CN103073330B - Method for preparing mullite-corundum porous ceramic by taking active yeast as pore forming agent - Google Patents
Method for preparing mullite-corundum porous ceramic by taking active yeast as pore forming agent Download PDFInfo
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Abstract
The invention discloses a method for preparing mullite-corundum porous ceramic by taking active yeast as a pore forming agent. The mullite-corundum porous ceramic is prepared by taking AlOOH and silica micropowder as raw materials, absolute ethyl alcohol as a ball-milling medium and the active yeast as the pore forming agent, mixing all the raw materials, carrying out vacuum filtration forming on the mixed raw materials and carrying out direct reaction and high-temperature sintering, wherein the active yeast is prepared by culturing dry yeast in 30-40-DEG C deionized water. According to the method disclosed by the invention, the active yeast is used as the pore forming agent and is uniform in size which is 2-5 Mu m; in addition, the yeast carries negative charges in a solution, and the raw material AlOOH powder and the silica micropowder carry positive charges in the solution; and the raw material powder can be well adsorbed on the surface of the yeast by using the electrostatic interaction, and therefore the porous material finally prepared is narrow in pore diameter range and uniform in pore diameter distribution.
Description
Technical field
The present invention relates to porous ceramic film material field, relate in particular to and a kind ofly take active yeast and prepare the method for mullite-corundum porous ceramics as pore-forming material.
Background technology
Along with development, the process of industrialization of national economy are accelerated, problem of environmental pollution highlights.A large amount of three industrial wastes discharges, especially the discharge of industrial high temperature flue gas and motor-vehicle tail-gas, solid particulate has become the arch-criminal of municipal pollution.Therefore, carry out the research and development of filtering high-temperature flue gas, catalysis technique, the discharge that reduces solid particulate and toxic gas becomes the important ring in energy-saving and emission-reduction, environmental engineering.High temperature filtration body material except needs have high temperature resistant and corrosion-resistant, also need to there is certain porosity, intensity and good heat-shock resistance.Porous ceramic film material is owing to having that porosity is high, air permeance resistance is little, cleaning and regeneration is convenient and the feature such as high temperature resistant, high pressure, resistant to chemical media corrosion is as the separated optimal selection with purifying of high temperature fluid.
Porous ceramic matrices suitable material category is various, and wherein mullite-corundum compound matrix material is high temperature resistant owing to having, and heat-shock resistance is excellent, wear resistance is good, and intensity is high, good toughness, good and the Young's modulus high of creep resistance and resistance to fouling, becomes the more a kind of substrate material of research application.Premium properties based on mullite-corundum matrix material, its porous ceramic film material goods become the ideal chose of solid support material for the separation of industrial high temperature filtering flow and motor-vehicle tail-gas, solid particulate filtration, purification.In the preparation and application research of mullite-corundum composite porous ceramic material, people have also done a few thing in recent years, by different preparation synthetic methods, add different pore-forming materials, have prepared various mullite-corundum porous ceramic film materials.
Such as: people (the Yingchao Dong such as Yingchao Dong, Bin Lin, KuiXie, et.al., Journal of Alloys and Compounds, 47,2009,350-356) adopting W-Gum is that pore-forming material has been prepared mullite-corundum porous ceramic film support, porosity 40% left and right, and mean pore size is 26.21 μ m.
The people such as Han Huonian (Han Huonian, Li Qiang, Hong Yubin etc., functional materials, 3 phases 42 volumes, 2011,425-428) first by the precipitator method, prepare the aluminum oxide of superfine alumina powder parcel, with nanometer titanium dioxide pasc reaction and add pore-forming material and prepare mullite-corundum porous ceramic film support, porosity is 40.21% again, and mean pore size is 9.87 μ m.
People (Kiyoshi Okada, Shuhei Uchiyama, the ToshihiroIsobe such as Kiyoshi Okada, et al., Journal of the European Ceramic Society, 29,2009,2491-2497) by being added with organic fiber, prepared mullite porous ceramics.
In above-mentioned three open source literatures, be mainly that to take starch, graphite, organic fibre etc. be pore-forming material, by the method for mechanical ball milling, pore-forming material mixed with material powder, sintering obtains mullite-corundum porous ceramic film material.The defect existing is: when mechanical ball milling mixes, because the specific gravity difference of pore-forming material and material powder is larger, pore-forming material disperses inhomogeneous in base substrate, and the grain size of pore-forming material own is difficult to control, easily produce and reunite, the aperture of porous material skewness obtaining, pore size distribution range is wide, thereby reduced the sintering strength of porous ceramics, affected its result of use and work-ing life.
The technology close with the present invention is: China Patent Publication No. CN1442392A discloses a kind of preparation method of take the carborundum porous ceramics that yeast powder is pore-forming material, and it is with SiC, Al
2o
3, Suzhou soil and wilkinite be raw material, take dried yeast powder as pore-forming material, by sieving varigrained yeast powder, mix with ceramic size, drying, compression moulding sintering forms.The defect that the method exists is: owing to using dried yeast powder as pore-forming material, pore-forming material size is larger, cause the specific gravity difference of pore-forming material and material powder larger, and by mechanical ball milling method, mix with material powder equally, occur mixing uneven defect, and owing to adopting 1 granularity dried yeast powder, the porous ceramics pore size distribution range of preparation is wide, between 50-500 μ m, the uneven distribution in aperture has influence on the sintering strength of material equally.
Summary of the invention
In order to overcome existing preparation in mullite-corundum porous ceramic film material method because pore size distribution is uneven, size is difficult to control, the wide material sintering strength causing of pore size distribution range is low, the technological deficiency that filtering accuracy is low, the present invention puts forward a kind of preparation method of take the mullite-corundum porous ceramic film material that active yeast is pore-forming material, the method utilizes yeast to have uniform size (2-5 μ m), and surface is with the characteristic of negative charge, with the ceramic powder with positive charge by electrostatic attraction, make ceramic powder raw material be adsorbed in yeast surface, realize dispersed in ceramic raw material of yeast, thereby acquisition even aperture distribution, the mullite-corundum porous ceramics that intensity is high, to meet the requirement of the solid support materials such as industrial high temperature filtering flow and motor vehicle tail-gas purifying processing.
For achieving the above object, preparation method of the present invention is:
It is to take weight ratio as (3.1-7.1): 1 AlOOH and silicon powder are raw material, using dehydrated alcohol as ball-milling medium, take active yeast as pore-forming material, through mixing, vacuum filtration moulding, by direct reaction high temperature sintering, the porosity of the porous material after sintering is 40～62%, and aperture size is at 0.5-3 μ m.
Above-mentioned active yeast is to be cultivated and obtain in 30-40 ℃ of deionized water by dry yeast;
The weight percent content of above-mentioned each material purity is: pseudo-boehmite >=98%, silicon powder >=97%.
The detailed preparation method of mullite-corundum porous ceramic film material of the present invention is as follows:
The first step: the preparation of active yeast solution
First load weighted dried yeast powder is joined in 30-40 ℃ of deionized water, wherein the weight ratio of yeast and deionized water is (0.25-1): 100, fully stir, and cultivate and obtain active yeast solution;
Second step: the preparation of raw material fine powder
AlOOH and silicon powder are pressed to (3.1-7.1): 1 weight ratio weighs, and joins in ball grinder, usings dehydrated alcohol as ball-milling medium wet ball grinding, and material powder is mixed, after being dried, obtain raw material fine powder;
The weight percent of general compound, ball, alcohol is 1:(1.5～2.5): (0.6～0.9);
The 3rd step: the preparation of mullite-corundum porous ceramic film material
By above-mentioned powder raw material according to final mullite-corundum product weight: weight ratio dry yeast=10:(2-5) is added in yeast solution, constantly stir and form suspension, and to regulate suspension pH value is 8-9; Adopt vacuum filtration moulding to obtain biscuit the suspension being fully uniformly mixed, biscuit is high temperature sintering 2-4 hour under 1200-1400 ℃ of condition after drying, by direct reaction sintering method, obtains mullite-corundum porous ceramic film material.
Advantage of the present invention is:
1, because the present invention be take active yeast as pore-forming material, active yeast size homogeneous, size is at 2-5 μ m, and yeast is electronegative in solution, material powder AlOOH and silicon powder are positively charged in solution, utilize electrostatic interaction, can make material powder well be adsorbed in yeast surface, thereby make the aperture of porous material narrow range of final preparation, even aperture distribution, technique is simple.
2, the present invention utilizes the method for direct reaction sintering, in sintering process, by yeast removal, leave hole, and the activated alumina silicon powder direct and that activity is high that pseudo-boehmite decomposition generates reacts at the high mullite-corundum material of hole wall place generation intensity.
3, the prepared mullite-corundum porous ceramic film material of the present invention is high temperature resistant, intensity is high, void content is 40～62%, air vent aperture is evenly distributed, thermostability and chemical stability are good, can process for ceramic filtration membrane supporter, industrial high temperature filtering flow, separation and motor vehicle tail-gas purifying the solid support material of use, for realizing the application of mullite-corundum porous ceramic film material in industrial high temperature filtering flow and motor vehicle tail-gas purifying processing, lay a good foundation.
After testing: the void content of mullite-corundum porous ceramic film material prepared by the present invention be for can reach 40～62%, narrow pore size distribution range, pore size is even, and between 0.5-3 μ m, can improve well filtering separation precision.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction that adopts the synthetic porous ceramic film material of the inventive method.
Fig. 2 a is the stereoscan photograph of 1000 times of the amplifications of the prepared porous ceramic film material of the present invention;
Fig. 2 b is the stereoscan photograph of 5000 times of the amplifications of the prepared porous ceramic film material of the present invention.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment 1: the mass percent that the corundum content of take accounts for total mass is prepared burden as 5%, and inoculum of dry yeast is according to final mullite-corundum product weight: the weight ratio of dry yeast=10:5.
First by above-mentioned weight, take raw material: pseudo-boehmite 87.9g, silicon powder 27.6g, and material powder AlOOH and silicon powder are joined in planetary ball mill and mixed, the weight percent of compound, ball, dehydrated alcohol is 1:2:0.8, mixing time is 2 hours.Take dry yeast 50g, join in the deionized water of 10L30-40 ℃ and constantly stir 2 hours, cultivate and obtain yeast solution; The material powder that above-mentioned ball milling is mixed joins in cultured yeast solution and constantly and stirs 4 hours, obtains suspension.Then the moulding of suspension vacuum filtration is obtained to biscuit, put into baking oven and dry under 80 ℃ of conditions.Sample after oven dry burns till at 1200 ℃ of temperature, and soaking time is 2 hours, makes mullite-corundum porous ceramic film material, and the porosity of porous material is 57%, and folding strength is 32Mpa, and aperture is greatly between 0.5-3 μ m.
Embodiment 2: the mass percent that the corundum content of take accounts for total mass is prepared burden as 5%, and inoculum of dry yeast is according to final mullite-corundum product weight: the weight ratio of dry yeast=10:2.
First by following weight, take raw material: pseudo-boehmite 87.9g, silicon powder 27.6g, and material powder AlOOH and silicon powder are joined in planetary ball mill and mixed, the weight percent of compound, ball, dehydrated alcohol is 1:2:0.8, mixing time is 2 hours.Take dry yeast 20g, join in the deionized water of 10L30-40 ℃ and constantly stir 1 hour, cultivate and obtain yeast solution; The material powder that above-mentioned ball milling is mixed joins in cultured yeast solution and constantly and stirs 4 hours, obtains suspension.Then the moulding of suspension vacuum filtration is obtained to biscuit, put into baking oven and dry under 80 ℃ of conditions.Sample after oven dry burns till at 1200 ℃ of temperature, and soaking time is 2 hours, makes mullite-corundum porous ceramic film material, and the porosity of porous material is 41%, and folding strength is 65Mpa, and aperture is greatly between 0.5-3 μ m.
Embodiment 3: the mass percent that the corundum content of take accounts for total mass is prepared burden as 50%, and inoculum of dry yeast is according to final mullite-corundum product weight: the weight ratio of dry yeast=10:5.
First by following weight, take raw material: pseudo-boehmite 103.1g, silicon powder 14.8g, material powder AlOOH and silicon powder are joined in planetary ball mill and mixed, and the weight percent of compound, ball, dehydrated alcohol is 1:2:0.8, and mixing time is 1 hour.Take dry yeast 50g, join in the deionized water of 10L30-40 ℃ and constantly stir 1 hour, cultivate and obtain yeast solution; The material powder that above-mentioned ball milling is mixed, according to final mullite-corundum product weight: the ratio of dry yeast=10:5 joins in cultured yeast solution and constantly and stirs 6 hours, obtains suspension.Then the moulding of suspension vacuum filtration is obtained to biscuit, put into baking oven and dry under 90 ℃ of conditions.Sample after oven dry burns till at 1200 ℃ of temperature, and soaking time is 2 hours, makes mullite-corundum porous ceramic film material, and the porosity of porous material is 62%, and folding strength is 15Mpa, and aperture is greatly between 0.5-3 μ m.
Embodiment 4: the mass percent that the corundum content of take accounts for total mass is prepared burden as 20%, and inoculum of dry yeast is according to final mullite-corundum product weight: the weight ratio of dry yeast=10:5.
First by following weight, take raw material: pseudo-boehmite 93g, silicon powder 23.2g, joins material powder AlOOH and silicon powder in planetary ball mill and mixes, and the weight percent of compound, ball, dehydrated alcohol is 1:2:0.8, and mixing time is 1 hour.Take dry yeast 50g, join in the deionized water of 10L30-40 ℃ and constantly stir 1 hour, cultivate and obtain yeast solution; The material powder that above-mentioned ball milling is mixed, according to final mullite-corundum product weight: the ratio of dry yeast=10:5 joins in cultured yeast solution and constantly and stirs 4 hours, obtains suspension.Then the moulding of suspension vacuum filtration is obtained to biscuit, put into baking oven and dry under 80 ℃ of conditions.Sample after oven dry burns till at 1300 ℃ of temperature, and soaking time is 2 hours, makes mullite-corundum porous ceramic film material, and the porosity of porous material is 53%, and folding strength is 38Mpa, and aperture is greatly between 0.5-2 μ m.
Embodiment 5: the mass percent that the corundum content of take accounts for total mass is prepared burden as 20%, and inoculum of dry yeast is according to final mullite-corundum product weight: the weight ratio of dry yeast=10:5.
First by following weight, take raw material: pseudo-boehmite 93g, silicon powder 23.2g, joins material powder AlOOH and silicon powder in planetary ball mill and mixes, and the weight percent of compound, ball, dehydrated alcohol is 1:2:0.8, and mixing time is 1 hour.Take dry yeast 50g, join in the deionized water of 10L30-40 ℃ and constantly stir 1 hour, cultivate and obtain yeast solution; The material powder that above-mentioned ball milling is mixed, according to final mullite-corundum product weight: the ratio of dry yeast=10:5 joins in cultured yeast solution and constantly and stirs 4 hours, obtains suspension.Then the moulding of suspension vacuum filtration is obtained to biscuit, put into baking oven and dry under 80 ℃ of conditions.Sample after oven dry burns till at 1400 ℃ of temperature, and soaking time is 2 hours, makes mullite-corundum porous ceramic film material, and the porosity of porous material is 48%, and folding strength is 45Mpa, and aperture is greatly between 0.5-2 μ m.
In the present invention, the detection of folding strength is with reference to GB GB/T1965-1996 < < porous ceramics bending strength test method > >, and the detection of above-mentioned porosity is according to GB GB/T1966-1996 < < Porosity of Porous Ceramics, unit weight test method > >.
The X-ray powder diffraction of porous ceramic film material of the present invention and profile scanning electromicroscopic photograph are shown in respectively Fig. 1, Fig. 2 a, Fig. 2 b.From Fig. 1 X-ray powder diffraction, analyzed, the phase composition of material is mainly mullite and corundum.From Fig. 2 a, Fig. 2 b cross-section morphology, analyze, the pore size distribution of porous ceramic film material is very even, pore size is between 0.5-3 μ m, between Kong Yukong, mutually connect, and hole wall mullite-corundum phase densified sintering product, can effectively improve the intensity of porous ceramics, meet the requirement of the solid support material such as solution or gas filtration and motor vehicle tail-gas purifying processing in industrial production under normal temperature, hot conditions.
Claims (2)
1. take active yeast and prepare the method for mullite-corundum porous ceramics as pore-forming material for one kind, it is characterized in that, it is to take weight ratio as (3.1-7.1): 1 pseudo-boehmite and silicon powder are raw material, using dehydrated alcohol as ball-milling medium, take active yeast as pore-forming material, through mixing, vacuum filtration moulding, by direct reaction high temperature sintering, the porosity of the porous material after sintering is 40～62%, and aperture size is at 0.5-3 μ m;
Above-mentioned active yeast is to be cultivated and obtain in 30-40 ℃ of deionized water by dry yeast; The usage quantity of active yeast is according to final mullite-corundum product weight: weight ratio dry yeast=10:(2-5) is carried out proportioning;
The weight percent content of above-mentioned each material purity is: pseudo-boehmite >=98%, silicon powder >=97%.
2. the method for claim 1, is characterized in that, detailed step is as follows:
The first step: the preparation of active yeast solution
First load weighted dried yeast powder is joined in 30-40 ℃ of deionized water, wherein the weight ratio of yeast and deionized water is (0.25-1): 100, fully stir, and cultivate and obtain active yeast solution;
Second step: the preparation of raw material fine powder
Pseudo-boehmite and silicon powder are pressed to (3.1-7.1): 1 weight ratio weighs, and joins in ball grinder, usings dehydrated alcohol as ball-milling medium wet ball grinding, and material powder is mixed, after being dried, obtain raw material fine powder;
The 3rd step: the preparation of mullite-corundum porous ceramic film material
By above-mentioned powder raw material according to final mullite-corundum product weight: weight ratio dry yeast=10:(2-5) is added in yeast solution, constantly stir and form suspension, and to regulate pH of suspension value is 8-9; Adopt vacuum filtration moulding to obtain biscuit the suspension being fully uniformly mixed, biscuit is high temperature sintering 2-4 hour under 1200-1400 ℃ of condition after drying, by direct reaction sintering method, obtains mullite-corundum porous ceramic film material.
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| CN106083175B8 (en) * | 2016-06-28 | 2018-08-28 | 承德鑫焱热力有限公司 | A kind of preparation method of composite ceramics accumulation of heat basis material |
| CN106588085B (en) * | 2016-12-22 | 2019-07-16 | 哈尔滨工业大学 | A kind of preparation method of high-temperature-resistant structure type SiC porous ceramics |
| CN109336589B (en) * | 2018-11-02 | 2021-08-31 | 山东科技大学 | Method for preparing aluminum titanate mullite ceramic with hierarchical pore structure through microbial foaming |
| CN109467423B (en) * | 2018-12-21 | 2021-08-13 | 福建龙净环保股份有限公司 | Ceramic fiber reinforced high-temperature-resistant gas filtering material and preparation method thereof |
| CN111517750A (en) * | 2020-05-08 | 2020-08-11 | 广西玖醇科技有限公司 | Manufacturing process of ceramic product for accelerating alcohol alcoholization and alcohol alcoholization method |
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| CN1442392A (en) * | 2003-04-11 | 2003-09-17 | 中国科学院上海硅酸盐研究所 | Preparation method of silicon carbide porous ceramic using yeast powder as pore forming agent |
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| CN1442392A (en) * | 2003-04-11 | 2003-09-17 | 中国科学院上海硅酸盐研究所 | Preparation method of silicon carbide porous ceramic using yeast powder as pore forming agent |
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| Title |
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| JP特公平8-13449B2 1996.02.14 |
| Red clay-based porous ceramic with pores created by yeast-based foaming technique;Ruben L.Menchavez;《Journal of Materials Science》;20100707;第45卷;6511-6520 * |
| Ruben L.Menchavez.Red clay-based porous ceramic with pores created by yeast-based foaming technique.《Journal of Materials Science》.2010,第45卷6511-6520. |
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