CN111036092A - Preparation method of hydrophilic composite membrane - Google Patents
Preparation method of hydrophilic composite membrane Download PDFInfo
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- CN111036092A CN111036092A CN202010054744.7A CN202010054744A CN111036092A CN 111036092 A CN111036092 A CN 111036092A CN 202010054744 A CN202010054744 A CN 202010054744A CN 111036092 A CN111036092 A CN 111036092A
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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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
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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
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/027—Silicium oxide
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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
- B01D71/54—Polyureas; Polyurethanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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- 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
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Abstract
The invention discloses a preparation method of a hydrophilic composite membrane. Dissolving thermoplastic polyurethane particles and polyurethane hydrogel particles in a solvent to obtain a polyurethane solution, adding hydrophilic fumed silica powder into the polyurethane solution, stirring at a high speed to obtain a solid-liquid mixture, performing reduced pressure defoaming treatment, coating the mixture on a glass plate, soaking the glass plate into deionized water, curing to form a film, drying the film, and performing plasma discharge treatment after the film is peeled off to obtain the hydrophilic composite film. The polyurethane hydrogel and the hydrophilic fumed silica powder in the composite membrane prepared by the method have good mechanical properties, and the hydrophilicity of the membrane is obviously improved; the surface treatment of low-pressure plasma effectively improves the hydrophilicity of the membrane; the porous structure of the membrane also enhances the moisture absorption performance of the material.
Description
Technical Field
The invention relates to an organic-inorganic hybrid material, in particular to a preparation method of a hydrophilic composite membrane.
Background
In recent years, hydrophilic materials are more and more concerned by people, and the excellent hydrophilicity of the hydrophilic materials endows the materials with unique physicochemical properties, so that the hydrophilic materials have great development prospects in the aspect of environmental protection.
The hydrophilic fumed silica is fluffy white powder, is non-toxic, tasteless, pollution-free and high-temperature-resistant, has special physical and chemical properties, is used for improving a polyurethane material, and can improve the tensile strength, the tear resistance and the wear resistance.
The surface treatment of low temperature plasma is an effective hydrophilization surface treatment means, the particles in the plasma can break the chemical bonds of some organic macromolecules, and combine with free radicals in the plasma to form polar groups on the surface of the material, so that the hydrophilicity of the surface of the material can be obviously enhanced, and the performance of the matrix is not influenced.
Disclosure of Invention
The invention aims to provide a preparation method of a hydrophilic composite membrane, which has the advantages of easily obtained materials, simple process and environmental friendliness.
The invention is realized by the following technical scheme:
a preparation method of a hydrophilic composite membrane comprises the following steps:
(1) weighing 13-23 parts by weight of thermoplastic polyurethane particles, 15-30 parts by weight of dried polyurethane hydrogel particles and 110-130 parts by weight of solvent, adding the weighed materials into a reactor, stirring at a constant temperature of 60-80 ℃ for 2-4 hours to fully dissolve the thermoplastic polyurethane particles and the polyurethane hydrogel particles in the solvent, and cooling to room temperature to obtain a polyurethane solution;
(2) adding hydrophilic fumed silica powder into the polyurethane solution obtained in the step (1), wherein the mass ratio of the polyurethane solution to the hydrophilic fumed silica powder is 120-125: 15-23, and uniformly stirring by using a high-speed stirrer to obtain a solid-liquid mixture;
(3) decompressing and defoaming the solid-liquid mixture obtained in the step (2) for 0.5-1.5 h, uniformly coating the mixture on a glass plate, immersing the glass plate into deionized water, and drying the mixture in a drying oven after the solid-liquid mixture is completely cured into a film; (4) and (3) after the glass plate and the film are cooled, peeling the film, then putting the film into a low-pressure plasma processor, and carrying out plasma discharge treatment on the surface of the film for 0.5-3 min to obtain the hydrophilic composite film, wherein the output power is 80-120W, the plasma gas source is one of oxygen and nitrogen, and the pressure of the reaction chamber is 50-100 Pa.
After the hydrophilic composite membrane is taken out of the reactor, the membrane product can be cut into different sizes according to the requirement so as to meet the actual requirement.
Preferably, in step (1), the polyurethane hydrogel particles are nonionic polyurethane hydrogel particles.
Preferably, in the step (1), the thermoplastic polyurethane particles are polyester type thermoplastic polyurethane particles or/and polyether type thermoplastic polyurethane particles, and the shore hardness of the thermoplastic polyurethane particles is 55-70A.
Preferably, in step (1), the solvent is N, N-dimethylformamide or/and N, N-dimethylacetamide.
Preferably, in the step (2), the hydrophilic fumed silica is white powder with fineness of 2000-5000 meshes.
Preferably, in the step (2), the weight percentages of the thermoplastic polyurethane, the polyurethane hydrogel, the solvent and the hydrophilic fumed silica in the prepared solid-liquid mixture are as follows: 7.68-11.02% of thermoplastic polyurethane, 7.08-11.97% of polyurethane hydrogel, 62.66-72.87% of solvent and 10.88-16.05% of hydrophilic fumed silica.
Preferably, in the step (3), the total thickness of the hydrophilic composite membrane is controlled to be 0.36-0.6 mm by adjusting the thickness of the solid-liquid mixture coated on the glass plate.
Preferably, in the step (3), the drying temperature is 60-80 ℃, and the drying time is 2-4 h. Preferably, in the step (4), the plasma discharge treatment time is 1-3 min.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method of the hydrophilic composite membrane provided by the invention has the advantages of easily available materials, simplicity, practicability, low requirements on equipment and environmental friendliness.
(2) The polyurethane hydrogel and the hydrophilic fumed silica powder in the composite membrane prepared by the method have good mechanical properties, and the hydrophilicity of the membrane is obviously improved.
(3) The surface treatment of low-pressure plasma effectively improves the hydrophilicity of the membrane; the porous structure of the membrane also enhances the moisture absorption performance of the material.
Detailed Description
The present invention will be described in further detail by the following specific examples, wherein the raw materials are all industrial products, and the equipment is common industrial production equipment.
Example 1
(1) Weighing 5 kg of polyester type thermoplastic polyurethane particles with Shore hardness of 55A, stirring 6 kg of nonionic polyurethane hydrogel particles and 46 kg of N, N-dimethylformamide in a reactor at constant temperature of 60 ℃ for 3h to fully dissolve the polyester type thermoplastic polyurethane particles and the polyurethane hydrogel particles in a solvent, and cooling to room temperature to obtain a polyurethane solution;
(2) adding 7.13 kg of 2000-mesh hydrophilic fumed silica powder into the polyurethane solution obtained in the step (1), and uniformly stirring by using a high-speed stirrer to obtain a solid-liquid mixture;
(3) defoaming the solid-liquid mixture obtained in the step (2) under reduced pressure for 1h, uniformly coating the mixture on a glass plate, then soaking the glass plate into deionized water, placing the mixture in a drying oven after the solid-liquid mixture is completely cured into a film, drying the mixture at 80 ℃ for 3h, and controlling the total thickness of the film to be 0.36mm by adjusting the thickness of the solid-liquid mixture coated on the glass plate;
(4) after the glass plate and the film are cooled, peeling the film, then putting the film into a low-pressure plasma processor, carrying out plasma discharge treatment on the surface of the film for 1min, wherein the output power is 100 watts, a plasma gas source is oxygen, and the pressure of a reaction chamber is 50 Pa;
(5) and taking the membrane out of the reactor, and cutting the membrane product into a proper size according to the requirement to obtain the hydrophilic composite membrane product.
In the solid-liquid mixture obtained in this example, the mass percentage of the polyester-type thermoplastic polyurethane was 7.8%, the mass percentage of the polyurethane hydrogel was 9.36%, the mass percentage of the N, N-dimethylformamide was 71.73%, and the mass percentage of the hydrophilic fumed silica powder was 11.12%. The resulting film product was white in color and 0.36mm thick.
The hydrophilic experiment of the product prepared by the embodiment shows that the pure water contact angle of the hydrophilic film is 58.5 degrees, compared with the contact angle of a common polyurethane film, the contact angle is obviously reduced, water can be well spread on the surface of the composite film, and the excellent hydrophilic performance is reflected in the embodiment 2
(1) Weighing 7 kg of polyester type thermoplastic polyurethane particles with Shore hardness of 60A, stirring 10 kg of nonionic polyurethane hydrogel particles and 56 kg of N, N-dimethylformamide in a reactor at constant temperature of 70 ℃ for 3h to fully dissolve the polyester type thermoplastic polyurethane particles and the polyurethane hydrogel particles in a solvent, and cooling to room temperature to obtain a polyurethane solution;
(2) adding 10.95 kg of 2000-mesh hydrophilic fumed silica powder into the polyurethane solution obtained in the step (1), and uniformly stirring by using a high-speed stirrer to obtain a solid-liquid mixture;
(3) defoaming the solid-liquid mixture obtained in the step (2) under reduced pressure for 1h, uniformly coating the mixture on a glass plate, then soaking the glass plate into deionized water, placing the mixture in a drying oven after the solid-liquid mixture is completely cured into a film, drying the mixture at 70 ℃ for 3h, and controlling the total thickness of the film to be 0.42mm by adjusting the thickness of the solid-liquid mixture coated on the glass plate;
(4) after the glass plate and the film are cooled, peeling the film, then putting the film into a low-pressure plasma processor, carrying out plasma discharge treatment on the surface of the film for 1min, wherein the output power is 100 watts, a plasma gas source is oxygen, and the pressure of a reaction chamber is 60 Pa;
(5) and taking the membrane out of the reactor, and cutting the membrane product into a proper size according to the requirement to obtain the hydrophilic composite membrane product.
In the solid-liquid mixture obtained in this example, the mass percentage of the polyester-type thermoplastic polyurethane was 8.34%, the mass percentage of the polyurethane hydrogel was 11.91%, the mass percentage of N, N-dimethylformamide was 66.71%, and the mass percentage of the hydrophilic fumed silica powder was 13.04%. The resulting film product was white in color and 0.42mm thick.
The product prepared by the embodiment is subjected to a hydrophilic experiment, and the experimental result shows that the pure water contact angle of the hydrophilic film is 54.7 degrees, compared with the contact angle of a common polyurethane film, the contact angle is obviously reduced, water can be well spread on the surface of the composite film, and the excellent hydrophilic performance is reflected.
Example 3
(1) Weighing 10 kg of polyether type thermoplastic polyurethane particles with Shore hardness of 65A, stirring 10 kg of nonionic polyurethane hydrogel particles and 60 kg of N, N-dimethylacetamide in a reactor at constant temperature of 70 ℃ for 3h to fully dissolve the polyether type thermoplastic polyurethane particles and the polyurethane hydrogel particles in a solvent, and cooling to room temperature to obtain a polyurethane solution;
(2) adding 13.5 kg of 3000-mesh hydrophilic fumed silica powder into the polyurethane solution obtained in the step (1), and uniformly stirring by using a high-speed stirrer to obtain a solid-liquid mixture;
(3) defoaming the solid-liquid mixture obtained in the step (2) under reduced pressure for 1h, uniformly coating the mixture on a glass plate, then soaking the glass plate into deionized water, placing the mixture in a drying oven after the solid-liquid mixture is completely cured into a film, drying the mixture at 70 ℃ for 3h, and controlling the total thickness of the film to be 0.48mm by adjusting the thickness of the solid-liquid mixture coated on the glass plate;
(4) after the glass plate and the film are cooled, peeling the film, then putting the film into a low-pressure plasma processor, carrying out plasma discharge treatment on the surface of the film for 2min, wherein the output power is 100 watts, a plasma gas source is nitrogen, and the pressure of a reaction chamber is 80 Pa;
(5) and taking the membrane out of the reactor, and cutting the membrane product into a proper size according to the requirement to obtain the hydrophilic composite membrane product.
In the solid-liquid mixture obtained in this example, the mass percentage of the polyether thermoplastic polyurethane was 10.7%, the mass percentage of the polyurethane hydrogel was 10.7%, the mass percentage of N, N-dimethylformamide was 64.17%, and the mass percentage of the hydrophilic fumed silica powder was 14.44%. The resulting film product was white in color and 0.48mm thick.
The product prepared by the embodiment is subjected to a hydrophilic experiment, and the experimental result shows that the pure water contact angle of the hydrophilic film is 47.4 degrees, compared with the contact angle of a common polyurethane film, the contact angle is obviously reduced, water can be well spread on the surface of the composite film, and the excellent hydrophilic performance is reflected.
Example 4
(1) Weighing 13 kg of polyether type thermoplastic polyurethane particles with Shore hardness of 70A, putting 8.5 kg of nonionic polyurethane hydrogel particles and 78 kg of N, N-dimethylformamide in a reactor, stirring at constant temperature of 80 ℃ for 3h to fully dissolve the polyether type thermoplastic polyurethane particles and the polyurethane hydrogel particles in a solvent, and cooling to room temperature to obtain a polyurethane solution;
(2) adding 18.85 kg of 5000-mesh hydrophilic fumed silica powder into the polyurethane solution obtained in the step (1), and uniformly stirring by using a high-speed stirrer to obtain a solid-liquid mixture;
(3) carrying out 1h of decompression defoaming on the solid-liquid mixture obtained in the step (2), uniformly coating the solid-liquid mixture on a glass plate with a certain thickness, then immersing the glass plate into deionized water, placing the solid-liquid mixture in a drying box after the solid-liquid mixture is completely cured into a film, drying the film for 3h at the temperature of 80 ℃, and controlling the total thickness of the film to be 0.6mm by adjusting the thickness of the solid-liquid mixture coated on the glass plate;
(4) after the glass plate and the film are cooled, peeling the film, then putting the film into a low-pressure plasma processor, carrying out plasma discharge treatment on the surface of the film for 3min, wherein the output power is 100 watts, a plasma gas source is nitrogen, and the pressure of a reaction chamber is 100 Pa;
(5) and taking the membrane out of the reactor, and cutting the membrane product into a proper size according to the requirement to obtain the hydrophilic composite membrane product.
In the solid-liquid mixture obtained in the present example, the mass percentage of the polyether thermoplastic polyurethane was 10.98%, the mass percentage of the polyurethane hydrogel was 7.18%, the mass percentage of N, N-dimethylacetamide was 65.91%, and the mass percentage of the hydrophilic fumed silica powder was 15.93%. The obtained film product was white in color and 0.6mm in thickness.
The product prepared by the embodiment is subjected to a hydrophilic experiment, and the experiment result shows that the pure water contact angle of the hydrophilic film is 44.5 degrees, compared with the contact angle of a common polyurethane film, the contact angle is obviously reduced, water can be well spread on the surface of the composite film, and the excellent hydrophilic performance is reflected.
By observing the shapes of the lower surface and the cross section of the hydrophilic composite membrane prepared by the embodiment on an electron microscope, the surface of the hydrophilic composite membrane has a porous structure, and the cross section of the hydrophilic composite membrane has an asymmetric pore channel structure; the hydrophilic fumed silica particles are uniformly distributed on the composite membrane without obvious agglomeration.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of a hydrophilic composite membrane is characterized by comprising the following steps:
(1) weighing 13-23 parts by weight of thermoplastic polyurethane particles, 15-30 parts by weight of dried polyurethane hydrogel particles and 110-130 parts by weight of solvent, adding the weighed materials into a reactor, stirring at a constant temperature of 60-80 ℃ for 2-4 hours to fully dissolve the thermoplastic polyurethane particles and the polyurethane hydrogel particles in the solvent, and cooling to room temperature to obtain a polyurethane solution;
(2) adding hydrophilic fumed silica powder into the polyurethane solution obtained in the step (1), wherein the mass ratio of the polyurethane solution to the hydrophilic fumed silica powder is 120-125: 15-23, and uniformly stirring by using a high-speed stirrer to obtain a solid-liquid mixture;
(3) decompressing and defoaming the solid-liquid mixture obtained in the step (2) for 0.5-1.5 h, uniformly coating the mixture on a glass plate, immersing the glass plate into deionized water, and drying the mixture in a drying oven after the solid-liquid mixture is completely cured into a film;
(4) and (3) after the glass plate and the film are cooled, peeling the film, then putting the film into a low-pressure plasma processor, and carrying out plasma discharge treatment on the surface of the film for 0.5-3 min to obtain the hydrophilic composite film.
2. A method for preparing a hydrophilic composite membrane according to claim 1, wherein in step (1), the polyurethane hydrogel particles are nonionic polyurethane hydrogel particles.
3. The preparation method of the hydrophilic composite film according to claim 1, wherein in the step (1), the thermoplastic polyurethane particles are polyester thermoplastic polyurethane particles or/and polyether thermoplastic polyurethane particles, and the Shore hardness of the thermoplastic polyurethane particles is 55A-70A.
4. The method for preparing a hydrophilic composite membrane according to claim 1, wherein in the step (1), the solvent is N, N-dimethylformamide or/and N, N-dimethylacetamide.
5. The method for preparing a hydrophilic composite membrane according to claim 1, wherein in the step (2), the hydrophilic fumed silica is white powder with fineness of 2000-5000 mesh.
6. A method for preparing a hydrophilic composite membrane according to claim 1, wherein in the step (2), the weight percentages of the thermoplastic polyurethane, the polyurethane hydrogel, the solvent and the hydrophilic fumed silica in the prepared solid-liquid mixture are as follows: 7.68-11.02% of thermoplastic polyurethane, 7.08-11.97% of polyurethane hydrogel, 62.66-72.87% of solvent and 10.88-16.05% of hydrophilic fumed silica.
7. The method for preparing a hydrophilic composite membrane according to claim 1, wherein in the step (3), the total thickness of the hydrophilic composite membrane is controlled to be 0.36-0.6 mm by adjusting the thickness of the solid-liquid mixture coated on the glass plate.
8. The preparation method of the hydrophilic composite membrane according to claim 1, wherein in the step (3), the drying temperature is 60-80 ℃ and the drying time is 2-4 h.
9. The method for preparing the hydrophilic composite membrane according to claim 1, wherein in the step (4), the plasma discharge treatment time is 1-3 min.
10. The preparation method of the hydrophilic composite membrane according to claim 1, wherein in the step (4), the output power of the plasma processor is 80-120 w, the plasma gas source is one of oxygen and nitrogen, and the pressure of the reaction chamber is 50-100 Pa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112210112A (en) * | 2020-10-19 | 2021-01-12 | 闽江学院 | Surface self-cleaning raw lacquer composite film and preparation method thereof |
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