CN105693265A - Method for preparing aluminum oxide based porous ceramic membrane - Google Patents
Method for preparing aluminum oxide based porous ceramic membrane Download PDFInfo
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- CN105693265A CN105693265A CN201610014544.2A CN201610014544A CN105693265A CN 105693265 A CN105693265 A CN 105693265A CN 201610014544 A CN201610014544 A CN 201610014544A CN 105693265 A CN105693265 A CN 105693265A
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
Abstract
The invention discloses a method for preparing an aluminum oxide based porous ceramic membrane.The method comprises the following steps that firstly, glucose, tetrabutyl titanate and aluminum nitrate and magnesium nitrate are all dissolved in deionized water, then aluminum oxide powder with the particle size of 3-8 microns is added, and spray drying is performed after even mixing and mixing; the powder obtained after the spray drying is put into a mold and is molded under the pressure of 30-40 MPa, then heating is performed to reach 400-500 DEG C, heat preservation is performed to remove organic matter, the powder is cooled and then is put into an isostatic pressing machine for isostatic pressing, then heat preservation is performed at the temperature of 850-850 DEG C to remove redundant carbon, then heating is performed to reach 1350-1450 DEG C, and sintering is performed to obtain the aluminum oxide based porous ceramic membrane.The aluminum oxide based porous ceramic membrane prepared by means of the method is small in pore diameter and uniform in pore distribution.Water sources can be purified by utilizing the barrier and adsorption effects of the porous ceramic membrane, and the porous ceramic membrane has an important significance on wastewater treatment.
Description
Technical field
The present invention relates to a kind of method preparing porous material, be specifically related to a kind of method preparing alumina oxide matrix porous ceramic membrane, belong to materials science field。
Background technology
The application in the treatment of waste water of micropore ceramics membrane separation technique starts from phase early 1980s, and its advantage is able to ensure better and more reliable water quality, without chemical substance, is particularly suitable for high value added product。Inorganic ceramic film application in the treatment of waste water mainly includes processing oily waste water, textile waste, wastewater from chemical industry, radioactive wastewater, heavy metal-containing waste water, city domestic sewage and paper waste etc.。Ceramic membrane seepage slope technique has the advantage such as high flux, high stability, has extremely strong competitiveness and the huge market demand。
The tube wall of porous alumina ceramic film gathers micropore, under pressure, material liquid or gas are in membrane tube or film flows outside, and small-molecule substance (or liquid) is through film, macromolecular substances (or solid) is rejected by, thus reaching the purposes such as separation, concentration, purification and environmental protection。Porous alumina ceramic film has numerous advantages such as separation efficiency height, effect stability, chemical stability be good, acid and alkali-resistance, organic solvent-resistant, resistance to bacterium, high temperature resistant, antipollution, mechanical strength high, regenerability is good, separation process is simple, energy consumption is low, simple and convenient operation and maintenance, long service life。The separating property of porous alumina ceramic film and the micro structure such as the pore size of material and distribution, porosity, pore morphology have close relationship, its pore size can be adjusted at several nanometers to tens micrometer ranges, the screening from nanoscale (such as the NF membrane high rejection to multivalent ion) can be carried out, to visible oarse-grained separation (such as gas cleaning at high temperature), be with a wide range of applications。
Adding pore creating material method is a kind of traditional porous ceramics preparation method, this technique by adding the pore creating material such as carbon dust, starch in ceramic batch, utilizing pore creating material to occupy certain space in blank, after oversintering, pore creating material leaves matrix and forms the prepared porous ceramics of pore。Owing to the method can arbitrarily change pore creating material kind, addition and particle diameter thereof, thus can be made into the porous ceramics of various different pore size and gas cell distribution to meet different instructions for uses；And compared with conventional porous manufacturing method of ceramic, interpolation pore creating material method is with low cost, method simple, is suitable to industrialized mass。On the basis of traditional handicraft, Chinese patent CN104692779A is disclosed the adjuvant for combustion being composited by calcium-copper-titanium three element and prepares the aluminium oxide ceramics of micron order hole, but the proportion requirement of adjuvant for combustion is higher。Chinese patent CN101734909B discloses on the basis of original pore-creating pore former, add zirconium xerogel as reinforcing agent, magnesium xerogel as sintering aid, improve porosity and the intensity of aluminium oxide ceramics, but this method can not efficiently control the distribution of pores of porous alumina ceramic；And the intensity that the increase of porosity often leads to pottery sharply declines。
Summary of the invention
It is an object of the invention to provide and a kind of prepare that aperture is tiny, the method for even pore distribution and the high alumina oxide matrix porous ceramic membrane of intensity。
The method preparing alumina oxide matrix porous ceramic membrane that the present invention proposes, comprises the following steps:
(1) glucose that mass fraction is 40 ~ 95 parts, the butyl titanate of 2 ~ 6 parts, the aluminum nitrate of 2 ~ 5 parts, the magnesium nitrate of 1 ~ 2 part are fully dissolved in deionized water, are sufficiently stirred for mixing, it is thus achieved that mixed solution；
(2) in above-mentioned mixed solution, add the aluminium sesquioxide powder body that mass fraction is 100 parts, be subsequently placed in blender and stir mixing 0.5 ~ 2 hour；The medium particle diameter of described aluminium sesquioxide powder body is at 3 ~ 8 μm；
(3) mixed for above-mentioned stirring material is carried out spray drying, remove deionized water, it is thus achieved that powder body；
(4) powder body obtained after spray drying is put in mould, at the forming under the pressure of 30～40MPa, be then incubated 1～3 hour at 400～500 DEG C, place into after cooling in isostatic pressing machine, under 100～200MPa, carry out isostatic pressed；
(5) product after isostatic pressed is placed in stove, is incubated 2 ~ 6 hours at 850 ~ 950 DEG C, then continue to be warmed up to 1350 ~ 1450 DEG C and be incubated 2 ~ 4 hours, then cool to room temperature with the furnace, obtain alumina oxide matrix porous ceramic membrane。
The method have the advantages that in the deionized water solution by the aluminium sesquioxide powder body of particle diameter 3 ~ 8 μm being put into glucose, butyl titanate, aluminum nitrate and magnesium nitrate and carry out mix and blend, related auxiliaries being uniformly distributed at aluminium sesquioxide powder body particle surface can be realized, it is hereby achieved that tiny aperture and uniform hole；Introduce butyl titanate and magnesium nitrate as sintering aid, and product is carried out isostatic pressed again after 400～500 DEG C of insulations, it is possible to the sintering temperature effectively reducing ceramic membrane also improves its intensity。
Utilize iris action and the adsorption of porous ceramic film prepared by the present invention, it is possible to purify water source, sewage disposal is had important meaning。
Detailed description of the invention
Below in conjunction with example, the invention will be further described。
Embodiment 1:
The glucose that mass fraction is 95 parts, the butyl titanate of 2 parts, the aluminum nitrate of 2 parts, the magnesium nitrate of 1 part are fully dissolved in deionized water, are sufficiently stirred for mixing, it is thus achieved that mixed solution；Add in above-mentioned mixed solution mass fraction be 100 parts, the aluminium sesquioxide powder body of medium particle diameter 5 μm, be subsequently placed in blender stirring mixing 1 hour；Mixed for above-mentioned stirring material is carried out spray drying, removes deionized water, it is thus achieved that powder body。The powder body obtained after above-mentioned spray drying is put in mould, at the forming under the pressure of 30MPa, is then warmed up to 450 DEG C and is incubated 2 hours, place into after cooling in isostatic pressing machine, under 200MPa, carry out isostatic pressed。Product after isostatic pressed is placed in high temperature furnace, is warmed up to 900 DEG C and is incubated 4 hours, then continue to be warmed up to 1450 DEG C and be incubated 3 hours, then cool to room temperature with the furnace, namely obtain alumina oxide matrix porous ceramic membrane。
Embodiment 2:
The glucose that mass fraction is 40 parts, the butyl titanate of 6 parts, the aluminum nitrate of 5 parts, the magnesium nitrate of 2 parts are fully dissolved in deionized water, are sufficiently stirred for mixing, it is thus achieved that mixed solution；Add in above-mentioned mixed solution mass fraction be 100 parts, the aluminium sesquioxide powder body of medium particle diameter 6 μm, be subsequently placed in blender stirring mixing 2 hours；Mixed for above-mentioned stirring material is carried out spray drying, removes deionized water, it is thus achieved that powder body。The powder body obtained after above-mentioned spray drying is put in mould, at the forming under the pressure of 40MPa, is then warmed up to 500 DEG C and is incubated 1 hour, place into after cooling in isostatic pressing machine, under 100MPa, carry out isostatic pressed。Product after isostatic pressed is placed in high temperature furnace, is warmed up to 850 DEG C and is incubated 6 hours, then continue to be warmed up to 1350 DEG C and be incubated 4 hours, then cool to room temperature with the furnace, obtain alumina oxide matrix porous ceramic membrane。
Embodiment 3:
The glucose that mass fraction is 60 parts, the butyl titanate of 4 parts, the aluminum nitrate of 3 parts, the magnesium nitrate of 1.5 parts are fully dissolved in deionized water, are sufficiently stirred for mixing, it is thus achieved that mixed solution；Add in above-mentioned mixed solution mass fraction be 100 parts, the aluminium sesquioxide powder body of medium particle diameter 8 μm, be subsequently placed in blender stirring mixing 0.5 hour；Mixed for above-mentioned stirring material is carried out spray drying, removes deionized water, it is thus achieved that powder body。The powder body obtained after above-mentioned spray drying is put in mould, at the forming under the pressure of 35MPa, is then warmed up to 400 DEG C and is incubated 3 hours, place into after cooling in isostatic pressing machine, under 150MPa, carry out isostatic pressed。Product after isostatic pressed is placed in high temperature furnace, is warmed up to 950 DEG C and is incubated 2 hours, then continue to be warmed up to 1400 DEG C and be incubated 2 hours, then cool to room temperature with the furnace, obtain alumina oxide matrix porous ceramic membrane。
Claims (1)
1. the method preparing alumina oxide matrix porous ceramic membrane, it is characterised in that comprise the steps:
(1) glucose that mass fraction is 40 ~ 95 parts, the butyl titanate of 2 ~ 6 parts, the aluminum nitrate of 2 ~ 5 parts, the magnesium nitrate of 1 ~ 2 part are fully dissolved in deionized water, are sufficiently stirred for mixing, it is thus achieved that mixed solution；
(2) in above-mentioned mixed solution, add the aluminium sesquioxide powder body that mass fraction is 100 parts, be subsequently placed in blender and stir mixing 0.5 ~ 2 hour；The medium particle diameter of described aluminium sesquioxide powder body is at 3 ~ 8 μm；
(3) mixed for above-mentioned stirring material is carried out spray drying, remove deionized water, it is thus achieved that powder body；
(4) powder body obtained after spray drying is put in mould, at the forming under the pressure of 30～40MPa, be then incubated 1～3 hour at 400～500 DEG C, place into after cooling in isostatic pressing machine, under 100～200MPa, carry out isostatic pressed；
(5) product after isostatic pressed is placed in stove, is incubated 2 ~ 6 hours at 850 ~ 950 DEG C, then continue to be warmed up to 1350 ~ 1450 DEG C and be incubated 2 ~ 4 hours, then cool to room temperature with the furnace, obtain alumina oxide matrix porous ceramic membrane。
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| CN201610014544.2A CN105693265B (en) | 2016-01-11 | 2016-01-11 | A kind of method for preparing alumina oxide matrix porous ceramic membrane |
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| CN201610014544.2A CN105693265B (en) | 2016-01-11 | 2016-01-11 | A kind of method for preparing alumina oxide matrix porous ceramic membrane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107973615A (en) * | 2016-10-24 | 2018-05-01 | 天津工业大学 | A kind of mesoporous γ-Al2O3Ceramic membrane and preparation method thereof |
| CN109650935A (en) * | 2019-02-15 | 2019-04-19 | 中国计量大学 | A kind of preparation method of the adjustable alumina porous ceramic film of hole shape |
| CN112044286A (en) * | 2020-09-08 | 2020-12-08 | 山东谷雨春生物科技有限公司 | Metal porous membrane tube and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01308888A (en) * | 1988-06-08 | 1989-12-13 | Asahi Optical Co Ltd | Production of porous ceramic material |
| CN103553600A (en) * | 2013-09-24 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | Porous ferroelectric ceramic with uniform pore distribution and low dielectric loss and preparation method thereof |
| CN104163615A (en) * | 2014-07-18 | 2014-11-26 | 西安建筑科技大学 | Slag based mesoporous material and preparation method thereof |
| CN104446635A (en) * | 2014-11-10 | 2015-03-25 | 西北工业大学 | Method for preparing closed-pore porous heat-insulating alumina ceramic |
-
2016
- 2016-01-11 CN CN201610014544.2A patent/CN105693265B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01308888A (en) * | 1988-06-08 | 1989-12-13 | Asahi Optical Co Ltd | Production of porous ceramic material |
| CN103553600A (en) * | 2013-09-24 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | Porous ferroelectric ceramic with uniform pore distribution and low dielectric loss and preparation method thereof |
| CN104163615A (en) * | 2014-07-18 | 2014-11-26 | 西安建筑科技大学 | Slag based mesoporous material and preparation method thereof |
| CN104446635A (en) * | 2014-11-10 | 2015-03-25 | 西北工业大学 | Method for preparing closed-pore porous heat-insulating alumina ceramic |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107973615A (en) * | 2016-10-24 | 2018-05-01 | 天津工业大学 | A kind of mesoporous γ-Al2O3Ceramic membrane and preparation method thereof |
| CN109650935A (en) * | 2019-02-15 | 2019-04-19 | 中国计量大学 | A kind of preparation method of the adjustable alumina porous ceramic film of hole shape |
| CN109650935B (en) * | 2019-02-15 | 2022-03-22 | 中国计量大学 | Preparation method of porous alumina ceramic membrane with adjustable pore shape |
| CN112044286A (en) * | 2020-09-08 | 2020-12-08 | 山东谷雨春生物科技有限公司 | Metal porous membrane tube and preparation method and application thereof |
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| CN105693265B (en) | 2018-04-20 |
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