CN101591164A - The preparation method of alumina porous ceramic - Google Patents
The preparation method of alumina porous ceramic Download PDFInfo
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- CN101591164A CN101591164A CNA2008100167146A CN200810016714A CN101591164A CN 101591164 A CN101591164 A CN 101591164A CN A2008100167146 A CNA2008100167146 A CN A2008100167146A CN 200810016714 A CN200810016714 A CN 200810016714A CN 101591164 A CN101591164 A CN 101591164A
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Abstract
The invention provides the preparation method of a method of porous alumina ceramics; comprise the preparation of suspension ceramic slurry; foaming; moulding and burning till; it is characterized in that: it is the bubble of 5～600 μ m that the suspension ceramic slurry for preparing is added a certain amount of whipping agent powerful stirring certain hour formation diameter in nitrogen environment; add initiator and catalyzer continuation stirring then and obtained the porous slurry in 0.5～3 minute; the porous slurry is injected non-suction mould; room temperature was placed 1 minute～48 hours under nitrogen protection; be 10 minutes～6 hours curing moldings 60～150 ℃ following time of temperature then; demoulding drying then; the water ratio of base substrate is lower than below the 0.5wt%; with dried base substrate degreasing, and burn till under certain condition.Because ceramic powder is evenly distributed in the suspension ceramic slurry, and adopt special foam theory, make the many and size of the porous slurry bubble that makes, be evenly distributed, even by its alumina porous ceramic base substrate microstructure, density of making, the alumina porous ceramic yield rate height that makes.
Description
Technical field
The present invention relates to the preparation method of a method of porous alumina ceramics, belong to the porous ceramics preparing technical field.
Background technology
The tradition porous ceramics be adopt slip casting, extrude, ramming and etc. traditional production method productions such as static pressure, prepare porous ceramics by the particle packing and the method for adding pore forming agent.Because production technique and technology limitation, the alumina porous ceramic aperture of production and density distribution is inhomogeneous, intensity is low and production cost is high in use is easy to generate stress concentration, causes cracking.
Summary of the invention
The object of the present invention is to provide a kind of porous ceramics even aperture distribution that can overcome above-mentioned defective, make and production cost is low, the preparation method of the alumina porous ceramic of product excellent working performance, its technical scheme is:
The preparation method of one method of porous alumina ceramics; comprise the preparation of suspension ceramic slurry; foaming; moulding and burning till; wherein the preparation of suspension ceramic slurry is with the organic monomer formation organic solution that is dissolved in the water by a certain percentage; organic solution and dispersion agent mix the back by a certain percentage and adjust required pH and make mixed organic solvents; with granularity be then the alumina-ceramic powder of 0.2～5-and mixed organic solvents by a certain percentage thorough mixing make the suspension ceramic slurry; it is characterized in that: the suspension ceramic slurry adds a certain amount of whipping agent powerful certain hour that stirs in nitrogen environment; forming hole diameter by the control churning time is the bubble of 5～600 μ m; add initiator and catalyzer continuation stirring then and obtained the porous slurry in 0.5～3 minute; the porous slurry is injected non-suction mould; room temperature was placed 1 minute～48 hours under nitrogen protection; be 10 minutes～6 hours curing moldings 60～150 ℃ following time of temperature then; demoulding drying then; the water ratio of base substrate is lower than below the 0.5wt%, burns till under certain condition then.
The preparation method of described alumina porous ceramic, organic solution is dissolved in by organic monomer 1～75wt% in the water of 25～99wt% and forms, wherein the component of organic monomer is N, N-methylene radical acrylamide and acrylamide, its weight percent is 1～10: 90～99, organic solution and dispersion agent by weight percentage 85～97: 3～15 mix after, again its pH value is adjusted to 8～11, promptly make mixed organic solvents.
The preparation method of described alumina porous ceramic, dispersion agent adopts the polyacrylic acid ammonium solution, its concentration is 20～60wt%, it is 40～60wt% ammoniacal liquor or 40～60wt% lactic acid that the pH value is adjusted agent, promptly to reduce the pH value of mixed organic solvents, the pH value is adjusted agent and is adopted 40～60wt% lactic acid, otherwise the pH value is adjusted agent employing 40～60wt% ammoniacal liquor.
The preparation method of described alumina porous ceramic, with alumina-ceramic powder and mixed organic solvents according to weight percent 60～90: 10～40 add ballstone after mixing grind after, vacuum-treat does not have bubble to overflow to slurry again, makes even suspension ceramic slurry.
The preparation method of described alumina porous ceramic, the alumina-ceramic powder is the mixture of aluminum oxide powder 80～100wt%, clay 0～20wt%, talcum 0～10wt%, yttrium oxide 0～2wt%, silicon nitride 0～2wt% and magnesiumcarbonate 0～5wt%.
The preparation method of described alumina porous ceramic, whipping agent is any of oxidized nicotinamide, lipid acid, hydroxy ethyl cellulose, alkyl acyl aminopropyl dimethylamine oxide compound, n-hexyl alcohol, normal heptane, alkylol amide phosphoric acid fat, fatty alcohol-polyoxyethylene ether phosphoric acid fat, octyl phenyl Soxylat A 25-7, ammonium polyacrylate, polyoxyethylenesorbitan sorbitan monooleate, rhamnolipid, n-Hexadecane Phenylsulfonic acid, and add-on is 0.001～5wt% of suspension ceramic slurry.
The preparation method of described alumina porous ceramic, it is the ammonium persulfate solution of 1～5wt% that initiator adopts concentration, add-on is 0.01～0.2wt% of suspension ceramic slurry, catalyzer adopts N, N, N, N-4-methyl hexamethylene diamine, add-on are 0.01～0.2wt% of suspension ceramic slurry.
The preparation method of described alumina porous ceramic, the suspension ceramic slurry brute force in nitrogen environment that is added with whipping agent stirred 1～20 minute, and the suspension ceramic slurry is fully foamed.
The preparation method of described alumina porous ceramic, alumina porous ceramic was fired in 1400～1700 ℃ temperature range 10～180 minutes, made alumina porous ceramic.
The present invention compared with prior art, its advantage is: because ceramic powder is evenly distributed in the suspension ceramic slurry, and adopt special foam theory, make the many and size of the porous slurry bubble that makes, be evenly distributed, even by its alumina porous ceramic base substrate microstructure, density of making, the alumina porous ceramic yield rate height that makes at last.
Embodiment
Embodiment 1
Step is:
1, preparation alumina-ceramic powder: granularity is that the alumina powder jointed 80wt% of 0.5 μ m and clay 20wt% are mixed.
2, preparation mixed organic solvents: with N, N-methylene radical acrylamide and acrylamide dissolve in the water with 2: 98 mixed organic monomers that get of weight percent, the weight percent of organic monomer and water is 5: 95, make organic solution, the polyacrylic acid ammonium solution dispersion agent that with organic solution and concentration is 40wt% again mixes with 9: 1 weight ratio, be that the ammoniacal liquor of 50wt% adjusts to 9 with the pH value of mixed solution with concentration then, promptly make mixed organic solvents.
3, preparation suspension ceramic slurry: after adding the ballstone grinding after the mixed organic solvents that alumina-ceramic powder and the step 2 of step 1 gained made mixes according to 4: 1 weight ratio, vacuum-treat does not have bubble to overflow to slurry again, makes even suspension ceramic slurry.
4; moulding: the suspension ceramic slurry is added 0.01wt% hydroxy ethyl cellulose whipping agent under nitrogen protection; stirring velocity is the powerful stirring of 200 rev/mins rotating speed 4 minutes; the concentration that adds 0.01wt% then is the initiator ammonium persulfate solution of 4wt% and the N of 0.01wt%; N; N; N-4-methyl hexamethylene diamine catalyzer; restir obtained the porous slurry in 3 minutes; the porous slurry is injected in the non-suction mould then; room temperature is placed after 48 hours 60 ℃ of temperature under nitrogen protection; time is curing molding under 6 hours the condition; the demoulding is dried to water ratio and is lower than below the 0.5wt% then, forms the alumina porous ceramic base substrate.
5, burn till: base substrate was fired under 1400 ℃ temperature 60 minutes, made alumina porous ceramic.
The purity of testing used proportion material is technical pure.
The alumina porous ceramic intensity that obtains is 10MPa, and density is 0.4g/cm
3
Embodiment 2:
Step is:
1, preparation alumina-ceramic powder: granularity is that alumina powder jointed 90wt%, the clay 7wt% of 2 μ m and talcum 3wt% are mixed.
2, preparation mixed organic solvents: with N, N-methylene radical acrylamide and acrylamide dissolve in the water with 5: 95 mixed organic monomers that get of weight percent, the weight ratio of organic monomer and water is 1: 4, make organic solution, the polyacrylic acid ammonium solution dispersion agent that with organic solution and concentration is 60wt% again mixes with 97: 3 weight percent, be that the ammoniacal liquor of 60wt% adjusts to 10 with the pH value of mixed solution with concentration then, promptly make mixed organic solvents.
3, preparation suspension ceramic slurry: after adding the ballstone grinding after the mixed organic solvents that alumina-ceramic powder and the step 2 of step 1 gained made mixes according to 7: 3 weight ratio, vacuum-treat does not have bubble to overflow to slurry again, makes even suspension ceramic slurry.
4; blank forming: the suspension ceramic slurry is added 0.5wt% polyoxyethylenesorbitan sorbitan monooleate whipping agent under nitrogen protection; stirring velocity is the powerful stirring of 100 rev/mins rotating speed 20 minutes; the concentration that adds 0.1wt% then is the ammonium persulfate solution initiator of 2wt% and the N of 0.1wt%; N; N; N-4-methyl hexamethylene diamine catalyzer; restir obtained the porous slurry in 1 minute; the porous slurry is injected in the non-suction mould then; room temperature was placed after 24 hours under nitrogen protection; again 90 ℃ of temperature; curing molding under the condition of 1 hour time; the demoulding is dried to water ratio and is lower than below the 0.5wt% then, forms the alumina porous ceramic base substrate.
5, burn till: base substrate was fired under 1500 ℃ temperature 180 minutes, made alumina porous ceramic.
The purity of testing used proportion material is technical pure.
The alumina porous ceramic intensity that obtains is 8MPa, and density is 0.6g/cm
3
Embodiment 3:
Step is:
1, preparation alumina-ceramic powder: granularity is that alumina powder jointed 97wt%, the yttrium oxide 1wt% of 5 μ m and magnesiumcarbonate 2wt% are mixed.
2, preparation mixed organic solvents: with N, N-methylene radical acrylamide and acrylamide dissolve in the water with 10: 90 mixed organic monomers that get of weight percent, the weight percent of organic monomer and water is 70: 30, make organic solution, the polyacrylic acid ammonium solution dispersion agent that with organic solution and concentration is 20wt% again mixes with 85: 15 weight percent, be that the ammoniacal liquor of 40wt% adjusts to 11 with the pH value of mixed solution with concentration then, promptly make mixed organic solvents.
3, preparation suspension ceramic slurry: after adding the ballstone grinding after the mixed organic solvents that alumina-ceramic powder and the step 2 of step 1 gained made mixes according to 17: 3 weight ratio, vacuum-treat does not have bubble to overflow to slurry again, makes even suspension ceramic slurry.
4; blank forming: the suspension ceramic slurry is added 3wt% alkyl acyl aminopropyl dimethylamine oxide compound whipping agent under nitrogen protection; stirring velocity is the powerful stirring of 150 rev/mins rotating speed 12 minutes; the concentration that adds 0.2wt% then is the ammonium persulfate solution initiator of 1wt% and the N of 0.2wt%; N; N; N-4-methyl hexamethylene diamine catalyzer; restir obtained the porous slurry in 0.5 minute; the porous slurry is injected in the non-suction mould then; room temperature was placed after 5 minutes under nitrogen protection; again 90 ℃ of temperature; curing molding under the condition of 30 minutes time; the demoulding is dried to water ratio and is lower than below the 0.5wt% then, forms the alumina porous ceramic base substrate.
5, burn till: base substrate was fired under 1600 ℃ temperature 120 minutes, made alumina porous ceramic.
The purity of testing used proportion material is technical pure.
The alumina porous ceramic intensity that obtains is 7MPa, and density is 0.8g/cm
3
Embodiment 4:
Step is:
1, preparation alumina-ceramic powder: granularity is that alumina powder jointed 97wt%, the silicon nitride 2wt% of 2 μ m and magnesiumcarbonate 1wt% are mixed.
2, preparation mixed organic solvents: with N, N-methylene radical acrylamide and acrylamide dissolve in the water with 10: 90 mixed organic monomers that get of weight percent, the weight percent of organic monomer and water is 70: 30, make organic solution, the polyacrylic acid ammonium solution dispersion agent that with organic solution and concentration is 20wt% again mixes with 85: 15 weight percent, be that the ammoniacal liquor of 40wt% adjusts to 11 with the pH value of mixed solution with concentration then, promptly make mixed organic solvents.
3, preparation suspension ceramic slurry: after adding the ballstone grinding after the mixed organic solvents that alumina-ceramic powder and the step 2 of step 1 gained made mixes according to 17: 3 weight ratio, vacuum-treat does not have bubble to overflow to slurry again, makes even suspension ceramic slurry.
4; blank forming: the suspension ceramic slurry is added 3wt% alkyl acyl aminopropyl dimethylamine oxide compound whipping agent under nitrogen protection; stirring velocity is the powerful stirring of 150 rev/mins rotating speed 12 minutes; the concentration that adds 0.2wt% then is the ammonium persulfate solution initiator of 1wt% and the N of 0.2wt%; N; N; N-4-methyl hexamethylene diamine catalyzer; restir obtained the porous slurry in 0.5 minute; the porous slurry is injected in the non-suction mould then; room temperature was placed after 5 minutes under nitrogen protection; again 90 ℃ of temperature; curing molding under the condition of 30 minutes time, the demoulding is dried to water ratio and is lower than below the 0.5wt% then, forms the alumina porous ceramic base substrate.
5, burn till: base substrate was fired under 1650 ℃ temperature 120 minutes, made alumina porous ceramic.
The purity of testing used proportion material is technical pure.
The alumina porous ceramic intensity that obtains is 15MPa, and density is 0.8g/cm
3
Claims (9)
1; the preparation method of one method of porous alumina ceramics; comprise the preparation of suspension ceramic slurry; foaming; moulding and burning till; wherein the preparation of suspension ceramic slurry is with the organic monomer formation organic solution that is dissolved in the water by a certain percentage; organic solution and dispersion agent mix the back by a certain percentage and adjust required pH and make mixed organic solvents; with granularity be then the alumina-ceramic powder of 0.2～5 μ m and mixed organic solvents by a certain percentage thorough mixing make the suspension ceramic slurry; it is characterized in that: the suspension ceramic slurry adds a certain amount of whipping agent powerful certain hour that stirs in nitrogen environment; forming hole diameter by the control churning time is the bubble of 5～600 μ m; add initiator and catalyzer continuation stirring then and obtained the porous slurry in 0.5～3 minute; the porous slurry is injected non-suction mould; room temperature was placed 1 minute～48 hours under nitrogen protection; be 10 minutes～6 hours curing moldings 60～150 ℃ following time of temperature then; demoulding drying then; the water ratio of base substrate is lower than below the 0.5wt%, burns till under certain condition then.
2, the preparation method of alumina porous ceramic as claimed in claim 1, it is characterized in that: organic solution is dissolved in by organic monomer 1～75wt% in the water of 25～99wt% and forms, wherein the component of organic monomer is N, N-methylene radical acrylamide and acrylamide, its weight percent is 1～10: 90～99, organic solution and dispersion agent by weight percentage 85～97: 3～15 mix after, again its pH value is adjusted to 8～11, promptly make mixed organic solvents.
3, the preparation method of alumina porous ceramic as claimed in claim 1 or 2, it is characterized in that: dispersion agent adopts the polyacrylic acid ammonium solution, its concentration is 20～60wt%, it is 40～60wt% ammoniacal liquor or 40～60wt% lactic acid that the pH value is adjusted agent, promptly to reduce the pH value of mixed organic solvents, the pH value is adjusted agent and is adopted 40～60wt% lactic acid, otherwise the pH value is adjusted agent employing 40～60wt% ammoniacal liquor.
4, the preparation method of alumina porous ceramic as claimed in claim 1, it is characterized in that: with alumina-ceramic powder and mixed organic solvents according to weight percent 60～90: 10～40 add ballstone after mixing grind after, vacuum-treat does not have bubble to overflow to slurry again, makes even suspension ceramic slurry.
5, the preparation method of alumina porous ceramic as claimed in claim 1 is characterized in that: the alumina-ceramic powder is the mixture of aluminum oxide powder 80～100wt%, clay 0～20wt%, talcum 0～10wt%, yttrium oxide 0～2wt%, silicon nitride 0～2wt% and magnesiumcarbonate 0～5wt%.
6, the preparation method of alumina porous ceramic as claimed in claim 1, it is characterized in that: whipping agent is any of oxidized nicotinamide, lipid acid, hydroxy ethyl cellulose, alkyl acyl aminopropyl dimethylamine oxide compound, n-hexyl alcohol, normal heptane, alkylol amide phosphoric acid fat, fatty alcohol-polyoxyethylene ether phosphoric acid fat, octyl phenyl Soxylat A 25-7, ammonium polyacrylate, polyoxyethylenesorbitan sorbitan monooleate, rhamnolipid, n-Hexadecane Phenylsulfonic acid, and add-on is 0.001～5wt% of suspension ceramic slurry.
7, the preparation method of alumina porous ceramic as claimed in claim 1, it is characterized in that: it is the ammonium persulfate solution of 1～5wt% that initiator adopts concentration, add-on is 0.01～0.2wt% of suspension ceramic slurry, catalyzer adopts N, N, N, the N-4-methyl hexamethylene diamine, add-on is 0.01～0.2wt% of suspension ceramic slurry.
8, the preparation method of alumina porous ceramic as claimed in claim 1 is characterized in that: be added with suspension ceramic slurry powerful stirring 1～20 minute in nitrogen environment of whipping agent, the suspension ceramic slurry is fully foamed.
9, the preparation method of alumina porous ceramic as claimed in claim 1 is characterized in that: alumina porous ceramic was fired in 1400～1700 ℃ temperature range 10～180 minutes, made alumina porous ceramic.
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| CN102659398A (en) * | 2012-04-25 | 2012-09-12 | 中钢集团洛阳耐火材料研究院有限公司 | Method for manufacturing light magnesia-alumina spinel insulation materials |
| CN102659427A (en) * | 2012-04-25 | 2012-09-12 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method for light refractory raw material |
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| CN104311095A (en) * | 2014-09-25 | 2015-01-28 | 山东理工大学 | Method for preparing porous ceramic from active alumina precursor |
| CN104311109A (en) * | 2014-10-09 | 2015-01-28 | 山东理工大学 | Method for preparing foamed ceramic through foaming, injection molding and cementing of aluminum dihydrogen phosphate |
| CN104909752A (en) * | 2015-05-19 | 2015-09-16 | 铜陵宏正网络科技有限公司 | Alumina fiber reinforced gypsum ceramic matrix composite and preparation method thereof |
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| CN100334041C (en) * | 2005-06-23 | 2007-08-29 | 华东理工大学 | Porous ceramics preparation method |
| CN100384781C (en) * | 2006-12-06 | 2008-04-30 | 中国科学院上海硅酸盐研究所 | Method for preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process |
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| CN102659398A (en) * | 2012-04-25 | 2012-09-12 | 中钢集团洛阳耐火材料研究院有限公司 | Method for manufacturing light magnesia-alumina spinel insulation materials |
| CN102659427A (en) * | 2012-04-25 | 2012-09-12 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method for light refractory raw material |
| CN102659398B (en) * | 2012-04-25 | 2014-02-26 | 中钢集团洛阳耐火材料研究院有限公司 | Method for manufacturing light magnesia-alumina spinel insulation materials |
| CN102964083A (en) * | 2012-10-26 | 2013-03-13 | 安徽艾柯泡塑股份有限公司 | Modified soy protein foaming agent for concrete |
| CN102964083B (en) * | 2012-10-26 | 2014-05-07 | 安徽艾柯泡塑股份有限公司 | Modified soy protein foaming agent for concrete |
| CN104311095A (en) * | 2014-09-25 | 2015-01-28 | 山东理工大学 | Method for preparing porous ceramic from active alumina precursor |
| CN104311095B (en) * | 2014-09-25 | 2017-09-22 | 山东理工大学 | The method that porous ceramics is prepared with activated alumina presoma |
| CN104311109A (en) * | 2014-10-09 | 2015-01-28 | 山东理工大学 | Method for preparing foamed ceramic through foaming, injection molding and cementing of aluminum dihydrogen phosphate |
| CN104909752A (en) * | 2015-05-19 | 2015-09-16 | 铜陵宏正网络科技有限公司 | Alumina fiber reinforced gypsum ceramic matrix composite and preparation method thereof |
| CN116444287A (en) * | 2023-04-19 | 2023-07-18 | 国发环保新材料(江门)有限公司 | Foamed ceramic production process and equipment |
| CN116444287B (en) * | 2023-04-19 | 2024-05-07 | 国发环保新材料(江门)有限公司 | Foamed ceramic production process and equipment |
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