TWI854657B - Solids granule preparation method - Google Patents

Abstract

A solids granule and preparation method thereof are disclosed. The solids granule includes: a polymer material; an organic solvent; a plasticizer; a bracing granule material; and an auxiliary material; wherein, by weight percentage, the polymer material is 30~60%, the organic solvent is 10~20%, the plasticizer is 15~25%, the bracing granule material is 0.5~10%, and the auxiliary material is 10~15 %. Thereby, a supporting feature of solids granule and its production method could be provided.

Description

Solid particle glue preparation method

The present invention relates to a method for preparing a solid particle colloid, and in particular to a method for preparing a solid particle colloid with support.

General electrolyte colloids, especially when applied to products made of glass, acrylic or other substrates, such as large-area window glass for buildings or current skylight glass for cars and electric vehicles, still have the following disadvantages, such as poor light transmittance, poor conductivity, and uneven concentration distribution. In addition, when applied to large-area substrates, there are more stress and structural force issues that need to be solved. For example, high-rise window glass or current car and electric vehicle windshields are prone to deformation when the substrate is subjected to headwind for a long time, and deformation is likely to cause subsequent substrate rupture under uncertain circumstances, causing danger. In view of the above and other problems, traditional electrolyte colloids need to be improved.

In order to solve the above and other problems, the purpose of the present invention is to provide a method for preparing solid particle glue.

Another purpose of the present invention is to provide a solid particle glue having functions such as high light transmittance, high conductivity and good heat insulation effect.

Another purpose of the present invention is to provide a solid particle colloid that has the functions of providing colloid stability and support.

Another purpose of the present invention is to provide a method for preparing solid particle glue, which has the characteristics of fast process and convenient storage.

Another purpose of the present invention is to provide a solid particle glue and a method for making the same. The solid particle glue can be applied to glass, acrylic or other transparent substrates and can be used for light transmission and heat insulation.

To achieve the above and other purposes, the solid particle glue of the present invention comprises: a polymer material, an organic solvent, a plasticizer, a supporting particle material and an auxiliary material, wherein the weight percentage of the polymer material is 30-60%, the weight percentage of the organic solvent is 10-20%, the weight percentage of the plasticizer is 15-25%, the weight percentage of the supporting particle is 0.5-10%, and the weight percentage of the auxiliary material is 10-15%.

In some embodiments of the present invention, the polymer material is a thermoplastic polymer material or a thermosetting polymer selected from the group consisting of polyvinyl butyral (PVB), vinyl acetate copolymer (EVA), epoxy resin (EP), polyethylene (PE), polyester resin (UPR) and vinyl ester (VER).

In some embodiments of the present invention, the organic solvent is selected from propylene carbonate (PC), ethylene carbonate (EC), butyl propyl carbonate (γ-BL), N-methyl-pyrrolidine (NMP), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), diethyl carbonate (DEC), vinylene carbonate (VC), fluoroethylene carbonate (FEC) or ethyl acetate (EA) and is a high dielectric solvent mixture composed of any one or two or more thereof.

In some embodiments of the present invention, the plasticizer is selected from the group consisting of diethylene glycol monobutyl ether, diisopropyl phthalate (DINP), benzyl butyl phthalate (BBzP, BBP), dioctyl phthalate (DOP, DnOP), diisopropyl phthalate (DIDP), triethyl citrate or adipic acid.

In some embodiments of the present invention, the supporting particle material is preferably fumed silica (FS), silicon oxide (SiO ₂ ), graphite, graphene (rGO), graphene oxide (GO), silica gel or polymethyl methacrylate (PMMA), any one of the above or a mixture of two or more thereof.

In some embodiments of the present invention, the auxiliary material is a toner, a UV absorber, a light stabilizer, a temperature stabilizer (such as ethylene glycol), an antioxidant, lithium hexafluorophosphate (LiPF ₆ ), lithium tetrafluoroborate (LiBF ₄ ), lithium perchlorate (LiClO ₄ ), lithium hexafluoroarsenic phosphate (LiAsF ₆ ), lithium trifluoromethanesulfonate (LiCF ₃ SO ₃ ), lithium bis(trifluoromethylsulfonyl)borate (LiBOB), lithium difluorooxalatoborate (LiODFB), lithium bis(trifluoromethylsulfonyl)imide (LiTFSI), lithium bis(fluorosulfonyl)imide (LiFSI), lithium difluorophosphate (LiPO ₂ F ₂ ), lithium tetrafluorooxalatophosphate (LiFOP), titanium dioxide (TiO ₂ ) powder, tungsten oxide (WO ₃ ) powder or metal powder, any one of the above or a mixture of two or more thereof.

To achieve the above and other purposes, the solid particle preparation method of the present invention comprises: a drying and dehydration step, placing a polymer material at a reaction temperature of 40-80°C for a reaction time of 10-40 minutes to perform dehydration and drying to obtain a dry polymer material; a material mixing step, stirring and dispersing the dry polymer material and a plasticizer with a stirrer, and then mixing a support particle material, an organic solvent and After the auxiliary materials are uniformly mixed, they are added to a stirrer for high-speed uniform stirring to produce a premixed material; and a mixing and rubber-making step, the premixed material is placed in a twin-screw mixer and the reaction temperature is gradually increased to 70-120°C, and the reaction is carried out for 1-15 minutes to obtain a colloid, and the twin-screw mixer is used to fully and uniformly stir the colloid, and the end of the mixer can be combined with a plate press or an extrusion die to produce an embryonic rubber block.

In some embodiments of the present invention, an extrusion granulation step (S3) is further included, wherein the embryonic rubber mass produced in the mixing and rubber-making step (S2) is reinforced using a sieve mill or a bite-type strong pressure sieve mill, and then the materials are mixed evenly using a double-shaft kneader and extruded, and then a high-speed granulator is used to form a granular solid particle rubber.

In some embodiments of the present invention, in the extrusion granulation step, the working temperature is 20-50°C, the extrusion pressure is 0.1-2 MPa, and the particle size of the produced granular solid particle glue is 10 nanometers (nm) to 10 millimeters (mm).

In some embodiments of the present invention, a first solid particle film production step is further included, and the first solid particle film production step is performed after the extrusion granulation step. The first solid particle film production step includes: a heating reaction sub-step, placing the granular solid particle gel at a reaction temperature of 60-120°C for 2-10 minutes; a gelling reaction sub-step, using a mixer to form a plastic solid particle gel from the granular solid particle gel; a melting reaction sub-step, heating the plastic solid particle gel at 80-150°C to melt and form a fluidized solid particle gel; A fluid colloid; a film forming sub-step, in which the fluid colloid is injected into the coating head cavity by the pressure, and the top of the coating head is a fine slit outlet with an adjustable caliber. The fluid colloid flows out of the fine slit outlet of the coating head evenly, and the fluid colloid is formed into a film on the release film as it is coated; and a first cooling forming sub-step, in which the film is rapidly cooled by an air knife to control the film thickness to produce a solid particle film.

In some embodiments of the present invention, a second solid particle film production step is further included, and the second solid particle film production step is performed after the mixing and gelling step. The second solid particle film production step includes: an extrusion casting sub-step, in which the embryonic colloid is first heated to 60-120°C by extrusion casting to become a thick colloid; a colloid refining sub-step, in which the thick colloid is heated and extruded, wherein the extrusion temperature is 80-150°C, and a second cooling molding sub-step, after the thick colloid is heated and extruded, the wind pressure through the air knife nozzle is 95-1000 kPa, and the extrusion pressure is 0.5-2 million Pascals (MPa), and the thick colloid is formed into a solid particle film with a thickness of 0.01-3 mm.

S0: Drying and dehydration step

S1: Material mixing step

S2: Mixing and rubber making step

S3: Extrusion granulation step

S41: The first solid particle film production step

S42: Second solid particle film production step

S410: Heating reaction sub-step

S411: Gelatinization reaction sub-step

S412: Melting reaction sub-step

S413: Film forming sub-step

S414: First cooling and forming sub-step

S420: Extrusion and spreading step

S421: Colloid refining step

S422: Second cooling and molding sub-step

Figure 1 is a flow chart of an embodiment of the solid particle colloid preparation method of the present invention.

Figure 2 is a flow chart of another embodiment of the solid particle colloid preparation method of the present invention.

Figure 3 is a flow chart of another embodiment of the solid particle colloid preparation method of the present invention.

Figure 4 is a flow chart of another embodiment of the solid particle colloid preparation method of the present invention.

In order to make the above and other purposes, effects, and features more clearly understood, some preferred embodiments are cited below, and detailed descriptions are made with reference to the attached drawings. Without departing from the spirit of the creation, this creation has multiple implementation methods and is not limited to the details specifically described in the implementation methods below. The drawings may not be drawn according to the actual scale and are only provided for illustrating the embodiments.

The solid particle glue of this embodiment includes: a polymer material, an organic solvent, a plasticizer, a supporting particle material and an auxiliary material, wherein the weight percentage of the polymer material is 30-60%, the weight percentage of the organic solvent is 10-20%, the weight percentage of the plasticizer is 15-25%, the weight percentage of the supporting particle is 0.5-10%, and the weight percentage of the auxiliary material is 10-15%.

Preferably, the polymer material is a thermoplastic polymer material or a thermosetting polymer selected from the group consisting of polyvinyl butyral (PVB), vinyl acetate copolymer (EVA), epoxy resin (EP), polyethylene (PE), polyester resin (UPR) and vinyl ester (VER).

Preferably, the organic solvent is selected from propylene carbonate (PC), ethylene carbonate (EC), butyl propyl carbonate (γ-BL), N-methyl-pyrrolidine (NMP), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), diethyl carbonate (DEC), vinylene carbonate (VC), fluoroethylene carbonate (FEC) or ethyl acetate (EA) and is a high dielectric solvent mixture composed of any one or two or more thereof.

Preferably, the plasticizer is selected from the group consisting of diethylene glycol monobutyl ether, diisopropyl phthalate (DINP), benzyl butyl phthalate (BBzP, BBP), dioctyl phthalate (DOP, DnOP), diisopropyl phthalate (DIDP), triethyl citrate or adipic acid.

Preferably, the supporting particle material can be an insulator, conductor, semiconductor or polymer material. The supporting particle material is preferably selected from fumed silica (FS), silicon oxide ( _SiO2 ), graphite, graphene (rGO), graphene oxide (GO), silica gel or polymethyl methacrylate (PMMA), any one of the above or a mixture of two or more thereof, wherein the length of the supporting particle material is between 30 and 100 micrometers ( μm ).

When the solid particle glue is applied to substrates such as glass or acrylic, especially large-area substrates such as high-rise window glass or car windshields, the solid particles can buffer the deformation caused by the pressure generated when the glass faces the wind. This is mainly because the solid particles in the solid particle glue have the function of changing stress and improving mechanical strength, which can prevent the glass from breaking due to long-term pressure from facing the wind.

Preferably, the auxiliary material is a toner, a UV absorber, a light stabilizer, a temperature stabilizer (such as ethylene glycol), an antioxidant, lithium hexafluorophosphate (LiPF ₆ ), lithium tetrafluoroborate (LiBF ₄ ), lithium perchlorate (LiClO ₄ ), lithium hexafluoroarsenic phosphate (LiAsF ₆ ), lithium trifluoromethanesulfonate (LiCF ₃ SO ₃ ), lithium bis(trifluoromethylsulfonyl)imide (LiTFSI), lithium bis(fluorosulfonyl)imide (LiFSI), lithium difluorophosphate (LiPO ₂ F ₂ ), lithium tetrafluorooxalatephosphate (LiFOP), titanium dioxide (TiO ₂ ) powder, tungsten oxide (WO ₃ ) powder or metal powder, any one of the above or a mixture of two or more thereof.

The heat insulation effect of the solid particle glue of the present invention is close to the lightweight and heat insulation effect of vacuum glass. It utilizes the non-heat accumulation and diversity of thermal conductivity coefficients of the colloidal material composition, such as the application of silicone materials to effectively block the transfer of heat energy. In general, the manufacturing process of traditional vacuum glass is relatively complicated and cumbersome, mainly because vacuuming is a difficult procedure. Therefore, the solid particle glue of the present invention can effectively shield heat energy by reflecting infrared or ultraviolet rays and constructing low thermal conductivity, which can replace the effect of vacuum glass. It has better heat insulation effect than traditional heat insulation paper that absorbs heat and will not age and deteriorate.

FIG1 is a flow chart of an embodiment of the solid particle glue preparation method of the present invention, please refer to FIG1. The solid particle glue preparation method of the present invention comprises: a drying and dehydration step (S0), placing a polymer material at a reaction temperature of 40-80°C for 10-40 minutes to perform dehydration and drying to obtain a dry polymer material; a material mixing step (S1), stirring and dispersing the dry polymer material and a plasticizer uniformly with a stirrer, and then mixing a support particle material, an organic solvent and an auxiliary agent. After the materials are uniformly mixed, a stirrer is added to stir uniformly at high speed to produce a premixed material; and a mixing and rubber-making step (S2) is performed, wherein the premixed material is placed in a twin-screw mixer and the reaction temperature is gradually increased to 70-120°C, and the reaction is carried out for 1-15 minutes to obtain a colloid, and the twin-screw mixer is used to fully and uniformly stir the colloid, and then the end of the mixer is combined with a plate press or an extrusion die to produce an embryonic rubber block.

FIG2 is a flow chart of an embodiment of the solid particle glue production method of the present invention, please refer to FIG2. Preferably, an extrusion granulation step (S3) is further included. The extrusion granulation step (S3) uses a squeegee or a bite-type strong pressure squeegee to mix the embryonic rubber block produced in the mixing and making glue step (S2), and then uses a double-axis kneader to mix the materials evenly, and then extrude the materials to form granular solid particle glue with a high-speed granulator.

Preferably, in the extrusion granulation step (S3), the working temperature is 20-50°C, the extrusion pressure is 0.1-2 MPa, and the particle size of the produced granular solid particle glue is 0.1-10 mm.

FIG3 is a flow chart of an embodiment of the method for preparing solid particle glue of the present invention. Please refer to FIG3 . Preferably, the solid particle glue manufacturing method of the present invention further comprises a first solid particle glue film production step (S41), and the first solid particle glue film production step (S41) is performed after the extrusion granulation step (S3), wherein the first solid particle glue film production step (S41) comprises: a heating reaction step (S410), placing the granular solid particle glue at a reaction temperature of 60-120°C for 2-10 minutes; a gelling reaction sub-step (S411), using a mixer to form the granular solid particle glue into a plastic solid particle colloid; a melting reaction sub-step (S412), wherein the granular solid particle glue is heated to 100°C and heated to 200°C for 2-10 minutes; a heating reaction sub-step (S413), wherein the granular solid particle glue is heated to 100°C and heated to 200°C for 2-10 minutes; a heating reaction sub-step (S414), wherein the granular solid particle glue is heated to 100°C and heated to 200°C for 2-10 minutes; a heating reaction sub-step (S415), wherein the granular solid particle glue is heated to 100°C and heated to 200°C for 2-10 minutes; a heating reaction sub-step (S416), wherein the granular solid particle glue is heated to 100°C and heated to 200°C for 2-10 minutes; a heating reaction sub-step (S417), wherein the granular solid particle glue is heated to 100°C and heated to 200°C for 2-10 minutes; a heating reaction sub-step (S418), wherein the granular solid particle glue is heated to 100°C and heated to 200°C for 2-10 minutes; a heating reaction sub-step (S419), wherein the granular solid particle glue is heated to 100°C and heated to 200°C for 2-1 S412), the plastic solid particle colloid is heated and melted at 80-150°C to form a fluid colloid; a film forming sub-step (S413), the fluid colloid is injected into the coating head cavity by pressure, the top of the coating head is a slit outlet with an adjustable caliber, the fluid colloid The fluid colloid flows out from the slit outlet of the coating head uniformly, and the fluid colloid runs on the release film to form a colloid film as it is coated; and a first cooling and forming sub-step (S414), the colloid film is quickly cooled by 0~25℃ through compressed air by an air knife, and the thickness of the colloid film is controlled by a roller to produce a solid particle colloid film.

FIG4 is a flow chart of an embodiment of the solid particle glue manufacturing method of the present invention, please refer to FIG4. Preferably, the solid particle glue manufacturing method of the present invention further includes a second solid particle glue film production step (S42), and the second solid particle glue film production step (S42) is performed after the mixing glue making step (S2), wherein the second solid particle glue film production step (S42) includes: an extrusion casting sub-step (S420), in which the embryonic glue block is first heated at 60-120°C to become a thick colloid by extrusion casting; a colloid refining sub-step A first step (S421) is to heat and extrude the thick colloid, wherein the extrusion temperature is 80-150°C; and a second cooling and molding sub-step (S422) is to heat and extrude the thick colloid, and the air pressure through the air knife nozzle is about 95-1000 kPa, the extrusion pressure is 0.5-2 MPa, and the compressed gas temperature is 0-25°C, and the thick colloid is formed into a solid particle film with a thickness of 0.01-3 mm.

In summary, the solid particle glue of the present invention has high cohesive mechanical properties and low fluidity due to the specific components and specific ratios between the components, and the components are evenly dispersed by mixing. The solid particle glue can be used to prepare high electronic insulation ion conductivity glue, high electronic conductivity solid glue or low thermal conductivity insulation glue, and further achieves high ion conductivity, no need for spacers, and can be glued to glass and plastic, achieving high safety without leakage, and at the same time has colloid support, high adhesion, high light transmittance and high conductivity.

In addition, the solid particle glue of the present invention can be applied to the electrolyte layer of electrochromic components and can be made using glue technology. In addition, in known energy storage components such as supercapacitors, lithium polymer batteries, and electrolytes of superbatteries, an isolation film is required to separate the electrodes to prevent the electrodes from conducting. When the solid particle glue of the present invention is made into an ion-conducting glue film, it can be directly used between the two electrodes as a spacer and ion transfer and electron blocking functions. In addition, other applications such as organic optoelectronic components, organic solar components, bioglass, etc. can be designed to be safer and more effective in protecting the UV resistance of organisms and protected objects through the ultraviolet light shielding and visible light transparency characteristics of the glue layer in the laminated glass product design.

This creation has been disclosed using the above-mentioned preferred embodiments, but they are not used to limit this creation. Those with ordinary knowledge in the technical field to which this creation belongs can clearly understand that this creation is not limited to the details of the above-mentioned illustrative implementation methods. The implementation methods are only for explaining this creation, not for limiting this creation. This creation is based on the scope of the patent application, not on the above-mentioned description. The meaning of the scope of the patent application and its equivalent scope are all within the scope of the patent right of this creation.

S0: Drying and dehydration step

S1: Material mixing step

S2: Mixing and rubber making step

Claims (3)

A method for preparing a solid particle glue comprises: a drying and dehydration step (S0), placing a polymer material at a reaction temperature of 40-80°C for a reaction time of 10-40 minutes, dehydrating and drying to obtain a dry polymer material, wherein the polymer material is a thermoplastic polymer material or a thermosetting polymer selected from polyvinyl butyral (PVB), vinyl acetate copolymer (EVA), epoxy resin (EP), A group consisting of any two or more of polyethylene (PE), polyester resin (UPR) and vinyl ester (VER); a material mixing step (S1), wherein the dried polymer material and a plasticizer are uniformly stirred and dispersed, and then a support particle material, an organic solvent and an auxiliary material are uniformly mixed, and then the above-mentioned separately mixed materials are uniformly stirred again at a high speed to prepare a pre-mixed material; a mixing and glue making step ( S2), placing the premixed material in a twin-screw mixer, gradually raising the reaction temperature to 70-120°C, reacting for 1-15 minutes to obtain a colloid, and making the colloid completely and evenly stirred, and producing a green rubber block at the end of the twin-screw mixer by a plate press or an extrusion die; and an extrusion granulation step (S3), using a ripper to granulate the green rubber block produced in the mixing and granulation step (S2). Or a bite-type strong pressure Lina type close kneading machine is used for strengthening, and then a double-shaft kneading machine is used to mix the materials evenly and then extrude them, and then a high-speed granulator is used to form a granular solid particle glue, wherein, in the extrusion granulation step (S3), the working temperature is 20~50℃, the extrusion pressure is 0.1~2 million Pascals (MPa), and the particle size of the granular solid particle glue produced is 0.1~10 mm. The method for preparing the solid particle glue as described in claim 1, further comprising a first solid particle glue film production step (S41), the first solid particle glue film production step (S41) being performed after the extrusion granulation step (S3), wherein the first solid particle glue film production step (S41) comprises: a heating reaction sub-step (S410), placing the granular solid particle glue at a reaction temperature of 60-120°C for 2-10 minutes; a gelling reaction sub-step (S411), using a mixer to form the granular solid particle glue into a plastic solid particle colloid; a melting reaction sub-step (S412), wherein the granular solid particle glue is heated to 120°C for 2-10 minutes; and a melting reaction sub-step (S413). The plastic solid particle colloid is heated and melted at 80-150°C to form a fluid colloid; a film forming sub-step (S413) is performed to inject the fluid colloid into the coating head cavity by pressure, and the top of the coating head is a slit outlet with an adjustable caliber. The colloid flows out from the slit outlet of the coating head uniformly, and the fluid colloid runs on the release film to form a colloid film; and, a first cooling and forming sub-step (S414), the colloid film is quickly cooled by 0~25℃ using compressed air by an air knife, and the thickness of the colloid film is controlled by a roller to produce a solid particle colloid film. The solid particle glue production method as described in claim 2, wherein the second solid particle glue film production step (S42) is further included. The second solid particle glue film production step (S42) is performed after the mixing glue production step (S2), wherein the second solid particle glue film production step (S42) includes: an extrusion casting sub-step (S420), wherein the embryo glue block is first heated at 60-120°C to become a viscous colloid by an extrusion casting method; a colloid refining sub-step (S421), the thick colloid is heated and extruded, wherein the extrusion temperature is 80-150°C; and, a second cooling and molding sub-step (S422), after the thick colloid is heated and extruded, the air pressure through the air knife nozzle is 95-1000 kPa, the extrusion pressure is 0.5-2 MPa, and the compressed gas temperature is 0-25°C, the thick colloid is formed into a solid particle film with a thickness of 0.01-3 mm.

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