CN112406244B - High-performance laminated glass intermediate polymer film material and preparation method thereof - Google Patents
High-performance laminated glass intermediate polymer film material and preparation method thereof Download PDFInfo
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- CN112406244B CN112406244B CN202011249209.3A CN202011249209A CN112406244B CN 112406244 B CN112406244 B CN 112406244B CN 202011249209 A CN202011249209 A CN 202011249209A CN 112406244 B CN112406244 B CN 112406244B
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/42—Layered products comprising a layer of synthetic resin comprising condensation resins of aldehydes, e.g. with phenols, ureas or melamines
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/285—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyethers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
- B32B27/322—Layered products comprising a layer of synthetic resin comprising polyolefins comprising halogenated polyolefins, e.g. PTFE
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0223—Vinyl resin fibres
- B32B2262/0238—Vinyl halide, e.g. PVC, PVDC, PVF, PVDF
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0261—Polyamide fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/558—Impact strength, toughness
Abstract
The invention provides a high-performance laminated glass intermediate polymer film material and a preparation method thereof, wherein the preparation method comprises the following steps: a) Dissolving a polymer in an organic solvent to obtain an electrospinning solution; b) Carrying out electrostatic spinning on the substrate by adopting the electrospinning solution obtained in the step a) to obtain a substrate with polymer fibers on the surface; c) Taking two substrates with polymer fibers on the surfaces obtained in the step b), placing a functional film between the two substrates, contacting one surface with the polymer fibers with the film, carrying out hot pressing, and removing the substrates to obtain the high-performance laminated glass intermediate polymer film material. The preparation method prepares the fibers through an electrostatic spinning process, and then permeates the fibers into the polymer film through hot pressing to obtain the electrospun fiber reinforced polymer film material, the mechanical property of the material is obviously improved, and the material is particularly suitable for high-impact-resistance sandwich glass intermediate film materials.
Description
Technical Field
The invention relates to the technical field of polymer film materials, in particular to a high-performance sandwich glass intermediate polymer film material and a preparation method thereof.
Background
The common glass can be broken under the common impact, more long-strip-shaped sharp fragments can be generated, and great threat is caused to the safety of a human body. The tempered glass is broken under the impact of large force, once broken, the whole glass is burst into fine particles without acute angles due to internal prestress, and a little broken glass remains in the frame. Even if the laminated glass is broken under impact, the generated fragments can be adhered to the interlayer intermediate film, so that the fragment splashing condition is greatly reduced, and the personal safety is well guaranteed.
The laminated glass is prepared by placing the polymer adhesive film between two or more toughened glass substrates and performing hot pressing, is the safe glass with excellent performance, and has excellent performance in the aspects of safety, security protection, sound insulation, radiation protection and the like compared with the traditional common glass. With the development and progress of society, the application of the laminated glass in automobile glass, high-rise buildings, military industry fields and daily life is more and more extensive. Meanwhile, the impact resistance of the laminated glass is further improved, the extreme application requirements in more projects are met, and the light and safe functions can be maintained, so that a laminated glass intermediate polymer adhesive film material with high mechanical property needs to be developed, and the reports on the aspect show that the laminated glass intermediate polymer adhesive film material is not suitable for the project application.
Disclosure of Invention
In view of the above, the present invention aims to provide a high-performance laminated glass intermediate polymer film material and a preparation method thereof, the preparation method provided by the present invention prepares fibers through an electrostatic spinning process, and then permeates the fibers into a polymer film through hot pressing to obtain an electrospun fiber reinforced polymer film material, wherein the material has significantly improved mechanical properties, and is particularly suitable for a high-impact resistant laminated glass intermediate film material.
The invention provides a preparation method of a high-performance laminated glass intermediate polymer film material, which comprises the following steps:
a) Dissolving a polymer in an organic solvent to obtain an electrospinning solution;
b) Carrying out electrostatic spinning on the substrate by adopting the electrospinning solution obtained in the step a) to obtain a substrate with polymer fibers on the surface;
c) Taking two substrates with polymer fibers on the surfaces obtained in the step b), placing a functional film between the two substrates, and enabling one surface with the polymer fibers to be in contact with the film, carrying out hot pressing, and then removing the substrates to obtain the high-performance sandwich glass intermediate polymer film material.
Preferably, the polymer in step a) is selected from one or more of polyvinylidene fluoride, polyamide, polytetramethylene adipamide and polycarbonate.
Preferably, the organic solvent in step a) is selected from one or more of dimethylformamide, dimethylacetamide, dimethylsulfoxide, formic acid, acetic acid, hexafluoroisopropanol, phenol, benzene, toluene, tetrahydrofuran, acetone, dichloromethane and chloroform.
Preferably, the mass fraction of the electrospinning solution in the step a) is 3wt% to 30wt%.
Preferably, the inner diameter of the spinning needle adopted in the electrostatic spinning process in the step b) is 0.1 mm-1.0 mm, and the distance between the tip and the substrate is 5 cm-30 cm.
Preferably, the electric field intensity of the electrostatic spinning in the step b) is 2kV to 35kV, and the advancing speed of the electrospinning solution is 0.05mL/h to 1.50mL/h.
Preferably, the functional film in step c) is selected from a PVB film, an EVA film or a PU film.
Preferably, the hot pressing in the step c) has the tabletting temperature of 50-190 ℃ and the pressure of 1.0-1.5 MPa.
The invention also provides a high-performance laminated glass intermediate polymer film material prepared by the preparation method of the technical scheme.
The invention provides a high-performance sandwich glass intermediate polymer film material and a preparation method thereof, wherein the preparation method comprises the following steps: a) Dissolving a polymer in an organic solvent to obtain an electrospinning solution; b) Carrying out electrostatic spinning on the substrate by adopting the electrospinning solution obtained in the step a) to obtain a substrate with polymer fibers on the surface; c) Taking two substrates with polymer fibers on the surfaces obtained in the step b), placing a functional film between the two substrates, and contacting one surface with the polymer fibers with the film, and carrying out hot pressing to obtain the high-performance laminated glass intermediate polymer film material. Compared with the prior art, the preparation method provided by the invention prepares the fibers through an electrostatic spinning process, and then permeates the fibers into the polymer film through hot pressing to obtain the electrospun fiber reinforced polymer film material, the mechanical property of the material is obviously improved, and the material is particularly suitable for the high-impact-resistance laminated glass intermediate film material.
In addition, the preparation method provided by the invention can realize the regulation and control of the light transmittance of the interlayer glass by controlling the reaction conditions, maintain the good light transmittance of the product and have wide application prospect.
Drawings
FIG. 1 is a schematic diagram of an electrospinning test apparatus and a process flow provided by an embodiment of the present invention;
FIG. 2 is a flow chart of the preparation of a high-performance polymer film material in the middle of a laminated glass provided by an embodiment of the present invention;
FIG. 3 is a scanning electron micrograph of the morphology of the fibers of example 1 of the present invention;
FIG. 4 shows the results of light transmittance of the laminated glass in example 1 of the present invention;
FIG. 5 shows the impact resistance results of the laminated glass of example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a high-performance laminated glass intermediate polymer film material, which comprises the following steps:
a) Dissolving a polymer in an organic solvent to obtain an electrospinning solution;
b) Carrying out electrostatic spinning on the substrate by adopting the electrospinning solution obtained in the step a) to obtain a substrate with polymer fibers on the surface;
c) Taking two substrates with polymer fibers on the surfaces obtained in the step b), placing a functional film between the two substrates, and contacting one surface with the polymer fibers with the film, and carrying out hot pressing to obtain the high-performance laminated glass intermediate polymer film material.
According to the invention, firstly, a polymer is dissolved in an organic solvent to obtain an electrospinning solution. In the present invention, the polymer is preferably selected from one or more of polyvinylidene fluoride, polyamide, polytetramethylene adipamide, and polycarbonate. The source of the polymer is not particularly limited in the present invention, and commercially available products of the above-mentioned polyvinylidene fluoride, polyamide, polytetramethylene adipamide and polycarbonate, which are well known to those skilled in the art, may be used.
In the present invention, the organic solvent is preferably selected from one or more of dimethylformamide, dimethylacetamide, dimethylsulfoxide, formic acid, acetic acid, hexafluoroisopropanol, phenol, benzene, toluene, tetrahydrofuran, acetone, dichloromethane, chloroform. In a preferred embodiment of the present invention, the organic solvent is a mixed organic solvent of Dimethylformamide (DMF) and Acetone (ACE); the volume ratio of DMF to ACE is preferably (3-5): 1. the source of the organic solvent is not particularly limited in the present invention, and commercially available products of the above-mentioned dimethylformamide, dimethylacetamide, dimethylsulfoxide, formic acid, acetic acid, hexafluoroisopropanol, phenol, benzene, toluene, tetrahydrofuran, acetone, dichloromethane and chloroform, which are well known to those skilled in the art, may be used.
The dissolving mode is not particularly limited in the invention, and the technical scheme of magnetic stirring well known to those skilled in the art can be adopted.
In the present invention, the mass fraction of the electrospinning solution is preferably 3 to 30wt%, more preferably 5 to 20wt%.
After the electrospinning solution is obtained, the obtained electrospinning solution is used for carrying out electrostatic spinning on a substrate to obtain the substrate with the polymer fibers on the surface. In the present invention, the substrate is preferably selected from a polyimide film, a polyphenylene sulfide film, a polyether ether ketone film, a polytetrafluoroethylene film or a liquid crystal polymer film. The source of the substrate in the present invention is not particularly limited, and commercially available products of the above polyimide film, polyphenylene sulfide film, polyether ether ketone film, polytetrafluoroethylene film and liquid crystal polymer film, which are well known to those skilled in the art, may be used. The substrate is adopted, so that the substrate can be conveniently separated from the obtained high-performance laminated glass intermediate polymer membrane material after subsequent hot pressing.
In the invention, the electrostatic spinning is a simple and effective method for preparing a nano-fiber membrane material, and a polymer solution with certain viscosity is stretched to form fibers with diameters ranging from nanometer to micrometer under the action of electrostatic force generated by a high-voltage electric field; the nanofiber membrane obtained by electrostatic spinning generally has certain porosity, continuous fibers and adjustable diameters.
The structural schematic diagram of the electrostatic spinning test device and the process flow provided by the invention is shown in figure 1; wherein, (1) is the injection pump, (2) is the spinneret, (3) is the collection device, (4) is the high voltage power supply; the syringe pump (syringe) used may be a 5mL medical syringe known to those skilled in the art. In the invention, the inner diameter of the spinning needle adopted in the electrostatic spinning process is preferably 0.1 mm-1.0 mm; the distance between the tip of the spinneret needle and the glass substrate is preferably 5 cm-30 cm.
In the invention, the electric field intensity of the electrostatic spinning is preferably 2 kV-35 kV; the preferred advancing speed of the electrospinning solution for electrostatic spinning is 0.05 mL/h-1.50 mL/h; the time for the electrostatic spinning is preferably 10min to 60min.
After the substrate with the polymer fibers on the surface is obtained, the invention takes two obtained substrates with the polymer fibers on the surface, places the functional film between the two substrates, and contacts the surface with the polymer fibers with the film for the laminated glass, and carries out hot pressing to obtain the high-performance laminated glass intermediate polymer film material. In the present invention, the functional film is preferably selected from a PVB film, an EVA film, or a PU film.
In the present invention, the purpose of the hot pressing is to hot press the polymer fibers into the functional film; in the hot pressing process, the functional film is melted and filled in holes formed by polymer fibers, and is taken down after the room temperature is recovered, so that a modified polymer film material is obtained, small-sized fiber yarns are embedded in the polymer film material, and the mechanical property of the film is improved; in addition, by accurately controlling conditions, better light transmittance can be maintained after hot pressing.
The hot pressing apparatus of the present invention is not particularly limited, and a vulcanizing machine well known to those skilled in the art may be used. In the invention, the tabletting temperature of the hot pressing is preferably 50-190 ℃, and more preferably 110-140 ℃; the pressure of the hot pressing is preferably 1.0MPa to 1.5MPa; the time for hot pressing is preferably 10min to 60min.
The preparation method provided by the invention prepares the fiber by an electrostatic spinning method, and then permeates the fiber into the polymer membrane by hot pressing to obtain the electro-spinning fiber reinforced polymer membrane material, and the flow chart of the whole preparation method is shown in figure 2; wherein, (1) is a high temperature resistant film, (2) is a polymer fiber, (3) is a polymer film, and (4) is a high-performance polymer film. The polymer film material prepared by the preparation method has obviously improved mechanical properties, and is particularly suitable for high-impact-resistance laminated glass intermediate film materials.
The invention also provides a high-performance laminated glass intermediate polymer film material prepared by the preparation method of the technical scheme. According to the invention, the nano-fibers are added on the two sides of the functional film to form a nano-fiber frame, so that the product has excellent mechanical properties while being simple and convenient; in addition, the obtained high-performance laminated glass intermediate polymer film material has fiber morphology.
The invention provides a high-performance laminated glass intermediate polymer film material and a preparation method thereof, wherein the preparation method comprises the following steps: a) Dissolving a polymer in an organic solvent to obtain an electrospinning solution; b) Carrying out electrostatic spinning on the substrate by adopting the electrospinning solution obtained in the step a) to obtain a substrate with polymer fibers on the surface; c) Taking two substrates with polymer fibers on the surfaces obtained in the step b), placing a functional film between the two substrates, and contacting one surface with the polymer fibers with the functional film, and carrying out hot pressing to obtain the high-performance laminated glass intermediate polymer film material. Compared with the prior art, the preparation method provided by the invention has the advantages that the fibers are prepared by the electrostatic spinning process, and then the fibers are infiltrated into the polymer film through hot pressing to obtain the electrospun fiber reinforced polymer film material, the mechanical property of the material is obviously improved, and the material is particularly suitable for the high-impact-resistance laminated glass intermediate film material.
In addition, the preparation method provided by the invention can realize the regulation and control of the light transmittance of the interlayer glass by controlling the reaction conditions, maintain the good light transmittance of the product and have wide application prospect.
To further illustrate the present invention, the following examples are provided for illustration. The drugs and solvents used in the following examples of the present invention are commercially available.
Example 1
(1) Dissolving polyamide-6 (PA 6) in formic acid organic solvent to prepare PA6 solution with mass fraction of 13.0wt%, namely electrospinning solution.
(2) An electrostatic spinning test device is adopted, electrostatic spinning is carried out on a polyimide film substrate under the condition that the electric field intensity is 21kV, as shown in figure 1, an injector of the electrostatic spinning test device is a 5mL medical injector, the inner diameter of a spinning needle is 0.34mm, the needle is flat, the distance between the tip of the spinning needle and a receiving plate (substrate) is 20cm, an electrospinning solution is spun at the advancing speed of 0.3mL/h, the electrospinning time is 30min respectively, the substrate with PA6 fibers on the surface is obtained, the fiber morphology is shown in figure 3, and the fiber diameter is about ninety nanometers.
(3) Taking two substrates with PA6 fibers on the surfaces obtained in the step (2), placing a PVB film between the two glass substrates, enabling one surface with the PA6 fibers to be in contact with the PVB film, then pressing the substrates by a vulcanizing machine, enabling the pressing temperature to be 130 ℃, the pressure to be 1.0MPa and the time to be 20min, and removing the polyimide film to obtain a high-performance laminated glass intermediate polymer film material, so that the prepared laminated glass has good light transmittance, shown in figure 4 and excellent impact resistance, shown in figure 5.
Example 2
(1) Polyvinylidene fluoride (PVDF) was dissolved in DMF: ACE =4:1 (volume ratio) to prepare a PVDF solution with the mass fraction of 11.0wt%, namely an electrospinning solution.
(2) An electrostatic spinning test device is adopted to carry out electrostatic spinning on a polyimide film substrate under the condition that the electric field intensity is 15kV, as shown in figure 1, an injector of the electrostatic spinning test device is a 5mL medical injector, the inner diameter of a spinning needle is 0.34mm, the needle is flat, the distance between the tip of the spinning needle and a receiving plate (substrate) is 15cm, an electrospinning solution is spun at the advancing speed of 0.5mL/h, and the electrospinning time is 40min respectively, so that the substrate with PVDF fibers on the surface is obtained.
(3) Taking two substrates with the PVDF fibers on the surfaces, obtained in the step (2), placing a PVB film between the two glass substrates, enabling the surface with the PVDF fibers to be in contact with the PVB film, then tabletting by using a vulcanizing machine, wherein the tabletting temperature is 130 ℃, the pressure is 1.0MPa, and the time is 20min, and removing the polyimide film to obtain the high-performance laminated glass intermediate polymer film material.
Example 3
(1) Polyvinylidene fluoride (PVDF) was dissolved in DMF: ACE =4:1 (volume ratio) to prepare a PVDF solution with the mass fraction of 12.0wt%, namely an electrospinning solution.
(2) An electrostatic spinning test device is adopted to carry out electrostatic spinning on a polyimide film substrate under the condition that the electric field intensity is 15kV, as shown in figure 1, an injector of the electrostatic spinning test device is a 5mL medical injector, the inner diameter of a spinning needle is 0.34mm, the needle is flat, the distance between the tip of the spinning needle and a receiving plate (substrate) is 15cm, an electrospinning solution is spun at the advancing speed of 0.5mL/h, and the electrospinning time is 10min respectively, so that the substrate with PVDF fibers on the surface is obtained.
(3) Taking two substrates with the PVDF fibers on the surfaces obtained in the step (2), placing a PVB film between the two glass substrates, enabling the PVB film to be in contact with the PVDF fibers on one surface, then pressing the substrates by using a vulcanizing machine, and removing the polyimide film to obtain the high-performance laminated glass intermediate polymer film material, wherein the pressing temperature is 130 ℃, the pressure is 1.0MPa, and the time is 20 min.
Example 4
(1) Polyvinylidene fluoride (PVDF) was dissolved in DMF: ACE =4:1 (volume ratio) to prepare a PVDF solution with the mass fraction of 14.0wt%, namely an electrospinning solution.
(2) Adopting an electrostatic spinning test device, carrying out electrostatic spinning on a polyimide film substrate under the condition that the electric field intensity is 15kV, as shown in figure 1, wherein an injector of the electrostatic spinning test device is a 5mL medical injector, the inner diameter of a spinning needle is 0.34mm, the needle is flat, the distance between the tip of the spinning needle and a receiving plate (substrate) is 15cm, an electrospinning solution is spun at a propelling speed of 0.5mL/h, and the electrospinning time is 40min respectively, so as to obtain the substrate with the PVDF fibers on the surface.
(3) Taking two substrates with the PVDF fibers on the surfaces, obtained in the step (2), placing a PVB film between the two glass substrates, enabling the surface with the PVDF fibers to be in contact with the PVB film, then tabletting by using a vulcanizing machine, wherein the tabletting temperature is 130 ℃, the pressure is 1.0MPa, and the time is 20min, and removing the polyimide film to obtain the high-performance laminated glass intermediate polymer film material.
Example 5
(1) Polyvinylidene fluoride (PVDF) was dissolved in DMF: ACE =4:1 (volume ratio) to prepare a PVDF solution with the mass fraction of 11.0wt%, namely an electrospinning solution.
(2) An electrostatic spinning test device is adopted to carry out electrostatic spinning on a polytetrafluoroethylene film substrate under the condition that the electric field intensity is 16kV, as shown in figure 1, an injector of the electrostatic spinning test device is a 5mL medical injector, the inner diameter of a spinning needle is 0.34mm, the needle is flat, the distance between the tip of the spinning needle and a receiving plate (substrate) is 14cm, an electrospinning solution is spun at the advancing speed of 0.6mL/h, and the electrospinning time is 40min respectively, so that the substrate with PVDF fibers on the surface is obtained.
(3) Taking two substrates with the PVDF fibers on the surfaces obtained in the step (2), placing an EVA film between the two glass substrates, enabling one surface with the PVDF fibers to be in contact with the EVA film, then performing tabletting by adopting a vulcanizing machine, and taking off a polytetrafluoroethylene film to obtain the high-performance laminated glass intermediate polymer film material, wherein the tabletting temperature is 110 ℃, the pressure is 1.0MPa, and the time is 20 min.
Example 6
(1) Polyvinylidene fluoride (PVDF) was dissolved in DMF: ACE =4:1 (volume ratio) to prepare a PVDF solution with the mass fraction of 12.0wt%, namely an electrospinning solution.
(2) Adopting an electrostatic spinning test device, carrying out electrostatic spinning on a polytetrafluoroethylene film substrate under the condition that the electric field intensity is 15kV, as shown in figure 1, wherein an injector of the electrostatic spinning test device is a 5mL medical injector, the inner diameter of a spinning needle is 0.34mm, the needle is flat, the distance between the tip of the spinning needle and a receiving plate (substrate) is 15cm, an electrospinning solution is spun at a propelling speed of 0.5mL/h, and the electrospinning time is 20min respectively, so as to obtain the substrate with the PVDF fibers on the surface.
(3) Taking two substrates with the PVDF fibers on the surfaces obtained in the step (2), placing an EVA film between the two glass substrates, enabling the side with the PVDF fibers to be in contact with the PVB film, then carrying out tabletting by adopting a vulcanizing machine, wherein the tabletting temperature is 110 ℃, the pressure is 1.0MPa, and the time is 20min, and removing the polytetrafluoroethylene film to obtain the high-performance laminated glass intermediate polymer film material.
Example 7
(2) Dissolving polyamide-6 (PA 6) in formic acid organic solvent to prepare PA6 solution with mass fraction of 13.0wt%, namely electrospinning solution.
(2) An electrostatic spinning test device is adopted to carry out electrostatic spinning on the polyetheretherketone film substrate under the condition that the electric field intensity is 21kV, as shown in figure 1, an injector of the electrostatic spinning test device is a 5mL medical injector, the inner diameter of a spinning needle is 0.34mm, the needle is flat, the distance between the tip of the spinning needle and a receiving plate (substrate) is 20cm, an electrospinning solution is spun at the advancing speed of 0.4mL/h, and the electrospinning time is 40min respectively, so that the substrate with PA6 fibers on the surface is obtained.
(3) Taking two substrates with PA6 fibers on the surfaces obtained in the step (2), placing a PU film between the two glass substrates, enabling one surface with the PA6 fibers to be in contact with the PU film, then adopting a vulcanizing machine to perform tabletting, wherein the tabletting temperature is 120 ℃, the pressure is 1.0MPa, and the time is 20min, and removing the polyether-ether-ketone film to obtain the high-performance interlayer glass intermediate polymer film material.
Example 8
(1) Polyvinylidene fluoride (PVDF) was dissolved in DMF: ACE =4:1 (volume ratio) to prepare a PVDF solution with the mass fraction of 13.0wt%, namely an electrospinning solution.
(2) Adopting an electrostatic spinning test device, carrying out electrostatic spinning on a polyetheretherketone film substrate under the condition that the electric field intensity is 15kV, as shown in figure 1, wherein an injector of the electrostatic spinning test device is a 5mL medical injector, the inner diameter of a spinning needle is 0.34mm, the needle is flat, the distance between the tip of the spinning needle and a receiving plate (substrate) is 15cm, an electrospinning solution is spun at a propelling speed of 0.5mL/h, and the electrospinning time is 40min respectively, so as to obtain the substrate with the PVDF fibers on the surface.
(3) Taking two substrates with PVDF fibers on the surfaces obtained in the step (2), placing a PU film between the two glass substrates, enabling the side with the PVDF fibers to be in contact with the PVB film, then carrying out tabletting by adopting a vulcanizer, wherein the tabletting temperature is 120 ℃, the pressure is 1.0MPa, and the time is 20min, and removing the polyether-ether-ketone film to obtain the high-performance laminated glass intermediate polymer film material.
Comparative example 1
Taking two polyimide film substrates, placing a PVB film between the two substrates, then tabletting by using a vulcanizing machine, wherein the tabletting temperature is 130 ℃, the pressure is 1.0MPa, and the time is 20min, and removing the polyimide film to obtain the film.
Comparative example 2
Taking two polytetrafluoroethylene film substrates, placing an EVA film between the two substrates, then tabletting by using a vulcanizing machine, wherein the tabletting temperature is 110 ℃, the pressure is 1.0MPa, and the time is 20min, and removing the polytetrafluoroethylene film to obtain the film.
Comparative example 3
Taking two polyether-ether-ketone film substrates, placing the PU film between the two substrates, then tabletting by using a vulcanizing machine, wherein the tabletting temperature is 120 ℃, the pressure is 1.0MPa, and the time is 20min, and removing the polyether-ether-ketone film to obtain the film.
The mechanical properties of the high-performance laminated glass intermediate polymer film materials obtained by the preparation methods provided in examples 1 to 8 and the films obtained by the preparation methods provided in comparative examples 1 to 3 were tested according to the national standard GB/T13022-1991, and the results are shown in Table 1.
TABLE 1 data of mechanical properties of high-performance polymer film materials for laminated glasses prepared by the preparation methods provided in examples 1-8 and films prepared by the preparation methods provided in comparative examples 1-3
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. A preparation method of a high-performance laminated glass intermediate polymer film material comprises the following steps:
a) Dissolving polyamide-6 in formic acid organic solvent to prepare polyamide-6 solution with mass fraction of 13.0wt%, or dissolving polyvinylidene fluoride in dimethylformamide and acetone at volume ratio of 4:1, preparing a polyvinylidene fluoride solution with the mass fraction of 11.0wt%, 12.0wt%, 13.0wt% or 14.0wt% in the mixed organic solvent to obtain an electrospinning solution;
b) Carrying out electrostatic spinning on the substrate by adopting the electrospinning solution obtained in the step a) to obtain a substrate with polymer fibers on the surface;
c) Taking two substrates with polymer fibers on the surfaces obtained in the step b), placing a functional film between the two substrates, and enabling one surface with the polymer fibers to be in contact with the film, carrying out hot pressing, and then removing the substrates to obtain a high-performance sandwich glass intermediate polymer film material; the functional film is selected from a PVB film, an EVA film or a PU film; the hot pressing temperature is 50-190 ℃, the pressure is 1.0-1.5 MPa, and the time is 10-60 min.
2. The method of claim 1, wherein the electrospinning process in step b) uses a spinneret tip having an inner diameter of 0.1mm to 1.0mm and a tip-to-base distance of 5cm to 30cm.
3. The preparation method according to claim 1, wherein the electric field strength of the electrostatic spinning in the step b) is 2kV to 35kV, and the advancing rate of the electrospinning solution is 0.05mL/h to 1.50mL/h.
4. A high-performance laminated glass intermediate polymer film material, which is characterized by being prepared by the preparation method of any one of claims 1 to 3.
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| CN101069822A (en) * | 2007-03-06 | 2007-11-14 | 天津大学 | Method for preparing PVDF super-fine fiber film with good mechanics-performance |
| CN101538746A (en) * | 2008-03-17 | 2009-09-23 | 国家纳米科学中心 | Principle and novel method for preparing orientation-controllable electrostatic spinning nano polymer fibers |
| CN101705593A (en) * | 2009-10-29 | 2010-05-12 | 无锡中科光远生物材料有限公司 | Shaping method of ultrafine fiber membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101069822A (en) * | 2007-03-06 | 2007-11-14 | 天津大学 | Method for preparing PVDF super-fine fiber film with good mechanics-performance |
| CN101538746A (en) * | 2008-03-17 | 2009-09-23 | 国家纳米科学中心 | Principle and novel method for preparing orientation-controllable electrostatic spinning nano polymer fibers |
| CN101705593A (en) * | 2009-10-29 | 2010-05-12 | 无锡中科光远生物材料有限公司 | Shaping method of ultrafine fiber membrane |
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