CN102512977A - Al2O3-SiO2 ceramic membrane and preparation method thereof - Google Patents
Al2O3-SiO2 ceramic membrane and preparation method thereof Download PDFInfo
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- CN102512977A CN102512977A CN2011103580274A CN201110358027A CN102512977A CN 102512977 A CN102512977 A CN 102512977A CN 2011103580274 A CN2011103580274 A CN 2011103580274A CN 201110358027 A CN201110358027 A CN 201110358027A CN 102512977 A CN102512977 A CN 102512977A
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Abstract
The invention discloses a Al2O3-SiO2 ceramic membrane which comprises a support body and a separation layer and is characterized in that the separation layer is prepared by coating a membrane making solution comprising nano SiO2, PVA (polyvinyl acetate), glycerol and water on the inner surface of the support body by adopting a melting-sol-gel process. The invention also discloses a preparation method of the Al2O3-SiO2 ceramic membrane, and the method comprises the following steps of: preparing the nano Al2O3 support body by adopting a blended particle sintering process; and coating the membrane making solution comprising the nano SiO2, the PVA, the glycerol and the like on the inner surface of the support body by adopting the melting-sol-gel process to form the Al2O3-SiO2 ceramic membrane. By adopting the technical scheme, the Al2O3-SiO2 ceramic membrane has the characteristics of low cost, simpleness and easiness for acquisition, increased membrane flux, high mechanical strength, pollution resistance, uniform membrane aperture, thin membrane wall, large permeation flux, raw material saving, easy realization of miniaturization and simplified structure of separation equipment, and the like.
Description
Technical field
The present invention relates to the film separation field, particularly a kind of Al2O3-SiO2 ceramic membrane and preparation method thereof.
Background technology
The research of ceramic membrane starts from the forties in 20th century, and its development can be divided into three phases.Enter into period with inorganic micro filtering membrane and milipore filter from the nuclear industry of the isotopic separation that is used for uranium and to be master's fluid separation applications period and to be the all-round developing period of core with the membrane catalytic reaction.The nineties in 20th century, the research that the appearance of sol-gel technique indicates inoranic membrane gets into three phases with using, and is the conceptual phase of ceramic membrane separator-combination of reactors member of advocating peace with the gas separating application promptly.
The ceramic membrane isolation technics is owing to have separations, concentrated, purifying and refining function concurrently; Efficient, energy-saving and environmental protection are arranged again, molecular level filters and filter process is simple, be easy to characteristic such as control; Therefore; Be widely used in food, medicine, biology, environmental protection, chemical industry, metallurgy, the energy, oil, water treatment, electronics, field such as bionical, produced huge economic benefit and social benefit, become one of most important means in the separation science.
The ceramic membrane technology of preparing is so that it has ferroelectricity at one or more layers ceramic membrane of matrix surface preparation; Biologically active; Or improve the surface engineering technology of performances such as its wear-resisting, anti-corrosion, high temperature resistant and antimicrobial erosion; Played important effect, and shown the irreplaceable advantage of other products in fields such as environmental protection, chemical industry and bioengineering.Moreover, ceramic membrane also will play a significant role in the separating technology in fields such as the energy, resource and health.Therefore, the inorganic ceramic filter membrane will become the very wide a kind of material of prospect, to solving problems such as china natural resources shortage, environmental pollution, all play crucial effect.
The main technology of preparing of inorganic ceramic membrane has at present: sol-gel process, solid particles sintering process, split-phase method, chemical vapour deposition technique, physical vaporous deposition etc.Perforated membrane mainly is ultrafiltration and micro-filtration membrane at present, and its preparation method is main with particles sintering method and sol-gel process.The former is mainly used in the preparation miillpore filter, and the latter mainly is used for preparing milipore filter.The 1950's, France, the U.S. etc. have developed successively that gas such as various SiC, mullite, ZrO2, ceramic fibre, liquid filter, microbiological treatment is used the micropore ceramic filter element, are mainly used in chemical industry, food, beverage and water treatment field.The seventies in 20th century, Japan and other countries has obtained bigger progress at high temperature gas cleaning, flue gas ash removal aspect the research of porous ceramics filtering material.Since the eighties in 20th century, abroad obtain bigger breakthrough again in the research of ceramic membrane and Application and Development, the research of refractory ceramics hot gas purge technical elements.Along with the expansion of the scope of application, its material also develops into material high temperature resistant, corrosion-resistant, heat shock resistance by common clay, like SiC, cordierite, mullite, ZrO2 and SiO2 etc.Since the nineties in 20th century, the material kind of preparation inorganic separating film is more and more, and commonly used has: metal, glass, Al2O3, SiO2, TiO2, SiC, Si3N4 and alumino-silicate etc., that wherein the most frequently used is Al2O3.
At present, inorganic ceramic membrane is used maximum obstacle and is mainly contained aspect two in water treatment, first complicate fabrication process, and cost is high, costs an arm and a leg; It two is membrane flux problems, only overcomes the filtration flux that film pollutes and improve film, could really promote the use of the every field of water treatment.
Summary of the invention
To the problems referred to above, the objective of the invention is to design a kind of low cost of manufacture, Al2O3-SiO2 ceramic membrane that membrane flux is big and preparation method thereof.
For reaching the problems referred to above; Technical scheme proposed by the invention is: a kind of Al2O3-SiO2 ceramic membrane; Comprise supporter and separating layer, it is characterized in that: described separating layer adopt preparation liquid that nanometer SiO2, PVA, glycerine, water forms through dissolve-gel method is coated on the supporting layer inner surface and makes.
Further, the component of each material is respectively nanometer SiO2 13%, PVA 15%, glycerine 10-22%, water 50-57% in the described preparation liquid.
Further, the thickness of described separating layer is 50-60 μ m.
Further, raw materials used and each the constituent mass percentage of described supporter is respectively: ceramic film support powder 90-95%, pore creating material 1-5%, binding agent 0.5-5%, sintering aid 0.5-5%.
Further; Described ceramic film support powder is nanometer Al2O3; Described binding agent is any one or a few of polyvinyl alcohol, polyacrylic acid or phenolic resins; Described sintering aid is any one perhaps several kinds the mixing in kaolin, bentonite, the magnesia, and described pore creating material is a carbon dust.
The invention still further relates to the preparation method of above-mentioned Al2O3-SiO2 ceramic membrane, it is characterized in that: comprise the steps:
Step 1: with the raw materials used mixing and stirring of supporter, use blend particles sintering method, under 1200 ℃-1600 ℃ of temperature, sintering time 4-6h, lower the temperature naturally supporter;
Step 2: mix back ageing 24h under the environment about 20 ℃ to the nanometer SiO2 of different proportionings and water, the PVA and the glycerine that add different proportion again obtain preparation liquid as additive;
Step 3: preparation liquid repeatedly is coated on the ceramic film support inner surface, to the surface evenly till, place dryly, put into sintering furnace to the ceramic membrane after parching in 800 ℃ of following sintering at last, promptly get the Al2O3-SiO2 ceramic membrane.
Further, raw materials used and each the constituent mass percentage of described supporter is respectively: ceramic film support powder 90-95%, pore creating material 1-5%, binding agent 0.5-5%, sintering aid 0.5-5%.
Further; Described ceramic film support powder is nanometer Al2O3; Described binding agent is any one or a few of polyvinyl alcohol, polyacrylic acid or phenolic resins; Described sintering aid is any one perhaps several kinds the mixing in kaolin, bentonite, the magnesia, and described pore creating material is a carbon dust.
Further, the component of each material is respectively nanometer SiO2 13%, PVA 15%, glycerine 10-22%, water 50-57% in the described preparation liquid.
Further, described coating number of times is preferred 3-5 time.
Further, the thickness of described separating layer is 50-60 μ m.
In sum, Al2O3-SiO2 ceramic membrane of the present invention adopts nanometer Al2O3 as primary raw material; Carbon dust is a pore creating material, utilizes blend particles sintering method, preparation nanometer Al2O3 supporter; And adopt to dissolve-the gel method preparation liquid that materials such as coated with nano SiO2, PVA, glycerine are formed on the supporter inner surface; Problems such as formation Al2O3-SiO2 ceramic membrane has solved the cost of manufacture height, and membrane aperture is inhomogeneous.Adopt technique scheme, have with low cost, be simple and easy to, membrane flux strengthens, mechanical strength is high, anti-pollution.Membrane aperture is even, membranous wall is thin, the big and conservation of permeation flux, be easy to realize the separation equipment miniaturization, characteristics such as simplify the structure.
The specific embodiment
Following specific embodiment further specifies the present invention.
(1) preparation of Al2O3-SiO2 ceramic membrane
Step 1: the preparation of supporter
With the raw materials used mixing and stirring of supporter, use blend particles sintering method, under 1200 ℃-1600 ℃ of temperature, sintering time 4-6h, cooling naturally gets supporter; Raw materials used and each the constituent mass percentage of supporter is respectively: ceramic film support powder 90-95%; Pore creating material 1-5%, binding agent 0.5-5%, sintering aid 0.5-5%; Described ceramic film support powder is nanometer Al2O3; Described binding agent is any one or a few of polyvinyl alcohol, polyacrylic acid or phenolic resins, and described sintering aid is any one perhaps several kinds the mixing in kaolin, bentonite, the magnesia, and described pore creating material is a carbon dust.
Step 2: the preparation of preparation liquid
Mix back ageing 24h under the environment about 20 ℃ to the nanometer SiO2 of different proportionings and water, the PVA and the glycerine that add different proportion again obtain preparation liquid as additive; Each the quality of material percentage of ceramic membrane separating layer for preparing different apertures is shown in table one.
Table one
| Membrane aperture/μ m | Nanometer SiO2/% | PVA/％ | Glycerine/% | Water/% | Coating number of times/inferior |
| 0.05 | 13 | 15 | 10 | 62 | 5 |
| 0.1 | 13 | 15 | 15 | 57 | 5 |
| 0.2 | 13 | 15 | 18 | 54 | 4 |
| 0.5 | 13 | 15 | 22 | 50 | 3 |
Step 3: preparation liquid repeatedly is coated on the ceramic film support inner surface; Apply number of times preferred 3-5 time; The thickness of separating layer is that 50-60 μ m is advisable, to the surface evenly till, place dry; Put into sintering furnace to the ceramic membrane after parching in 800 ℃ of following sintering at last, promptly get the Al2O3-SiO2 ceramic membrane.
(2) measurement of Al2O3-SiO2 ceramic membrane parameter
The ceramic membrane in the different apertures that prepare gained is tested greater than the average rejection and the initial film flux of the particle of 0.5 μ m diameter in the sewage, and the gained result sees table two.
Table two
| Membrane aperture/μ m | Rejection/% | Initial film flux/(m 3·m -2·h -1) |
| 0.05 | 99.9 | 0.08 |
| 0.1 | 99.8 | 0.45 |
| 0.2 | 99.5 | 1.59 |
| 0.5 | 99.3 | 5.50 |
Although specifically show and introduced the present invention in conjunction with preferred embodiment; But the those skilled in the art should be understood that; In the spirit and scope of the present invention that do not break away from appended claims and limited; In form with on the details the present invention is made various variations, be protection scope of the present invention.
Claims (10)
1. an Al2O3-SiO2 ceramic membrane comprises supporter and separating layer, it is characterized in that: described separating layer adopt preparation liquid that nanometer SiO2, PVA, glycerine, water forms through dissolve-gel method is coated on the supporting layer inner surface and makes.
2. a kind of Al2O3-SiO2 ceramic membrane according to claim 1 is characterized in that: the component of each material is respectively nanometer SiO2 13%, PVA 15%, glycerine 10-22%, water 50-57% in the described preparation liquid.
3. a kind of Al2O3-SiO2 ceramic membrane according to claim 1 is characterized in that: the thickness of described separating layer is 50-60 μ m.
4. a kind of Al2O3-SiO2 ceramic membrane according to claim 1; It is characterized in that: raw materials used and each the constituent mass percentage of described supporter is respectively: ceramic film support powder 90-95%; Pore creating material 1-5%, binding agent 0.5-5%, sintering aid 0.5-5%.
5. a kind of Al2O3-SiO2 ceramic membrane according to claim 1; It is characterized in that: described ceramic film support powder is nanometer Al2O3; Described binding agent is any one or a few of polyvinyl alcohol, polyacrylic acid or phenolic resins; Described sintering aid is any one perhaps several kinds the mixing in kaolin, bentonite, the magnesia, and described pore creating material is a carbon dust.
6. the preparation method of an Al2O3-SiO2 ceramic membrane is characterized in that, comprises the steps:
Step 1: with the raw materials used mixing and stirring of supporter, use blend particles sintering method, under 1200 ℃-1600 ℃ of temperature, sintering time 4-6h, lower the temperature naturally supporter;
Step 2: mix back ageing 24h under the environment about 20 ℃ to nanometer SiO2 and water, add PVA again and glycerine obtains preparation liquid as additive;
Step 3: preparation liquid repeatedly is coated on the ceramic film support inner surface, to the surface evenly till, place dryly, put into sintering furnace to the ceramic membrane after parching in 800 ℃ of following sintering at last, promptly get the Al2O3-SiO2 ceramic membrane.
7. the preparation method of a kind of Al2O3-SiO2 ceramic membrane according to claim 6; It is characterized in that: raw materials used and each the constituent mass percentage of described supporter is respectively: ceramic film support powder 90-95%; Pore creating material 1-5%, binding agent 0.5-5%, sintering aid 0.5-5%.
8. the preparation method of a kind of Al2O3-SiO2 ceramic membrane according to claim 6 is characterized in that: the component of each material is respectively nanometer SiO2 13%, PVA 15%, glycerine 10-22%, water 50-57% in the described preparation liquid.
9. the preparation method of a kind of Al2O3-SiO2 ceramic membrane according to claim 6; It is characterized in that: described ceramic film support powder is nanometer Al2O3; Described binding agent is any one or a few of polyvinyl alcohol, polyacrylic acid or phenolic resins; Described sintering aid is any one perhaps several kinds the mixing in kaolin, bentonite, the magnesia, and described pore creating material is a carbon dust.
10. the preparation method of a kind of Al2O3-SiO2 ceramic membrane according to claim 6 is characterized in that: described coating number of times is 3-5 time.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103736401A (en) * | 2014-01-10 | 2014-04-23 | 天津市环境保护科学研究院 | Inorganic film for treating organic waste water under catalysis of ozone and preparation method of film |
| CN104587846A (en) * | 2014-12-24 | 2015-05-06 | 长安大学 | Method for preparing porous ceramic filter membrane by low-temperature sintering |
| CN104785119A (en) * | 2014-01-18 | 2015-07-22 | 刘旭红 | Tubular type ceramic filter element and preparation method thereof |
| CN105903272A (en) * | 2016-05-09 | 2016-08-31 | 河南省豫星华晶微钻有限公司 | Ceramic filter core containing nanometer carbon crystal and nanometer diamond alkene blends |
| CN106587268A (en) * | 2016-11-02 | 2017-04-26 | 深圳市康源环境纳米科技有限公司 | Ceramic membrane, component of ceramic membrane, contact chamber, processing system and method for heavy metal wastewater |
| CN107698258A (en) * | 2017-08-03 | 2018-02-16 | 浙江理工大学 | A kind of ceramic membrane painting method |
| CN108046788A (en) * | 2017-12-08 | 2018-05-18 | 刘惠强 | A kind of preparation method of self-cleaning ceramic film |
| CN108658270A (en) * | 2017-11-27 | 2018-10-16 | 江苏久吾高科技股份有限公司 | A kind of processing method and processing device of titanium white production waste water |
| CN111153684A (en) * | 2018-11-08 | 2020-05-15 | 中国石油化工股份有限公司 | Ceramic membrane and preparation method and application thereof |
| CN111253148A (en) * | 2020-01-20 | 2020-06-09 | 浙江乾仕智能科技有限公司 | Ceramic filter membrane preparation method and ceramic filter membrane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1686920A (en) * | 2005-04-05 | 2005-10-26 | 南京工业大学 | Preparation method of ceramic microfiltration membrane |
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- 2011-11-14 CN CN2011103580274A patent/CN102512977A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686920A (en) * | 2005-04-05 | 2005-10-26 | 南京工业大学 | Preparation method of ceramic microfiltration membrane |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103736401A (en) * | 2014-01-10 | 2014-04-23 | 天津市环境保护科学研究院 | Inorganic film for treating organic waste water under catalysis of ozone and preparation method of film |
| CN104785119A (en) * | 2014-01-18 | 2015-07-22 | 刘旭红 | Tubular type ceramic filter element and preparation method thereof |
| CN104587846A (en) * | 2014-12-24 | 2015-05-06 | 长安大学 | Method for preparing porous ceramic filter membrane by low-temperature sintering |
| CN104587846B (en) * | 2014-12-24 | 2016-05-18 | 长安大学 | A kind of low-temperature sintering is prepared the method for porous ceramics filter membrane |
| CN105903272A (en) * | 2016-05-09 | 2016-08-31 | 河南省豫星华晶微钻有限公司 | Ceramic filter core containing nanometer carbon crystal and nanometer diamond alkene blends |
| CN106587268B (en) * | 2016-11-02 | 2019-12-20 | 深圳市康源环境纳米科技有限公司 | Ceramic membrane and component thereof, contact tank, heavy metal wastewater treatment system and method |
| CN106587268A (en) * | 2016-11-02 | 2017-04-26 | 深圳市康源环境纳米科技有限公司 | Ceramic membrane, component of ceramic membrane, contact chamber, processing system and method for heavy metal wastewater |
| CN107698258A (en) * | 2017-08-03 | 2018-02-16 | 浙江理工大学 | A kind of ceramic membrane painting method |
| CN108658270A (en) * | 2017-11-27 | 2018-10-16 | 江苏久吾高科技股份有限公司 | A kind of processing method and processing device of titanium white production waste water |
| CN108046788A (en) * | 2017-12-08 | 2018-05-18 | 刘惠强 | A kind of preparation method of self-cleaning ceramic film |
| CN111153684A (en) * | 2018-11-08 | 2020-05-15 | 中国石油化工股份有限公司 | Ceramic membrane and preparation method and application thereof |
| CN111153684B (en) * | 2018-11-08 | 2022-06-17 | 中国石油化工股份有限公司 | Ceramic membrane and preparation method and application thereof |
| CN111253148A (en) * | 2020-01-20 | 2020-06-09 | 浙江乾仕智能科技有限公司 | Ceramic filter membrane preparation method and ceramic filter membrane |
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Application publication date: 20120627 |