CN114159983A - Backwashing-resistant organic tubular membrane and preparation method thereof - Google Patents
Backwashing-resistant organic tubular membrane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a backwash-resistant organic tubular membrane and a preparation method thereof, and the method comprises the following steps: (1) preparing an organic tubular base membrane in a sintering mode; (2) preparing a high molecular solution, injecting the high molecular solution into the tubular base membrane, and pretreating to obtain a membrane tube with an initial active separation layer; (3) and immersing the pretreated initial membrane tube in a coagulating bath for phase separation to obtain the organic tubular membrane. In the preparation process of the organic tubular membrane, the membrane casting solution is completely filled into the base membrane by pressure to obtain an active separation layer on the inner surface and a membrane layer on the outer surface, wherein the active separation layer on the inner surface is fully contacted with the tubular base membrane, and the uniform membrane layer exists on the outer surface, so that the backwashing resistance of the active separation layer of the tubular membrane is greatly improved; the preparation process of the tubular membrane is simple, and the separation hole structure of the membrane is uniform and easy to control.
Description
Technical Field
The invention belongs to the technical field of membrane preparation, and particularly relates to a backwashing-resistant organic tubular membrane and a preparation method thereof.
Background
The membrane separation technology can realize the high-efficiency separation of liquid-liquid and solid-liquid. The membrane material can be divided into hollow fiber membrane, flat membrane and tubular membrane. The tubular membrane is a high-efficiency separation membrane material, wherein the organic tubular membrane mainly comprises a supporting structure and an active separation layer. The support structure of the organic tubular membrane is generally a tubular base membrane composed of non-woven fabrics, meshes and sintered particles, and the main function of the base membrane is to provide mechanical support, so that the organic tubular membrane has higher strength. The active separation layer of the organic tubular membrane is generally an ultrafiltration membrane or microfiltration membrane structure. The pipe cavity is large, the strength of the membrane is high, and the material separation can be carried out at a high flow rate, so that the pollution resistance is high, the device can be used for solid-liquid separation, treating materials containing a large amount of pollutants such as particles and the like, and can replace the traditional coagulation sedimentation tank in the separation process.
The separation layer of the organic tubular membrane is generally obtained by a method of high-molecular membrane casting liquid phase separation, and the main preparation method comprises the following steps: and coating the organic polymer membrane casting solution on the inner wall or the outer wall of the supporting tube to prepare the membrane. However, the preparation process is complicated and mainly comprises the preparation of a tubular base film, the coating of an organic polymer and the phase separation curing film forming. Patent CN109647226A discloses a method for preparing an organic tubular membrane with a composite structure, and a nonwoven fabric supported tubular membrane is prepared. Patent CN104888619A discloses a method for preparing organic tubular composite membrane, which comprises welding a support membrane into a base membrane, and then coating a membrane, wherein the support membrane is mainly made of non-woven fabric. The preparation method of the organic tubular membrane based on the non-woven fabric support generally comprises the following steps: the supporting tube is obtained by ultrasonic welding, the high molecular casting solution is coated on the inner wall of the supporting tube, and the high molecular casting solution is converted into a film in a coagulating bath. However, when highly polluted materials are separated and materials containing solid particles are separated, the membrane is easy to be polluted and needs to be frequently backwashed, and the organic tubular membrane based on the non-woven fabric has insufficient strength, so that the backwashing process is easy to deform and the separation efficiency is influenced. Therefore, how to prepare the tubular membrane for effective separation of the materials and the separation layer is resistant to back washing with high frequency and high strength is a key technical problem to be solved.
Patent CN108854581A discloses a preparation method of a high-strength composite tubular membrane, which comprises sintering high molecular resins with large and small particle sizes in a composite die respectively, wherein the membrane flux obtained by the method is large, the effective separation layer is obtained by sintering uniform particles, deep pollution is easy to occur in the filtration process, and the recovery of backwashing on the flux is low. In addition, the organic tubular membrane based on the sintered tube support is prepared by coating a polymer casting solution on the inner surface of a tubular base membrane to obtain a highly precise separation layer. The tubular membrane has higher strength due to the support composed of the sintered particles, and the tubular base membrane can keep the structural form unchanged under the conditions of high strength and high-frequency back washing. An active separation layer can be obtained by a phase separation method, and the regulation and control of separation precision are realized. Patent CN102343218A discloses a method for preparing a composite tubular membrane, in which a base membrane is immersed in a membrane casting solution for coating, the material consumption is high, the membrane casting solution is easily polluted by impurities on a sintered tube, the membrane preparation steps are many, and the difficulty in controlling the pore structure is high. Patent CN111408273A discloses an organic tubular membrane, a tubular membrane component and a tubular membrane unit, wherein the organic tubular membrane in the patent is divided into two layers, namely a base membrane layer and a surface membrane layer, and the surface membrane layer is easy to fall off after long-term back washing in the application process of the membrane.
Therefore, aiming at the treatment of wastewater containing certain solid particles and high-concentration pollutants, under the operating condition of high flow rate, the high-performance tubular membrane not only has higher separation precision, but also has higher strength, can realize backwashing, and the separation skin layer can resist the impact of backwashing. The problems can be effectively solved by using a high-strength sintering pipe as a base film and coating a separation skin layer with high separation precision and backwashing resistance.
Disclosure of Invention
In order to solve the problems, the invention provides a backwashing-resistant organic tubular membrane and a preparation method thereof.
The invention adopts the following technical scheme that,
a preparation method of a backwashing-resistant organic tubular membrane comprises the following steps:
(1) preparing an organic tubular base membrane in a sintering mode;
mixing the polymer particles, injecting the mixture into a mold for sintering, and cooling to obtain a tubular base membrane with a pore structure; cleaning polymer particles which are not completely bonded on the tubular base film, and drying to obtain the tubular base film for coating;
(2) preparing a membrane casting solution;
mixing a polymer, a solvent and an additive, stirring and dissolving at 25-80 ℃, filtering to remove impurities in the solution after the polymer, the solvent and the additive are completely dissolved, and standing or defoaming the filtered polymer solution in vacuum to obtain a membrane casting solution;
(3) injecting the casting solution obtained in the step (2) into the pores on the tubular base membrane obtained in the step (1) through a coating head of a coating machine, and pretreating to obtain a tubular base membrane containing an initial active separation layer;
(4) and (4) immersing the tubular base membrane containing the initial active separation layer obtained in the step (3) in a gel bath to complete phase separation, so as to obtain the organic tubular membrane.
Further, the polymer particles in the step (1) are any one or more of polyethylene, polypropylene, polytetrafluoroethylene, polyvinylidene fluoride and polyether ether ketone.
Further, the solution for cleaning the tubular base membrane in the step (1) is one or a mixture of N, N-dimethylformamide, N-dimethylacetamide, 1, 4-dioxane, N-methylpyrrolidone, concentrated sulfuric acid and water.
Further, the thickness of the tubular base membrane obtained in the step (1) is 0.5-5mm, the porosity is 10% -70%, the coating pressure is 0.1-2MPa, and the coating speed is 5-100 cm/min.
Further, the macromolecule in the step (2) is: one or more of polyvinylidene fluoride, polyether ether ketone, polyether sulfone, polysulfone, polyvinyl chloride and polyetherimide.
Further, the additive in the step (2) is: one or more of water, inorganic chloride, polyethylene glycol, glycerol, diethylene glycol, polyvinylpyrrolidone, graphene oxide, sulfonated graphene oxide and carbon nanotubes; the solvent in the step (2) is: one or more of N, N-dimethylformamide, N-dimethylacetamide, 1, 4-dioxane, N-methylpyrrolidone, concentrated sulfuric acid and methanesulfonic acid.
Further, the mass ratio of the added polymer to the additive in the step (2) is 100:1 to 1:1, and the mass ratio of the solvent in the casting solution is 80-60%.
Further, the pretreatment process in the step (3) is as follows: scraping the excessive casting film liquid on the inner surface and the outer surface of the tubular base film, and then standing the tubular base film for 0-30min or introducing nitrogen or air with the humidity of 20-100% for 10-100 s.
Further, the gel bath in the step (4) is an aqueous solution containing a solvent, the type of the solvent is the same as that in the step (2), the gel bath is composed of an aqueous solution with the mass concentration of the solvent of 0-50%, and the temperature of the solution is 20-90 ℃.
The back-flush resistant organic tubular membrane prepared according to the method comprises a tubular base membrane, an active separation layer on the inner surface of the membrane and a high polymer membrane layer on the outer surface of the membrane.
Advantageous effects
(1) The back-flushing resistant organic tubular membrane consists of a tubular base membrane and a separation layer structure, wherein the separation layer is obtained by separating a membrane casting solution in the tubular base membrane. The lower layer pore structure of the tubular membrane active separation layer is filled in the pores of the tubular base membrane, and the membrane also comprises an even outer surface membrane layer, so that the strength of the tubular membrane is increased, and the anti-recoil performance of the active separation layer on the tubular membrane is greatly improved.
(2) The method comprises the steps of controllably injecting the casting solution into the tubular base film, and controlling the immersion speed of the casting solution through the film coating pressure and speed, wherein the prepared casting solution enters pores of the tubular base film under the action of air pressure or pump pressure; the casting solution has less material consumption, easy control of the membrane preparation process and high production efficiency.
(3) The organic tubular membrane produced by the invention not only has high mechanical strength of the tubular base membrane, but also has high-efficiency separation performance of a separation layer obtained by phase separation.
Description of the drawings:
FIG. 1 is a schematic diagram of the structure of a tubular membrane made according to the present invention.
Fig. 2 is a sectional structure and a surface structure of the tubular membrane prepared in example 1.
Fig. 3 is a sectional structure and a surface structure of the tubular membrane prepared in example 2.
Detailed Description
The tubular membrane preparation process is described first below, with the following steps:
(1) preparing an organic tubular base membrane in a sintering mode;
mixing the polymer particles, injecting the mixture into a mold for sintering, and cooling to obtain a tubular base membrane with a pore structure; cleaning polymer particles which are not completely bonded on the tubular base film, and drying to obtain the tubular base film for coating;
(2) preparing a membrane casting solution;
mixing a polymer, a solvent and an additive, stirring and dissolving at 25-80 ℃, filtering to remove impurities in the solution after the polymer, the solvent and the additive are completely dissolved, and standing or defoaming the filtered polymer solution in vacuum to obtain a membrane casting solution;
(3) injecting the casting solution obtained in the step (2) into the pores on the tubular base membrane obtained in the step (1) through a coating head of a coating machine, and pretreating to obtain a tubular base membrane containing an initial active separation layer;
(4) and (4) immersing the tubular base membrane containing the initial active separation layer obtained in the step (3) in a gel bath to complete phase separation, so as to obtain the organic tubular membrane.
In each of the following examples, the tubular membrane was prepared using the procedure described above.
Example 1
And sintering to obtain the tubular base membrane made of polypropylene, wherein the wall thickness of the tubular base membrane is 2.5mm, and the porosity is 32%. According to the mass ratio, polyvinylidene fluoride: diethylene glycol: n, N-dimethylacetamide is 15: 5: 80. mixing and stirring at 80 ℃ to dissolve, and then filtering by a stainless steel filter screen. And (4) vacuum defoaming is adopted to obtain the casting solution for the coating.
The casting solution enters a coating head under the conveying of a gear pump, and the tubular base film is coated, wherein the coating speed is 10cm/min, and the coating pressure is controlled at 0.3 MPa. And scraping the redundant casting film liquid on the inner surface and the outer surface of the tubular base film after coating, introducing air with the humidity of 50%, treating for 1min, and putting into a hydrogel bath at 50 ℃ to obtain the macromolecular tubular film.
The properties of the film were as follows: the pure water flux was 2300 liters per square meter per hour and the average pore size of the membrane was 200 nm. The cross-sectional structure of the film was observed by a scanning electron microscope to obtain fig. 2.
The membrane is subjected to intermittent back flushing under 0.3MPa, and the separation performance of the membrane is kept unchanged after 1000-hour back flushing.
Example 2
Sintering to obtain the tubular base membrane made of the polytetrafluoroethylene material, wherein the wall thickness of the tubular base membrane is 5mm, and the porosity is 55%. According to the mass ratio, polyvinylidene fluoride: polyethylene glycol: n-methylpyrrolidone is 11: 20: 80. mixing and stirring at 80 ℃ to dissolve, and then filtering by a stainless steel filter screen. Standing for 24 hours for defoaming, and obtaining the casting solution for coating.
And (3) feeding the casting solution into a coating head under the action of air pressure, and coating the tubular base film at a coating speed of 1m/min and under a coating pressure of 0.1 MPa. And scraping redundant casting film liquid on the inner surface and the outer surface of the tubular base film after coating, standing for 1min, and putting into a 80-DEG hydrogel bath to obtain the macromolecular tubular film.
The properties of the film were as follows: pure water flux 1820 liters per square meter per hour, and the average pore size of the membrane is 0.5 micron.
The cross-sectional structure of the film was observed by a scanning electron microscope to obtain fig. 3.
The membrane is subjected to intermittent back flushing under 0.4MPa, and the separation performance of the membrane is kept unchanged after 1000-hour back flushing.
Example 3
Sintering to obtain the tubular base membrane made of the polytetrafluoroethylene material, wherein the wall thickness of the tubular base membrane is 5mm, and the porosity is 60%. According to the mass ratio, polyether-ether-ketone: polypyrrolidone: the concentrated sulfuric acid is 11: 1: stirring at 88 deg.C and 25 deg.C for dissolution, and filtering with stainless steel filter screen. Standing for 24 hours for defoaming, and obtaining the casting solution for coating.
And (3) feeding the casting solution into a coating head under the action of air pressure, and coating the tubular base film at a coating speed of 20cm/min and under a coating pressure of 1.9 MPa. And scraping redundant casting film liquid on the inner surface and the outer surface of the tubular base film after coating, standing for 1min, and putting into 30-DEG gel bath water to obtain the macromolecular tubular film.
The properties of the film were as follows: pure water flux 120 liters per square meter per hour, and average pore size of the membrane 50 nm.
The membrane is subjected to intermittent back flushing under 0.3MPa, and the separation performance of the membrane is kept unchanged after 1000-hour back flushing.
Example 4
Sintering to obtain the tubular base membrane made of polyethylene, wherein the wall thickness of the tubular base membrane is 8mm, and the average pore diameter is 90 mu m. According to the mass ratio, polyether sulfone: polypyrrolidone: n, N-dimethylformamide is 16: 10: the mixture was dissolved by stirring at 74, 80 ℃ and then filtered through a stainless steel sieve. Standing for 24 hours for defoaming, and obtaining the casting solution for coating.
And (3) feeding the casting solution into a coating head under the action of air pressure, and coating the tubular base film at a coating speed of 50cm/min and under a coating pressure of 1 MPa. And scraping the redundant casting film liquid on the inner surface and the outer surface of the tubular base film after coating, standing for 0.5min, and then putting into a gel bath aqueous solution containing 30% of N, N-dimethylformamide by mass, wherein the gel bath temperature is 30 ℃, so as to obtain the macromolecular tubular film.
The properties of the film were as follows: the pure water flux was 650 liters per square meter per hour and the average pore diameter of the membrane was 150 nm.
The membrane is subjected to intermittent back flushing under 0.3MPa, and the separation performance of the membrane is kept unchanged after 500-hour back flushing.
Claims (10)
1. The preparation method of the back-flushing-resistant organic tubular membrane is characterized by comprising the following steps of:
(1) preparing an organic tubular base membrane in a sintering mode;
mixing the polymer particles, injecting the mixture into a mold for sintering, and cooling to obtain a tubular base membrane with a pore structure; cleaning polymer particles which are not completely bonded on the tubular base film, and drying to obtain the tubular base film for coating;
(2) preparing a membrane casting solution;
mixing a polymer, a solvent and an additive, stirring and dissolving at 25-80 ℃, filtering to remove impurities in the solution after the polymer, the solvent and the additive are completely dissolved, and standing or defoaming the filtered polymer solution in vacuum to obtain a membrane casting solution;
(3) injecting the casting solution obtained in the step (2) into the pores on the tubular base membrane obtained in the step (1) through a coating head of a coating machine, and pretreating to obtain a tubular base membrane containing an initial active separation layer;
(4) immersing the tubular base membrane containing the initial active separation layer obtained in step (3) in a gel bath to complete phase separation to obtain an organic tubular membrane.
2. The preparation method according to claim 1, wherein the polymer particles in step (1) are any one or more of polyethylene, polypropylene, polytetrafluoroethylene, polyvinylidene fluoride and polyether ether ketone.
3. The preparation method according to claim 1, wherein the solution for cleaning the tubular base membrane in step (1) is one or more of N, N-dimethylformamide, N-dimethylacetamide, 1, 4-dioxane, N-methylpyrrolidone, concentrated sulfuric acid and water.
4. The production method according to claim 1, wherein the tubular base film obtained in step (1) has a thickness of 0.5 to 5mm, a porosity of 10 to 70%, a film coating pressure of 0.1 to 2MPa, and a film coating speed of 5 to 100 cm/min.
5. The method according to claim 1, wherein the polymer in step (2) is: one or more of polyvinylidene fluoride, polyether ether ketone, polyether sulfone, polysulfone, polyvinyl chloride and polyetherimide.
6. The method according to claim 1, wherein the additive in step (2) is: one or more of water, inorganic chloride, polyethylene glycol, glycerol, diethylene glycol, polyvinylpyrrolidone, graphene oxide, sulfonated graphene oxide and carbon nanotubes; the solvent in the step (2) is: one or more of N, N-dimethylformamide, N-dimethylacetamide, 1, 4-dioxane, N-methylpyrrolidone, concentrated sulfuric acid and methanesulfonic acid.
7. The preparation method according to claim 1, wherein the mass ratio of the added polymer to the additive in the step (2) is 100:1 to 1:1, and the mass ratio of the solvent in the casting solution is 80% -60%.
8. The method according to claim 1, wherein the pretreatment step of step (3) is: scraping the excessive casting solution on the inner surface and the outer surface of the tubular base film, and then standing the tubular base film for 0-30min or introducing nitrogen or staying in air with the humidity of 20-100% for 10-100 seconds.
9. The method according to claim 1, wherein the gelling bath in step (4) is an aqueous solution containing a solvent, the kind of the solvent is the same as that in step (2), the gelling bath is composed of an aqueous solution having a solvent mass concentration of 0 to 50%, and the temperature of the solution is 20 to 90 ℃.
10. The backwash-resistant organic tubular membrane produced by the method as claimed in any one of claims 1 to 9, wherein the organic tubular membrane comprises a tubular base membrane, an active separation layer at an inner surface of the membrane, and a polymeric membrane layer at an outer surface of the membrane.
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| CN116535786A (en) * | 2023-04-25 | 2023-08-04 | 深圳市华之美科技有限公司 | Fixing film for printer or copier, and preparation method and application thereof |
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