CN101417215A - Ordered porous ceramic film and preparation method thereof - Google Patents

Ordered porous ceramic film and preparation method thereof Download PDF

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Publication number
CN101417215A
CN101417215A CNA200810143685XA CN200810143685A CN101417215A CN 101417215 A CN101417215 A CN 101417215A CN A200810143685X A CNA200810143685X A CN A200810143685XA CN 200810143685 A CN200810143685 A CN 200810143685A CN 101417215 A CN101417215 A CN 101417215A
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China
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porous ceramic
ceramic film
ordered
ordered porous
fiber
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CNA200810143685XA
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伍协
冯延林
陈振华
周治德
李桂银
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Abstract

The invention relates to an orderly porous ceramic film and a preparation method thereof. Normal ceramic aggregate and adhesive are adopted and the orderly fiber is used as pore-forming agent, the proportion is shown as follows: 25 percent-50 percent of ceramic aggregate, 15-20 percent of adhesive, 25-30 percent of water and 10-27 percent of orderly fiber; the porous ceramic film, with the aperture of 100-200 microns, porosity of 50-70 percent, strength of 20-40MPa and flux of 3000-110,000L.m<-2><-1> is formed by an enwinding method and is provided with two-dimensional communicated straight through holes which are arranged in order. The preparation method can achieve the quick forming of the ceramic film, has high yield, low production cost, simple process and the like, and can be directly applied to the preparation of orderly porous ceramic film products.

Description

A kind of ordered porous ceramic film and preparation method thereof
Technical field
The present invention relates to a kind of ordered porous ceramic film and preparation method thereof, especially a kind of ordered porous ceramic film and technology of preparing thereof that is applicable to fields such as Separation of Solid and Liquid, vehicle exhaust processing, gas cleaning at high temperature, purification of waste water and chemical industry catalysis.
Background technology
Order design and research to the hole of ceramic membrane is the important directions of material science development, and Zhang G J etc. utilizes cotton fiber to make pore creating material, by the coated with ceramic slurry, prepares the porous ceramics of some ordered through hole, and its aperture is about 100 microns.Along with the development of nanometer technology, now people focus on by organic polymer to be masterplate, to prepare some ordered porous poromerics by self-assembling reaction.Some sulfur-containing compounds such as mercaptan and the thiophenols etc. of using in self assembling process more.The Jin Z.Zhang of the U.S. etc. prepares nano level micropore and mesoporous ordered porous material by self assembly, not only has extraordinary separating effect, and have functions such as photoelectricity, expanded the developing direction of ceramic membrane greatly, He Lan Twente university and professor Larbot etc. use sol-gel technology preparing pellumina, its aperture can reach 1-3nm in addition, porosity surpasses 50%, can be used as micro-filtration membrane, milipore filter uses, and is a current very important based ceramic film material.
The ceramic membrane technology of China also is in the primary stage, and Xu Nanping has deep research aspect ceramic membrane, and the portioned product of exploitation has been applied in the industry, is mainly used in the solid-liquid division, just the part of traditional ceramic membrane is improved.It is the synthetic 13X zeolite molecular sieve of raw material that the purification of waste water new technology adopts natural minerals, by the ionic adsorption exchange interaction, removes the heavy metal ion in the waste water.Eluent with preparation elutes the heavy metal ion that the 13X zeolite molecular sieve adsorbs, and molecular sieve can repeatedly recycle through reactivating.Add precipitating reagent and make the heavy metal ion in the eluent be precipitated as metal sulfide, through the recyclable heavy metal element of high melt.These ceramic membranes all belong to the scope of unordered porous ceramic film, still exist the regeneration of ceramic membrane very difficult, defectives such as film weak point in service life.The Shi Jianlin of Shanghai silicate research institute etc. have prepared the mesoporous material of better performances by self assembly, and fenestra is distributed with certain ordered, but also far from practical application.
Therefore, be necessary existing ceramic membrane technology of preparing is improved, be in order and be the straight type through hole of two dimension, and its filtration flux and recyclability are better than existing ceramic membrane with the hole that obtains porous ceramic film.
Summary of the invention
Technical problem to be solved by this invention provides the straight type through hole of a kind of two dimension, the hole is orderly, filtration flux is big and recyclability is strong porous ceramic film and preparation method thereof.
In order to address the above problem, through work for many years, the present invention adopts percent of ordinary ceramic aggregate and bond, make pore creating material with ordered fiber, adopt the preparation of winding method to portal the footpath at 100-200 microns, porosity is 50%-70%, intensity is at 20-40MPa, and filtration flux is at 3000-110000L.m -2.h -1, regeneration is simple, and the porous ceramic film of the straight type through hole of two-dimentional UNICOM is arranged in order and is formed in the hole.
Technical scheme of the present invention is: a kind of ordered porous ceramic film and preparation method thereof is characterized in that adopting following row prescription and preparation method:
(1) prescription
Ceramic aggregate 23%-50%; Bond 15%-20%; Water 25%-30%; Ordered fiber 10%-27%.
Ceramic aggregate is meant wherein a kind of, perhaps multiple or whole such as aluminium oxide, spodumene, quartz, porcelain powder, carborundum and cordierite, can be combined into composition by arbitrary proportion; Bond is wherein a kind of, perhaps multiple or whole such as calcium carbonate, brium carbonate, bentonite, Suzhou soil feldspar, glass dust and boron frit, can be combined into composition by arbitrary proportion; Described ordered fiber is wherein a kind of, perhaps multiple or whole such as nylon fiber, carbon fiber and measuring fiber, can be combined into composition by arbitrary proportion.
(2) preparation method
A, batching.Ceramic aggregate, bond, water are prepared burden by the formula rate requirement;
B, ball milling.With above-mentioned compound ball milling 24 hours in ball mill, wherein material: ballstone=1:2 obtains ceramic size;
C, brushing or dip-coating.The ceramic size that the B step is made adopts brushing or dip-coating on ordered fiber,
Obtain the hanging ordered fiber;
D, moulding and drying.With C step gained hanging ordered fiber, be wound on the wrapping machine cylindricly in self-control, speed of wrap at 0.1MPa, obtains the ceramic membrane green compact at 1m/min, pressure, and 120 ℃ of dryings 24 hours;
E, sintering.Above-mentioned ceramic membrane green compact are put into kiln carry out sintering,,, obtain the ordered porous ceramic film crude green body 1150 ℃-1400 ℃ insulations 2-6 hours 700 ℃-900 ℃ insulations 1-2 hours;
F, cutting.Ordered porous ceramic runic in the E step is adopted the cutting two ends and polish, promptly get the ordered porous ceramic film finished product.
Among the present invention, the batching of ordered porous ceramic film, ball milling, brushing, dip-coating, drying, sintering, be cut into known technology.
The present invention has following advantage and effect:
(1) directly adopt ordered fiber to make pore creating material, simultaneously fiber is arranged towards a direction, can very simply prepare portals is arranged with preface, and the hole is the straight type through hole of two dimension;
(2) by regulating the size that fibre diameter just can adjustment aperture;
(3) by regulating the hanging amount of ordered fiber, the porosity that just can regulate ceramic membrane.
(4) adopt the winding method can realize the rapid shaping of ceramic membrane, the yield rate height, characteristics such as production cost is low, and technology is simple can directly apply to prepared in batches ordered porous ceramic film product.
The specific embodiment
The explanation that the following stated example is detailed the present invention.In example, unless otherwise indicated, all umbers and percentage are all by weight.
Embodiment 1
1, takes by weighing aluminium oxide 300 grams by prescription, Suzhou soil 70 grams, brium carbonate 70 grams, calcium carbonate 8 grams, bentonite 2 grams, water 280 grams, ordered fiber 270 grams.
2, the ceramic powder in 1 step was added in the ball mill mixing and ball milling 24 hours, material: ballstone=1:2.
3, ceramic size 730 grams with the preparation of 2 steps adopt brushing on 270 gram ordered fibers, obtain 1000g hanging ordered fiber.
4, gained hanging ordered fiber in 3 steps is twined on the wrapping machine in self-control, speed of wrap at 0.1MPa, obtains 1 on ceramic membrane green compact at 1m/min, pressure, and 120 ℃ of dryings 24 hours.
5,41 on step gained ceramic membrane green compact are put into silicon carbide rod furnace and carry out sintering, programming rate is controlled at 5 ℃ of-10 ℃/min, 700 ℃ of insulations 2 hours, 1350 ℃ of insulations 4 hours, obtains 1 of ordered porous ceramic film crude green body again.
6, with cutting machine the ordered porous ceramic film two ends are cut away and polished, just obtain 1 of ordered porous ceramic film finished product.
Embodiment 2
1, takes by weighing cordierite 400 grams by the prescription requirement, brium carbonate 70 grams, calcium carbonate 80 grams, bentonite 1 gram, feldspar 4 grams, water 280 grams, ordered fiber 170 grams;
2, the ceramic powder in 1 step was added in the ball mill mixing and ball milling 24 hours, material: ballstone=1:2 obtains ceramic size 830 grams.
3,830 gram ceramic sizes with the preparation of 2 steps adopt brushing on 170 gram ordered fibers, obtain 1000 gram hanging ordered fibers.
4, the ordered fiber that gained in 3 steps is had a ceramic size twines on the self-control wrapping machine, speed of wrap be 1m/min, pressure at 0.1MPa, obtain 1 on ceramic membrane green compact, and 120 ℃ of dryings 24 hours.
5,41 on step gained ceramic membrane green compact are put into silicon carbide rod furnace and carry out sintering, programming rate is controlled at 5 ℃ of-10 ℃/min, 700 ℃ of insulations 1 hour, 1250 ℃ of insulations 4 hours, obtains the ordered porous ceramic film crude green body again.
6, with cutting machine ordered porous ceramic film crude green body two ends are cut away and polished, just obtain 1 of ordered porous ceramic film finished product.
Embodiment 3
1, take by weighing spodumene 3500 grams by the prescription requirement, low temperature frit 650 grams, calcium carbonate 650 grams, bentonite 80 grams, feldspar 120 grams, water 3000 grams add ordered fiber 2000 grams.
2, the ceramic powder in 1 step was added in the ball mill mixing and ball milling 24 hours, material: ballstone=1:2 obtains ceramic size 8000 grams.
3,8000 gram ceramic sizes with the preparation of 2 steps adopt brushing on 2000 gram ordered fibers, obtain 10000g hanging ordered fiber.
4, gained hanging ordered fiber in 3 steps is twined on the wrapping machine in self-control, speed of wrap be 1m/min, pressure at 0.1MPa, obtain 10 on ceramic membrane green compact, and 120 ℃ of dryings 24 hours.
5,4 10 on step gained ceramic membrane green compact are put into silicon carbide rod furnace and carry out sintering, programming rate is controlled at 5 ℃ of-10 ℃/min, 700 ℃ of insulations 1 hour, 1150 ℃ of insulations 4 hours, obtains the ordered porous ceramic film crude green body again.
6, with cutting machine ordered porous ceramic film crude green body two ends are cut away and polished, just obtain 10 of ordered porous ceramic film finished products.
Embodiment 4
1, takes by weighing aluminium oxide 400 grams, spodumene 800 grams, quartzy 500 grams, porcelain powder 600 grams, carborundum 1000 grams, cordierite 700 grams by the prescription requirement; Water 2800 grams; Calcium carbonate 80 grams, brium carbonate 580 grams, bentonite 10 grams, Suzhou soil 500 grams, feldspar 40 grams, glass dust 100 grams, boron frit 200 grams, nylon fiber 600 grams, carbon fiber 500 gram measuring fibers 600 grams.
2, the ceramic powder in 1 step was added in the ball mill mixing and ball milling 24 hours, material: ballstone=1:2 obtains ceramic size 8300 grams.
3,8300 gram ceramic sizes with the preparation of 2 steps adopt brushing on 1700 gram ordered fibers, obtain 10000 gram hanging ordered fibers.
4, the ordered fiber that gained in 3 steps is had a ceramic size twines on the self-control wrapping machine, speed of wrap be 1m/min, pressure at 0.1MPa, obtain 10 on ceramic membrane green compact, and 120 ℃ of dryings 24 hours.
5,41 on step gained ceramic membrane green compact are put into silicon carbide rod furnace and carry out sintering, programming rate is controlled at 5 ℃ of-10 ℃/min, 700 ℃ of insulations 1 hour, 1250 ℃ of insulations 4.5 hours, obtains the ordered porous ceramic film crude green body again.
6, with cutting machine ordered porous ceramic film crude green body two ends are cut away and polished, just obtain 10 of ordered porous ceramic film finished products.

Claims (6)

1. an ordered porous ceramic film is characterized in that: adopt following prescription: (by weight percentage)
Ceramic aggregate 23%-50%; Bond 15%-20%; Water 25%-30%; Ordered fiber 10%-27%.
2. according to the described ordered porous ceramic film of claim 1, it is characterized in that: described ceramic aggregate is wherein a kind of such as aluminium oxide, spodumene, quartz, porcelain powder, carborundum and cordierite or their arbitrary proportion composition.
3. according to the described ordered porous ceramic film of claim 1, it is characterized in that: described bond is wherein a kind of such as calcium carbonate, brium carbonate, bentonite, Suzhou soil feldspar, glass dust and boron frit or their arbitrary proportion composition; Described ordered fiber is wherein a kind of such as nylon fiber, carbon fiber and measuring fiber or their arbitrary proportion composition.
4. a method for preparing the described ordered porous ceramic film of claim 1 is characterized in that: adopt steps such as batching, ball milling, brushing or dip-coating, moulding, drying, sintering, cutting.
5. according to the preparation method of the described ordered porous ceramic film of claim 4, it is characterized in that: described moulding is that to adopt the self-control wrapping machine to carry out ceramic membrane Wrapping formed.
6. according to the preparation method of the described ordered porous ceramic film of claim 4, it is characterized in that: described sintering is meant porcelain film green compact is put into kiln, 700 ℃-900 ℃ insulations 1-2 hours, 1150 ℃-1400 ℃ insulations 2-6 hours, obtain the ordered porous ceramic film crude green body.
CNA200810143685XA 2008-11-24 2008-11-24 Ordered porous ceramic film and preparation method thereof Pending CN101417215A (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101851100A (en) * 2010-05-21 2010-10-06 南京工业大学 Preparation method of ceramic membrane with different surface roughness
CN102515817A (en) * 2011-11-16 2012-06-27 伍协 Hollow fiber ceramic membrane and preparation method thereof
CN105413482A (en) * 2015-12-03 2016-03-23 仇颖超 Preparation method of porous ceramic membrane
CN105771475A (en) * 2016-03-16 2016-07-20 江苏省陶瓷研究所有限公司 Ceramic membrane for filtering high-temperature smoke and preparation method thereof
CN106587948A (en) * 2016-12-14 2017-04-26 安徽瑞研新材料技术研究院有限公司 Ceramic membrane material
CN108793971A (en) * 2018-06-12 2018-11-13 佛山市华强协兴陶瓷有限公司 A kind of environmental protection water purification ceramic material and preparation method thereof
CN111744372A (en) * 2020-07-06 2020-10-09 广州市还原科技有限公司 Porous ultrafiltration ceramic material, product containing material and preparation of porous ultrafiltration ceramic material
CN112159239A (en) * 2020-09-28 2021-01-01 景德镇陶瓷大学 Preparation method of roll type ceramic membrane support and ceramic membrane product thereof
CN112675712A (en) * 2020-12-10 2021-04-20 景德镇陶瓷大学 Preparation method of roll-type ceramic membrane, prepared product and filtration water purifier
CN112694140A (en) * 2019-10-22 2021-04-23 陈鹤鹏 Novel filtering material
CN112791511A (en) * 2020-12-21 2021-05-14 扬州大学 Oriented porous structure material for filtration and preparation method thereof
CN115504807A (en) * 2022-09-29 2022-12-23 聊城大学 Method for preparing porous ceramic with uniform pore diameter
WO2023023905A1 (en) * 2021-08-23 2023-03-02 深圳市安芯精密组件有限公司 Atomization core structural member and preparation method therefor
RU2815671C1 (en) * 2021-08-23 2024-03-19 Шэньчжэнь Аньсинь Пресижен Компонентс Ко., Лтд. Structural element for spraying core and method of its manufacturing

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101851100B (en) * 2010-05-21 2012-11-21 南京工业大学 Preparation method of ceramic membrane with different surface roughness
CN101851100A (en) * 2010-05-21 2010-10-06 南京工业大学 Preparation method of ceramic membrane with different surface roughness
CN102515817A (en) * 2011-11-16 2012-06-27 伍协 Hollow fiber ceramic membrane and preparation method thereof
CN105413482A (en) * 2015-12-03 2016-03-23 仇颖超 Preparation method of porous ceramic membrane
CN105771475A (en) * 2016-03-16 2016-07-20 江苏省陶瓷研究所有限公司 Ceramic membrane for filtering high-temperature smoke and preparation method thereof
CN106587948A (en) * 2016-12-14 2017-04-26 安徽瑞研新材料技术研究院有限公司 Ceramic membrane material
CN108793971A (en) * 2018-06-12 2018-11-13 佛山市华强协兴陶瓷有限公司 A kind of environmental protection water purification ceramic material and preparation method thereof
CN112694140A (en) * 2019-10-22 2021-04-23 陈鹤鹏 Novel filtering material
CN111744372B (en) * 2020-07-06 2022-06-28 广州市还原科技有限公司 Porous ultrafiltration ceramic material, product containing material and preparation of product
CN111744372A (en) * 2020-07-06 2020-10-09 广州市还原科技有限公司 Porous ultrafiltration ceramic material, product containing material and preparation of porous ultrafiltration ceramic material
CN112159239A (en) * 2020-09-28 2021-01-01 景德镇陶瓷大学 Preparation method of roll type ceramic membrane support and ceramic membrane product thereof
CN112159239B (en) * 2020-09-28 2022-07-15 景德镇陶瓷大学 Preparation method of roll-type ceramic membrane support and ceramic membrane product thereof
CN112675712A (en) * 2020-12-10 2021-04-20 景德镇陶瓷大学 Preparation method of roll-type ceramic membrane, prepared product and filtration water purifier
CN112675712B (en) * 2020-12-10 2022-07-15 景德镇陶瓷大学 Preparation method of roll-type ceramic membrane, prepared product and filtration water purifier
CN112791511A (en) * 2020-12-21 2021-05-14 扬州大学 Oriented porous structure material for filtration and preparation method thereof
WO2023023905A1 (en) * 2021-08-23 2023-03-02 深圳市安芯精密组件有限公司 Atomization core structural member and preparation method therefor
RU2815671C1 (en) * 2021-08-23 2024-03-19 Шэньчжэнь Аньсинь Пресижен Компонентс Ко., Лтд. Structural element for spraying core and method of its manufacturing
CN115504807A (en) * 2022-09-29 2022-12-23 聊城大学 Method for preparing porous ceramic with uniform pore diameter
CN115504807B (en) * 2022-09-29 2023-08-08 聊城大学 Method for preparing porous ceramic with uniform pore diameter

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Application publication date: 20090429