CN112011282B - 3D protective film and preparation process thereof - Google Patents
3D protective film and preparation process thereof Download PDFInfo
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Abstract
The invention discloses a 3D protective film and a preparation process thereof, wherein the protective film comprises a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA film layer, a high-viscosity silica gel layer and a fluorine release film layer from top to bottom; the self-repairing TPU film layer adopts a coated hot-melt TPU with good tensile strength, elongation at break and tearing strength, white carbon black is used as a reinforcing adhesive, propylene glycol butyl ether is used as a dispersing agent, and molybdenum disulfide is used as a lubricating agent, so that the coated hot-melt TPU obtains a good lubricating effect, the friction coefficient is greatly reduced, and the repairing effect is improved; the antibacterial filler is prepared by wrapping silver nitrate with alkalized beta-cyclodextrin, so that silver ions can be slowly released to achieve a lasting antibacterial property; the arc-shaped grating layer structure enables the 3D protective film to have good stereoscopic vision effect after being applied to electronic products.
Description
Technical Field
The invention relates to the technical field of screen protection films, in particular to a 3D protection film and a preparation process thereof.
Background
With the popularization of touch screens of electronic products, the screen becomes an operation part, and long-time operation is inevitable and may cause operation on the screen, so people usually stick a protective film on the screen. The early protective film is simple, has no special structure, and does not have the function of preventing the screen from being broken. Along with the development of screen, tempering membrane, 2.5D tempering membrane, 3D tempering membrane etc. have appeared, and this type of protection film can not only prevent that the screen from being scratched, must prevent falling the ability moreover, and the laminating degree with the screen has also obtained promoting by a wide margin simultaneously.
The prior art (CN108116020A) discloses a 3D curved screen TPU protective film and a preparation method thereof, wherein the protective film comprises a matte film layer, a first OCA adhesive layer, a self-repairing layer, a TPU film layer, a bottom coating, a second OCA adhesive layer, a transparent PET layer, a high-viscosity low-peeling silica gel layer and a fluorine film layer which are sequentially attached from top to bottom; the invention has ingenious structural design, reasonably takes the TPU film layer as a base material, has good flexibility, and can be attached to the surface of a 3D curved screen; the TPU film layer is coated with the self-repairing layer, so that the repairing effect is good, and the service life of the TPU film layer is prolonged; wholly peel off the silica gel layer through high viscidity low and closely laminate on the 3D face screen that needs to be protected, carry out the guard action of high strength to 3D face screen. The following technical problems are found through research: 1) the TPU film has no good self-repairing performance, poor tensile strength and insufficient and durable antibacterial performance; 2) do not possess supporting two-sided tectorial membrane hot pressing equipment for production efficiency is low, and the 3D protection film of producing does not possess good fineness and sealed effect.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide a 3D protective film and a preparation process thereof.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a 3D protective film which comprises a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA adhesive layer, a high-viscosity silica gel layer and a fluorine release film layer from top to bottom;
the self-repairing TPU film layer is obtained by coating and curing a self-repairing TPU mixture, and the preparation method of the self-repairing TPU mixture comprises the following steps: according to the weight parts, 80-100 parts of coated hot-melt TPU, 4-8 parts of white carbon black, 5-10 parts of propylene glycol butyl ether, 0.3-0.8 part of molybdenum disulfide and 0.3-0.6 part of antibacterial filler are sequentially added into a reaction kettle, the temperature is increased to 200-220 ℃ at the speed of 10-20 ℃/min, the temperature is increased while stirring is carried out, the stirring speed is 200-300r/min, and the heat preservation and the stirring are carried out for 1-2 hours to obtain the antibacterial polyurethane;
the specific gravity of the coated hot melt grade TPU is 1.11-1.15g/cm3The tensile strength is 32-34MPa, the elongation at break is 510-530 percent, and the tear strength is 110-120 kN/m; SiO of the white carbon black2The content is more than or equal to 96 percent, the particle size is 6-8 mu m, the specific surface area is 220-2/g。
As a further aspect of the present invention, the preparation method of the antibacterial filler is as follows: dissolving 25-30g of beta-cyclodextrin in 150mL of sodium hydroxide solution with the concentration of 0.5mol/L and stirring for 20-30min to obtain a cyclodextrin solution; weighing 1.6-2.2g of silver nitrate, and dissolving in 140mL of ethanol with the volume of 120-; adding the antibacterial agent solution into cyclodextrin solution, heating in water bath at 60-70 deg.C for 4-6 hr, concentrating under reduced pressure to remove water and ethanol, and drying at 80-100 deg.C.
As a further scheme of the invention, the thickness of the dummy film layer and the fluorine release film layer is 40-60 μm, the thickness of the first OCA adhesive layer and the second OCA adhesive layer is 15-18 μm, the thickness of the self-repairing TPU film layer is 100-160 μm, the thickness of the high-viscosity silica gel layer is 18-25 μm, and the grating layer is a grid-shaped stripe which is uniformly arranged.
The invention also provides a preparation process of the 3D protective film, which comprises the following steps:
s1, sequentially adding the coated hot-melt TPU, white carbon black, propylene glycol butyl ether, molybdenum disulfide and antibacterial filler into a reaction kettle, heating to 60-70 ℃, uniformly stirring, heating to 90-100 ℃, stirring for 1-2 hours, and extruding for granulation; introducing the extruded particles into a casting machine to be extruded and cast to obtain a self-repairing TPU film layer, wherein the extrusion temperature is 195-205 ℃;
s2, winding the self-repairing TPU film layer on a unwinding roll of double-faced film-covered hot-pressing equipment, penetrating the unwinding roll, a position between a first upper hot-pressing column and a first lower hot-pressing column and a straightening roll, driving the unwinding roll by a motor to unwind the self-repairing TPU film, and performing hot-pressing molding on the first upper hot-pressing column and the first lower hot-pressing column when passing through a first hot-pressing mechanism;
s3, when the self-repairing TPU film passes through the first film covering mechanism, opening a first adjusting valve and a second adjusting valve, injecting OCA glue in an OCA glue tank into a first upper liquid injection region through a first liquid injection pipe, injecting OCA glue into a first lower liquid injection region through a second liquid injection pipe, and injecting the OCA glue into the upper surface and the lower surface of the self-repairing TPU film after entering an expansion section and a liquid injection section;
s4, enabling a self-repairing TPU film with upper and lower surfaces covered with OCA glue to enter a space between a second upper hot pressing column and a second lower hot pressing column, driving a cam to rotate by a motor, driving a piston to be compressed in a piston cylinder by the cam, enabling a first upper hot pressing area and a first lower hot pressing area to be extruded, and enabling first upper hot pressing rollers and first lower hot pressing rollers which are arranged in a staggered mode to be subjected to hot extrusion, so that an arc-shaped grating layer is formed between the OCA glue layer and the self-repairing TPU film layer, and a film semi-finished product consisting of the first OCA glue layer, the grating layer, the self-repairing TPU film layer and the second OCA glue layer;
s5, enabling a film semi-finished product consisting of the first OCA adhesive layer, the grating layer, the self-repairing TPU film layer and the second OCA adhesive layer to enter a space between a second upper liquid injection region and a second lower liquid injection region through a straightening roller, opening a third regulating valve and a fourth regulating valve, enabling a dummy film layer liquid in a dummy film layer liquid tank to enter the second upper liquid injection region through a third liquid injection pipe, enabling a high-viscosity silica gel layer liquid in the high-viscosity silica gel layer liquid tank to enter the second lower liquid injection region through a fourth liquid injection pipe, enabling the upper surface of the first OCA adhesive layer to be covered with the dummy film layer liquid, and enabling the lower surface of the second OCA adhesive layer to be covered with the high-viscosity silica gel layer;
s6, the cam drives the piston to compress in the piston cylinder body, so that a third upper hot pressing column and a third lower hot pressing column are extruded, and a second upper hot pressing roller and a second lower hot pressing roller are subjected to hot extrusion to obtain a semi-finished film product consisting of a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA adhesive layer and a high-viscosity silica gel layer;
s7, feeding a semi-finished product of the film consisting of the matte film layer, the first OCA adhesive layer, the grating layer, the self-repairing TPU film layer, the second OCA adhesive layer and the high-viscosity silica gel layer into a space between a fourth upper hot pressing column and a third lower liquid injection region through a straightening roller, opening a fifth adjusting valve, covering fluorine release film layer liquid in a fluorine release film layer liquid tank on the lower surface of the semi-finished product of the film through a fifth liquid injection pipe, and carrying out hot press molding on the third upper hot pressing roller to obtain a semi-finished product of the 3D protective film;
and S8, winding the 3D protective film semi-finished product on a winding drum through a winding roller.
As a further scheme of the invention, the temperature of the step S2 hot press molding is 60-80 ℃, the step S4 hot extrusion temperature is 90-110 ℃, the step S6 hot extrusion temperature is 100-120 ℃, and the step S7 hot press molding temperature is 90-110 ℃.
As a further scheme of the invention, the winding speed of the winding roller is the same as the unwinding speed of the unwinding roller and is 2-3 cm/s.
The invention has the beneficial effects that:
1. the 3D protective film comprises a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA adhesive layer, a high-viscosity silica gel layer and a fluorine release film layer from top to bottom; the self-repairing TPU film layer adopts a coated hot-melt TPU with good tensile strength, elongation at break and tearing strength, white carbon black is used as a reinforcing adhesive, propylene glycol butyl ether is used as a dispersing agent, and molybdenum disulfide is used as a lubricating agent, so that the coated hot-melt TPU obtains a good lubricating effect, the friction coefficient is greatly reduced, and the repairing effect is improved; the antibacterial filler is prepared by wrapping silver nitrate with alkalized beta-cyclodextrin, so that silver ions can be slowly released to achieve a lasting antibacterial property; the arc-shaped grating layer structure enables the 3D protective film to have good stereoscopic vision effect after being applied to electronic products. Detecting that the light transmittance is more than 90%, scratching 1 x 10mm on the film in a repair experiment, blowing for 20s by a hot air blower at the temperature of 45 ℃ in the repair experiment, standing for 5min, and observing that only slight scratches are formed; the tensile strength is 35.8-36.4MPa, the bacteriostasis rate of escherichia coli is 89-92%, and the bacteriostasis rate of staphylococcus aureus is 86-91%.
2. The preparation process of the 3D protective film comprises the steps of firstly preparing a self-repairing TPU film layer, then carrying out double-sided coating or hot pressing on the self-repairing TPU film layer by adopting double-sided film-coating hot pressing equipment to sequentially obtain each hierarchical structure, and carrying out hot press molding on the self-repairing TPU film layer by using a first upper hot pressing column and a first lower hot pressing column; OCA glue in the OCA glue tank is injected into the first upper liquid injection region through the first liquid injection pipe and is injected into the first lower liquid injection region through the second liquid injection pipe, and the OCA glue enters the expansion section and the liquid injection section and is injected into the upper surface and the lower surface of the self-repairing TPU film; extruding the first upper hot pressing area and the first lower hot pressing area, and hot extruding the first upper hot pressing rollers and the first lower hot pressing rollers which are arranged in a staggered mode to enable a fluctuant grating layer to be formed between the OCA adhesive layer and the self-repairing TPU film layer, so that a film semi-finished product consisting of the first OCA adhesive layer, the grating layer, the self-repairing TPU film layer and the second OCA adhesive layer is obtained; the matte layer liquid in the matte layer liquid tank enters a second upper liquid injection area through a third liquid injection pipe, and the high-viscosity silica gel layer liquid in the high-viscosity silica gel layer liquid tank enters a second lower liquid injection area through a fourth liquid injection pipe, so that the upper surface of the first OCA glue layer is covered with the matte layer liquid, and the lower surface of the second OCA glue layer is covered with the high-viscosity silica gel layer liquid; carrying out hot extrusion on the second upper hot-pressing roller and the second lower hot-pressing roller to obtain a semi-finished film product consisting of a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA film layer and a high-viscosity silica gel layer; the fluorine release film layer liquid in the fluorine release film layer liquid tank passes through a fifth liquid injection pipe and then covers the lower surface of the film semi-finished product, and a third upper hot press roller is used for hot press forming to obtain a 3D protective film semi-finished product; a plurality of hot pressing mechanisms and tectorial membrane mechanism have improved the production efficiency of 3D protection film, and the 3D protection film of producing possesses good fineness and sealed effect.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic structural diagram of a double-sided laminating hot-pressing apparatus according to the present invention.
Fig. 2 is a partial enlarged view of the invention at a in fig. 1.
Fig. 3 is a partial enlarged view of the present invention at B in fig. 1.
Fig. 4 is a partial enlarged view of the invention at C in fig. 1.
Fig. 5 is an enlarged view of a portion of the invention at D in fig. 1.
In the figure: 1. hot-pressing the shell; 2. placing the winding drum; 3. unwinding rollers; 4. a wind-up roll; 5. winding the roll; 6. a piston cylinder; 7. an oil nip; 8. a piston; 9. a cam; 11. a first upper heat pressing column; 12. a first lower hot pressing column; 13. a first upper liquid injection zone; 14. a first lower liquid pouring zone; 15. a first liquid injection pipe; 16. a first regulating valve; 17. a second liquid injection pipe; 18. a second regulating valve; 19. a liquid injection part; 20. a second upper hot pressing column; 21. a second lower hot pressing column; 22. a first upper hot pressing zone; 23. a first lower hot nip; 24. a first upper hot press roll; 25. a first lower hot press roll; 26. a second upper liquid injection zone; 27. a second lower pour zone; 28. a third liquid injection pipe; 29. a third regulating valve; 30. a fourth liquid injection pipe; 31. a fourth regulating valve; 32. a third upper hot pressing column; 33. a third lower hot pressing column; 34. a second upper hot nip; 35. a second lower hot nip; 36. a second upper hot press roll; 37. a second lower hot press roll; 38. a fourth upper hot pressing column; 39. a third lower pour zone; 40. a third upper hot press roll; 41. a fifth liquid injection pipe; 42. a straightening roll; 43. a fifth regulating valve; 191. an expansion section; 192. a liquid injection section; 193. a liquid storage section.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious 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.
Example 1
Referring to fig. 1 to 5, the 3D protective film of the present embodiment includes, from top to bottom, a matte film layer, a first OCA adhesive layer, a grating layer, a self-repairing TPU film layer, a second OCA adhesive layer, a high-viscosity silica gel layer, and a fluorine release film layer; the thickness of the matte film layer and the fluorine release film layer is 40-60 mu m, the thickness of the first OCA adhesive layer and the second OCA adhesive layer is 15-18 mu m, the thickness of the self-repairing TPU film layer is 100-160 mu m, the thickness of the high-viscosity silica gel layer is 18-25 mu m, and the grating layer is grid-shaped stripes which are uniformly arranged.
The self-repairing TPU film layer is obtained by coating and curing a self-repairing TPU mixture, and the preparation method of the self-repairing TPU mixture comprises the following steps: according to parts by weight, 95 parts of hot-melt-grade coated TPU, 7 parts of white carbon black, 7 parts of propylene glycol butyl ether, 0.6 part of molybdenum disulfide and 0.4 part of antibacterial filler are sequentially added into a reaction kettle, the temperature is increased to 215 ℃ at the speed of 16 ℃/min, the temperature is increased while stirring, the stirring speed is 260r/min, and the heat preservation and the stirring are carried out for 1.5 hours to obtain the antibacterial polyurethane; the specific gravity of the coated hot melt grade TPU is 1.11-1.15g/cm3The tensile strength is 32-34MPa, the elongation at break is 510-530 percent, and the tear strength is 110-120 percentkN/m; SiO of the white carbon black2The content is more than or equal to 96 percent, the particle size is 6-8 mu m, the specific surface area is 220-2/g。
The preparation method of the antibacterial filler comprises the following steps: dissolving 27g of beta-cyclodextrin in 136mL of sodium hydroxide solution with the concentration of 0.5mol/L, and stirring for 25min to obtain a cyclodextrin solution; weighing 1.8g of silver nitrate, and dissolving in 132mL of ethanol to obtain an antibacterial agent solution; adding the antibacterial agent solution into cyclodextrin solution, heating in 65 deg.C water bath for 5.5 hr, concentrating under reduced pressure to remove water and ethanol, and drying at 92 deg.C.
The preparation process of the 3D protective film of the embodiment includes the following steps:
s1, sequentially adding the coated hot-melt TPU, white carbon black, propylene glycol butyl ether, molybdenum disulfide and antibacterial filler into a reaction kettle, heating to 65 ℃, uniformly stirring, heating to 92 ℃, stirring for 1.2 hours, and extruding for granulation; introducing the extruded particles into a casting machine to be extruded and cast to obtain a self-repairing TPU film layer, wherein the extrusion temperature is 201 ℃;
s2, winding the self-repairing TPU film layer on the unwinding cylinder 2 of the double-faced film-covering hot-pressing equipment, penetrating through the unwinding roller 3, a position between the first upper hot-pressing column 11 and the first lower hot-pressing column 12 and the straightening roller 42, driving the unwinding cylinder 2 by a motor to unwind the self-repairing TPU film, and performing hot-pressing forming on the first upper hot-pressing column 11 and the first lower hot-pressing column 12 when passing through the first hot-pressing mechanism;
s3, when the self-repairing TPU film passes through the first film covering mechanism, the first adjusting valve 16 and the second adjusting valve 18 are opened, OCA glue in the OCA glue tank is injected into the first upper liquid injection zone 13 through the first liquid injection pipe 15 and is injected into the first lower liquid injection zone 14 through the second liquid injection pipe 17, and the OCA glue enters the expansion section 191 and the liquid injection section 192 and then is injected into the upper surface and the lower surface of the self-repairing TPU film;
s4, enabling a self-repairing TPU film with OCA glue coated on the upper and lower surfaces to enter a space between a second upper hot pressing column 20 and a second lower hot pressing column 21, driving a cam 9 to rotate by a motor, driving a piston 8 to be compressed in a piston cylinder body 6 by the cam 9, extruding a first upper hot pressing area 22 and a first lower hot pressing area 23, and thermally extruding first upper hot pressing rollers 24 and first lower hot pressing rollers 25 which are arranged in a staggered mode to form an arc-shaped grating layer between an OCA glue layer and a self-repairing TPU film layer, so that a film semi-finished product consisting of the first OCA glue layer, the grating layer, the self-repairing TPU film layer and the second OCA glue layer is obtained;
s5, enabling a semi-finished film product composed of the first OCA adhesive layer, the grating layer, the self-repairing TPU film layer and the second OCA adhesive layer to enter a space between the second upper liquid injection region 26 and the second lower liquid injection region 27 through a straightening roller, opening a third adjusting valve 29 and a fourth adjusting valve 31, enabling the dummy film layer liquid in the dummy film layer liquid tank to enter the second upper liquid injection region 26 through a third liquid injection pipe 28, enabling the high-viscosity silica gel layer liquid in the high-viscosity silica gel layer liquid tank to enter the second lower liquid injection region 27 through a fourth liquid injection pipe 30, enabling the upper surface of the first OCA adhesive layer to be covered with the dummy film layer liquid, and enabling the lower surface of the second OCA adhesive layer to be covered with the high-viscosity silica gel layer;
s6, the cam 9 drives the piston 8 to compress in the piston cylinder 6, so that the third upper hot-pressing column 32 and the third lower hot-pressing column 33 are extruded, and the second upper hot-pressing roller 36 and the second lower hot-pressing roller 37 are subjected to hot extrusion to obtain a semi-finished film product consisting of a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA (optical clear adhesive) layer and a high-viscosity silica gel layer;
s7, feeding a semi-finished film product consisting of a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA film layer and a high-viscosity silica gel layer into a space between the fourth upper hot pressing column 38 and the third lower liquid injection zone 39 through a straightening roller 42, opening a fifth adjusting valve 43, covering fluorine release film layer liquid in a fluorine release film layer liquid tank on the lower surface of the semi-finished film product through a fifth liquid injection pipe 41, and carrying out hot press molding on the third upper hot pressing roller 40 to obtain a semi-finished 3D protective film product;
and S8, winding the 3D protective film semi-finished product on a winding drum 5 through a winding roller 4.
Wherein the hot press forming temperature in the step S2 is 75 ℃, the hot extrusion temperature in the step S4 is 106 ℃, the hot extrusion temperature in the step S6 is 110 ℃, and the hot press forming temperature in the step S7 is 105 ℃. The winding speed of the winding roller 4 is the same as the unwinding speed of the unwinding roller 3 and is 2.6 cm/s.
The 3D protective film of the embodiment is detected to have the light transmittance of more than 90 percent, 1 x 10mm scratches are firstly drawn on the film in a repair experiment, after the film is swept by a hot air blower at 45 ℃ for 20s in the experiment, the film is kept still for 5min, only slight scratches are observed, the tensile strength is 36.4MPa, the antibacterial rate of escherichia coli is 92 percent, and the antibacterial rate of staphylococcus aureus is 91 percent.
Example 2
Referring to fig. 1 to 5, the 3D protective film of the present embodiment includes, from top to bottom, a matte film layer, a first OCA adhesive layer, a grating layer, a self-repairing TPU film layer, a second OCA adhesive layer, a high-viscosity silica gel layer, and a fluorine release film layer; the thickness of the matte film layer and the fluorine release film layer is 40-60 mu m, the thickness of the first OCA adhesive layer and the second OCA adhesive layer is 15-18 mu m, the thickness of the self-repairing TPU film layer is 100-160 mu m, the thickness of the high-viscosity silica gel layer is 18-25 mu m, and the grating layer is grid-shaped stripes which are uniformly arranged.
The self-repairing TPU film layer is obtained by coating and curing a self-repairing TPU mixture, and the preparation method of the self-repairing TPU mixture comprises the following steps: according to the weight parts, 88 parts of hot-melt-grade coated TPU, 6 parts of white carbon black, 9 parts of propylene glycol butyl ether, 0.7 part of molybdenum disulfide and 0.5 part of antibacterial filler are sequentially added into a reaction kettle, the temperature is raised to 216 ℃ at the speed of 18 ℃/min, the stirring is carried out while the temperature is raised, the stirring speed is 230r/min, and the heat preservation and the stirring are carried out for 1.3 hours to obtain the antibacterial polyurethane; the specific gravity of the coated hot melt grade TPU is 1.11-1.15g/cm3The tensile strength is 32-34MPa, the elongation at break is 510-530 percent, and the tear strength is 110-120 kN/m; SiO of the white carbon black2The content is more than or equal to 96 percent, the particle size is 6-8 mu m, the specific surface area is 220-2/g。
The preparation method of the antibacterial filler comprises the following steps: dissolving 29g of beta-cyclodextrin in 142mL of sodium hydroxide solution with the concentration of 0.5mol/L, and stirring for 28min to obtain a cyclodextrin solution; weighing 2.1g of silver nitrate, and dissolving in 135mL of ethanol to obtain an antibacterial agent solution; adding the antibacterial agent solution into cyclodextrin solution, heating in 67 deg.C water bath for 5 hr, concentrating under reduced pressure to remove water and ethanol, and drying at 95 deg.C.
The preparation process of the 3D protective film in this embodiment is different from that in embodiment 1, in step S1, sequentially adding the coated hot-melt TPU, white carbon black, propylene glycol butyl ether, molybdenum disulfide, and the antibacterial filler into a reaction kettle, heating to 70 ℃, uniformly stirring, heating to 98 ℃, stirring for 1.7 hours, and extruding for granulation; introducing the extruded particles into a casting machine to be extruded and cast to obtain a self-repairing TPU film layer, wherein the extrusion temperature is 203 ℃; the hot press forming temperature of the step S2 is 75 ℃, the hot extrusion temperature of the step S4 is 106 ℃, the hot extrusion temperature of the step S6 is 113 ℃, and the hot press forming temperature of the step S7 is 103 ℃. The winding speed of the winding roller 4 is the same as the unwinding speed of the unwinding roller 3 and is 2.2 cm/s.
The 3D protective film of the embodiment is detected to have the light transmittance of more than 90 percent, 1 x 10mm scratches are firstly drawn on the film in a repair experiment, after the film is swept by a hot air blower at 45 ℃ for 20s in the experiment, the film is kept still for 5min, only slight scratches are observed, the tensile strength is 36.0MPa, the antibacterial rate of escherichia coli is 91 percent, and the antibacterial rate of staphylococcus aureus is 88 percent.
Example 3
Referring to fig. 1 to 5, the 3D protective film of the present embodiment includes, from top to bottom, a matte film layer, a first OCA adhesive layer, a grating layer, a self-repairing TPU film layer, a second OCA adhesive layer, a high-viscosity silica gel layer, and a fluorine release film layer; the thickness of the matte film layer and the fluorine release film layer is 40-60 mu m, the thickness of the first OCA adhesive layer and the second OCA adhesive layer is 15-18 mu m, the thickness of the self-repairing TPU film layer is 100-160 mu m, the thickness of the high-viscosity silica gel layer is 18-25 mu m, and the grating layer is grid-shaped stripes which are uniformly arranged.
The self-repairing TPU film layer is obtained by coating and curing a self-repairing TPU mixture, and the preparation method of the self-repairing TPU mixture comprises the following steps: according to the weight parts, 90 parts of hot-melt coated TPU, 8 parts of white carbon black, 9 parts of propylene glycol butyl ether, 0.7 part of molybdenum disulfide and 0.3 part of antibacterial filler are sequentially added into a reaction kettle, the temperature is raised to 206 ℃ at the speed of 18 ℃/min, the stirring is carried out while the temperature is raised, the stirring speed is 260r/min, and the heat preservation and the stirring are carried out for 1.5 hours to obtain the antibacterial polyurethane; the specific gravity of the coated hot melt grade TPU is 1.11-1.15g/cm3The tensile strength is 32-34MPa, the elongation at break is 510-530 percent, and the tear strength is 110-120 kN/m; SiO of the white carbon black2The content is more than or equal to 96 percent, the particle size is 6-8 mu m, the specific surface area is 220-2/g。
The preparation method of the antibacterial filler comprises the following steps: dissolving 27g of beta-cyclodextrin in 136mL of sodium hydroxide solution with the concentration of 0.5mol/L, and stirring for 25min to obtain a cyclodextrin solution; weighing 1.8g of silver nitrate, and dissolving in 132mL of ethanol to obtain an antibacterial agent solution; adding the antibacterial agent solution into cyclodextrin solution, heating in 65 deg.C water bath for 5.5 hr, concentrating under reduced pressure to remove water and ethanol, and drying at 92 deg.C.
The preparation process of the 3D protective film in this embodiment is different from that in embodiment 1, in step S1, sequentially adding the coated hot-melt TPU, white carbon black, propylene glycol butyl ether, molybdenum disulfide, and the antibacterial filler into a reaction kettle, heating to 69 ℃, stirring uniformly, heating to 96 ℃, stirring for 2 hours, and extruding for granulation; introducing the extruded particles into a casting machine to be extruded and cast to obtain a self-repairing TPU film layer, wherein the extrusion temperature is 204 ℃; the hot press forming temperature of the step S2 is 76 ℃, the hot extrusion temperature of the step S4 is 108 ℃, the hot extrusion temperature of the step S6 is 114 ℃, and the hot press forming temperature of the step S7 is 105 ℃. The winding speed of the winding roller 4 is the same as the unwinding speed of the unwinding roller 3 and is 3 cm/s.
The 3D protective film of the embodiment is detected to have the light transmittance of more than 90 percent, 1 x 10mm scratches are firstly drawn on the film in a repair experiment, after the film is swept by a hot air blower at 45 ℃ for 20s in the experiment, the film is kept still for 5min, only slight scratches are observed, the tensile strength is 35.8MPa, the antibacterial rate of escherichia coli is 89 percent, and the antibacterial rate of staphylococcus aureus is 86 percent.
Example 4
Referring to fig. 1-5, the present embodiment provides a double-sided film-coating hot-pressing apparatus, including a hot-pressing housing 1, an unwinding cylinder 2, an unwinding roller 3, a winding roller 4, and a winding cylinder 5, wherein the unwinding cylinder 2 is wound with a self-repairing TPU film and is disposed on one side of the hot-pressing housing 1, the unwinding roller 3 is disposed between the unwinding cylinder 2 and the hot-pressing housing 1, the winding cylinder 5 is wound with a 3D protective film semi-finished product and is disposed on the other side of the hot-pressing housing 1, and the winding roller 4 is disposed between the winding cylinder 5 and the hot-pressing housing 1.
The cross-section of hot pressing casing 1 is rectangle, and one side center part of hot pressing casing 1 is equipped with piston cylinder body 6, and the inside of hot pressing casing 1 is equipped with oil pressure district 7, and piston cylinder body 6 and oil pressure district 7 intercommunication and the inside hydraulic oil that is full of the two, and the radial direction slip of piston cylinder body 6 is provided with piston 8, and the piston contact is provided with cam 9, and cam 9 passes through motor drive piston 8 and follows piston cylinder body 6 radial movement. The inner cavity of the hot pressing shell 1 is sequentially provided with a first hot pressing mechanism, a first laminating mechanism, a second hot pressing mechanism, a second laminating mechanism, a third hot pressing mechanism and a laminating hot pressing mechanism from the side close to the piston cylinder 6 to the side far away from the piston cylinder 6.
The first hot pressing mechanism comprises a first upper hot pressing column 11 and a first lower hot pressing column 12, the first upper hot pressing column 11 and the first lower hot pressing column 12 are T-shaped and are symmetrically arranged, one end of each of the first upper hot pressing column 11 and the corresponding end of the corresponding first lower hot pressing column 12 are slidably connected with the oil pressure area 7, and the area opposite to the other end of each of the first upper hot pressing column 11 and the corresponding area of the corresponding first lower hot pressing column 12 penetrates through the self-repairing TPU film. First tectorial membrane mechanism includes that first notes liquid district 13, first liquid district 14 of annotating once, and first notes liquid district 13 and first liquid district 14 of annotating once are the bellows on first, and first notes liquid district 13 is connected with OCA glue can through first notes liquid pipe 15, first governing valve 16 on first, and first liquid district 14 of pouring down is connected with OCA glue can through second notes liquid pipe 17, second governing valve 18. The bottom of the first upper liquid injection zone 13 and the top of the first lower liquid injection zone 14 are provided with liquid injection parts 19 correspondingly. The liquid injection part 19 comprises an expansion section 191 and liquid injection sections 192, the expansion section 191 is arranged at the bottom of the first upper liquid injection area 13 and the top of the first lower liquid injection area 14, the liquid injection sections 192 are distributed at the end parts of the expansion section 191 in a horizontal array mode, and liquid storage sections 193 are connected between the adjacent liquid injection sections 192.
Hot pressing column 20, hot pressing column 21 under the second are drawn together to hot pressing mechanism on the second and include that hot pressing column 20, hot pressing column 21 are T shape and symmetry setting under the second on the second, hot pressing column 20 and second one end and oil pressure district 7 sliding connection of hot pressing column 21 down on the second, and the relative region of other end has passed interior outer surface hot pressing and has had the semi-manufactured goods of membrane of constituteing by first OCA glue film, selfreparing TPU rete, second OCA glue film. The bottom of the second upper hot pressing column 20 is provided with a first upper hot pressing area 22, the top of the second lower hot pressing column 21 is provided with a first lower hot pressing area 23, a plurality of first upper hot pressing rollers 24 are arranged in parallel in the first upper hot pressing area 22, a plurality of first lower hot pressing rollers 25 are arranged in parallel in the first lower hot pressing area 23, the first upper hot pressing rollers 24 and the first lower hot pressing rollers 25 are arranged in a staggered mode, the distance between the bottom of the first upper hot pressing rollers 24 and the top of the first lower hot pressing rollers 25 is 0.1-0.3 mu m, and the diameters of the first upper hot pressing rollers 24 and the first lower hot pressing rollers 25 are 0.5-0.8 mu m.
The second laminating mechanism comprises a second upper liquid injection area 26 and a second lower liquid injection area 27, the second upper liquid injection area 26 and the second lower liquid injection area 27 are both corrugated pipes, the second upper liquid injection area 26 is connected with the dumb film layer liquid tank through a third liquid injection pipe 28 and a third regulating valve 29, and the second lower liquid injection area 27 is connected with the high-viscosity silica gel layer liquid tank through a fourth liquid injection pipe 30 and a fourth regulating valve 31. The bottom of the second upper liquid injection zone 26 and the top of the second lower liquid injection zone 27 are provided with liquid injection parts 19.
Third hot pressing mechanism includes hot pressing post 32 on the third that hot pressing mechanism includes the third, hot pressing post 33 under the third, hot pressing post 32 on the third, hot pressing post 33 is T shape and symmetry setting down under the third, hot pressing post 32 and third are gone up hot pressing post 33's one end and oil pressure district 7 sliding connection down on the third, the relative region of other end has passed inside and outside surface hot pressing has the semi-manufactured goods of membrane of compriseing dumb rete, first OCA glue film, the grating layer, the selfreparing TPU rete, the OCA glue film of second, high viscose silica gel layer. The bottom of hot pressing post 32 is equipped with hot nip 34 on the third, and the top of hot pressing post 33 is equipped with hot nip 35 under the second under the third, and hot nip 34 is gone up to the second parallel is equipped with hot-pressing roller 36 on a plurality of second, and hot nip 35 is gone up to the second parallel is equipped with hot-pressing roller 37 under a plurality of second, and hot-pressing roller 36 and second hot-pressing roller 37 symmetry setting are gone up to the second.
The film laminating hot-pressing mechanism comprises a fourth upper hot-pressing column 38 and a third lower liquid injection area 39, wherein the fourth upper hot-pressing column 38 is inverted T-shaped, one end of the fourth upper hot-pressing column is connected with the oil pressure area 7 in a sliding mode, and the other end of the fourth upper hot-pressing column is provided with a plurality of parallel third upper hot-pressing rollers 40. The third lower liquid injection zone 39 is a corrugated pipe and is connected with the fluorine release film layer liquid tank through a fifth liquid injection pipe 41 and a fifth regulating valve 43, and the top of the third lower liquid injection zone 39 is correspondingly provided with a liquid injection part 19.
Straightening rollers 42 are arranged between the first hot-pressing mechanism and the first film laminating mechanism, between the second hot-pressing mechanism and the second film laminating mechanism, between the second film laminating mechanism and the third hot-pressing mechanism, and between the third hot-pressing mechanism and the film laminating hot-pressing mechanism.
The working method of the double-sided laminating hot-pressing equipment of the embodiment is as follows:
s1, winding the self-repairing TPU film layer on the unwinding roll 2, enabling the self-repairing TPU film layer to penetrate through the unwinding roll 3, a position between the first upper hot pressing column 11 and the first lower hot pressing column 12 and the straightening roll 42, enabling the motor to drive the unwinding roll 2 to unwind the self-repairing TPU film, and enabling the first upper hot pressing column 11 and the first lower hot pressing column 12 to be subjected to hot press forming when passing through the first hot pressing mechanism;
s2, when the self-repairing TPU film passes through the first film covering mechanism, the first adjusting valve 16 and the second adjusting valve 18 are opened, OCA glue in the OCA glue tank is injected into the first upper liquid injection zone 13 through the first liquid injection pipe 15 and is injected into the first lower liquid injection zone 14 through the second liquid injection pipe 17, and the OCA glue enters the expansion section 191 and the liquid injection section 192 and then is injected into the upper surface and the lower surface of the self-repairing TPU film;
s3, enabling a self-repairing TPU film with OCA glue coated on the upper and lower surfaces to enter a space between a second upper hot pressing column 20 and a second lower hot pressing column 21, driving a cam 9 to rotate by a motor, driving a piston 8 to be compressed in a piston cylinder body 6 by the cam 9, extruding a first upper hot pressing area 22 and a first lower hot pressing area 23, and thermally extruding first upper hot pressing rollers 24 and first lower hot pressing rollers 25 which are arranged in a staggered mode to form an arc-shaped grating layer between an OCA glue layer and a self-repairing TPU film layer, so that a film semi-finished product consisting of the first OCA glue layer, the grating layer, the self-repairing TPU film layer and the second OCA glue layer is obtained;
s4, enabling a semi-finished film product composed of the first OCA adhesive layer, the grating layer, the self-repairing TPU film layer and the second OCA adhesive layer to enter a space between the second upper liquid injection region 26 and the second lower liquid injection region 27 through a straightening roller, opening a third adjusting valve 29 and a fourth adjusting valve 31, enabling the dummy film layer liquid in the dummy film layer liquid tank to enter the second upper liquid injection region 26 through a third liquid injection pipe 28, enabling the high-viscosity silica gel layer liquid in the high-viscosity silica gel layer liquid tank to enter the second lower liquid injection region 27 through a fourth liquid injection pipe 30, enabling the upper surface of the first OCA adhesive layer to be covered with the dummy film layer liquid, and enabling the lower surface of the second OCA adhesive layer to be covered with the high-viscosity silica gel layer;
s5, the cam 9 drives the piston 8 to compress in the piston cylinder 6, so that the third upper hot-pressing column 32 and the third lower hot-pressing column 33 are extruded, and the second upper hot-pressing roller 36 and the second lower hot-pressing roller 37 are subjected to hot extrusion to obtain a semi-finished film product consisting of a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA (optical clear adhesive) layer and a high-viscosity silica gel layer;
s6, feeding a semi-finished film product consisting of a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA film layer and a high-viscosity silica gel layer into a space between the fourth upper hot pressing column 38 and the third lower liquid injection zone 39 through a straightening roller 42, opening a fifth adjusting valve 43, covering fluorine release film layer liquid in a fluorine release film layer liquid tank on the lower surface of the semi-finished film product through a fifth liquid injection pipe 41, and carrying out hot press molding on the third upper hot pressing roller 40 to obtain a semi-finished 3D protective film product;
and S7, winding the 3D protective film semi-finished product on a winding drum 5 through a winding roller 4.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (1)
1. A3D protective film is characterized by comprising a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA adhesive layer, a high-viscosity silica gel layer and a fluorine release film layer from top to bottom;
the self-repairing TPU film layer is obtained by coating and curing a self-repairing TPU mixture, and the preparation method of the self-repairing TPU mixture comprises the following steps: according to the weight parts, 80-100 parts of coated hot-melt TPU, 4-8 parts of white carbon black, 5-10 parts of propylene glycol butyl ether, 0.3-0.8 part of molybdenum disulfide and 0.3-0.6 part of antibacterial filler are sequentially added into a reaction kettle, the temperature is increased to 200-220 ℃ at the speed of 10-20 ℃/min, the temperature is increased while stirring is carried out, the stirring speed is 200-300r/min, and the heat preservation and the stirring are carried out for 1-2 hours to obtain the antibacterial polyurethane;
the specific gravity of the coated hot melt grade TPU is 1.11-1.15g/cm3The tensile strength is 32-34MPa, the elongation at break is 510-530 percent, and the tear strength is 110-120 kN/m; SiO of the white carbon black2The content is more than or equal to 96 percent, the particle size is 6-8 mu m, the specific surface area is 220-2/g；
The preparation method of the antibacterial filler comprises the following steps: dissolving 25-30g of beta-cyclodextrin in 150mL of sodium hydroxide solution with the concentration of 0.5mol/L and stirring for 20-30min to obtain a cyclodextrin solution; weighing 1.6-2.2g of silver nitrate, and dissolving in 140mL of ethanol with the volume of 120-; adding the antibacterial agent solution into cyclodextrin solution, heating in water bath at 60-70 deg.C for 4-6 hr, concentrating under reduced pressure to remove water and ethanol, and drying at 80-100 deg.C;
the thickness of the matte film layer and the fluorine release film layer is 40-60 mu m, the thickness of the first OCA adhesive layer and the second OCA adhesive layer is 15-18 mu m, the thickness of the self-repairing TPU film layer is 100-160 mu m, the thickness of the high-viscosity silica gel layer is 18-25 mu m, and the grating layer is uniformly arranged grid-shaped stripes;
the preparation process of the 3D protective film comprises the following steps:
s1, sequentially adding the coated hot-melt TPU, white carbon black, propylene glycol butyl ether, molybdenum disulfide and antibacterial filler into a reaction kettle, heating to 60-70 ℃, uniformly stirring, heating to 90-100 ℃, stirring for 1-2 hours, and extruding for granulation; introducing the extruded particles into a casting machine to be extruded and cast to obtain a self-repairing TPU film layer, wherein the extrusion temperature is 195-205 ℃;
s2, winding the self-repairing TPU film layer on an unwinding cylinder (2) of double-faced film-covering hot-pressing equipment, enabling the self-repairing TPU film layer to penetrate through an unwinding roller (3), a position between a first upper hot-pressing column (11) and a first lower hot-pressing column (12) and a straightening roller (42), driving the unwinding cylinder (2) by a motor to unwind the self-repairing TPU film, and carrying out hot-pressing forming on the first upper hot-pressing column (11) and the first lower hot-pressing column (12) when passing through a first hot-pressing mechanism;
s3, when the self-repairing TPU film passes through the first film covering mechanism, opening a first adjusting valve (16) and a second adjusting valve (18), injecting OCA glue in an OCA glue tank into a first upper liquid injection zone (13) through a first liquid injection pipe (15), injecting the OCA glue into a first lower liquid injection zone (14) through a second liquid injection pipe (17), and injecting the OCA glue into the upper surface and the lower surface of the self-repairing TPU film after entering an expansion section (191) and a liquid injection section (192);
s4, enabling a self-repairing TPU film with upper and lower surfaces covered with OCA glue to enter a space between a second upper hot pressing column (20) and a second lower hot pressing column (21), driving a cam (9) to rotate by a motor, driving a piston (8) to compress in a piston cylinder body (6) by the cam (9), enabling a first upper hot pressing area (22) and a first lower hot pressing area (23) to be extruded, and enabling first upper hot pressing rollers (24) and first lower hot pressing rollers (25) which are arranged in a staggered mode to be subjected to hot extrusion, so that an arc-shaped grating layer is formed between the OCA glue layer and the TPU film layer, and a film semi-finished product consisting of the first OCA glue layer, the grating layer, the self-repairing TPU film layer and the second OCA glue layer is obtained;
s5, enabling a semi-finished film product consisting of the first OCA adhesive layer, the grating layer, the self-repairing TPU film layer and the second OCA adhesive layer to enter a space between a second upper liquid injection area (26) and a second lower liquid injection area (27) through a straightening roller, opening a third regulating valve (29) and a fourth regulating valve (31), enabling a dummy film layer liquid in a dummy film layer liquid tank to enter the second upper liquid injection area (26) through a third liquid injection pipe (28), enabling a high-viscosity silica gel layer liquid in a high-viscosity silica gel layer liquid tank to enter the second lower liquid injection area (27) through a fourth liquid injection pipe (30), covering the upper surface of the first OCA adhesive layer with the dummy film layer liquid, and covering the lower surface of the second OCA adhesive layer with the high-viscosity silica gel layer liquid;
s6, a cam (9) drives a piston (8) to compress in a piston cylinder body (6), so that a third upper hot-pressing column (32) and a third lower hot-pressing column (33) are extruded, a second upper hot-pressing roller (36) and a second lower hot-pressing roller (37) are subjected to hot extrusion, and a semi-finished film product consisting of a matte film layer, a first OCA adhesive layer, a grating layer, a self-repairing TPU film layer, a second OCA adhesive layer and a high-viscosity silica gel layer is obtained;
s7, feeding a semi-finished film product consisting of a matte film layer, a first OCA (optical clear adhesive) layer, a grating layer, a self-repairing TPU (thermoplastic polyurethane) film layer, a second OCA film layer and a high-viscosity silica gel layer between a fourth upper hot pressing column (38) and a third lower liquid injection zone (39) through a straightening roller (42), opening a fifth adjusting valve (43), covering fluorine release film layer liquid in a fluorine release film layer liquid tank on the lower surface of the semi-finished film product after passing through a fifth liquid injection pipe (41), and carrying out hot press molding on a third upper hot pressing roller (40) to obtain a semi-finished 3D protective film product;
s8, winding the 3D protective film semi-finished product on a winding drum (5) through a winding roller (4);
the hot press molding temperature of the step S2 is 60-80 ℃, the hot extrusion temperature of the step S4 is 90-110 ℃, the hot extrusion temperature of the step S6 is 100-120 ℃, and the hot press molding temperature of the step S7 is 90-110 ℃;
the winding speed of the winding roller (4) is the same as the unwinding speed of the unwinding roller (3) and is 2-3 cm/s.
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| CN110713801A (en) * | 2018-07-15 | 2020-01-21 | 浙江磊峰塑料科技有限公司 | Electromagnetic shielding film and preparation method thereof |
| CN208682286U (en) * | 2018-08-01 | 2019-04-02 | 汕头市银海印务有限公司 | A kind of dry type laminating machine |
| CN110628354A (en) * | 2019-10-16 | 2019-12-31 | 深圳市弘海电子材料技术有限公司 | High-light-reflection cover film and manufacturing method thereof |
| CN111231190A (en) * | 2020-01-20 | 2020-06-05 | 滁州市玉林聚氨酯有限公司 | Preparation method of antibacterial stain-resistant polyurethane tire |
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2020
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