodiment 2, stirring uniformly to obtain ceramic slurry, wherein Al 2 O 3 Clay, polypropylene glycol, polyacrylamide, silica sol, and the mass ratio of the modified SiC ceramic flaky particles to water is 2:1.2:0.1:0.12:6:65:30;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, wherein the sintering parameters are that the temperature is raised to 1080 ℃, the heat is preserved for 2 hours, and naturally cooling is carried out, so that the SiC foam ceramic is obtained.
Example 6
The foam ceramic filter comprises a multi-layer filter structure, wherein the filter structure comprises a foam structure layer and a wavy electrostatic spinning layer, the pores of the electrostatic spinning layer gradually decrease from top to bottom, the porosity of the foam layer is unchanged along the flowing direction, the porosity of the wavy electrostatic spinning layer gradually increases from top to bottom along the flowing direction, and the pore diameter gradually decreases from top to bottom;
the preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a wavy structure by using polyurethane sponge, laminating a polyurethane electrostatic spinning film into a wavy shape, wherein the height from the crest to the trough of the foam structure layer and the electrostatic spinning layer is 14mm, the distance from the crest to the crest is 15mm, the thickness of the foam structure layer is 10mm, the porosity of the foam structure layer is 80%, the porosity of the electrostatic spinning layer is 9mm, the porosity of the electrostatic spinning layer is changed from 80% to 90% along the flowing direction, and the foam structure layer and the electrostatic spinning film layer are compounded in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Mixing clay uniformly, adding water, stirring and mixing uniformly, sequentially adding polypropylene glycol and polyacrylamide, stirring uniformly, adding silica sol, stirring uniformly, adding the modified SiC ceramic flake particles prepared in the embodiment 3, stirring uniformly to obtain ceramic slurry, wherein Al 2 O 3 Clay, polypropylene glycol, polyacrylamide, silica sol, modified SiC ceramic flaky particles and water in a mass ratio of 1:0.6:0.06:0.06:4:58:24;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, wherein the sintering parameters are that the temperature is raised to 950 ℃, the heat is preserved for 4 hours, and the SiC foam ceramic is obtained after natural cooling.
Example 7
The foam ceramic filter comprises a multi-layer filter structure, wherein the filter structure comprises a foam structure layer and a wavy electrostatic spinning layer, the pores of the electrostatic spinning layer gradually decrease from top to bottom, the porosity of the foam layer is unchanged along the flowing direction, the porosity of the wavy electrostatic spinning layer gradually increases from top to bottom along the flowing direction, and the pore diameter gradually decreases from top to bottom;
the preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a wavy structure by using polyurethane sponge, laminating a polyurethane electrostatic spinning film into a wavy shape, wherein the height from the crest to the trough of the foam structure layer and the electrostatic spinning layer is 18mm, the distance from the crest to the crest is 15mm, the thickness of the foam structure layer is 15mm, the porosity of the foam structure layer is 90%, the porosity of the electrostatic spinning layer is 6mm, the porosity of the electrostatic spinning layer is changed from 90% to 95% along the flowing direction, and the foam structure layer and the electrostatic spinning film layer are compounded in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Mixing clay uniformly, adding water, stirring and mixing uniformly, sequentially adding polypropylene glycol and polyacrylamide, stirring uniformly, adding silica sol, stirring uniformly, adding the modified SiC ceramic flake particles prepared in the embodiment 3, stirring uniformly to obtain ceramic slurry, wherein Al 2 O 3 Clay, polypropylene glycol, polyacrylamide, silica sol, modified SiC ceramic flaky particles and water in a mass ratio of 2:01:0.08:0.1:5:60:28;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, wherein the sintering parameters are that the temperature is raised to 1050 ℃, the heat is preserved for 3 hours, and the SiC foam ceramic is obtained after natural cooling.
Example 8
The foam ceramic filter comprises a multi-layer filter structure, wherein the filter structure comprises a foam structure layer and a wavy electrostatic spinning layer, the pores of the electrostatic spinning layer gradually decrease from top to bottom, the porosity of the foam layer is unchanged along the flowing direction, the porosity of the wavy electrostatic spinning layer gradually increases from top to bottom along the flowing direction, and the pore diameter gradually decreases from top to bottom;
the preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a wavy structure by using polyurethane sponge, laminating a polyurethane electrostatic spinning film into a wavy shape, wherein the height from the crest to the trough of the foam structure layer and the electrostatic spinning layer is 15mm, the distance from the crest to the crest is 15mm, the thickness of the foam structure layer is 15mm, the porosity of the foam structure layer is 85%, the porosity of the electrostatic spinning layer is 7mm, the porosity of the electrostatic spinning layer is changed from 85% to 92% along the flowing direction, and the foam structure layer and the electrostatic spinning film layer are compounded in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Mixing clay uniformly, adding water, stirring and mixing uniformly, sequentially adding polypropylene glycol and polyacrylamide, stirring uniformly, adding silica sol, stirring uniformly, adding the modified SiC ceramic flake particles prepared in the embodiment 3, stirring uniformly to obtain ceramic slurry, wherein Al 2 O 3 Clay, polypropylene glycol, polyacrylamide, silica sol, modified SiC ceramic platelet particles and water in a mass ratio of 1.2:0.8:0.06:0.08:4.5:60:26;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, wherein the sintering parameters are that the temperature is raised to 1020 ℃, the temperature is kept for 3.5 hours, and naturally cooling to obtain the SiC foam ceramic.
Comparative example 1
The foam ceramic filter comprises a multi-layer filter structure, wherein the filter structure comprises a foam structure layer and a wavy electrostatic spinning layer, the pores of the electrostatic spinning layer gradually decrease from top to bottom, the porosity of the foam layer is unchanged along the flowing direction, the porosity of the wavy electrostatic spinning layer gradually increases from top to bottom along the flowing direction, and the pore diameter gradually decreases from top to bottom;
the preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a wavy structure by using polyurethane sponge, laminating a polyurethane electrostatic spinning film into a wavy shape, wherein the height from the crest to the trough of the foam structure layer and the electrostatic spinning layer is 20mm, the distance from the crest to the crest is 20mm, the thickness of the foam structure layer is 15mm, the porosity of the foam structure layer is 90%, the electrostatic spinning layer is 5mm, the porosity of the foam structure layer is changed from 90% to 95% along the flowing direction, and the foam structure layer and the electrostatic spinning film layer are compounded in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Mixing clay uniformly, adding water, stirring and mixing uniformly, sequentially adding polypropylene glycol and polyacrylamide, stirring uniformly, adding silica sol, stirring uniformly, adding SiC particles, stirring uniformly to obtain ceramic slurry, wherein Al 2 O 3 Clay, polypropylene glycol, polyacrylamide, silica sol, siC particles and water in a mass ratio of 2:1.2:0.1:0.12:6:65:30;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, wherein the sintering parameters are that the temperature is raised to 1080 ℃, the heat is preserved for 2 hours, and naturally cooling is carried out, so that the SiC foam ceramic is obtained.
Comparative example 2
The foam ceramic filter comprises a multi-layer filter structure, wherein the filter structure comprises a foam structure layer and an electrostatic spinning layer, the pores of the electrostatic spinning layer gradually decrease from top to bottom, the porosity of the foam layer is unchanged along the flowing direction, the porosity of the electrostatic spinning layer gradually increases from top to bottom along the flowing direction, and the pore diameter gradually decreases from top to bottom;
the preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a specified size by using polyurethane sponge and a polyurethane electrostatic spinning film layer, wherein the thickness of the foam structure layer is 15mm, the porosity of the foam structure layer is 85%, the electrostatic spinning layer is 7mm, the porosity of the foam structure layer is changed from 85% to 92% along the flowing direction, and the foam structure layer and the electrostatic spinning film layer are compounded in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Mixing clay uniformly, adding water, stirring and mixing uniformly, sequentially adding polypropylene glycol and polyacrylamide, stirring uniformly, adding silica sol, stirring uniformly, adding the modified SiC ceramic flake particles prepared in the embodiment 3, stirring uniformly to obtain ceramic slurry, wherein Al 2 O 3 Clay, polypropylene glycol, polyacrylamide, silica sol, modified SiC ceramic flaky particles and water in a mass ratio of 1.2:0.8:0.06:0.08:4.5:60:26;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, wherein the sintering parameters are that the temperature is raised to 1020 ℃, the temperature is kept for 3.5 hours, and naturally cooling to obtain the SiC foam ceramic.
Comparative example 3
A ceramic foam filter comprising a multi-layer filter structure, the filter structure comprising a foam structure layer;
the preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a specified size by using polyurethane sponge, wherein the thickness of the foam structure layer is 30mm, and the porosity of the foam structure layer is 85%;
s2, preparing ceramic slurry: al is added with 2 O 3 After the clay is uniformly mixedAdding water, stirring, mixing, sequentially adding polypropylene glycol and polyacrylamide, stirring, adding silica sol, stirring, adding the modified SiC ceramic flake particles prepared in example 3, stirring to obtain ceramic slurry, wherein Al 2 O 3 Clay, polypropylene glycol, polyacrylamide, silica sol, modified SiC ceramic flaky particles and water in a mass ratio of 1.2:0.8:0.06:0.08:4.5:60:26;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, wherein the sintering parameters are that the temperature is raised to 1020 ℃, the temperature is kept for 3.5 hours, and naturally cooling to obtain the SiC foam ceramic.
Comparative example 4
The preparation method of the SiC ceramic flaky particles comprises the following steps:
adding ethyl orthosilicate into an ethanol solution, then adding polyvinylpyrrolidone and N, N-dimethylformamide, stirring uniformly to obtain a spinning solution, carrying out electrostatic spinning on the spinning solution, presintering at 200 ℃ for 3 hours, presintering at 380 ℃ for 3 hours in Ar atmosphere, carrying out carbonization and reduction at 1500 ℃ for 2 hours after the heating rate is 3 ℃/min, obtaining a SiC fiber film, and crushing the SiC fiber film to obtain SiC ceramic flaky particles;
the foam ceramic filter comprises a multi-layer filter structure, wherein the filter structure comprises a foam structure layer and a wavy electrostatic spinning layer, the pores of the electrostatic spinning layer gradually decrease from top to bottom, the porosity of the foam layer is unchanged along the flowing direction, the porosity of the wavy electrostatic spinning layer gradually increases from top to bottom along the flowing direction, and the pore diameter gradually decreases from top to bottom;
the preparation method of the foam ceramic filter comprises the following steps:
s1, selecting a base material: cutting the foam structure layer into a wavy structure by using polyurethane sponge, laminating a polyurethane electrostatic spinning film into a wavy shape, wherein the height from the crest to the trough of the foam structure layer and the electrostatic spinning layer is 18mm, the distance from the crest to the crest is 15mm, the thickness of the foam structure layer is 15mm, the porosity of the foam structure layer is 90%, the porosity of the electrostatic spinning layer is 6mm, the porosity of the electrostatic spinning layer is changed from 90% to 95% along the flowing direction, and the foam structure layer and the electrostatic spinning film layer are compounded in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Mixing clay uniformly, adding water, stirring and mixing uniformly, sequentially adding polypropylene glycol and polyacrylamide, stirring uniformly, adding silica sol, stirring uniformly, adding SiC ceramic flaky particles, stirring uniformly to obtain ceramic slurry, wherein Al 2 O 3 Clay, polypropylene glycol, polyacrylamide, silica sol, siC ceramic platelet particles and water in a mass ratio of 2:01:0.08:0.1:5:60:28;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, wherein the sintering parameters are that the temperature is raised to 1050 ℃, the heat is preserved for 3 hours, and the SiC foam ceramic is obtained after natural cooling.
Comparing various indexes of the finished product, the main performance indexes of the finished product are as follows (according to national standard):
it is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (9)
1. The utility model provides a foam ceramic filter, its characterized in that includes multilayer filtration, filtration is including foam structure layer and wave formula electrostatic spinning layer, and the aperture from the top down of electrostatic spinning layer diminishes gradually, foam layer is unchangeable along flow direction porosity, wave formula electrostatic spinning layer increases from top to bottom along flow direction porosity, and the aperture diminishes gradually from top to bottom.
2. The method for preparing a ceramic foam filter according to claim 1, comprising the steps of:
s1, selecting a base material: cutting the foam structure layer into a wavy structure by using polyurethane sponge, laminating a polyurethane electrostatic spinning film into a wavy shape, and compounding the foam structure layer and the electrostatic spinning film layer in a needling mode;
s2, preparing ceramic slurry: al is added with 2 O 3 Adding water after clay is uniformly mixed, stirring and uniformly mixing, sequentially adding polypropylene glycol and polyacrylamide, stirring and uniformly mixing, adding silica sol, stirring and uniformly mixing, adding modified SiC ceramic flaky particles, and stirring and uniformly mixing to obtain ceramic slurry;
s3, preparing a ceramic precast block: immersing the substrate into the ceramic slurry, taking out the substrate containing the ceramic slurry, extruding, drying, immersing the substrate into the ceramic slurry once again, and drying to obtain the SiC foam ceramic precast block;
s4, preparing foamed ceramics: and (3) placing the SiC foam ceramic precast block into a heating furnace for sintering, and naturally cooling to obtain the SiC foam ceramic.
3. The method for preparing the foam ceramic filter according to claim 2, wherein: the preparation method of the modified SiC ceramic flaky particles comprises the following steps:
s11, adding ethyl orthosilicate into an ethanol solution, then adding polyvinylpyrrolidone and N, N-dimethylformamide, uniformly stirring to obtain a spinning solution, carrying out electrostatic spinning on the spinning solution, and carrying out presintering to obtain a SiC fiber membrane;
s12, weighing a certain amount of cerium nitrate, yttrium nitrate, sodium dodecyl sulfate and urea to be dissolved in deionized water together, stirring at 30-40 ℃ to be fully dissolved, immersing the SiC fiber membrane prepared in the step S11 into the mixed solution, raising the temperature of the solution to 70-80 ℃ to react and precipitate, and then taking out the SiC fiber membrane to be sintered to obtain the modified SiC fiber membrane;
s13, crushing the modified SiC fiber membrane prepared in the step 12 to obtain modified SiC ceramic flaky particles.
4. The method for preparing the foam ceramic filter according to claim 2, wherein: al in the step S1 2 O 3 The mass ratio of clay, polypropylene glycol, polyacrylamide, silica sol, modified SiC ceramic flaky particles and water is 1-2:0.5-1.2:0.05-0.1:0.05-0.12:2-6:55-65:20-30.
5. The method for preparing the foam ceramic filter according to claim 2, wherein: and the sintering parameters in the step S3 are that the temperature is raised to 890-1080 ℃, and the temperature is kept for 2-4 hours.
6. A method of making a ceramic foam filter according to claim 3, wherein: the presintering temperature in the step S11 is 180-200 ℃ and the presintering time is 2-4h.
7. A method of making a ceramic foam filter according to claim 3, wherein: in the step S12, the molar ratio of cerium nitrate to yttrium nitrate to sodium dodecyl sulfate to urea is 2:3-8:20:22.
8. A method of making a ceramic foam filter according to claim 3, wherein: the sintering parameters in the step S12 are pre-sintering 2.5-3.5 h at 360-400 ℃ in Ar atmosphere, and after the heating rate is 3 ℃/min, carbonizing and reducing 2h at 1480-1500 ℃ and the heating rate is 2-3 ℃/min.
9. A method of making a ceramic foam filter according to claim 3, wherein: the particle size of the modified SiC ceramic flake particles in the step S14 is 20-50um.
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