CN111138987B - Polyurethane acoustic adhesive film and production method thereof - Google Patents
Polyurethane acoustic adhesive film and production method thereof Download PDFInfo
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- CN111138987B CN111138987B CN202010020605.2A CN202010020605A CN111138987B CN 111138987 B CN111138987 B CN 111138987B CN 202010020605 A CN202010020605 A CN 202010020605A CN 111138987 B CN111138987 B CN 111138987B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/24—Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/241—Polyolefin, e.g.rubber
- C09J7/243—Ethylene or propylene polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/35—Heat-activated
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2423/00—Presence of polyolefin
- C09J2423/10—Presence of homo or copolymers of propene
- C09J2423/106—Presence of homo or copolymers of propene in the substrate
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Abstract
The invention discloses a production method of a polyurethane acoustic adhesive film, which is characterized by comprising the following steps: step S1, chain extension of amino-terminated polyurethane; step S2, preparing epoxy rosin; step S3, preparing glue solution; and step S4, coating. The invention also discloses a production method of the polyurethane acoustic adhesive film. The polyurethane acoustic adhesive film disclosed by the invention has the advantages of good weather resistance, excellent mechanical property, high bonding strength, excellent adhesiveness at room temperature, good performance stability and long service life, and can be used as a hot melt adhesive and a pressure-sensitive adhesive.
Description
Technical Field
The invention relates to the technical field of film materials, in particular to a polyurethane acoustic adhesive film and a production method thereof.
Background
An electroacoustic transducer, also referred to as an acoustic transducer, is a device that can convert an electrical signal (i.e. a voltage) into an alternating acoustic pressure (i.e. an acoustic signal), or vice versa. Acoustic transducers are used for various types of loudspeakers and microphones, in particular for micro-loudspeakers for applications in mobile phones, laptops, tablets, games, headsets, hands-free speakerphones, modern televisions and also in the automotive field.
The acoustic membrane is one of the key components of an electroacoustic transducer, and the acoustic signal is generated by the movement of the acoustic membrane of the loudspeaker, which is mechanically driven, for example, by a voice coil. The acoustic membrane with excellent performance is a precondition for ensuring the electroacoustic conversion efficiency of the electroacoustic transducer, and the mass of the acoustic membrane directly influences the sound transmission quality and the service life of an acoustic device. With the development of the electronic industry, the electroacoustic transducer needs to continuously meet higher requirements of consumers on product performance and to perfectly present the nature of sound, so that the acoustic membrane of the core component of the electroacoustic transducer also has higher and higher performance requirements, and the electroacoustic transducer not only needs to have excellent mechanical performance, but also needs to have better temperature resistance, acceptable fatigue performance and better performance stability so as to have longer service life of the transducer.
The acoustic film in the prior art is generally manufactured by coating and attaching a plurality of layers of thermoplastic resin, and the layers of thermoplastic resin are bonded by an acoustic adhesive film, for example, WO 2008/056286 discloses a multilayer film for an acoustic device, in which a thermoplastic material is used. The outer membrane facing the surface is preferably a softer material which can be melted and used to establish a direct connection with other components of the acoustic device. Preferably, one layer is rigid, for example polycarbonate, and the other layer is a softer material, for example PU, thermoplastic elastomers being considered particularly suitable. However, these materials are often not laminated well by gluing and are prone to delamination, which reduces their useful life. It can be seen that there is a need for an improved acoustic adhesive film for use in the prior art.
At present, acoustic adhesive films on the market are all in thousands of autumn, but the defects that the heat resistance, the bonding strength and the weather resistance are required to be further improved and the dielectric constant under high frequency is required to be further reduced exist generally. Thermoplastic polyurethane elastomers (TPU) are widely used for bonding products such as shoes, electronics, and medical products, and various properties of the TPU as an adhesive are generally adjusted by controlling molecular chain segments in the polymerization process of the TPU.
Therefore, the development of a polyurethane acoustic adhesive film is very important to promote the development of the acoustic adhesive film industry.
Disclosure of Invention
The invention mainly aims to provide a polyurethane acoustic adhesive film and a production method thereof, wherein the production method is simple and feasible, has small dependence on equipment and high production efficiency and yield, is suitable for continuous large-scale production, and has higher popularization and application values; the prepared polyurethane acoustic adhesive film has the advantages of good weather resistance, excellent mechanical property, high bonding strength, excellent adhesiveness at room temperature, good performance stability and long service life, and can be used as a hot melt adhesive and a pressure-sensitive adhesive.
In order to achieve the above object, the present invention provides a method for producing a polyurethane acoustic adhesive film, comprising the steps of:
step S1, chain extension of amino-terminated polyurethane: adding 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione and amino-terminated polyurethane into a high boiling point solvent, adding a basic catalyst into the solvent, stirring the mixture to react for 10 to 15 hours at the temperature of between 75 and 85 ℃, performing rotary evaporation to remove the solvent, adding acetone and water in a mass ratio of 1 (3-4) into the mixture, separating the mixture, taking an organic phase, and performing rotary evaporation to remove the acetone to obtain polyurethane based on imidazolidinone;
step S2, preparation of epoxy rosin: adding hydrogenated rosin, epoxy chloropropane and sodium hydroxide into N-methyl pyrrolidone, stirring and reacting for 3-5 hours at 70-80 ℃, cooling to room temperature, performing rotary evaporation to remove the N-methyl pyrrolidone, washing for 3-6 times with water, and performing rotary evaporation to remove water to obtain epoxy rosin;
step S3, preparation of glue solution: adding the imidazolidinone-based polyurethane prepared in the step S1 and the epoxy rosin prepared in the step S2 into acetone, carrying out ultrasonic treatment for 10-15 minutes, adding bis (chloromethyl) tetramethyldisilazane and dichloromethyl triethoxysilane, and uniformly stirring to obtain a glue solution;
step S4, coating: uniformly coating the glue solution on the upper surface and the lower surface of a clean BPPO (styrene-propylene-diene monomer) basement membrane by using an elcometer3700 scraper coater, then putting the basement membrane into an oven, drying the basement membrane at 85-95 ℃ for 4-8min to remove the solvent, and simultaneously performing heating, crosslinking and curing; and after taking out, respectively sticking the light-stripping release film and the heavy-stripping release film on the upper surface and the lower surface of the BPPO base film coated with the glue solution for protection, thus obtaining the polyurethane acoustic glue film.
Further, in step S1, the molar ratio of the 5, 5-dimethyl-1, 3-di (oxiranylmethyl) imidazolidine-2, 4-dione, the amino-terminated polyurethane, the high boiling point solvent, and the basic catalyst is 1:1 (6-10) to (0.3-0.5).
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the alkaline catalyst is at least one of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
Preferably, the amino-terminated polyurethane has an average molecular weight of 1836, and for the preparation in advance, the preparation method refers to: example 1 of chinese invention patent CN 201110382645.2.
Further, in the step S2, the molar ratio of the hydrogenated rosin to the epichlorohydrin to the sodium hydroxide to the N-methylpyrrolidone is 1:1, (0.5-0.8) to (6-10).
Further, in step S3, the mass ratio of the imidazolidinone-based polyurethane to the epoxy rosin to the acetone to the bis (chloromethyl) tetramethyldisilazane to the dichloromethyltriethoxysilane is (3-5): (2-3): (0.1-0.2): 0.3.
Preferably, the light-stripping release film is one of a PE release film, a PET release film, an OPP release film and a PC release film.
Preferably, the heavy-peeling release film is one of a PS release film, a PMMA release film and a BOPP release film.
Another object of the present invention is to provide a polyurethane acoustic adhesive film obtained according to the method for producing a polyurethane acoustic adhesive film.
Due to the application of the technical scheme, the invention has the following beneficial effects:
(1) the polyurethane acoustic adhesive film disclosed by the invention is simple and feasible in production method, small in equipment dependence, high in production efficiency and yield, suitable for continuous large-scale production and high in popularization and application value.
(2) The polyurethane acoustic adhesive film disclosed by the invention overcomes the defects that the heat resistance, the bonding strength and the weather resistance of the traditional acoustic adhesive film are required to be further improved and the dielectric constant under high frequency is required to be further reduced; the defects that polyurethane in the prior art has good adhesive property at a high temperature, but has poor adhesive property at room temperature and is difficult to be directly used for an acoustic adhesive film are overcome; the adhesive has the advantages of good weather resistance, excellent mechanical property, large bonding strength, excellent adhesiveness at room temperature, good performance stability and long service life, and can be used as a hot melt adhesive and a pressure-sensitive adhesive.
(3) The invention discloses a polyurethane acoustic adhesive film, which is characterized in that firstly, a polycondensation reaction (epoxy group and terminal amino group reaction) between 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione and terminal amino group polyurethane is utilized to carry out chain extension on the terminal amino group polyurethane, an imidazolidine structure and a hydroxyl structure (generated after the reaction of an epoxy group and the terminal amino group) are introduced, and the existence of active groups enables the adhesive film to have higher bonding strength; bis (chloromethyl) tetramethyldisilazane and dichloromethyl triethoxysilane are added into the glue solution, chlorine in the two substances is easy to react with amino on a polyurethane molecular chain based on imidazolidinone to form a three-dimensional network structure, the comprehensive performance is further improved, and a silazane structure and an ethoxy structure are introduced through the two substances, so that the bonding strength and the weather resistance are further improved.
Detailed Description
The following description is provided to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
The average molecular weight of the amino-terminated polyurethane in the embodiment of the invention is 1836, and the preparation method refers to the following steps: example 1 of chinese invention patent CN 201110382645.2; the raw materials were all purchased commercially.
Example 1
The production method of the polyurethane acoustic adhesive film is characterized by comprising the following steps of:
step S1, chain extension of amino-terminated polyurethane: adding 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione and amino-terminated polyurethane into dimethyl sulfoxide, adding sodium hydroxide into the dimethyl sulfoxide, stirring the mixture at 75 ℃ for reaction for 10 hours, then performing rotary evaporation to remove the solvent, adding acetone and water in a mass ratio of 1:3 into the mixture, performing liquid separation, taking an organic phase, and performing rotary evaporation to remove the acetone to obtain polyurethane based on imidazolidinone; the molar ratio of the 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione to the amino-terminated polyurethane to the dimethyl sulfoxide to the sodium hydroxide is 1:1:6: 0.3;
step S2, preparation of epoxy rosin: adding hydrogenated rosin, epoxy chloropropane and sodium hydroxide into N-methyl pyrrolidone, stirring and reacting at 70 ℃ for 3 hours, cooling to room temperature, removing the N-methyl pyrrolidone by rotary evaporation, washing with water for 3 times, and removing water by rotary evaporation to obtain epoxy rosin; the molar ratio of the hydrogenated rosin to the epichlorohydrin to the sodium hydroxide to the N-methyl pyrrolidone is 1:1:0.5: 6;
step S3, preparation of glue solution: adding the imidazolidinone-based polyurethane prepared in the step S1 and the epoxy rosin prepared in the step S2 into acetone, performing ultrasonic treatment for 10 minutes, adding bis (chloromethyl) tetramethyldisilazane and dichloromethyl triethoxysilane, and uniformly stirring to obtain a glue solution; the mass ratio of the imidazolidinone-based polyurethane to the epoxy rosin to the acetone to the bis (chloromethyl) tetramethyldisilazane to the dichloromethyltriethoxysilane is 3:2:0.1: 0.3;
step S4, coating: uniformly coating the glue solution on the upper surface and the lower surface of a clean BPPO (boron-propylene oxide) basement membrane by using an elcometer3700 scraper coater, then putting the BPPO basement membrane into an oven, drying the BPPO basement membrane at 85 ℃ for 4min to remove the solvent, and simultaneously performing the heating, crosslinking and curing effects; taking out, respectively sticking a light-stripping release film and a heavy-stripping release film on the upper surface and the lower surface of the BPPO base film coated with the glue solution for protection to obtain a polyurethane acoustic glue film; the light stripping release film is a PE release film; the heavy-stripping release film is a PS release film.
A polyurethane acoustic adhesive film obtained according to the production method of the polyurethane acoustic adhesive film.
Example 2
The production method of the polyurethane acoustic adhesive film is characterized by comprising the following steps of:
step S1, chain extension of amino-terminated polyurethane: adding 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione and amino-terminated polyurethane into N, N-dimethylformamide, adding potassium hydroxide into the N, N-dimethylformamide, stirring the mixture at 77 ℃ for reaction for 11 hours, then performing rotary evaporation to remove the solvent, adding acetone and water in a mass ratio of 1:3.2 into the mixture, performing liquid separation, taking an organic phase, and performing rotary evaporation to remove the acetone to obtain imidazolidinone-based polyurethane; the molar ratio of the 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione to the amino-terminated polyurethane to the N, N-dimethylformamide to the potassium hydroxide is 1:1:7.5: 0.35;
step S2, preparation of epoxy rosin: adding hydrogenated rosin, epoxy chloropropane and sodium hydroxide into N-methyl pyrrolidone, stirring and reacting for 3.5 hours at 72 ℃, cooling to room temperature, removing the N-methyl pyrrolidone by rotary evaporation, washing for 4 times by water, and removing water by rotary evaporation to obtain epoxy rosin; the molar ratio of the hydrogenated rosin to the epichlorohydrin to the sodium hydroxide to the N-methyl pyrrolidone is 1:1:0.65: 7.5;
step S3, preparation of glue solution: adding the imidazolidinone-based polyurethane prepared in the step S1 and the epoxy rosin prepared in the step S2 into acetone, performing ultrasonic treatment for 11 minutes, adding bis (chloromethyl) tetramethyldisilazane and dichloromethyl triethoxysilane, and uniformly stirring to obtain a glue solution; the mass ratio of the imidazolidinone-based polyurethane to the epoxy rosin to the acetone to the bis (chloromethyl) tetramethyldisilazane to the dichloromethyltriethoxysilane is 3.5:2.3:0.13: 0.3;
step S4, coating: uniformly coating the glue solution on the upper surface and the lower surface of a clean BPPO (boron-propylene oxide) basement membrane by using an elcometer3700 scraper coater, then putting the BPPO basement membrane into an oven, drying the BPPO basement membrane at 87 ℃ for 5min to remove the solvent, and simultaneously performing the functions of heating, crosslinking and curing; taking out, respectively sticking a light-stripping release film and a heavy-stripping release film on the upper surface and the lower surface of the BPPO base film coated with the glue solution for protection to obtain a polyurethane acoustic glue film; the light stripping release film is a PET release film; the heavy-stripping release film is a PMMA release film.
A polyurethane acoustic adhesive film obtained according to the production method of the polyurethane acoustic adhesive film.
Example 3
The production method of the polyurethane acoustic adhesive film is characterized by comprising the following steps of:
step S1, chain extension of amino-terminated polyurethane: adding 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione and amino-terminated polyurethane into N, N-dimethylacetamide, adding sodium carbonate into the N, N-dimethylacetamide, stirring the mixture at 80 ℃ for reaction for 13 hours, then performing rotary evaporation to remove the solvent, adding acetone and water in a mass ratio of 1:3.5 into the mixture, performing liquid separation, taking an organic phase, and performing rotary evaporation to remove the acetone to obtain imidazolidinone-based polyurethane; the molar ratio of the 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-diketone to the amino-terminated polyurethane to the N, N-dimethylacetamide to the sodium carbonate is 1:1:8: 0.4;
step S2, preparation of epoxy rosin: adding hydrogenated rosin, epoxy chloropropane and sodium hydroxide into N-methyl pyrrolidone, stirring and reacting for 4 hours at 75 ℃, cooling to room temperature, performing rotary evaporation to remove the N-methyl pyrrolidone, washing with water for 5 times, and performing rotary evaporation to remove water to obtain epoxy rosin; the molar ratio of the hydrogenated rosin to the epoxy chloropropane to the sodium hydroxide to the N-methyl pyrrolidone is 1:1:0.7: 8;
step S3, preparation of glue solution: adding the imidazolidinone-based polyurethane prepared in the step S1 and the epoxy rosin prepared in the step S2 into acetone, performing ultrasonic treatment for 13 minutes, adding bis (chloromethyl) tetramethyldisilazane and dichloromethyl triethoxysilane, and uniformly stirring to obtain a glue solution; the mass ratio of the imidazolidinone-based polyurethane to the epoxy rosin to the acetone to the bis (chloromethyl) tetramethyldisilazane to the dichloromethyltriethoxysilane is 4:2.5:0.15: 0.3;
step S4, coating: uniformly coating the glue solution on the upper surface and the lower surface of a clean BPPO (boron-propylene oxide) basement membrane by using an elcometer3700 scraper coater, then putting the BPPO basement membrane into an oven, drying the BPPO basement membrane at 90 ℃ for 6min to remove the solvent, and simultaneously performing the heating, crosslinking and curing effects; taking out, respectively sticking a light-stripping release film and a heavy-stripping release film on the upper surface and the lower surface of the BPPO base film coated with the glue solution for protection to obtain a polyurethane acoustic glue film; the light stripping release film is an OPP release film; the heavy-peeling release film is a BOPP release film.
A polyurethane acoustic adhesive film obtained according to the production method of the polyurethane acoustic adhesive film.
Example 4
The production method of the polyurethane acoustic adhesive film is characterized by comprising the following steps of:
step S1, chain extension of amino-terminated polyurethane: adding 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione and amino-terminated polyurethane into a high boiling point solvent, adding a basic catalyst into the solvent, stirring the mixture at 84 ℃ for reaction for 14 hours, then performing rotary evaporation to remove the solvent, adding acetone and water in a mass ratio of 1:3.8 into the mixture, performing liquid separation, taking an organic phase, and performing rotary evaporation to remove the acetone to obtain polyurethane based on imidazolidinone; the molar ratio of the 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-diketone to the amino-terminated polyurethane to the high boiling point solvent to the basic catalyst is 1:1:9: 0.45; the high-boiling-point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1:2:3: 4; the alkaline catalyst is prepared by mixing sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate according to a mass ratio of 1:2:3: 2;
step S2, preparation of epoxy rosin: adding hydrogenated rosin, epoxy chloropropane and sodium hydroxide into N-methyl pyrrolidone, stirring and reacting for 4.8 hours at 78 ℃, cooling to room temperature, removing the N-methyl pyrrolidone by rotary evaporation, washing for 5 times by water, and removing water by rotary evaporation to obtain epoxy rosin; the molar ratio of the hydrogenated rosin to the epichlorohydrin to the sodium hydroxide to the N-methyl pyrrolidone is 1:1:0.75: 9;
step S3, preparation of glue solution: adding the imidazolidinone-based polyurethane prepared in the step S1 and the epoxy rosin prepared in the step S2 into acetone, performing ultrasonic treatment for 14.5 minutes, adding bis (chloromethyl) tetramethyldisilazane and dichloromethyl triethoxysilane, and uniformly stirring to obtain a glue solution; the mass ratio of the imidazolidinone-based polyurethane to the epoxy rosin to the acetone to the bis (chloromethyl) tetramethyldisilazane to the dichloromethyltriethoxysilane is 4.8:2.8:0.18: 0.3;
step S4, coating: uniformly coating the glue solution on the upper surface and the lower surface of a clean BPPO (crosslinked polystyrene oxide) basement membrane by using an elcometer3700 scraper coater, then putting the BPPO basement membrane into an oven, drying the BPPO basement membrane at 93 ℃ for 7min to remove the solvent, and simultaneously performing the heating crosslinking curing function; taking out, respectively sticking a light-stripping release film and a heavy-stripping release film on the upper surface and the lower surface of the BPPO base film coated with the glue solution for protection to obtain a polyurethane acoustic glue film; the light stripping release film is a PC release film; the heavy-stripping release film is a PS release film.
A polyurethane acoustic adhesive film obtained according to the production method of the polyurethane acoustic adhesive film.
Example 5
The production method of the polyurethane acoustic adhesive film is characterized by comprising the following steps of:
step S1, chain extension of amino-terminated polyurethane: adding 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione and amino-terminated polyurethane into N-methylpyrrolidone, adding potassium carbonate into the N-methylpyrrolidone, stirring the mixture at 85 ℃ for reaction for 15 hours, then performing rotary evaporation to remove the solvent, adding acetone and water in a mass ratio of 1:4 into the mixture, performing liquid separation, taking an organic phase, and performing rotary evaporation to remove the acetone to obtain polyurethane based on the imidazolidinone; the molar ratio of the 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione to the amino-terminated polyurethane to the N-methylpyrrolidone to the potassium carbonate is 1:1:10: 0.5;
step S2, preparation of epoxy rosin: adding hydrogenated rosin, epoxy chloropropane and sodium hydroxide into N-methyl pyrrolidone, stirring and reacting for 5 hours at 80 ℃, cooling to room temperature, removing the N-methyl pyrrolidone by rotary evaporation, washing with water for 6 times, and removing water by rotary evaporation to obtain epoxy rosin; the molar ratio of the hydrogenated rosin to the epichlorohydrin to the sodium hydroxide to the N-methyl pyrrolidone is 1:1:0.8: 10;
step S3, preparation of glue solution: adding the imidazolidinone-based polyurethane prepared in the step S1 and the epoxy rosin prepared in the step S2 into acetone, performing ultrasonic treatment for 15 minutes, adding bis (chloromethyl) tetramethyldisilazane and dichloromethyl triethoxysilane, and uniformly stirring to obtain a glue solution; the mass ratio of the imidazolidinone-based polyurethane to the epoxy rosin to the acetone to the bis (chloromethyl) tetramethyldisilazane to the dichloromethyltriethoxysilane is 5:3:0.2: 0.3;
step S4, coating: uniformly coating the glue solution on the upper surface and the lower surface of a clean BPPO (boron-propylene oxide) basement membrane by using an elcometer3700 scraper coater, then putting the BPPO basement membrane into an oven, drying the BPPO basement membrane at 95 ℃ for 8min to remove the solvent, and simultaneously performing the heating, crosslinking and curing effects; taking out, respectively sticking a light-stripping release film and a heavy-stripping release film on the upper surface and the lower surface of the BPPO base film coated with the glue solution for protection to obtain a polyurethane acoustic glue film; the light stripping release film is a PE release film; the heavy stripping release film is a PMMA release film.
A polyurethane acoustic adhesive film obtained according to the production method of the polyurethane acoustic adhesive film.
Comparative example 1
The invention provides a polyurethane acoustic adhesive film, the formula and the production method of which are similar to those of example 1, except that amino-terminated polyurethane is used for replacing polyurethane based on imidazolidinone.
Comparative example 2
The invention provides a polyurethane acoustic adhesive film, the formula and the production method of which are similar to those of example 1, except that hydrogenated rosin is used for replacing epoxy rosin.
Comparative example 3
The invention provides a polyurethane acoustic adhesive film, the formula and the production method of which are similar to those of example 1, except that bis (chloromethyl) tetramethyldisilazane and dichloromethyltriethoxysilane are not added.
The polyurethane acoustic adhesive films produced in the above examples 1 to 5 and comparative examples 1 to 3 were subjected to the related performance tests, and the test results are shown in table 1; the test method is as follows:
(1) thickness uniformity: and (3) testing each roll, namely taking the film material to be 50cm long, selecting 1 point every 10cm in the width direction, selecting 10 points altogether, selecting 10 points at intervals of 10cm in the length direction, and selecting 10 points in the same manner to respectively test the thickness of 20 points, wherein the thickness to be tested must be measured by a micrometer with the precision of 0.1 um.
(2) Adhesive force: sampling 1 volume of 3 groups of data in each batch, testing the adhesive force of the SUS304 mirror panel according to the left, middle and right positions, and then averaging; the adhesive force is a value measured at a tensile angle of 90 degrees and a peel speed of 300 mm/min in accordance with jis z 0237.
(3) Retention force: sampling 1 volume of 3 groups of data in each batch, testing the retention force at 40 ℃ according to the left, middle and right positions, and then taking an average value; the test method was tested with reference to GB 4851-1998.
(4) Initial adhesion: sampling 1 volume of 3 groups of data in each batch, testing the initial adhesive force according to the left, middle and right positions, and then taking an average value; the test method refers to GB/T4852-2002 standard for testing.
(5) Releasing force of the release film: sampling 1 volume of 3 groups of data in each batch, testing the release force according to the left position, the middle position and the right position, and then taking an average value; separately testing the light peeling release force and the heavy peeling release force; the test method refers to the GB/T2792-2014 standard for testing.
TABLE 1
| Item | Tolerance of thickness | Adhesive force | Retention force | Initial adhesion | Light peel off from mold | Heavy peel release force |
| Unit of | μm | N/25mm | mm | - | g/50mm | g/50mm |
| Example 1 | ±1.5 | 4.3 | 8.3 | 8 | 7 | 32 |
| Example 2 | ±1.5 | 4.4 | 8.5 | 8 | 7 | 34 |
| Example 3 | ±1.5 | 4.6 | 8.8 | 8 | 8 | 35 |
| Example 4 | ±1.5 | 4.7 | 9.0 | 9 | 8 | 37 |
| Example 5 | ±1.5 | 4.9 | 9.2 | 9 | 8 | 38 |
| Comparative example 1 | ±1.5 | 3.6 | 7.6 | 6 | 5 | 28 |
| Comparative example 2 | ±1.5 | 4.0 | 8.1 | 7 | 6 | 30 |
| Comparative example 3 | ±1.5 | 3.5 | 7.8 | 6 | 5 | 27 |
As can be seen from table 1, the thickness tolerance of the polyurethane acoustic adhesive film disclosed in the embodiment of the present invention is ± 1.5 um; the adhesive force is more than or equal to 4.3N/25 mm; the retention force is more than or equal to 8.3 mm; the initial adhesion is 8-9; the light release force is (7-8) g/50 mm; the heavy release force is (32-38) g/50 mm; it can be seen that it has a much superior bond strength, which is a result of the synergy of the components.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The production method of the polyurethane acoustic adhesive film is characterized by comprising the following steps of:
step S1, chain extension of amino-terminated polyurethane: adding 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-dione and amino-terminated polyurethane into a high boiling point solvent, adding a basic catalyst into the solvent, stirring the mixture to react for 10 to 15 hours at the temperature of between 75 and 85 ℃, performing rotary evaporation to remove the solvent, adding acetone and water in a mass ratio of 1 (3-4) into the mixture, separating the mixture, taking an organic phase, and performing rotary evaporation to remove the acetone to obtain polyurethane based on imidazolidinone; the molar ratio of the 5, 5-dimethyl-1, 3-di (ethylene oxide methyl) imidazolidine-2, 4-diketone to the amino-terminated polyurethane to the high boiling point solvent to the basic catalyst is 1:1 (6-10) to 0.3-0.5;
step S2, preparation of epoxy rosin: adding hydrogenated rosin, epoxy chloropropane and sodium hydroxide into N-methyl pyrrolidone, stirring and reacting for 3-5 hours at 70-80 ℃, cooling to room temperature, performing rotary evaporation to remove the N-methyl pyrrolidone, washing for 3-6 times with water, and performing rotary evaporation to remove water to obtain epoxy rosin; the molar ratio of the hydrogenated rosin to the epichlorohydrin to the sodium hydroxide to the N-methyl pyrrolidone is 1:1 (0.5-0.8) to (6-10);
step S3, preparation of glue solution: adding the imidazolidinone-based polyurethane prepared in the step S1 and the epoxy rosin prepared in the step S2 into acetone, carrying out ultrasonic treatment for 10-15 minutes, adding bis (chloromethyl) tetramethyldisilazane and dichloromethyl triethoxysilane, and uniformly stirring to obtain a glue solution; the mass ratio of the polyurethane based on the imidazolidinone, the epoxy rosin, the bis (chloromethyl) tetramethyldisilazane and the dichloromethyltriethoxysilane is (3-5) to (2-3) to (0.1-0.2) to 0.3;
step S4, coating: uniformly coating the glue solution on the upper surface and the lower surface of a clean BPPO (crosslinked polystyrene oxide) basement membrane by using an elcometer3700 scraper coater, then putting the BPPO basement membrane into an oven, drying the BPPO basement membrane at 85-95 ℃ for 4-8min to remove the solvent, and simultaneously performing heating, crosslinking and curing; and after taking out, respectively sticking the light-stripping release film and the heavy-stripping release film on the upper surface and the lower surface of the BPPO base film coated with the glue solution for protection, thus obtaining the polyurethane acoustic glue film.
2. The method for producing a polyurethane acoustic adhesive film according to claim 1, wherein the high boiling point solvent is at least one of dimethylsulfoxide, N-dimethylformamide, N-dimethylacetamide, and N-methylpyrrolidone.
3. The method for producing the polyurethane acoustic adhesive film according to claim 1, wherein the basic catalyst is at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, and potassium carbonate.
4. The method for producing a polyurethane acoustic adhesive film according to claim 1, wherein the light release film is one of a PE release film, a PET release film, an OPP release film, and a PC release film.
5. The method for producing a polyurethane acoustic adhesive film according to claim 1, wherein the heavy release liner is one of a PS release liner, a PMMA release liner, and a BOPP release liner.
6. A polyurethane acoustic adhesive film produced by the method for producing a polyurethane acoustic adhesive film according to any one of claims 1 to 5.
7. The polyurethane acoustic adhesive film of claim 6, wherein the polyurethane acoustic film has a thickness tolerance of ± 1.5 um; the adhesive force is more than or equal to 4.3N/25 mm; the retention force is more than or equal to 8.3 mm; the initial adhesion is 8-9; the light release force is (7-8) g/50 mm; the heavy release force is (32-38) g/50 mm.
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| US3971745A (en) * | 1973-12-21 | 1976-07-27 | Minnesota Mining And Manufacturing Company | Amino terminated ionic polyurethane emulsion with polyepoxide emulsion |
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| CN109796768A (en) * | 2019-01-28 | 2019-05-24 | 湖南七纬科技有限公司 | A kind of LED encapsulation material and preparation method thereof |
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| CN101407709B (en) * | 2008-11-26 | 2012-10-17 | 厦门大学 | Preparation of alcohol-soluble bicomponent polyurethane laminating adhesive |
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| US3971745A (en) * | 1973-12-21 | 1976-07-27 | Minnesota Mining And Manufacturing Company | Amino terminated ionic polyurethane emulsion with polyepoxide emulsion |
| CN109467643A (en) * | 2018-09-29 | 2019-03-15 | 苏州市新广益电子有限公司 | A kind of LCP glue film and preparation method thereof for FPC industry |
| CN109796768A (en) * | 2019-01-28 | 2019-05-24 | 湖南七纬科技有限公司 | A kind of LED encapsulation material and preparation method thereof |
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