CN117531383A - Temperature response separation membrane and preparation method thereof - Google Patents
Temperature response separation membrane and preparation method thereof Download PDFInfo
- Publication number
- CN117531383A CN117531383A CN202311753984.6A CN202311753984A CN117531383A CN 117531383 A CN117531383 A CN 117531383A CN 202311753984 A CN202311753984 A CN 202311753984A CN 117531383 A CN117531383 A CN 117531383A
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- Prior art keywords
- temperature
- parts
- separation membrane
- responsive
- responsive separation
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- 238000000926 separation method Methods 0.000 title claims abstract description 37
- 239000012528 membrane Substances 0.000 title claims abstract description 35
- 230000004044 response Effects 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 19
- 229920006254 polymer film Polymers 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000002798 polar solvent Substances 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005266 casting Methods 0.000 claims description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 11
- 239000002033 PVDF binder Substances 0.000 claims description 9
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 7
- 230000001112 coagulating effect Effects 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000004745 nonwoven fabric Substances 0.000 claims description 6
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical group CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 5
- 239000013557 residual solvent Substances 0.000 claims description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical group CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- 238000007790 scraping Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 229920002301 cellulose acetate Polymers 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 229920002521 macromolecule Polymers 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 239000010865 sewage Substances 0.000 abstract description 2
- 230000004907 flux Effects 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading 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
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
-
- 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
- B01D67/0002—Organic membrane manufacture
-
- 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
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/36—Polytetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/02—Aerobic processes
- C02F3/12—Activated sludge processes
- C02F3/1236—Particular type of activated sludge installations
- C02F3/1268—Membrane bioreactor systems
Abstract
The invention belongs to the technical field of sewage treatment material processing and preparation, and discloses a temperature response separation membrane and a preparation method thereof. The temperature response separation membrane comprises the following components in parts by weight: 12-20 parts of polymer film material, 60-85 parts of polar solvent, 0.5-2 parts of temperature control reagent, 6-10 parts of polymer pore-forming agent and 0.5-2 parts of additive. The preparation process is simple in process, continuous, easy to realize industrialization, convenient and easy to control in operation, energy-saving, cost-reducing, and meanwhile, the prepared temperature-responsive separation membrane can respond to the temperature of separated feed liquid.
Description
Technical Field
The invention belongs to the technical field of sewage treatment material processing and preparation, and particularly relates to a temperature response separation membrane and a preparation method thereof.
Background
PVDF membranes are widely used in water treatment and biological separation systems due to their excellent properties. However, PVDF membranes are susceptible to contamination by proteins, polysaccharides, etc. during use due to their hydrophilicity. In recent years, environmental-irritant films, such as temperature, pH, light, electricity, and the like, have received attention from researchers. Wherein the separation effect and filtration performance of the temperature-responsive membrane are affected by the temperature of the feed liquid.
The common preparation method of the temperature thermal response film comprises two methods, one is blending modification, the method is widely applied to industrial manufacture, and the other is to synthesize a functionalized thermosensitive material by adopting methods such as plasma treatment, illumination grafting and the like or graft the thermosensitive material on the film material.
Therefore, a new temperature-responsive separation membrane and a preparation method thereof are needed to be proposed, which reduce the manufacturing cost and improve the hydrophilic performance and the anti-pollution performance.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art and provides a temperature response separation membrane and a preparation method thereof. The preparation process is simple in process, continuous, easy to realize industrialization, convenient and easy to control in operation, energy-saving, cost-reducing, and meanwhile, the prepared temperature-responsive separation membrane can respond to the temperature of separated feed liquid.
In order to achieve the above object, the present invention provides, in one aspect, a temperature-responsive separation membrane comprising, in parts by weight: 12-20 parts of polymer film material, 60-85 parts of polar solvent, 0.5-2 parts of temperature control reagent, 6-10 parts of polymer pore-forming agent and 0.5-2 parts of additive.
According to the present invention, preferably, the temperature-responsive separation membrane comprises the following components in parts by weight: 15-20 parts of polymer film material, 65-82 parts of polar solvent, 0.5-1.5 parts of temperature control reagent, 7-9 parts of polymer pore-forming agent and 0.5-1.5 parts of additive.
According to the present invention, preferably, the polymer film material is polyvinylidene fluoride and/or polytetrafluoroethylene.
According to the present invention, preferably, the polar solvent is dimethylacetamide and/or N-methylpyrrolidone.
According to the present invention, preferably, the temperature control agent is N-isopropylacrylamide.
According to the invention, the polymer pore-forming agent is preferably polyvinylpyrrolidone with a polymerization degree of K15-K90, and preferably the polymer pore-forming agent is polyvinylpyrrolidone PVPK-15 and/or polyvinylpyrrolidone PVPK-30.
According to the invention, preferably, the additive is glycerol and/or cellulose acetate.
In another aspect, the present invention provides a method for preparing the temperature-responsive separation membrane, which includes the steps of:
s1: mixing and stirring the polar solvent, the temperature control reagent and the macromolecule pore-forming agent uniformly to obtain a mixed solution;
s2: drying the polymer film material to constant weight to obtain dried polymer film material powder, mixing and stirring the dried polymer film material powder, the mixed solution and the additive uniformly to obtain film casting solution, and sealing, standing and defoaming the film casting solution;
s3: the defoamed casting solution is coated on non-woven fabrics in a scraping way, and after a first preset time, the non-woven fabrics coated with the casting solution in a scraping way are immersed in a coagulating bath of water for curing, so that a cured film is obtained; and after removing the residual solvent on the surface of the solidified film, immersing the solidified film into a coagulating bath of water again for a second preset time, taking out and naturally airing to obtain the temperature response separation film.
According to the present invention, preferably, in step S1, the stirring time is 7 to 10 hours, and the stirring rate is 100rpm to 150rpm.
According to the present invention, preferably, in step S2, the stirring speed is 150rpm to 250rpm.
According to the invention, preferably, said step S2 is carried out at 15-30 ℃.
According to the present invention, preferably, in step S3:
the thickness of the scraper used for the blade coating is 100-2000 mu m;
the first preset time is 15-45s;
removing the residual solvent on the surface of the cured film by water washing;
the second preset time is 24-48h.
According to the invention, preferably, said step S3 is carried out at 15-30 ℃.
The technical scheme of the invention has the following beneficial effects:
the invention adopts a blending modification method, utilizes a solution phase inversion process, takes a polymer membrane material as a matrix, preferably takes N isopropyl acrylamide as a temperature control reagent, and prepares a temperature response separation membrane under the condition of a polar solvent.
The preparation process is simple in process, continuous, easy to realize industrialization, convenient and easy to control in operation, energy-saving, cost-reducing, and meanwhile, the prepared temperature-responsive separation membrane can respond to the temperature of separated feed liquid.
The temperature responsive separation membrane of the present invention can be used in membrane bioreactors.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular descriptions of exemplary embodiments of the invention as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the invention.
Fig. 1 shows an SEM image of the surface morphology of a temperature responsive separation membrane provided in example 1 of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the preferred embodiments of the present invention are described below, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Example 1
The present embodiment provides a temperature-responsive separation membrane comprising, in parts by weight: 18 parts of polyvinylidene fluoride, 70 parts of dimethylacetamide, 1 part of N isopropyl acrylamide, 15 parts of polyvinylpyrrolidone PVPK-15 parts and 1.5 parts of glycerin.
The preparation method of the temperature response separation membrane comprises the following steps:
s1: mixing and stirring the dimethylacetamide, N isopropyl acrylamide and polyvinylpyrrolidone PVPK-15 for 8 hours at 150rpm to obtain a mixed solution;
s2: drying the polyvinylidene fluoride to constant weight, removing water to obtain dried polyvinylidene fluoride powder, mixing and stirring the dried polyvinylidene fluoride powder, the mixed solution and glycerol at room temperature and 150rpm uniformly, fully dissolving the polyvinylidene fluoride powder to obtain casting solution, and sealing, standing and defoaming at room temperature;
s3: spreading the defoamed casting solution (the thickness of a scraper is 150 mu m) on non-woven fabrics, and immersing the non-woven fabrics with the casting solution spread thereon into a coagulating bath of water for curing after 15-45s to obtain a cured film; and after removing the residual solvent on the surface of the solidified film, immersing the solidified film into a coagulating bath of water again for 36 hours, taking out, and naturally airing at room temperature to obtain the temperature response separation film, wherein the surface microscopic morphology of the temperature response separation film is shown in figure 1.
Test case
The test example was conducted to examine pure water flux performance at different temperatures of the temperature responsive separation membrane of example 1, and the results are shown in table 1.
TABLE 1
| Pure water flux (LMH) at 25 DEG C | Pure water flux (LMH) at 35 DEG C | |
| Example 1 | 24.36(±0.59) | 37.84(±1.18) |
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.
Claims (10)
1. A temperature responsive separation membrane, characterized in that the temperature responsive separation membrane comprises the following components in parts by weight: 12-20 parts of polymer film material, 60-85 parts of polar solvent, 0.5-2 parts of temperature control reagent, 6-10 parts of polymer pore-forming agent and 0.5-2 parts of additive.
2. The temperature-responsive separation membrane of claim 1, wherein the temperature-responsive separation membrane comprises, in parts by weight: 15-20 parts of polymer film material, 65-82 parts of polar solvent, 0.5-1.5 parts of temperature control reagent, 7-9 parts of polymer pore-forming agent and 0.5-1.5 parts of additive.
3. The temperature-responsive separation membrane according to claim 1 or 2, wherein,
the polymer film material is polyvinylidene fluoride and/or polytetrafluoroethylene;
the polar solvent is dimethylacetamide and/or N-methylpyrrolidone;
the temperature control reagent is N isopropyl acrylamide;
the high molecular pore-forming agent is polyvinylpyrrolidone with a polymerization degree of K15-K90;
the additive is glycerol and/or cellulose acetate.
4. A temperature responsive separation membrane according to claim 3, wherein the polymeric pore forming agent is polyvinylpyrrolidone PVPK-15 and/or polyvinylpyrrolidone PVPK-30.
5. The method for producing a temperature-responsive separation membrane according to any one of claims 1 to 4, comprising the steps of:
s1: mixing and stirring the polar solvent, the temperature control reagent and the macromolecule pore-forming agent uniformly to obtain a mixed solution;
s2: drying the polymer film material to constant weight to obtain dried polymer film material powder, mixing and stirring the dried polymer film material powder, the mixed solution and the additive uniformly to obtain film casting solution, and sealing, standing and defoaming the film casting solution;
s3: the defoamed casting solution is coated on non-woven fabrics in a scraping way, and after a first preset time, the non-woven fabrics coated with the casting solution in a scraping way are immersed in a coagulating bath of water for curing, so that a cured film is obtained; and after removing the residual solvent on the surface of the solidified film, immersing the solidified film into a coagulating bath of water again for a second preset time, taking out and naturally airing to obtain the temperature response separation film.
6. The method for producing a temperature-responsive separation membrane according to claim 5, wherein in step S1, the stirring time is 7 to 10 hours, and the stirring rate is 100rpm to 150rpm.
7. The method for producing a temperature-responsive separation membrane according to claim 5, wherein, in step S2, the stirring speed is 150rpm to 250rpm.
8. The method for producing a temperature-responsive separation membrane according to claim 7, wherein the step S2 is performed at 15 to 30 ℃.
9. The method for producing a temperature-responsive separation membrane according to claim 5, wherein, in step S3:
the thickness of the scraper used for the blade coating is 100-2000 mu m;
the first preset time is 15-45s;
removing the residual solvent on the surface of the cured film by water washing;
the second preset time is 24-48h.
10. The method for producing a temperature-responsive separation membrane according to claim 9, wherein the step S3 is performed at 15-30 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311753984.6A CN117531383A (en) | 2023-12-19 | 2023-12-19 | Temperature response separation membrane and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311753984.6A CN117531383A (en) | 2023-12-19 | 2023-12-19 | Temperature response separation membrane and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117531383A true CN117531383A (en) | 2024-02-09 |
Family
ID=89790094
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311753984.6A Pending CN117531383A (en) | 2023-12-19 | 2023-12-19 | Temperature response separation membrane and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117531383A (en) |
-
2023
- 2023-12-19 CN CN202311753984.6A patent/CN117531383A/en active Pending
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