CN111939773A - Preparation method of PVDF (polyvinylidene fluoride) film - Google Patents
Preparation method of PVDF (polyvinylidene fluoride) film Download PDFInfo
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- CN111939773A CN111939773A CN202010830210.9A CN202010830210A CN111939773A CN 111939773 A CN111939773 A CN 111939773A CN 202010830210 A CN202010830210 A CN 202010830210A CN 111939773 A CN111939773 A CN 111939773A
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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
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
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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
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/20—By influencing the flow
- B01D2321/2066—Pulsated flow
- B01D2321/2075—Ultrasonic treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/04—Characteristic thickness
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
Abstract
A preparation method of a PVDF film comprises the following specific steps: s1, adding an absolute ethyl alcohol solution and a strong base solution into the PVDF powder; s2, heating and stirring the solution, filtering, adjusting the pH value, filtering, washing and drying to obtain powder; s3, adding N-N dimethylformamide, acrylic acid and azobisisobutyronitrile into the powder under the nitrogen atmosphere, mixing, and performing suction filtration, washing and drying to obtain modified powder; s4, adding polyoxyethylene and dopamine into the powder, and stirring; s5, defoaming the solution, uniformly coating the defoamed solution on the surface of a flat plate, and curing and forming to obtain a filter membrane; s7, activating the surface of the filter membrane in a plasma environment; and (3) carrying out grafting reaction on the gaseous DMAA and the surface of the filter membrane in a vacuum state, and then reacting with 4-bromobutyric acid to obtain the PVDF modified filter membrane. The preparation method of the PVDF film provided by the invention is simple to operate and can obtain the high-performance PVDF film.
Description
Technical Field
The invention relates to the technical field of PVDF film preparation, in particular to a preparation method of a PVDF film.
Background
About 97% of the water on earth is seawater, and fresh water only occupies 2.5% of the total water reserve of the ball; the problems of economic development, population growth, environmental pollution and the like generate great demand on fresh water resources, and the shortage of water resources and increasingly serious water pollution become bottlenecks which restrict social progress and economic development. The ultrafiltration technology has high removal rate on turbid liquid, organic substances (such as humus substances), giardia lamblia, viruses and the like due to simple operation and easy automation, and is widely considered as a very promising technology in the aspect of drinking water production; polyvinylidene fluoride (PVDF for short) which is one of ultrafiltration membrane materials has great potential in the application field of separation membranes due to excellent heat resistance, mechanical property, radiation resistance, chemical stability and the like; because fluorine atoms are symmetrically distributed, the whole molecule shows non-polarity, the surface energy of the polymer is very low, and thus, the PVDF filter membrane has weak anti-pollution capability and is easy to generate membrane pollution. Membrane fouling shortens the use of filtration membranes; therefore, the application provides a preparation method of the PVDF film.
Disclosure of Invention
Objects of the invention
In order to solve the technical problems in the background art, the invention provides a preparation method of a PVDF film, which is simple to operate and can obtain the PVDF film with strong hydrophilicity and good stain resistance.
(II) technical scheme
In order to solve the problems, the invention provides a preparation method of a PVDF film, which comprises the following specific steps:
s1, adding an absolute ethyl alcohol solution into the PVDF powder to obtain a mixed solution A; stirring the mixed solution A and adding a certain amount of strong base solution to obtain mixed solution B;
s2, heating the mixed solution B to 45-65 ℃, stirring at the speed of 80-120 r/mim for 10-20 min, performing suction filtration, and adjusting the pH of the mixed solution B to 7 to obtain a mixed solution C;
s3, carrying out suction filtration, washing and drying on the mixed solution C to obtain PVDF pretreated powder D;
s4, adding N-N dimethylformamide, acrylic acid and azobisisobutyronitrile into the PVDF pretreated powder D under the nitrogen atmosphere, and uniformly mixing at 60-80 ℃ to obtain a mixture E; wherein the mixing time is 20-40 min;
s5, carrying out suction filtration, washing and drying on the mixture E to obtain modified PVDF powder F;
s6, adding polyoxyethylene and dopamine into the modified PVDF powder F, and uniformly stirring to obtain a mixed solution G;
s6, defoaming the mixed solution G, uniformly coating the mixed solution G on the surface of a flat plate by using a film scraping rod, curing and molding the flat plate in water, and molding the mixed solution G on the surface of the flat plate to obtain a PVDF filter membrane H;
s7, activating the surface of the PVDF filter membrane H in a plasma environment; and (3) carrying out grafting reaction on gaseous DMAA and the surface of the PVDF filter membrane in a vacuum state, and then reacting with 4-bromobutyric acid to obtain the PVDF modified filter membrane I.
Preferably, the mass ratio of the PVDF powder to the absolute ethyl alcohol solution in S1 is 1: 15-23.
Preferably, the strong alkali solution in S1 is potassium hydroxide solution.
Preferably, the mixed solution A in S1 is added with strong alkali solution, heated to 50-75 ℃, and stirred at the speed of 80-150 r/min for 10-25 min.
Preferably, the mass ratio of the PVDF pre-treatment powder D, N-N dimethylformamide, acrylic acid and azobisisobutyronitrile in S4 is as follows: 3-13: 80-130: 12-17: 0.2 to 0.7.
Preferably, the mass ratio of the polyoxyethylene to the dopamine in S6 is 1: 0.4-3.7.
Preferably, the time for placing the flat plate in water for curing and forming in S6 is 22-36 h.
Preferably, the thickness of the PVDF filter membrane H in S6 is 100-300 μm.
Preferably, the processing power under the plasma environment is 8-25W, and the processing time is 20-150 s;
the power of the grafting reaction is 8-25W, and the reaction time is 40-200 s.
Preferably, the PVDF filter membrane H and the PVDF modified filter membrane I are washed before the activation of the PVDF filter membrane H and after the PVDF modified filter membrane I is obtained.
The technical scheme of the invention has the following beneficial technical effects:
the preparation method of the PVDF film provided by the invention does not need special equipment, and the implementation process of the PVDF film is simple and easy to control, so that the preparation method is worthy of popularization; the obtained PVDF film has strong hydrophilicity, stable physical performance, good pollution resistance and stable sewage treatment effect; the thickness of the prepared PVDF film is controlled to be 100-300 mu m, and the surface area of the PVDF film is greatly improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Example 1
The preparation method of the PVDF film provided by the invention comprises the following specific steps:
s1, adding an absolute ethyl alcohol solution into the PVDF powder to obtain a mixed solution A; stirring the mixed solution A and adding a certain amount of strong base solution to obtain mixed solution B;
s2, heating the mixed solution B to 45, stirring for 10min at the speed of 80r/mim, performing suction filtration, and adjusting the pH value of the mixed solution B to 7 to obtain a mixed solution C;
s3, carrying out suction filtration, washing and drying on the mixed solution C to obtain PVDF pretreated powder D;
s4, adding N-N dimethylformamide, acrylic acid and azobisisobutyronitrile into the PVDF pretreated powder D under the nitrogen atmosphere, and uniformly mixing at 60 ℃ to obtain a mixture E; wherein the mixing time is 20 min;
s5, carrying out suction filtration, washing and drying on the mixture E to obtain modified PVDF powder F;
s6, adding polyoxyethylene and dopamine into the modified PVDF powder F, and uniformly stirring to obtain a mixed solution G;
s6, defoaming the mixed solution G, uniformly coating the mixed solution G on the surface of a flat plate by using a film scraping rod, curing and molding the flat plate in water, and molding the mixed solution G on the surface of the flat plate to obtain a PVDF filter membrane H;
s7, activating the surface of the PVDF filter membrane H in a plasma environment; and (3) carrying out grafting reaction on gaseous DMAA and the surface of the PVDF filter membrane in a vacuum state, and then reacting with 4-bromobutyric acid to obtain the PVDF modified filter membrane I.
In an alternative embodiment, the mass ratio of the PVDF powder to the absolute ethanol solution in S1 is 1: 15.
In an alternative embodiment, the strong alkali solution in S1 is potassium hydroxide solution.
In an alternative embodiment, mixed liquor A in S1 is heated to 50 ℃ after adding strong alkali solution, and stirred for 10min at the speed of 80 r/min.
In an alternative embodiment, the mass ratio of the PVDF pre-treatment powder D, N-N dimethylformamide, acrylic acid and azobisisobutyronitrile in S4 is: 3:80:12: 0.2.
in an alternative embodiment, the mass ratio of polyethylene oxide to dopamine in S6 is 1: 0.4.
In an alternative embodiment, the time for setting and forming the flat plate in water in S6 is 22 h.
In an alternative embodiment, the PVDF membrane H in S6 has a thickness of 100 μm.
In an alternative embodiment, the processing power in the plasma environment is 8W, and the processing time is 20 s;
the grafting reaction power was 8W and the reaction time was 40 s.
In an optional embodiment, the PVDF filter membrane H and the PVDF-modified filter membrane I are cleaned before the activation of the PVDF filter membrane H and after the PVDF-modified filter membrane I is obtained; wherein, both the PVDF filter membrane H and the PVDF modified filter membrane I adopt absolute ethyl alcohol and deionized water for ultrasonic cleaning.
Example 2
The preparation method of the PVDF film provided by the invention comprises the following specific steps:
s1, adding an absolute ethyl alcohol solution into the PVDF powder to obtain a mixed solution A; stirring the mixed solution A and adding a certain amount of strong base solution to obtain mixed solution B;
s2, heating the mixed solution B to 52 ℃, stirring for 14min at the speed of 95r/mim, performing suction filtration, and adjusting the pH value of the mixed solution B to 7 to obtain a mixed solution C;
s3, carrying out suction filtration, washing and drying on the mixed solution C to obtain PVDF pretreated powder D;
s4, adding N-N dimethylformamide, acrylic acid and azobisisobutyronitrile into the PVDF pretreated powder D under the nitrogen atmosphere, and uniformly mixing at 67 ℃ to obtain a mixture E; wherein the mixing time is 28 min;
s5, carrying out suction filtration, washing and drying on the mixture E to obtain modified PVDF powder F;
s6, adding polyoxyethylene and dopamine into the modified PVDF powder F, and uniformly stirring to obtain a mixed solution G;
s6, defoaming the mixed solution G, uniformly coating the mixed solution G on the surface of a flat plate by using a film scraping rod, curing and molding the flat plate in water, and molding the mixed solution G on the surface of the flat plate to obtain a PVDF filter membrane H;
s7, activating the surface of the PVDF filter membrane H in a plasma environment; and (3) carrying out grafting reaction on gaseous DMAA and the surface of the PVDF filter membrane in a vacuum state, and then reacting with 4-bromobutyric acid to obtain the PVDF modified filter membrane I.
In an alternative embodiment, the mass ratio of the PVDF powder to the absolute ethanol solution in S1 is 1: 18.
In an alternative embodiment, the strong alkali solution in S1 is potassium hydroxide solution.
In an alternative embodiment, the temperature of mixed liquor A in S1 is raised to 62 ℃ after adding the strong base solution, and the mixed liquor is stirred for 17min at the speed of 100 r/min.
In an alternative embodiment, the mass ratio of the PVDF pre-treatment powder D, N-N dimethylformamide, acrylic acid and azobisisobutyronitrile in S4 is: 5:108:14: 0.5.
in an alternative embodiment, the mass ratio of polyethylene oxide to dopamine in S6 is 1: 1.8.
In an alternative embodiment, the time for setting and forming the flat plate in water in S6 is 24 h.
In an alternative embodiment, the PVDF membrane H in S6 has a thickness of 160 μm.
In an alternative embodiment, the processing power in the plasma environment is 15W, and the processing time is 60 s;
the grafting reaction power was 15W and the reaction time was 80 s.
In an optional embodiment, the PVDF filter membrane H and the PVDF-modified filter membrane I are cleaned before the activation of the PVDF filter membrane H and after the PVDF-modified filter membrane I is obtained; wherein, both the PVDF filter membrane H and the PVDF modified filter membrane I adopt absolute ethyl alcohol and deionized water for ultrasonic cleaning.
Example 3
The preparation method of the PVDF film provided by the invention comprises the following specific steps:
s1, adding an absolute ethyl alcohol solution into the PVDF powder to obtain a mixed solution A; stirring the mixed solution A and adding a certain amount of strong base solution to obtain mixed solution B;
s2, heating the mixed solution B to 60 ℃, stirring for 18min at the speed of 110r/mim, performing suction filtration, and adjusting the pH value of the mixed solution B to 7 to obtain a mixed solution C;
s3, carrying out suction filtration, washing and drying on the mixed solution C to obtain PVDF pretreated powder D;
s4, adding N-N dimethylformamide, acrylic acid and azobisisobutyronitrile into the PVDF pretreated powder D under the nitrogen atmosphere, and uniformly mixing at 75 ℃ to obtain a mixture E; wherein the mixing time is 20-35 min;
s5, carrying out suction filtration, washing and drying on the mixture E to obtain modified PVDF powder F;
s6, adding polyoxyethylene and dopamine into the modified PVDF powder F, and uniformly stirring to obtain a mixed solution G;
s6, defoaming the mixed solution G, uniformly coating the mixed solution G on the surface of a flat plate by using a film scraping rod, curing and molding the flat plate in water, and molding the mixed solution G on the surface of the flat plate to obtain a PVDF filter membrane H;
s7, activating the surface of the PVDF filter membrane H in a plasma environment; and (3) carrying out grafting reaction on gaseous DMAA and the surface of the PVDF filter membrane in a vacuum state, and then reacting with 4-bromobutyric acid to obtain the PVDF modified filter membrane I.
In an alternative embodiment, the mass ratio of the PVDF powder to the absolute ethanol solution in S1 is 1: 20.
In an alternative embodiment, the strong alkali solution in S1 is potassium hydroxide solution.
In an alternative embodiment, mixed liquor A in S1 is heated to 70 ℃ after adding strong alkali solution, and stirred for 22min at the speed of 120 r/min.
In an alternative embodiment, the mass ratio of the PVDF pre-treatment powder D, N-N dimethylformamide, acrylic acid and azobisisobutyronitrile in S4 is: 7:119:15: 0.6.
in an alternative embodiment, the mass ratio of polyethylene oxide to dopamine in S6 is 1: 2.5.
In an alternative embodiment, the time for setting and forming the flat plate in water in S6 is 30 h.
In an alternative embodiment, the PVDF membrane H in S6 has a thickness of 240 μm.
In an alternative embodiment, the processing power in the plasma environment is 20W, and the processing time is 100 s;
the grafting reaction power was 20W and the reaction time was 120 s.
In an optional embodiment, the PVDF filter membrane H and the PVDF-modified filter membrane I are cleaned before the activation of the PVDF filter membrane H and after the PVDF-modified filter membrane I is obtained; wherein, both the PVDF filter membrane H and the PVDF modified filter membrane I adopt absolute ethyl alcohol and deionized water for ultrasonic cleaning.
Example 4
The preparation method of the PVDF film provided by the invention comprises the following specific steps:
s1, adding an absolute ethyl alcohol solution into the PVDF powder to obtain a mixed solution A; stirring the mixed solution A and adding a certain amount of strong base solution to obtain mixed solution B;
s2, heating the mixed solution B to 65 ℃, stirring at the speed of 120r/mim for 20min, performing suction filtration, and adjusting the pH value of the mixed solution B to 7 to obtain a mixed solution C;
s3, carrying out suction filtration, washing and drying on the mixed solution C to obtain PVDF pretreated powder D;
s4, adding N-N dimethylformamide, acrylic acid and azobisisobutyronitrile into the PVDF pretreated powder D under the nitrogen atmosphere, and uniformly mixing at 80 ℃ to obtain a mixture E; wherein the mixing time is 40 min;
s5, carrying out suction filtration, washing and drying on the mixture E to obtain modified PVDF powder F;
s6, adding polyoxyethylene and dopamine into the modified PVDF powder F, and uniformly stirring to obtain a mixed solution G;
s6, defoaming the mixed solution G, uniformly coating the mixed solution G on the surface of a flat plate by using a film scraping rod, curing and molding the flat plate in water, and molding the mixed solution G on the surface of the flat plate to obtain a PVDF filter membrane H;
s7, activating the surface of the PVDF filter membrane H in a plasma environment; and (3) carrying out grafting reaction on gaseous DMAA and the surface of the PVDF filter membrane in a vacuum state, and then reacting with 4-bromobutyric acid to obtain the PVDF modified filter membrane I.
In an alternative embodiment, the mass ratio of the PVDF powder to the absolute ethanol solution in S1 is 1: 23.
In an alternative embodiment, the strong alkali solution in S1 is potassium hydroxide solution.
In an alternative embodiment, the temperature of mixed liquor A in S1 is raised to 75 ℃ after adding the strong base solution, and the mixed liquor is stirred for 25min at the speed of 150 r/min.
In an alternative embodiment, the mass ratio of the PVDF pre-treatment powder D, N-N dimethylformamide, acrylic acid and azobisisobutyronitrile in S4 is: 13:130:17: 0.7.
in an alternative embodiment, the mass ratio of polyethylene oxide to dopamine in S6 is 1: 3.7.
In an alternative embodiment, the time for setting and forming the flat plate in water in S6 is 36 h.
In an alternative embodiment, the PVDF membrane H in S6 has a thickness of 300. mu.m.
In an alternative embodiment, the processing power in the plasma environment is 25W, and the processing time is 150 s;
the grafting reaction power was 25W and the reaction time was 200 s.
In an optional embodiment, the PVDF filter membrane H and the PVDF-modified filter membrane I are cleaned before the activation of the PVDF filter membrane H and after the PVDF-modified filter membrane I is obtained; wherein, both the PVDF filter membrane H and the PVDF modified filter membrane I adopt absolute ethyl alcohol and deionized water for ultrasonic cleaning.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (10)
1. The preparation method of the PVDF film is characterized by comprising the following specific steps:
s1, adding an absolute ethyl alcohol solution into the PVDF powder to obtain a mixed solution A; stirring the mixed solution A and adding a certain amount of strong base solution to obtain mixed solution B;
s2, heating the mixed solution B to 45-65 ℃, stirring at the speed of 80-120 r/mim for 10-20 min, performing suction filtration, and adjusting the pH of the mixed solution B to 7 to obtain a mixed solution C;
s3, carrying out suction filtration, washing and drying on the mixed solution C to obtain PVDF pretreated powder D;
s4, adding N-N dimethylformamide, acrylic acid and azobisisobutyronitrile into the PVDF pretreated powder D under the nitrogen atmosphere, and uniformly mixing at 60-80 ℃ to obtain a mixture E; wherein the mixing time is 20-40 min;
s5, carrying out suction filtration, washing and drying on the mixture E to obtain modified PVDF powder F;
s6, adding polyoxyethylene and dopamine into the modified PVDF powder F, and uniformly stirring to obtain a mixed solution G;
s6, defoaming the mixed solution G, uniformly coating the mixed solution G on the surface of a flat plate by using a film scraping rod, curing and molding the flat plate in water, and molding the mixed solution G on the surface of the flat plate to obtain a PVDF filter membrane H;
s7, activating the surface of the PVDF filter membrane H in a plasma environment; and (3) carrying out grafting reaction on gaseous DMAA and the surface of the PVDF filter membrane in a vacuum state, and then reacting with 4-bromobutyric acid to obtain the PVDF modified filter membrane I.
2. The method for preparing the PVDF film as claimed in claim 1, wherein the mass ratio of the PVDF powder to the absolute ethyl alcohol solution in S1 is 1: 15-23.
3. The method of claim 1, wherein the strong alkali solution of S1 is potassium hydroxide solution.
4. The method for preparing PVDF film as defined in claim 1, wherein the temperature of the mixed solution A in S1 is raised to 50-75 ℃ after adding strong alkali solution, and the mixed solution is stirred at 80-150 r/min for 10-25 min.
5. The method of claim 1, wherein the mass ratio of the PVDF pre-treatment powder D, N-N dimethylformamide, acrylic acid and azobisisobutyronitrile in S4 is: 3-13: 80-130: 12-17: 0.2 to 0.7.
6. The method for preparing the PVDF film as claimed in claim 1, wherein the mass ratio of the polyoxyethylene to the dopamine in S6 is 1: 0.4-3.7.
7. The method of claim 1, wherein the time for setting the flat plate in water in S6 is 22-36 h.
8. The method of claim 1, wherein the thickness of the PVDF membrane H in S6 is 100-300 μm.
9. The method for preparing a PVDF film as defined in claim 1, wherein the processing power in plasma environment is 8-25W, the processing time is 20-150 s;
the power of the grafting reaction is 8-25W, and the reaction time is 40-200 s.
10. The method of claim 1, wherein the PVDF membrane H and the PVDF-modified membrane I are washed before activation and after obtaining the PVDF-modified membrane I.
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