CN115608166A - Preparation method and application of super-hydrophobic membrane with high-temperature self-repairing performance - Google Patents

Preparation method and application of super-hydrophobic membrane with high-temperature self-repairing performance Download PDF

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CN115608166A
CN115608166A CN202211313608.0A CN202211313608A CN115608166A CN 115608166 A CN115608166 A CN 115608166A CN 202211313608 A CN202211313608 A CN 202211313608A CN 115608166 A CN115608166 A CN 115608166A
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membrane
super
film
hydrophobic
temperature self
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李正
牟航葵
刘禹霄
张兰河
李连杰
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Northeast Electric Power University
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Northeast Dianli University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/08—Thin film evaporation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/38—Hydrophobic membranes

Abstract

A preparation method and application of a super-hydrophobic membrane with high-temperature self-repairing performance relate to a preparation method and application of a super-hydrophobic membrane. The invention aims to solve the problems that the existing super-hydrophobic membrane for membrane distillation can cause the reduction of membrane flux and the great increase of the conductivity of permeate liquid after long-time operation, and the water treatment performance of the membrane can be reduced or even the membrane can not be continuously operated after acid cleaning. The method comprises the following steps: 1. performing Fenton reaction pretreatment; 2. preparing a bottom super-hydrophobic layer; 3. preparing a PVA middle layer; 4. preparing a top super-hydrophobic layer. A super-hydrophobic membrane with high-temperature self-repairing performance is used as a membrane for membrane distillation. The membrane with high-temperature self-repairing performance prepared by the invention has high super-hydrophobic performance and self-repairing performance. The invention can obtain the super-hydrophobic membrane with high-temperature self-repairing performance.

Description

Preparation method and application of super-hydrophobic membrane with high-temperature self-repairing performance
Technical Field
The invention relates to a preparation method and application of a super-hydrophobic membrane.
Background
The Membrane Distillation (MD) technology is a high-efficiency separation technology integrating the evaporation and membrane separation processes. In the face of the increasing shortage of water resources, the membrane distillation technology has the advantages of simple process, convenience in operation, low power consumption and the like, the steam pressure difference on two sides of the microporous hydrophobic membrane is used as a driving force, the hot side of the membrane is directly contacted with feed liquid, water in hot feed liquid is evaporated into steam on the membrane surface and then enters the cold side through membrane holes to be condensed, and other solute molecules cannot pass through the membrane, so that the separation or purification of a mixture is realized.
Due to the flow of the membrane distillation process, microporous hydrophobic membranes must be used as membranes for membrane distillation. The stronger the hydrophobicity, the more difficult the contaminants in the feed liquid will adhere to the membrane surface, thereby greatly increasing the run time. When the static contact angle of the film surface with water exceeds 150 ° and the rolling contact angle is less than 10 °, the film may be referred to as an ultrahydrophobic film. Due to the excellent resistance and self-cleaning performance of the super-hydrophobic membrane, the flux reduction caused by membrane pore wetting and membrane surface pollution can be better avoided. However, the superhydrophobic membrane is also contaminated to some extent after a long time operation, and a decrease in membrane flux and a large increase in the conductivity of the permeate occur. The membrane surface is cleaned by acid cleaning and other methods to effectively recover the membrane performance, but the water treatment performance of the membrane after cleaning is correspondingly reduced, even the membrane cannot be continuously operated.
Disclosure of Invention
The invention aims to solve the problems that the existing super-hydrophobic membrane for membrane distillation has reduced membrane flux and greatly increased conductivity of permeate liquid after long-time operation, and the water treatment performance of the membrane is reduced even the membrane cannot be continuously operated after acid cleaning, and provides a preparation method and application of the super-hydrophobic membrane with high-temperature self-repairing performance.
A preparation method of a super-hydrophobic membrane with high-temperature self-repairing performance is specifically completed according to the following steps:
1. pretreatment of Fenton reaction:
immersing PVDF-based membrane into FeSO 4 ·7H 2 O、H 2 O 2 Carrying out Fenton reaction under the heating condition in a mixed solution of absolute ethyl alcohol and deionized water, cleaning the PVDF base membrane by using sulfuric acid, and finally carrying out vacuum drying to obtain the pretreated PVDF base membrane;
2. preparing a bottom super-hydrophobic layer:
(1) firstly, siO is mixed 2 Dissolving the nano particles in cyclohexane, magnetically stirring, ultrasonically dispersing, dripping 1H,2H and 2H-perfluoro octyl trichlorosilane, and continuously ultrasonically dispersing to obtain PFTS/SiO 2 A solution;
(2) immersing the pretreated PVDF basal membrane into PFTS/SiO 2 Taking out the solution, and then drying the solution in vacuum to obtain a composite film containing the bottom super-hydrophobic layer;
3. preparing a PVA intermediate layer:
(1) mixing polyvinyl alcohol and deionized water, stirring under a heating condition, and adding absolute ethyl alcohol to obtain a mixed solution;
(2) uniformly casting the mixed solution onto a composite film containing a bottom super-hydrophobic layer, controlling the thickness of the mixed solution on the bottom super-hydrophobic layer by using a film coater, and finally drying at room temperature to obtain the composite film containing the PVA intermediate layer;
4. preparing a top super-hydrophobic layer:
PFTS/SiO using a spray gun 2 And spraying the solution on the surface of the composite membrane containing the PVA intermediate layer, standing, and then performing forced air drying to obtain the super-hydrophobic membrane with high-temperature self-repairing performance.
A super-hydrophobic membrane with high-temperature self-repairing performance is used as a membrane for membrane distillation.
The principle of the invention is as follows:
the invention uses PFTS (1H, 2H-perfluorooctyltrichlorosilane) to fluorinate SiO 2 Nano particles grafted on the surface of the membrane to reduce the surface energy, PVA dissolved in water at high temperature and ethanol as auxiliary material to prepare the intermediate layer, and fluorinated SiO 2 The solution is sprayed on the surface of the membrane by a spray deposition method to prepare the super-hydrophobic membrane with high-temperature self-repairing performance. PVA as an organic compound is soluble in an aqueous environment at 85 ℃ or higherWhen the super-hydrophobic surface of the surface layer is polluted or damaged, the super-hydrophobic surface of the surface layer is rubbed off by abrasive paper, and then the super-hydrophobic surface is treated for 30min in a water environment with the temperature of more than 85 ℃, so that the PVA layer is dissolved, and the super-hydrophobic layer on the surface of the bottom layer film is exposed, and the hydrophobic property of the super-hydrophobic layer is recovered. The polyvinyl alcohol film can permeate water vapor but hardly permeates alcohol vapor, and further cannot permeate organic solvent vapor, inert gas and the like, and the water-soluble temperature of the high-temperature water-soluble polyvinyl alcohol film is more than 85 ℃ and 60 ℃ higher than the hot-side temperature of the conventional film distillation process, so that the polyvinyl alcohol film is suitable for the modification process of the film for film distillation. Compared with the method of modifying the surface of the membrane by only using fluorosilane, the membrane with high-temperature self-repairing performance prepared by the invention has higher super-hydrophobic performance and self-repairing performance. The invention provides a preparation method of a super-hydrophobic film with high-temperature self-repairing performance.
The invention has the advantages that:
1. the invention mainly aims to solve the problem of poor durability in conventional membrane super-hydrophobic modification in the membrane distillation technology, and provides a preparation method of a super-hydrophobic membrane with high-temperature self-repairing performance 2 Grafting modification is carried out on the surface of the membrane, the PVA (polyvinyl alcohol) is used for casting the surface of the membrane to form a PVA layer, and then the fluorinated SiO is sprayed and deposited by a spray gun 2 Spraying the solution on a PVA layer on the surface of the membrane to prepare a P-P-S self-repairing super-hydrophobic membrane (a super-hydrophobic membrane with high-temperature self-repairing performance); due to the characteristic that PVA is soluble in water at high temperature, compared with an untreated PVDF base membrane, the P-P-S self-repairing membrane has excellent hydrophobic property and high-temperature self-repairing property; after the surface layer of the membrane is damaged, at the high temperature of more than 85 ℃, PVA is dissolved in water, the super-hydrophobic surface at the bottom is exposed, and the hydrophobicity of the membrane is recovered;
2. the method is simple to operate, improves the hydrophobicity and the durability of the membrane surface, and is beneficial to long-time and repeated operation in the membrane separation process;
3. the super-hydrophobic membrane with high-temperature self-repairing performance has stable water flux in the initial operation process, and the water flux is improved to a certain extent due to the reduction of the overall thickness of the membrane after the self-repairing process is finished.
Drawings
FIG. 1 is a process for preparing a superhydrophobic film having high temperature self-repairing properties and a self-repairing process in example 1;
fig. 2 is a contact angle in which (a) is a contact angle of the super-hydrophobic layer on top of the super-hydrophobic film having high temperature self-repairing property prepared in example 1, (b) is a contact angle after the super-hydrophobic layer on top of the super-hydrophobic film having high temperature self-repairing property prepared in example 1 is damaged, and (c) is a contact angle after the super-hydrophobic film having high temperature self-repairing property prepared in example 1 is repaired at high temperature;
FIG. 3 is an SEM image of a bottom super-hydrophobic layer on a composite film containing the bottom super-hydrophobic layer prepared in step two (2) of example 1;
FIG. 4 is an SEM photograph of a PVA intermediate layer on a composite membrane containing the PVA intermediate layer prepared in step three (2) of example 1;
FIG. 5 is an SEM image of a top super-hydrophobic layer on a super-hydrophobic film with high temperature self-repairing properties prepared in step four of example 1;
FIG. 6 is a water flux chart in which 1 is the water flux of the superhydrophobic film having high temperature self-repairing property prepared in the fourth step of example 1, and 2 is the water flux of the superhydrophobic film having high temperature self-repairing property prepared in example 1 after high temperature repairing;
fig. 7 is a permeate conductivity graph, in which 1 is the permeate conductivity of the super-hydrophobic film with high-temperature self-repairing performance prepared in the fourth step of example 1, and 2 is the permeate conductivity of the super-hydrophobic film with high-temperature self-repairing performance prepared in example 1 after high-temperature repairing.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, steps or conditions of the present invention may be made without departing from the spirit of the invention.
The first embodiment is as follows: the embodiment provides a preparation method of a super-hydrophobic film with high-temperature self-repairing performance, which is specifically completed according to the following steps:
1. fenton reaction pretreatment:
immersing PVDF-based film in FeSO 4 ·7H 2 O、H 2 O 2 Carrying out Fenton reaction under the heating condition in a mixed solution of absolute ethyl alcohol and deionized water, cleaning the PVDF base membrane by using sulfuric acid, and finally carrying out vacuum drying to obtain the pretreated PVDF base membrane;
2. preparing a bottom super-hydrophobic layer:
(1) firstly, siO is mixed 2 Dissolving nano particles in cyclohexane, magnetically stirring, ultrasonically dispersing, dripping 1H,2H and 2H-perfluoro octyl trichlorosilane, and continuously ultrasonically dispersing to obtain PFTS/SiO 2 A solution;
(2) immersing the pretreated PVDF basal membrane into PFTS/SiO 2 Taking out the solution, and then drying the solution in vacuum to obtain a composite film containing the bottom super-hydrophobic layer;
3. preparing a PVA intermediate layer:
(1) mixing polyvinyl alcohol and deionized water, stirring under a heating condition, and adding absolute ethyl alcohol to obtain a mixed solution;
(2) uniformly casting the mixed solution onto a composite film containing a bottom super-hydrophobic layer, controlling the thickness of the mixed solution on the bottom super-hydrophobic layer by using a film coater, and finally drying at room temperature to obtain the composite film containing the PVA intermediate layer;
4. preparing a top super-hydrophobic layer:
PFTS/SiO using a spray gun 2 And spraying the solution on the surface of the composite membrane containing the PVA intermediate layer, standing, and then performing forced air drying to obtain the super-hydrophobic membrane with high-temperature self-repairing performance.
The second embodiment is as follows: the first difference between the present embodiment and the present embodiment is: feSO described in step one 4 ·7H 2 Mass of O and H 2 O 2 The volume ratio of (1 g-2 g) to (5 mL-7 mL); h in the step one 2 O 2 The volume ratio of the absolute ethyl alcohol to the deionized water is (5-7) to (40-60). It is provided withThe steps are the same as those in the first embodiment.
The third concrete implementation mode: the difference between this embodiment and the first or second embodiment is: h in the step one 2 O 2 The mass fraction of (A) is 30%; the temperature of the Fenton reaction in the step one is 40-60 ℃, and the time of the Fenton reaction is 1-2 h; the mass fraction of the sulfuric acid in the step one is 98%; the temperature of the vacuum drying in the first step is 60-80 ℃. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode is as follows: the difference between this embodiment and one of the first to third embodiments is as follows: siO described in step two (1) 2 The mass ratio of the nano particles to the 1H, 2H-perfluorooctyltrichlorosilane to the cyclohexane is 1 (1-2) to 50. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the magnetic stirring speed in the step two (1) is 40 r/min-60 r/min, and the magnetic stirring time is 20 min-40 min; the ultrasonic dispersion time in the step two (1) is 15min to 25min, and the ultrasonic dispersion power is 350W to 500W. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: in the second step (2), the pretreated PVDF basement membrane is immersed into PFTS/SiO 2 The solution is kept for 3 to 5 hours; the temperature of the vacuum drying in the second step (2) is 60-80 ℃. The other steps are the same as those in the first to fifth embodiments.
The seventh concrete implementation mode: the difference between this embodiment and the first to sixth embodiments is: the mass ratio of the polyvinyl alcohol to the deionized water in the step three (1) is 1 (6-8); the volume ratio of the mass of the polyvinyl alcohol to the absolute ethyl alcohol in the step three (1) is (1 g-2 g) 1mL; the stirring temperature in the step three (1) is 70-80 ℃, and the stirring time is 1-2 h. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and the first to seventh embodiments is: and step three (2), controlling the thickness of the mixed solution on the super-hydrophobic composite membrane to be 400-600 mu m by using a coating device. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: the spraying pressure in the step four is 0.2MPa to 0.6MPa, the spraying distance is 10cm to 17cm, and the spraying is performed and then the mixture is kept stand for 20min to 40min; the temperature of the forced air drying in the fourth step is 60-70 ℃, and the time of the forced air drying is 3-5 h. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment is a superhydrophobic film having high-temperature self-repairing performance used as a film for membrane distillation.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1: a preparation method of a super-hydrophobic membrane with high-temperature self-repairing performance is specifically completed according to the following steps:
1. fenton reaction pretreatment:
PVDF-based film was immersed in 1.39g FeSO 4 ·7H 2 O、6mL H 2 O 2 50mL of absolute ethyl alcohol and 50mL of deionized water, then carrying out Fenton reaction for 1h at 50 ℃, cleaning the PVDF base membrane by using sulfuric acid, and finally carrying out vacuum drying at 70 ℃ to obtain the pretreated PVDF base membrane;
h in the step one 2 O 2 The mass fraction of (A) is 30%;
the mass fraction of the sulfuric acid in the step one is 98%;
2. preparing a bottom super-hydrophobic layer:
(1) firstly, siO is added 2 Dissolving nanoparticles in cyclohexane, magnetically stirring at 40r/min for 30min, ultrasonically dispersing at 450W for 20min, adding 1H, 2H-Perfluorooctyltrichlorosilane (PFTS), and continuously ultrasonically dispersing to obtain PFTS/SiO 2 A solution;
SiO described in step two (1) 2 Nanoparticles, 1H,1The mass ratio of H, 2H-perfluorooctyltrichlorosilane to cyclohexane is 1.5;
(2) immersing the pretreated PVDF basal membrane into PFTS/SiO 2 Taking out the solution for 4 hours, and then drying the solution in vacuum at 70 ℃ to obtain a composite membrane containing the bottom super-hydrophobic layer;
3. preparing a PVA intermediate layer:
(1) mixing 1g of polyvinyl alcohol and 7g of deionized water, stirring at 80 ℃ for 1h, and adding 1mL of absolute ethyl alcohol to obtain a mixed solution;
(2) uniformly casting the mixed solution onto a composite film containing a bottom super-hydrophobic layer, controlling the thickness of the mixed solution on the bottom super-hydrophobic layer by using a film coater, and finally drying at room temperature to obtain the composite film containing the PVA intermediate layer;
controlling the thickness of the mixed solution on the super-hydrophobic composite membrane to be 500 mu m by using a membrane coater in the step three (2);
4. preparing a top super-hydrophobic layer:
PFTS/SiO using a spray gun 2 Spraying the solution on the surface of the composite membrane containing the PVA intermediate layer, standing for 30min, and then performing forced air drying at 60 ℃ for 4h to obtain a super-hydrophobic membrane (P-P-S membrane) with high-temperature self-repairing performance;
the spraying pressure in the fourth step is 0.2MPa, and the spraying distance is 10cm.
Example 2: the present example is different from example 1 in that: siO described in step two (1) 2 The mass ratio of the nanoparticles, 1H, 2H-perfluorooctyltrichlorosilane and cyclohexane is 1. The other steps and parameters were the same as in example 1.
Example 3: the present example is different from example 1 in that: the spraying pressure in the fourth step is 0.5MPa, and the spraying distance is 15cm. The other steps and parameters were the same as in example 1.
The super-hydrophobic layer on the top of the super-hydrophobic membrane with high-temperature self-repairing performance prepared in the fourth step of example 1 is rubbed off by using sandpaper, and the hydrophobicity of the membrane is greatly reduced. At the moment, the membrane body is placed in a high-temperature water environment with the temperature of more than 85 ℃, and due to the high-temperature dissolution characteristic of PVA, the PVA middle layer can be dissolved, the super-hydrophobic layer at the bottom is exposed, and the self-repairing process is realized.
FIG. 1 is a process for preparing a superhydrophobic film having high temperature self-healing properties and a self-healing process in example 1;
fig. 2 is a contact angle in which (a) is a contact angle of the super-hydrophobic layer on top of the super-hydrophobic film having a high-temperature self-repairing property prepared in example 1, (b) is a contact angle after the super-hydrophobic layer on top of the super-hydrophobic film having a high-temperature self-repairing property prepared in example 1 is damaged, and (c) is a contact angle after the super-hydrophobic film having a high-temperature self-repairing property prepared in example 1 is repaired at a high temperature;
as can be seen from fig. 2, after the high temperature self-repairing process, the static water contact angle of the surface can be restored to the original value.
FIG. 3 is an SEM image of a bottom super-hydrophobic layer on a composite membrane including the bottom super-hydrophobic layer prepared in step two (2) of example 1;
FIG. 4 is an SEM photograph of a PVA intermediate layer on a composite film containing the PVA intermediate layer prepared in step three (2) of example 1;
FIG. 5 is an SEM image of the top super-hydrophobic layer on the super-hydrophobic film with high temperature self-repairing property prepared in step four of example 1;
as can be seen from fig. 3 to 5, the superhydrophobic film with high temperature self-repairing property prepared in step four of example 1 has a three-layer hierarchical structure, and when the PVA layer is successfully prepared, the superhydrophobic surface at the bottom is covered and protected; the particle states of the top super-hydrophobic surface prepared by the spray deposition method and the bottom super-hydrophobic surface prepared by the surface grafting method are different, but the hydrophobicity of the membrane can be greatly improved.
FIG. 6 is a water flux chart in which 1 is the water flux of the superhydrophobic film having high temperature self-repairing property prepared in the fourth step of example 1, and 2 is the water flux of the superhydrophobic film having high temperature self-repairing property prepared in example 1 after high temperature repairing;
as can be seen from fig. 6: the super-hydrophobic membrane with high-temperature self-repairing performance prepared in the fourth step of the embodiment 1 not only has stable water flux in the initial operation process, but also has the water flux improved to a certain extent due to the reduction of the whole thickness of the membrane after the self-repairing process is completed.
Fig. 7 is a graph showing the conductivity of permeate, in which 1 is the conductivity of permeate of the superhydrophobic film having high-temperature self-healing property prepared in the fourth step of example 1, and 2 is the conductivity of permeate after the superhydrophobic film having high-temperature self-healing property prepared in example 1 is subjected to high-temperature healing.
As can be seen from fig. 7, the superhydrophobic film having high-temperature self-healing property prepared in the fourth step of example 1 does not have a large increase in the permeant liquid conductivity of the film after the self-healing process is completed.

Claims (10)

1. A preparation method of a super-hydrophobic membrane with high-temperature self-repairing performance is characterized by comprising the following steps:
1. pretreatment of Fenton reaction:
immersing PVDF-based film in FeSO 4 ·7H 2 O、H 2 O 2 Carrying out Fenton reaction under the heating condition in a mixed solution of absolute ethyl alcohol and deionized water, cleaning the PVDF base membrane by using sulfuric acid, and finally carrying out vacuum drying to obtain the pretreated PVDF base membrane;
2. preparing a bottom super-hydrophobic layer:
(1) firstly, siO is added 2 Dissolving the nano particles in cyclohexane, magnetically stirring, ultrasonically dispersing, dripping 1H,2H and 2H-perfluoro octyl trichlorosilane, and continuously ultrasonically dispersing to obtain PFTS/SiO 2 A solution;
(2) immersing the pretreated PVDF basal membrane into PFTS/SiO 2 Taking out the solution, and then drying the solution in vacuum to obtain a composite film containing the bottom super-hydrophobic layer;
3. preparing a PVA intermediate layer:
(1) mixing polyvinyl alcohol and deionized water, stirring under a heating condition, and adding absolute ethyl alcohol to obtain a mixed solution;
(2) uniformly casting the mixed solution onto a composite film containing a bottom super-hydrophobic layer, controlling the thickness of the mixed solution on the bottom super-hydrophobic layer by using a film coater, and finally drying at room temperature to obtain the composite film containing the PVA intermediate layer;
4. preparing a top super-hydrophobic layer:
PFTS/SiO using a spray gun 2 And spraying the solution on the surface of the composite membrane containing the PVA intermediate layer, standing, and then performing forced air drying to obtain the super-hydrophobic membrane with high-temperature self-repairing performance.
2. The method for preparing superhydrophobic film with high temperature self-repairing property according to claim 1, wherein the FeSO is provided in step one 4 ·7H 2 Mass of O and H 2 O 2 The volume ratio of (1 g-2 g) to (5 mL-7 mL); h in the step one 2 O 2 The volume ratio of the absolute ethyl alcohol to the deionized water is (5-7) to (40-60).
3. The method according to claim 1, wherein the step of preparing the superhydrophobic film comprises a step of adding H 2 O 2 The mass fraction of (A) is 30%; the temperature of the Fenton reaction in the step one is 40-60 ℃, and the time of the Fenton reaction is 1-2 h; the mass fraction of the sulfuric acid in the step one is 98%; the temperature of the vacuum drying in the first step is 60-80 ℃.
4. The method for preparing the superhydrophobic film with high temperature self-repairing property according to claim 1, wherein the SiO in step two (1) 2 The mass ratio of the nano particles to the 1H, 2H-perfluorooctyltrichlorosilane to the cyclohexane is 1 (1-2) to 50.
5. The method for preparing the superhydrophobic film with the high-temperature self-repairing performance according to claim 1, wherein the magnetic stirring speed in the step two (1) is 40r/min to 60r/min, and the magnetic stirring time is 20min to 40min; the ultrasonic dispersion time in the step two (1) is 15min to 25min, and the ultrasonic dispersion power is 350W to 500W.
6. According toThe method for preparing the superhydrophobic film having the high temperature self-repairing property according to claim 1, wherein the pretreated PVDF base film is immersed in PFTS/SiO in the step two (2) 2 The solution is kept for 3 to 5 hours; the temperature of the vacuum drying in the step two (2) is 60-80 ℃.
7. The method for preparing the superhydrophobic film with the high-temperature self-repairing performance according to claim 1, wherein the mass ratio of the polyvinyl alcohol to the deionized water in the step three (1) is 1 (6-8); the volume ratio of the mass of the polyvinyl alcohol to the absolute ethyl alcohol in the step three (1) (1 g-2 g) is 1mL; the stirring temperature in the step three (1) is 70-80 ℃, and the stirring time is 1-2 h.
8. The method for preparing the superhydrophobic film with the high temperature self-repairing performance according to claim 1, wherein the thickness of the mixed solution on the superhydrophobic composite film in the step three (2) is controlled to be 400 μm to 600 μm by using a film coater.
9. The preparation method of the superhydrophobic film with high-temperature self-repairing performance according to claim 1, wherein the spraying pressure in the fourth step is 0.2 MPa-0.6 MPa, the spraying distance is 10 cm-17 cm, and the superhydrophobic film is left standing for 20 min-40 min after spraying; the temperature of the forced air drying in the fourth step is 60-70 ℃, and the time of the forced air drying is 3-5 h.
10. Use of the superhydrophobic film having high temperature self-healing property prepared by the preparation method according to claim 1, characterized in that the superhydrophobic film having high temperature self-healing property is used as a film for membrane distillation.
CN202211313608.0A 2022-10-25 2022-10-25 Preparation method and application of super-hydrophobic membrane with high-temperature self-repairing performance Pending CN115608166A (en)

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