CN106799169A - A kind of preparation method of ceramic super-filtering film - Google Patents
A kind of preparation method of ceramic super-filtering film Download PDFInfo
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- CN106799169A CN106799169A CN201710033016.6A CN201710033016A CN106799169A CN 106799169 A CN106799169 A CN 106799169A CN 201710033016 A CN201710033016 A CN 201710033016A CN 106799169 A CN106799169 A CN 106799169A
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- ceramic
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- colloidal sol
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/025—Aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
Abstract
The present invention relates to the preparation method of ceramic super-filtering film.The method is comprised the following steps：（1）Prepare Ceramic excessive filtration film support green compact；（2）By PVA add boehmite sol in, wherein, addition weight/mass percentage compositions of the PVA in colloidal sol be 0.4%~1.2%；（3）By step（1）Ceramic excessive filtration film support be placed in step（2）Dip-coating 5~7 seconds in the boehmite sol of PVA are added；（4）Then it is once sintered after drying.This method is using directly drying and sintering technique (one-step method) can prepare the α Al with dissymmetrical structure after dip-coating boehmite sol on supporter green compact2O3Ceramic membrane, with low cost, the advantage of steady quality.
Description
Technical field
The present invention relates to water treatment field, and in particular to a kind of preparation method of ceramic super-filtering film.
Background technology
Ceramic membrane is the one kind in inoranic membrane, belongs to the solid membrane material in membrane separation technique, mainly with different size
Inorganic ceramic material is formed as supporter through surface coating, high-temperature firing.
Ceramic membrane technology is the outstanding figure in membrane technology, and film is a kind of macromolecule chemical material, it have it is numerous can only be with micro-
The rice aperture that even nanometer is calculated, existing separation, concentration, purification and desalination function have efficient, energy-saving and environmental protection, molecular level mistake again
The features such as filter.Just be widely used in after membrane technology invention food processing, purification of water quality, environmental improvement, pharmaceuticals industry, chemical industry with
The fields such as petrochemical industry, for realizing the purification separation of product.Ceramic membrane is exactly to be made up of the ceramic material by high temperature sintering
Seperation film.Due to unique patience, before one becomes as film field is with the fastest developing speed, also most has development into market
One of kind of scape.
The preparation of usual ceramic membrane is divided into two steps, and one is the preparation of supporter, and two is the preparation of separating layer.Tool is prepared first
There is a supporter of larger aperture, then by colloidal sol-gel method, the method such as chemical vapour deposition technique is in supporting body surface coating, shape
The ceramic membrane of the dissymmetrical structure into more than with two-layer or two-layer.Typically only tens nanometers to several microns of coating layer thickness,
Main centrifugation is played in separation process.The preparation of the general supporter of prior art and separating layer is separately carried out, it is necessary to through excessive
Secondary sintering, and sintering process in whole ceramic membrane preparation cost than great, repeatedly to occupy the manufacturing cost of ceramic membrane high for sintering
Under not.
The content of the invention
In order to overcome the shortcomings of that prior art is above-mentioned, the present invention provides a kind of preparation method of ceramic super-filtering film, the present invention
Using one-step preparation process, the direct dip-coating colloidal sol on supporter green compact, step sintering after drying, prepare have it is asymmetric
The ceramic membrane of structure.Reduce sintering number obvious to reducing the effect of ceramic membrane preparation cost.
The present invention program is：
A kind of preparation method of ceramic super-filtering film, comprises the following steps：
（1）Prepare Ceramic excessive filtration film support green compact；
（2）By PVA add boehmite sol in, wherein, addition weight/mass percentage compositions of the PVA in colloidal sol be 0.4%~1.2%；
（3）By step（1）Ceramic excessive filtration film support be placed in step（2）Dip-coating 5~7 seconds in the boehmite sol of PVA are added；
（4）Then it is once sintered after drying.
Another preferred scheme of the invention is that the boehmite sol is isopropanol aluminum colloidal sol, aluminium isopropoxide in colloidal sol
0.28~0.32mol/L of concentration.
Another preferred scheme of the invention is, aluminium isopropoxide concentration 0.3mol/L in the isopropanol aluminum colloidal sol.
Another preferred scheme of the invention is that the boehmite sol is chlorination aluminum colloidal sol, concentration of aluminum chloride in colloidal sol
0.12~0.16mol/L.
Another preferred scheme of the invention is, concentration of aluminum chloride 0.15mol/L in the chlorination aluminum colloidal sol.
Another preferred scheme of the invention is that coating layer thickness is 1. 45~1.48 μm after the ceramic super-filtering film dip-coating.
Another preferred scheme of the invention is that coating layer thickness is 1. 47 μm after the ceramic super-filtering film dip-coating.
This use dip-coating boehmite sol on supporter green compact, it is once sintered after drying to prepare with dissymmetrical structure
Inorganic ceramic ultra-filtering film.Using the directly drying and sintering technique (one-step method) after dip-coating boehmite sol on supporter green compact
Prepare the α-Al with dissymmetrical structure2O3Ceramic membrane, greatly reduces the production cost of ceramic super-filtering film, overcomes existing
Technical costs defect high.
Specific embodiment：
The preferred embodiment of the present invention presented below, to help further understanding the present invention, but protection scope of the present invention is simultaneously
It is not limited only to these embodiments.
Embodiment 1
（1）Al is prepared using prior art2O3Ceramic film support green compact；
（2）By PVA add boehmite sol in, wherein, addition weight/mass percentage compositions of the PVA in colloidal sol be 1%
（3）By step（1）Ceramic excessive filtration film support green compact be placed in step（2）Dip-coating 6 in the boehmite sol of PVA is added
Second；
（4）Then it is once sintered after drying to obtain α-Al2O3 Ceramic membrane.
The boehmite sol is isopropanol aluminum colloidal sol, aluminium isopropoxide concentration 0.3mol/L in colloidal sol.
Drying temperature is 120 DEG C, and drying time is 2 hours, and sintering temperature is 1150 DEG C, sintering time 3 hours.
Embodiment 2
（1）Al is prepared using prior art2O3Ceramic film support green compact；
（2）By PVA add boehmite sol in, wherein, addition weight/mass percentage compositions of the PVA in colloidal sol be 1%
（3）By step（1）Ceramic excessive filtration film support green compact be placed in step（2）Dip-coating 15 in the boehmite sol of PVA is added
Second；
（4）Then it is once sintered after drying to obtain α-Al2O3 Ceramic membrane.
The boehmite sol is isopropanol aluminum colloidal sol, aluminium isopropoxide concentration 0.3mol/L in colloidal sol.
Drying temperature is 120 DEG C, and drying time is 1.5 hours, and sintering temperature is 1150 DEG C, sintering time 3 hours.
Embodiment 3
（1）Al is prepared using prior art2O3Ceramic film support green compact；
（2）By PVA add boehmite sol in, wherein, addition weight/mass percentage compositions of the PVA in colloidal sol be 0.5%；
（3）By step（1）Ceramic excessive filtration film support be placed in step（2）Dip-coating 3 seconds in the boehmite sol of PVA are added；
（4）Then it is once sintered after drying to obtain α-Al2O3 Ceramic membrane.
The boehmite sol is isopropanol aluminum colloidal sol, aluminium isopropoxide concentration 0.16mol/L in colloidal sol.
Drying temperature is 120 DEG C, and drying time is 1 hour, and sintering temperature is 1150 DEG C, sintering time 3 hours.
Embodiment 4
（1）Al is prepared using prior art2O3Ceramic film support green compact；
（2）By PVA add boehmite sol in, wherein, addition weight/mass percentage compositions of the PVA in colloidal sol be 0.5%；
（3）By step（1）Ceramic excessive filtration film support be placed in step（2）Dip-coating 9 seconds in the boehmite sol of PVA are added；
（4）Then it is once sintered after drying to obtain α-Al2O3 Ceramic membrane.
The boehmite sol is isopropanol aluminum colloidal sol, aluminium isopropoxide concentration 0.16mol/L in colloidal sol.
Drying temperature is 120 DEG C, and drying time is 2 hours, and sintering temperature is 1150 DEG C, sintering time 3 hours.
Embodiment 5
（1）Al is prepared using prior art2O3Ceramic film support green compact；
（2）By PVA add boehmite sol in, wherein, addition weight/mass percentage compositions of the PVA in colloidal sol be 0.5%；
（3）By step（1）Ceramic excessive filtration film support be placed in step（2）Dip-coating 15 seconds in the boehmite sol of PVA are added；
（4）Then it is once sintered after drying to obtain α-Al2O3 Ceramic membrane.
The boehmite sol is isopropanol aluminum colloidal sol, aluminium isopropoxide concentration 0.16mol/L in colloidal sol.
Drying temperature is 120 DEG C, and drying time is 2 hours, and sintering temperature is 1150 DEG C, sintering time 3 hours.
The integrality of the ceramic membrane obtained by embodiment 1-5 such as following table：
Table one：PVA adds the influence to isopropanol aluminum dissolved glue film defect
The comparative example of embodiment 6
（1）Al is prepared using prior art2O3Ceramic film support green compact；
（2）By step（1）Ceramic excessive filtration film support be placed in dip-coating 6 seconds in the boehmite sol for do not added PVA；
（4）Then it is once sintered after drying to obtain α-Al2O3 Ceramic membrane.
The boehmite sol is isopropanol aluminum colloidal sol, aluminium isopropoxide concentration 0.16mol/L in colloidal sol.
Drying temperature is 120 DEG C, and drying time is 44 clocks, and sintering temperature is 1150 DEG C, sintering time 3 hours.
Ceramic membrane cracking phenomena obtained by the method sintering is universal.
Embodiment 7
The present embodiment boehmite sol is changed to chlorination aluminum colloidal sol, and other conditions are with embodiment 1.
Embodiment 8
The present embodiment boehmite sol is changed to chlorination aluminum colloidal sol, and other conditions are with embodiment 2.
Embodiment 9
The present embodiment boehmite sol is changed to chlorination aluminum colloidal sol, and other conditions are with embodiment 3.
Embodiment 10
The present embodiment boehmite sol is changed to chlorination aluminum colloidal sol, and other conditions are with embodiment 4.
Embodiment 11
The present embodiment boehmite sol is changed to chlorination aluminum colloidal sol, and other conditions are with embodiment 5.
Ceramic film integrality obtained by embodiment 7-11 is as shown in the table：
Table two：PVA adds the influence to chlorination aluminum dissolved glue film integrality
After testing, the coating layer thickness of the ceramic super-filtering film obtained by the present invention and film rejection and the relation such as following table of flux：
Table three：Coating thickness and film rejection and flux relation
By experiment, PVA is directly added into aluminium isopropoxide and chlorination aluminum boehmite sol, the film time can be extended, had
Effect improves the integrality of coating sintering.In addition, suitably reducing chlorination aluminum boehmite sol concentration can improve the film time extremely
15s。
After testing, the film time is 6s on supporter green compact（Isopropanol aluminum collosol concentration 0.3mol/L, aluminium chloride
Collosol concentration 0.16mol/L processed）Even if drying stage is reduced to 1h and can also prepare the perfect sunken pottery for having separating layer
Porcelain film.
After testing, with the increase of film thickness, rejection rises, and flux declines, and voidage is unrelated with thickness.Work as film thickness
When reaching 1.47 μm, the rejection to PVA1750 is more than 90%, and molecular cut off is 75000.
Experimental result explanation is using a directly drying and sintering technique (step after dip-coating boehmite sol on supporter green compact
Method) α-Al2O3 ceramic membranes with dissymmetrical structure can be prepared.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of ceramic super-filtering film, it is characterized in that, comprise the following steps：
（1）Prepare Ceramic excessive filtration film support green compact；
（2）By PVA add boehmite sol in, wherein, addition weight/mass percentage compositions of the PVA in colloidal sol be 0.4%~1.2%；
（3）By step（1）Ceramic excessive filtration film support be placed in step（2）Dip-coating 5~7 seconds in the boehmite sol of PVA are added；
（4）Then it is once sintered after drying.
2. the preparation method of ceramic super-filtering film according to claim 1, it is characterized in that, the boehmite sol is aluminium isopropoxide
Colloidal sol processed, 0.28~0.32mol/L of aluminium isopropoxide concentration in colloidal sol.
3. the preparation method of ceramic super-filtering film according to claim 2, it is characterized in that, isopropyl in the isopropanol aluminum colloidal sol
Alcohol aluminum concentration 0.3mol/L.
4. the preparation method of ceramic super-filtering film according to claim 1, it is characterized in that, the boehmite sol is chlorination aluminum
Colloidal sol, 0.12~0.16mol/L of concentration of aluminum chloride in colloidal sol.
5. the preparation method of ceramic super-filtering film according to claim 4, it is characterized in that, aluminium chloride in the chlorination aluminum colloidal sol
Concentration 0.15mol/L.
6. the preparation method of ceramic super-filtering film according to claim 1, it is characterized in that, coating after the ceramic super-filtering film dip-coating
Thickness is 1.45~1.48 μm.
7. the preparation method of ceramic super-filtering film according to claim 6, it is characterized in that, coating after the ceramic super-filtering film dip-coating
Thickness is 1.47 μm.
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| CN201710033016.6A CN106799169A (en) | 2017-01-18 | 2017-01-18 | A kind of preparation method of ceramic super-filtering film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240492A (en) * | 2018-03-07 | 2019-09-17 | 海加尔(厦门)科技有限公司 | A kind of preparation method of the ceramic separation film supporter of acid and alkali-resistance |
| CN112939580A (en) * | 2021-01-29 | 2021-06-11 | 广西碧清源环保投资有限公司 | Preparation method of ceramic filtering membrane |
| CN113493349A (en) * | 2021-07-28 | 2021-10-12 | 苏州新能环境技术股份有限公司 | Resourceful treatment process for glass grinding wastewater |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101708435A (en) * | 2009-11-06 | 2010-05-19 | 华东理工大学 | Method for preparing asymmetric structure ceramic hollow fiber and tubular ultra-filtration membrane |
| KR20150092518A (en) * | 2014-02-05 | 2015-08-13 | 한국기계연구원 | Method for manufacturing porous clay-based ceramic membrane with ceramic coating layer and ceramic membrane manufactured thereby |
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2017
- 2017-01-18 CN CN201710033016.6A patent/CN106799169A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101708435A (en) * | 2009-11-06 | 2010-05-19 | 华东理工大学 | Method for preparing asymmetric structure ceramic hollow fiber and tubular ultra-filtration membrane |
| KR20150092518A (en) * | 2014-02-05 | 2015-08-13 | 한국기계연구원 | Method for manufacturing porous clay-based ceramic membrane with ceramic coating layer and ceramic membrane manufactured thereby |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240492A (en) * | 2018-03-07 | 2019-09-17 | 海加尔(厦门)科技有限公司 | A kind of preparation method of the ceramic separation film supporter of acid and alkali-resistance |
| CN110240492B (en) * | 2018-03-07 | 2020-07-28 | 海加尔(厦门)科技有限公司 | Preparation method of acid-alkali-resistant ceramic separation membrane support |
| CN112939580A (en) * | 2021-01-29 | 2021-06-11 | 广西碧清源环保投资有限公司 | Preparation method of ceramic filtering membrane |
| CN112939580B (en) * | 2021-01-29 | 2022-07-01 | 广西碧清源环保投资有限公司 | Preparation method of ceramic filtering membrane |
| CN113493349A (en) * | 2021-07-28 | 2021-10-12 | 苏州新能环境技术股份有限公司 | Resourceful treatment process for glass grinding wastewater |
| CN113493349B (en) * | 2021-07-28 | 2022-07-01 | 苏州新能环境技术股份有限公司 | Recycling treatment process for glass grinding wastewater |
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Application publication date: 20170606 |