CN104311095A - Method for preparing porous ceramic from active alumina precursor - Google Patents
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Abstract
The invention relates to a method for preparing high-strength and high-porosity ceramic by preparing an active alumina precursor from inorganic aluminum salt, adding ceramic fibers and ceramic powder into the active alumina precursor, and carrying out filtering, washing, molding and sintering. Concretely, the method comprises the following steps of adding a dispersant and short ceramic fibers into an inorganic aluminum salt solution, carrying out uniform dispersion, adding the dispersion liquid into a precipitating agent solution to obtain precipitates, adding ceramic powder into the precipitates, carrying out filtering and washing to obtain the precursor, mixing the precursor and a binder to obtain a uniform mixture, carrying out molding and drying to obtain a high-strength green blank, carrying out machining such as turning according to demand, and carrying out two-step sintering in atmosphere, wherein in the two-step sintering, the first sintering process comprises that activated aluminum oxide in the ceramic blank is transformed into alpha-alumina in reduction atmosphere or inert gas atmosphere and simultaneously, the organic matter is transformed into carbon, and the second sintering process comprises that the carbon is oxidized and volatilized in oxidation atmosphere so that the porous ceramic is obtained. Compared with the foamed ceramic which is prepared by the prior art and has a similar cost, the foamed ceramic prepared by the method has high ceramic strength and high porosity.
Description
Technical field
The present invention relates to field of ceramic preparation technology.Specifically, relate to and a kind of prepare activated alumina presoma by inorganic aluminate, add ceramic fiber and ceramic powder, filtration washing, shaping, burn till, the method for obtained high strength, high porosity ceramic.
Background technology
porous ceramics has that chemical stability is high, thermal conductivity is low and high temperature resistant, corrosion-resistant, the feature such as intensity is high, rigidity is large; be widely applied in fields such as metallurgy, chemical industry, environmental protection, the energy, biologies; as aspect [Wang Hui such as fluid purification filtration, purification separation, support of the catalyst, sound absorption damping, lagging material, biological and medicinal implant material, materials for wall and sensor materials; Zeng Lingke; Zhang Haiwen; Deng. porous ceramics-green functional material. Chinese pottery; 2002,38 (3); 6-8].Porous ceramics particularly as high temperature resistance and high strength lagging material requires that void content wants high, is preferably not less than 80vol%; Current its preparation method mainly contains following a few class:
(1) foaming rubber plastic material soaking method, proposed in 1963 by Schwartzwalder, its technological process is roughly as follows: first by shaped for the rubber and plastic object of foam form, then flood with ceramic size, extrude unnecessary slurry and drying, finally burnout rubber and plastic object, the ceramic layer that sintering is residual.The shortcoming of the method is, releases a large amount of toxic gas, cause environmental pollution when polymer template is discharged.
(2) be that solvent is by after gel casting forming with water, lyophilize mode is adopted to generate porous body, such as US Patent No. P8262957 (2012) and application number are the application documents of 201110247169.3, and the shortcoming of the method is that drying plant investment is large, energy consumption is too high, production efficiency is low.
(3) porous body is generated with casting after water, polymkeric substance and ceramic powder preparation slurry, such as application number is the Chinese patent application of 200610124005.0 is that aluminum oxide powder and water are mixed with ceramic size, add the modified starch of the ratio according to aluminum oxide powder 30-5Ovol%, mix through ball milling, after degassed, ceramic size is injected mould, be heated to 60-85 DEG C of insulation 5-60 minute, the dried base substrate of the demoulding obtains goods after sintering.Application number be 201210148603.7 Chinese patent proposition flour and ceramic powder mixed fermentation become porous green compact, be sintered into the method for porous ceramics again, its main drawback be consume polymkeric substance too many (such as flour volume is greater than ceramic powder volume), green strength is low.
(4) with injection molding after nitrogen gas foaming, porous body is synthesized by radical polymerization, such as application number is the patent application of 200810016714.6, get ceramic powder and water, the monomers such as acrylamide, whipping agent is made into slurry, strong stirring certain hour in nitrogen environment, become foam state, then additional initiator and catalyzer continuation are stirred and are obtained porous slurry in 0.5-3 minute, porous slurry is injected unwetted mould, room temperature places 1 minute-48 hours under nitrogen protection, then at the temperature of 60-150 DEG C, the time is 10 minutes-6 hours curing moldings, then the demoulding is dry, make the water ratio of base substrate lower than 0.5 below wt%, then burn till under certain condition.The main drawback of the method is that the cost that operates in nitrogen is very high and dried blank strength is very low.Although also have adopt acrylamide monomers batching slurry, with air foaming, gel casting forming, because oxygen has inhibition to radical polymerization, the blank strength causing this legal system standby is lower.
add ceramic powder with organic solvent and be made into slurry, remove organic solvent after gel casting forming and generate porous body, what such as Chen R F etc. proposed is that solvent adds organic monomer and ceramic powder with the trimethyl carbinol, remove the trimethyl carbinol after gel casting forming and generate porous body (Ceramics with ultra-low density fabricated by gelcasting:An unconventional view, Journal of the American Ceramic Society. Chen R F, Huang Y, Wang C A, et al. J. Am. Ceram. Soc., 2007, 90 (11): 3424-3429.), application number is the patent document proposition ethanamide of 200910071845.9 etc. is solvent.The main drawback of these class methods is organic solvents to environmental hazard is serious and cost is very high.
Summary of the invention
Activated alumina typically refers to gama-alumina or η-aluminum oxide, they have the spinel structure comprising more defect, and owing to having excellent surface properties, as surface-area is larger, strong surface adsorption property, surface acidity center, and vesicular structure, be widely used as catalyzer, carrier, dry sorbent material, be applied to petrochemical complex, Organic Chemical Industry, chemical fertilizer industry and environmental protection industry.Activated alumina is actually by the coalescent agglomerate of crystallite particles, there is the micropore differed in size in the inside of agglomerate.
In order to overcome existing high strength, high porosity porous ceramics processing cost high, to the deficiency such as environmental hazard is serious, the present invention proposes following solution: reference catalyst carrier field is about the technology of preparing of activated alumina, in inorganic aluminum salting liquid, add short ceramic fiber, add precipitation agent etc. after being uniformly dispersed and generate precipitation; Add ceramic powder again and stir evenly, filtration washing; Filter cake is mixed with organic bond, after shaping, dry, forms high strength green compact; The mechanical workouts such as turning can be carried out as required, then atmosphere sintering in two steps in High Temperature Furnaces Heating Apparatus.The first step under reducing atmosphere or inert atmosphere activated alumina in porcelain base become Alpha-alumina simultaneously organism become carbon; Oxidation of coal volatilizees by second step under oxidizing atmosphere, thus makes porous ceramics.
The preparation of activated alumina is generally formed 400-700 DEG C of roasting by the presoma prepared specially.The method preparing presoma can be divided three classes by main raw material used: (1) inorganic aluminate precipitator method, precursor species form prepared by this method belongs to boehmite [Liu's winter with short texture, Ye Zhiliang, Cao Jing, Deng. aluminium salt precipitation method prepares the research of low heap than false boehmite. Progress & New Products, 2003,17 (7): 29-32.] or aluminium carbonate ammonium [Yang Yong come, Ning Guiling, Lin Yuan etc. the development of aluminium carbonate ammonium. investigation of materials journal, 1999,13 (3): 269-274]; (2) aluminium alcoholates hydrolysis method; (3) aluminium hydroxide rapid dehydration method.The inorganic aluminate precipitator method are lower than aluminium alcoholates hydrolysis method cost, than aluminium hydroxide rapid dehydration method simple equipments, be the method that application is more at present.The present invention adopts the inorganic aluminate precipitator method to prepare activated alumina presoma exactly, then prepares porous ceramics with ceramic powder etc.
Activated alumina changes Alpha-alumina at 800-1500 DEG C, multiple crystallite particles coalescence is combined into alpha-alumina crystal, size of particles increases more than decades of times, and inside particles hole and the interparticle hole overwhelming majority disappear, and usually can not form the porous ceramics of high porosity.This has had no the reason preparing porous ceramics with activated alumina since may being porous ceramic technology development many decades.
In order to make activated alumina inside particles hole and the interparticle hole overwhelming majority remain in the porcelain body of sintering, the present invention does not directly prepare porous ceramics with activated alumina preparation porcelain, but prepares porous ceramics with activated alumina presoma preparation porcelain.Add organic dispersing agent and organic bond when preparing activated alumina presoma, and adopt two step atmosphere sintering techniques.The first step is with reference to the control climate technology of non-oxidized substance fine ceramics sintering, and under reducing atmosphere or inert atmosphere, organic dispersing agent and organic bond are heated and become carbon particulate, meanwhile presoma is heated and is converted into activated alumina; Numerous carbon particulate interts between activated alumina particulate, hinders the mutual coalescence of activated alumina particulate to combine.Along with temperature raises further, active oxidation aluminum particulate progressively changes alpha-alumina particle into, and the inside and outside of these alpha-alumina particles all exists carbon particulate.Second step is by carbon particulate voloxidation under oxidizing atmosphere, because no longer there is the Phase change shrinkage of aluminum oxide during this, the space shared by carbon particulate remaines in the porcelain body of sintering as hole, thus makes porous ceramics.The control climate technology of a part of technology that the present invention is prepared chemical field about activated alumina and non-oxidized substance fine ceramics sintering, organically be combined with oxide compound special cermacis technology of preparing, this cross-cutting combine with technique is novelty, is not apparent.
Embodiment
In order to prepare high intensity, porous pottery, the present invention has done improvement to the existing method preparing activated alumina presoma, in the solution be made into inorganic aluminate and water, add organic dispersing agent and short ceramic fiber, be added on after being uniformly dispersed in precipitant solution, generate precipitation.Add ceramic powder again, stir evenly, filtration washing; Filter cake is mixed with organic bond, forms high strength green compact after shaping, dry, can the mechanical workouts such as turning be carried out as required, then atmosphere sintering in two steps in High Temperature Furnaces Heating Apparatus.The first step is under reducing atmosphere or inert atmosphere, about 300 DEG C are risen to the heat-up rate of 2-9 DEG C/min, (during this, organic dispersing agent and organic bond are heated and become carbon particulate to use the heat-up rate of 0.3-3 DEG C/min to rise to about 800 DEG C from about 300 DEG C again, meanwhile presoma is heated and is converted into activated alumina), then use the heat-up rate of 1-7 DEG C/min to rise to sintering temperature (during this, active oxidation aluminum particulate progressively changes alpha-alumina particle into) from about 800 DEG C; Second step uses oxidizing atmosphere instead, is incubated 1-6h at a sintering temperature, is volatilized by oxidation of coal, thus makes porous ceramics; The preferred range of sintering temperature is between 1200-1600 DEG C.
Described inorganic aluminate, comprises acid mineral aluminium salt and basic mineral aluminium salt two class.Acid mineral aluminium salt comprises aluminum nitrate, aluminum chloride, Tai-Ace S 150, exsiccated ammonium alum, and its precipitation agent comprises ammoniacal liquor, sodium hydroxide, volatile salt, bicarbonate of ammonia, sodium metaaluminate; Basic mineral aluminium salt comprises sodium metaaluminate and potassium metaaluminate, and its precipitation agent comprises hydrochloric acid, sulfuric acid, nitric acid, acetic acid, formic acid, and acid mineral aluminium salt.Acid mineral aluminum salt solution preferred concentration is 0.1-1.5mol/L, and basic mineral aluminum salt solution preferred concentration is 0.4-5.0mol/L, and the ratio of inorganic aluminate and precipitation agent is advisable between 7-10 by the pH value having precipitated rear mother liquor.
Described organic dispersing agent comprises: water-soluble cellulose derivative, polyoxyethylene glycol, oxygen ethylene copolymer, polyacrylate, the Citrate trianions such as the water soluble starch derivatives such as pre-gelatinized starch, maltodextrin, Natvosol.Often add 100g inorganic aluminate correspondence and add 0.1-9.0g organic dispersing agent.
Described short ceramic fiber comprises: sapphire whisker, aluminium oxide-zirconium oxide conjugated fibre, mullite fiber, aluminum silicate fiber, silica fiber, basalt fibre, and staple length is 1-10mm; Often add 100g inorganic aluminate correspondence and add 1.0-35.0g ceramic fiber.
Described ceramic powder comprises: high temperature alumina, flint clay, kaolinite, quartz, feldspar, talcum, wollastonite, peridotites, spinel, zirconium white, yttrium oxide, calcium carbonate, magnesium oxide, rhombspar; Particle diameter is 10nm-30 μm, often adds 100g inorganic aluminate correspondence and adds 10-100g ceramic powder.
Described organic bond comprises: starch, treated starch, Natvosol, guar gum, modified guar, sesbania gum, modification sesbania gum, polyacrylamide, polyvinyl alcohol, alginates, polyacrylate.Often add 100g inorganic aluminate correspondence and add 7.0-75g organic bond.
Below embodiments of the present invention are illustrated:
Embodiment 1
First workshop section: precursor power.Get 375g nine water aluminum nitrate and be dissolved in 1.5kg water, add 7.5g maltodextrin as dispersion agent, after stirring and dissolving, add 90g sapphire whisker (length 2-7mm), stir 2h completely dispersed to fiber, obtain aluminum nitrate solution; Get 320g sodium metaaluminate and be dissolved in 1.2kg water, obtain precipitant solution.At room temperature, prepared aluminum nitrate solution is slowly added in the precipitant solution that fiercely stirred, subsequently and adds 200g high temperature alumina (being ground to median 1.3 μm in advance), 20g light magnesium oxide, continue at room temperature to stir 1h; Suction filtration in semi-solid to filter cake, filter cake add 70ml water, drains; Repeated washing filter cake like this 3 times.
Second workshop section: join porcelain, shaping, dry, burn till.Be transferred in mixer by washed filter cake, add 60g pre-gelatinized starch, proceed in vinyl disc after at room temperature mixing, make thinner, dry in the air under room temperature 4h; Compression moulding is the four stupefied cylinders of 10mmX10mmX60mm, and 60 DEG C of oven dry, obtain high strength green compact; Suppress 60 green compact altogether, got the high-temperature electric resistance furnace that controlled atmosphere put into by the dry green compact of a part, rise to 290 DEG C with 5 DEG C/min in a nitrogen atmosphere; After this, rise to 800 DEG C with 1 DEG C/min, rise to 1550 DEG C succeeded by 3 DEG C/min from 800 DEG C; Last constant temperature 3h in air atmosphere.With stove Temperature fall to 200 DEG C.
The average bending strength of the porous ceramics prepared thus is 1.65MPa, and mean porosities is 86vol%.
Comparative example 1
From embodiment 1 suppress and get 15 dry green compact, put into the high-temperature electric resistance furnace of controlled atmosphere, adopt the intensification temperature control program identical with embodiment 1, just take air atmosphere therebetween always, prepared porous ceramics hole rate is 39vol%, as can be seen here, two step atmosphere sintering methods are not adopted just can not to reach the target of high porosity.
Embodiment 2
First workshop section: precursor power.Get 6.6kg hydrazine aluminum sulfate and be dissolved in 10kg water, add 0.1kg ammonium citrate, after stirring and dissolving, add 1.2kg sapphire whisker (length 2-7mm), stir 3h completely dispersed to fiber, obtain alum liquor; Get 5.7kg volatile salt and be dissolved in 9kg water, obtain precipitant solution; At room temperature, prepared alum liquor is slowly added in the precipitant solution that fiercely stirred, adds the composite ceramic powder (be pre-mixed and be ground to median 1.8 μm) be made up of 1.6kg flint clay, 0.4kg quartz and 0.2kg feldspar subsequently, continue at room temperature to stir 1h; Suction filtration in semi-solid to filter cake, filter cake add 160ml water, drains; Repeated washing filter cake like this 3 times; Be transferred in Stainless Steel Disc by washed filter cake, 70 DEG C of oven dry, obtain powdery precursor.In lot production, precursor power can be carried out by Chemical Manufacture enterprise, for Production of Ceramics enterprise join porcelain, shaping, dry, burn till.
Second workshop section: join porcelain, shaping, dry, burn till.The powdery precursor prepared from the first workshop section mixed with 280g starch, add 3.5kg water, at room temperature mixing rear injection cavity size is in the stainless steel mould of 200mmX200mmX70mm, in 90 DEG C of baking ovens, be incubated 2h, becomes the wet base substrate of gelling properties; The demoulding, 60 DEG C of oven dry, obtain high strength green compact; A part cuts into the four stupefied cylinders being of a size of 10mmX10mmX60mm, putting into Sweet natural gas is the shuttle kiln of fuel, controlling coefficient of excess air is 0.93(reducing atmosphere), 300 DEG C are risen to the time of 1h, then slowly heat up, rise to 800 DEG C with the time of 7h, after this rise to 1370 DEG C with the time of 3h from 800 DEG C; Finally controlling coefficient of excess air is 1.12(oxidizing atmosphere), at 1370 DEG C of insulation 2h.With stove Temperature fall to 200 DEG C.
The average bending strength of the porous ceramics prepared thus is 1.29MPa, and mean porosities is 81vol%.
Comparative example 2
The large green compact obtained from embodiment 2 cut 20, the little green compact of four stupefied cylinders being of a size of 10mmX10mmX60mm, putting into Sweet natural gas is the shuttle kiln of fuel, adopt the intensification temperature control program identical with embodiment 2, just control coefficient of excess air is therebetween 1.12(oxidizing atmosphere always), prepared porous ceramics mean porosities is 32vol%, as can be seen here, two step atmosphere sintering methods are not adopted just can not to reach the target of high porosity.
fromabove-described embodiment can be found out, the foamed ceramics prepared by the inventive method, and the foamed ceramics intensity that the cost prepared than original technology is close is high, porosity is high.These embodiments are used for the explanation to claim, but not for limitations on the claims, protection scope of the present invention should be as the criterion with claims.
Claims (6)
1. the method with activated alumina precursor power porous ceramics, it is characterized in that: comprise Liang Ge workshop section, presoma is prepared by first workshop section, organic dispersing agent and short ceramic fiber is added in the solution be made into inorganic aluminate and water, be added on after being uniformly dispersed in precipitant solution and generate precipitation, add ceramic powder again and stir evenly, filtration washing, obtaining presoma; Porcelain, shaping, dry, sintering are joined by second workshop section, presoma is mixed with organic bond, high strength green compact are formed after shaping, dry, then atmosphere sintering in two steps in High Temperature Furnaces Heating Apparatus: the first step reducing atmosphere or inert atmosphere, first rise to about 300 DEG C with the heat-up rate of 2-9 DEG C/min, use the heat-up rate of 0.3-3 DEG C/min to rise to about 800 DEG C from about 300 DEG C again, then use the heat-up rate of 1-7 DEG C/min to rise to sintering temperature from about 800 DEG C; Second step uses oxidizing atmosphere instead, is incubated 1-6h at a sintering temperature; The preferred range of sintering temperature is between 1200-1600 DEG C.
2. the method preparing porous ceramics according to claim 1, is characterized in that: described inorganic aluminate, comprises acid mineral aluminium salt and basic mineral aluminium salt two class; Acid mineral aluminium salt comprises aluminum nitrate, aluminum chloride, Tai-Ace S 150, exsiccated ammonium alum, and its precipitation agent comprises ammoniacal liquor, sodium hydroxide, volatile salt, sodium carbonate, sodium bicarbonate, bicarbonate of ammonia, sodium metaaluminate; Basic mineral aluminium salt salt comprises sodium metaaluminate and potassium metaaluminate, and its precipitation agent comprises hydrochloric acid, sulfuric acid, nitric acid, acetic acid, formic acid, and acid mineral aluminium salt; Acid mineral aluminum salt solution concentration is 0.1-1.5mol/L, and basic mineral aluminum salt solution concentration is 0.4-5.0mol/L, and the ratio of inorganic aluminate and precipitation agent is determined between 7-10 according to the pH value of mother liquor after precipitin reaction.
3. the method preparing porous ceramics according to claim 1, is characterized in that: described organic dispersing agent comprises water-soluble cellulose derivative, polyoxyethylene glycol, oxygen ethylene copolymer, polyacrylate, the Citrate trianions such as the water soluble starch derivatives such as pre-gelatinized starch, maltodextrin, Natvosol; Often add 100g inorganic aluminate correspondence and add 0.1-9.0g organic dispersing agent.
4. the method preparing porous ceramics according to claim 1, it is characterized in that: described short ceramic fiber comprises: sapphire whisker, aluminium oxide-zirconium oxide conjugated fibre, mullite fiber, aluminum silicate fiber, silica fiber, basalt fibre, staple length is 1-10mm; Often add 100g inorganic aluminate correspondence and add 1.0-35g ceramic fiber.
5. the method preparing porous ceramics according to claim 1, it is characterized in that: described ceramic powder comprises: high temperature alumina, flint clay, kaolinite, quartz, feldspar, talcum, wollastonite, peridotites, spinel, zirconium white, yttrium oxide, calcium carbonate, magnesium oxide, rhombspar; Particle diameter is 10nm-30 μm, often adds 100g inorganic aluminate correspondence and adds 10-100g ceramic powder.
6. the method preparing porous ceramics according to claim 1, is characterized in that: described organic bond comprises: starch, treated starch, Natvosol, guar gum, modified guar, sesbania gum, modification sesbania gum, polyacrylamide, polyvinyl alcohol, alginates, polyacrylate; Often add 100g inorganic aluminate correspondence and add 7.0-75g organic bond.
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| CN111763097B (en) * | 2020-07-14 | 2022-08-26 | 淄博钛金窑炉科技有限公司 | Method for preparing porous ceramic by using coal gangue |
| CN112521161A (en) * | 2020-12-15 | 2021-03-19 | 无锡特科精细陶瓷有限公司 | Gel injection molding method of aluminum oxide-zirconium dioxide complex phase ceramic |
| CN113427002A (en) * | 2021-06-25 | 2021-09-24 | 哈尔滨工业大学 | Pressureless sintering preparation method of three-dimensional porous structure |
| CN113427002B (en) * | 2021-06-25 | 2022-06-21 | 哈尔滨工业大学 | Pressureless sintering preparation method of three-dimensional porous structure |
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