CN116550164A - Preparation method of nanofiltration ceramic membrane and product prepared by preparation method - Google Patents
Preparation method of nanofiltration ceramic membrane and product prepared by preparation method Download PDFInfo
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- CN116550164A CN116550164A CN202310595348.9A CN202310595348A CN116550164A CN 116550164 A CN116550164 A CN 116550164A CN 202310595348 A CN202310595348 A CN 202310595348A CN 116550164 A CN116550164 A CN 116550164A
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- 239000012528 membrane Substances 0.000 title claims abstract description 52
- 239000000919 ceramic Substances 0.000 title claims abstract description 49
- 238000001728 nano-filtration Methods 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000011148 porous material Substances 0.000 claims abstract description 11
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 38
- 229910052726 zirconium Inorganic materials 0.000 claims description 38
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 16
- 239000012065 filter cake Substances 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 229960000583 acetic acid Drugs 0.000 claims description 11
- 239000012362 glacial acetic acid Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- 239000007888 film coating Substances 0.000 claims description 6
- 238000009501 film coating Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 5
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 4
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005336 cracking Methods 0.000 abstract description 5
- 238000003980 solgel method Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 9
- 230000007547 defect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000009775 high-speed stirring Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- -1 polyoxyethylene Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 229910000449 hafnium oxide Inorganic materials 0.000 description 1
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- B01D71/05—Cermet materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
-
- 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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/26—Spraying processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/48—Influencing the pH
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/50—Control of the membrane preparation process
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Water Supply & Treatment (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a preparation method of a nanofiltration ceramic membrane and a product prepared by the preparation method. The invention not only further refines the aperture, but also effectively solves the problems of large shrinkage and cracking of the film layer in the process of preparing the nanofiltration ceramic film by the sol-gel method in the prior art, thereby effectively forming the continuous film. In addition, the preparation method is simple, has controllable and adjustable pore diameter of the membrane layer, is beneficial to popularization and application, and has positive promotion effect on application and development of nanofiltration ceramic membrane technology.
Description
Technical Field
The invention relates to the technical field of inorganic membranes, in particular to a preparation method of a nanofiltration ceramic membrane and a product prepared by the same.
Background
Nanofiltration, which is a pressure-driven membrane process, has separation characteristics between ultrafiltration and reverse osmosis, and has attracted increasing interest in many fields of application, such as sea water desalination, wastewater treatment and drinking water purification. Nanofiltration membranes are generally classified into two types, including organic and inorganic, according to the materials. Organic nanofiltration membranes have found various industrial applications, however, these organic membranes have disadvantages such as low thermal and chemical stability, poor mechanical strength, and the problem that membrane pore size is compressed under operating pressure conditions, resulting in a decrease in membrane permeation flux. For these drawbacks, it is possible to overcome by developing more efficient nanofiltration ceramic membranes. Therefore, the nanofiltration ceramic membrane has rapid development and has become a great hot spot for research in the technical field of membrane separation.
Currently, different types of oxide materials have been used to develop ceramic nanofiltration membranes. These oxide materials include aluminum oxide, titanium oxide, zirconium oxide, hafnium oxide, and the like. The zirconia membrane has higher chemical stability, so that the zirconia membrane is widely applied to the development of ceramic nanofiltration membranes. In the prior art, sol-gel method is generally adopted to prepare sol particles with smaller particle size, and the ceramic nanofiltration membrane is formed through gelation, drying and sintering. However, the prior art has major technical drawbacks: that is, the sol particles are finer, but the pores of the ceramic film carrier are thicker, so that the film liquid is easy to leak into the pores during film coating, and film formation cannot be performed. And secondly, the gel is easy to crack in the drying process, so that cracks appear on the membrane surface, and a continuous membrane cannot be formed, thereby causing the defect of the nanofiltration membrane.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a nanofiltration ceramic membrane, which comprises the steps of firstly pre-coating the surface of a ceramic base membrane by initial mixing of zirconium sol and nano zirconia to form a filter cake layer, and then spraying the nano zirconium sol on the surface to carry out surface modification so as to achieve the purpose of further refining the pore diameter, inhibit gel drying cracking and prevent cracking of the membrane layer. Another object of the present invention is to provide a product manufactured by the above-mentioned method for manufacturing a nanofiltration ceramic membrane.
The aim of the invention is realized by the following technical scheme:
the invention provides a preparation method of a nanofiltration ceramic membrane, which comprises the following steps:
(1) Preparation of zirconium sols
ZrOCl 2 .8H 2 O is dissolved in deionized water and stirred for 10 to 30 minutes under the water bath at the temperature of 2 to 5 ℃ to form uniform solution A; dissolving hexamethylenetetramine in deionized water to obtain a solution B; then adding the solution B into the solution A at the temperature of 2-5 ℃ under the stirring condition to obtain zirconium sol with the concentration of 0.8-2.0 mol/L;
(2) Preparation of mixed solution of nano zirconia and zirconium sol
Mixing 60-70wt% of zirconium sol, 10-25wt% of nano zirconium oxide, 6-12wt% of polyethylene oxide aqueous solution and 2-8wt% of glacial acetic acid aqueous solution to obtain a mixed solution C with a pH value of 1-3 and a viscosity of 20-60 mPa.s;
(3) Preparation of zirconium sol dispersion
Mixing 70-80 wt% of zirconium sol, 4-20 wt% of polyethylene oxide aqueous solution and 3-16 wt% of glacial acetic acid aqueous solution to obtain zirconium sol dispersion D with pH value of 1-3 and viscosity of 5-12 mPa.s;
(4) Coating and spraying of nanofiltration ceramic membranes
And (3) coating the mixed solution C on the surface of the ceramic base film by adopting a film coating method to form a filter cake layer, wherein the coating time is 5-20 s, spraying the zirconium sol dispersion solution D on the surface of the filter cake layer after drying, sintering at 500-600 ℃ after drying, and preserving heat for 20-60 min to form a separation film layer on the filter cake layer to prepare the nanofiltration ceramic film.
Further, in the step (2), the particle size of the nano zirconia is 10-40 nm; the concentration of the polyethylene oxide aqueous solution is 3-6wt% and the concentration of the glacial acetic acid aqueous solution is 24-40wt%. The aperture of the ceramic bottom film is 100-200 nm. And (3) in the step (4), the drying temperature is less than or equal to 25 ℃, and the drying time is 12-48 h.
Further, the thickness of the separation membrane layer is 2-10 mu m, and the average pore diameter is 2-10 nm.
A product made by the method of making a nanofiltration ceramic membrane as defined in the claims.
The invention has the following beneficial effects:
(1) The invention improves the technology on the basis of preparing the nanofiltration ceramic membrane by a sol-gel method, adopts a two-step coating method, and prevents zirconium sol from leaking into the pores of the ceramic base membrane by pre-coating a filter cake layer on the surface of the ceramic base membrane through mixing zirconium sol and nanometer zirconia. Then spraying nano zirconium sol on the surface to carry out surface modification, wherein on one hand, the sprayed sol fills pores in a filter cake layer; on the other hand, in the sintering process, the nano zirconia which is a sintering product of the gel also falls into the pores of the filter cake, so that the pore diameter of the nano-filtration ceramic membrane is further reduced.
(2) Glacial acetic acid is adopted in the sol and the film coating liquid to reduce the pH value and inhibit the gel from drying and cracking, so that the problems of large shrinkage and cracking of a film layer in the process of preparing the nanofiltration ceramic film by a sol-gel method in the prior art are effectively solved.
(3) The controllable adjustment of the aperture of the membrane layer is realized by adjusting the particle size of the nano zirconia and the mixing proportion of the nano zirconia and the zirconium sol. Therefore, the invention is beneficial to popularization and application, and has positive promotion effect on application and development of nanofiltration ceramic membrane technology.
Drawings
The invention will be described in further detail with reference to examples and figures:
FIG. 1 is a photograph of a surface and a cross-section of a nanofiltration ceramic membrane (a: surface; b: cross-section) obtained according to the first embodiment of the invention;
FIG. 2 is a photograph of a surface and a cross-section of a nanofiltration ceramic membrane obtained in example two of the present invention (a: surface; b: cross-section).
Detailed Description
Embodiment one:
the preparation method of the nanofiltration ceramic membrane comprises the following steps:
(1) Preparation of zirconium sols
ZrOCl 2 .8H 2 O is dissolved in deionized water, and is magnetically stirred for 15min at the temperature of 3 ℃ in water bath to form uniform solution A; dissolving hexamethylenetetramine in deionized water to obtain a solution B; then dropwise adding the solution B into the solution A at the temperature of 3 ℃ and under the condition of high-speed stirring to obtain zirconium sol with the concentration of 0.8 mol/L;
(2) Preparation of mixed solution of nano zirconia and zirconium sol
Mixing 70wt% of zirconium sol, 15wt% of zirconium oxide with the particle size of 20nm, 10wt% of polyoxyethylene aqueous solution with the concentration of 4wt% and 5wt% of glacial acetic acid aqueous solution with the concentration of 36% to obtain a mixed solution C with the pH value of 2.2 and the viscosity of 52 mPa.s;
(3) Preparation of zirconium sol dispersion
Mixing 80wt% of zirconium sol, 10wt% of polyethylene oxide aqueous solution with the concentration of 5wt% and 10wt% of glacial acetic acid aqueous solution with the concentration of 36wt% to obtain zirconium sol dispersion D with the pH value of 1.8 and the viscosity of 10.2 Pa.s;
(4) Coating and spraying of nanofiltration ceramic membranes
The method comprises the steps of coating a mixed solution C on the surface of a ceramic base film with the aperture of 100nm by adopting a film coating method to form a filter cake layer, wherein the coating time is 15s, spraying a zirconium sol dispersion solution D on the surface of the filter cake layer after drying, drying at the temperature of 20 ℃ for 36h, sintering at the temperature of 600 ℃, and preserving heat for 60min to form a separation film layer with the thickness of 5 mu m and the average aperture of 8nm on the filter cake layer, so as to prepare the nanofiltration ceramic film, wherein the surface of the nanofiltration ceramic film has no defects and cracks, and the aperture of the particle size meets the requirements, as shown in figure 1.
Embodiment two:
the preparation method of the nanofiltration ceramic membrane comprises the following steps:
(1) Preparation of zirconium sols
ZrOCl 2 .8H 2 O is dissolved in deionized water and magnetically stirred for 30min at the temperature of 5 ℃ in water bathForming a uniform solution A; dissolving hexamethylenetetramine in deionized water to obtain a solution B; then dropwise adding the solution B into the solution A at the temperature of 5 ℃ and under the condition of high-speed stirring to obtain zirconium sol with the concentration of 1.5 mol/L;
(2) Preparation of mixed solution of nano zirconia and zirconium sol
Mixing 63wt% of zirconium sol, 23wt% of zirconium oxide with the particle size of 10nm, 10wt% of polyoxyethylene aqueous solution with the concentration of 6wt% and 4wt% of glacial acetic acid aqueous solution with the concentration of 30% to obtain a mixed solution C with the pH value of 2.7 and the viscosity of 58 mPa.s;
(3) Preparation of zirconium sol dispersion
Mixing 75wt% of zirconium sol, 20wt% of polyethylene oxide aqueous solution with the concentration of 3wt% and 5wt% of glacial acetic acid aqueous solution with the concentration of 30wt% to obtain zirconium sol dispersion D with the pH value of 1.5 and the viscosity of 8.8 mPa.s;
(4) Coating and spraying of nanofiltration ceramic membranes
The method comprises the steps of coating a mixed solution C on the surface of a ceramic base film with the aperture of 200nm by adopting a film coating method to form a filter cake layer, wherein the coating time is 15 seconds, spraying a zirconium sol dispersion solution D on the surface of the filter cake layer after drying, drying at the temperature of 15 ℃ for 36 hours, sintering at the temperature of 550 ℃, and preserving heat for 30 minutes to form a separation film layer with the thickness of 4 mu m and the average aperture of 5nm on the filter cake layer, so as to prepare the nanofiltration ceramic film, wherein the surface of the nanofiltration ceramic film has no defects and cracks, and the aperture of the particle size meets the requirements, as shown in figure 2.
Claims (6)
1. The preparation method of the nanofiltration ceramic membrane is characterized by comprising the following steps of:
(1) Preparation of zirconium sols
ZrOCl 2 .8H 2 O is dissolved in deionized water and stirred for 10 to 30 minutes under the water bath at the temperature of 2 to 5 ℃ to form uniform solution A; dissolving hexamethylenetetramine in deionized water to obtain a solution B; then adding the solution B into the solution A at the temperature of 2-5 ℃ under the stirring condition to obtain zirconium sol with the concentration of 0.8-2.0 mol/L;
(2) Preparation of mixed solution of nano zirconia and zirconium sol
Mixing 60-70wt% of zirconium sol, 10-25wt% of nano zirconium oxide, 6-12wt% of polyethylene oxide aqueous solution and 2-8wt% of glacial acetic acid aqueous solution to obtain a mixed solution C with a pH value of 1-3 and a viscosity of 20-60 mPa.s;
(3) Preparation of zirconium sol dispersion
Mixing 70-80 wt% of zirconium sol, 4-20 wt% of polyethylene oxide aqueous solution and 3-16 wt% of glacial acetic acid aqueous solution to obtain zirconium sol dispersion D with pH value of 1-3 and viscosity of 5-12 mPa.s;
(4) Coating and spraying of nanofiltration ceramic membranes
And (3) coating the mixed solution C on the surface of the ceramic base film by adopting a film coating method to form a filter cake layer, wherein the coating time is 5-20 s, spraying the zirconium sol dispersion solution D on the surface of the filter cake layer after drying, sintering at 500-600 ℃ after drying, and preserving heat for 20-60 min to form a separation film layer on the filter cake layer to prepare the nanofiltration ceramic film.
2. The method for preparing the nanofiltration ceramic membrane according to claim 1, wherein the method comprises the following steps: the grain diameter of the nano zirconia in the step (2) is 10-40 nm; the concentration of the polyethylene oxide aqueous solution is 3-6wt% and the concentration of the glacial acetic acid aqueous solution is 24-40wt%.
3. The method for preparing the nanofiltration ceramic membrane according to claim 1, wherein the method comprises the following steps: the aperture of the ceramic bottom film is 100-200 nm.
4. The method for preparing the nanofiltration ceramic membrane according to claim 1, wherein the method comprises the following steps: and (3) in the step (4), the drying temperature is less than or equal to 25 ℃, and the drying time is 12-48 h.
5. The method for preparing the nanofiltration ceramic membrane according to claim 1, wherein the method comprises the following steps: the thickness of the separation membrane layer is 2-10 mu m, and the average pore diameter is 2-10 nm.
6. A product produced by the method for producing a nanofiltration ceramic membrane according to any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202310595348.9A CN116550164A (en) | 2023-05-25 | 2023-05-25 | Preparation method of nanofiltration ceramic membrane and product prepared by preparation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310595348.9A CN116550164A (en) | 2023-05-25 | 2023-05-25 | Preparation method of nanofiltration ceramic membrane and product prepared by preparation method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5585136A (en) * | 1995-03-22 | 1996-12-17 | Queen's University At Kingston | Method for producing thick ceramic films by a sol gel coating process |
| CN102743979A (en) * | 2012-07-12 | 2012-10-24 | 三达膜科技（厦门）有限公司 | Preparation method of zirconia ceramic ultrafiltration film |
| CN103360080A (en) * | 2013-07-18 | 2013-10-23 | 南京工业大学 | Method for preparation of ceramic nanofiltration membrane by improved sol-gel technique |
| CN109908764A (en) * | 2019-03-14 | 2019-06-21 | 景德镇陶瓷大学 | A kind of preparation method of Inorganic Nanofiltration Membranes and its product obtained |
| CN112759370A (en) * | 2019-10-18 | 2021-05-07 | 三达膜科技（厦门）有限公司 | Preparation method of high-strength ceramic filtering membrane |
-
2023
- 2023-05-25 CN CN202310595348.9A patent/CN116550164A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5585136A (en) * | 1995-03-22 | 1996-12-17 | Queen's University At Kingston | Method for producing thick ceramic films by a sol gel coating process |
| CN102743979A (en) * | 2012-07-12 | 2012-10-24 | 三达膜科技（厦门）有限公司 | Preparation method of zirconia ceramic ultrafiltration film |
| CN103360080A (en) * | 2013-07-18 | 2013-10-23 | 南京工业大学 | Method for preparation of ceramic nanofiltration membrane by improved sol-gel technique |
| CN109908764A (en) * | 2019-03-14 | 2019-06-21 | 景德镇陶瓷大学 | A kind of preparation method of Inorganic Nanofiltration Membranes and its product obtained |
| CN112759370A (en) * | 2019-10-18 | 2021-05-07 | 三达膜科技（厦门）有限公司 | Preparation method of high-strength ceramic filtering membrane |
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