CN111352253A - 1.591 refractive index PC blue light prevention lens and preparation method thereof - Google Patents

1.591 refractive index PC blue light prevention lens and preparation method thereof Download PDF

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CN111352253A
CN111352253A CN202010189760.7A CN202010189760A CN111352253A CN 111352253 A CN111352253 A CN 111352253A CN 202010189760 A CN202010189760 A CN 202010189760A CN 111352253 A CN111352253 A CN 111352253A
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刘建中
郭耀钟
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Jiangsu Xinshike Optoelectronics Technology Co ltd
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    • GPHYSICS
    • G02OPTICS
    • G02CSPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
    • G02C7/00Optical parts
    • G02C7/10Filters, e.g. for facilitating adaptation of the eyes to the dark; Sunglasses
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/10Block or graft copolymers containing polysiloxane sequences
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/14Protective coatings, e.g. hard coatings
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
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    • C08K3/08Metals
    • C08K2003/0806Silver
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

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  • Optics & Photonics (AREA)
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Abstract

The invention relates to a 1.591 refractive index PC blue light prevention lens and a preparation method thereof, belonging to the technical field of optical lens preparation. According to the invention, photosensitive acrylate groups are introduced into the organic silicon resin to prepare the hybrid organic silicon resin, phenyl groups are also introduced into the hybrid organic silicon resin, the excellent ultraviolet absorption performance of the phenyl groups is utilized to improve the ultraviolet resistance of the coating, meanwhile, the organic silicon resin is used as a coating base material to play a role in wear resistance and impact resistance, and then dichloromethane, zinc oxide and nano silver are added into the organic silicon resin, so that the coating and a PC lens are combined together through the mutual dissolution, winding and other effects, the adhesion of the coating is improved, the effective blocking of ultraviolet and short-wave blue light is achieved by utilizing the scattering effect of zinc oxide films and Ag nano particles in a back layer and a surface layer, and the organic silicon resin has a wide application prospect.

Description

1.591 refractive index PC blue light prevention lens and preparation method thereof
Technical Field
The invention relates to a 1.591 refractive index PC blue light prevention lens and a preparation method thereof, belonging to the technical field of optical lens preparation.
Background
PC is an abbreviation for polycarbonate. PC is a linear carbonate polyester in which the carbonate groups alternate with other groups, either aromatic or aliphatic, or both. Bisphenol a type PC is the most important industrial product. PC is an amorphous polymer in a nearly colorless glassy state, and has excellent optical properties and oxidation resistance. The PC high molecular weight resin has high toughness, the bending modulus can reach more than 2400MPa, and the resin can be processed into large rigid products. The main performance defects of PC are insufficient hydrolysis resistance stability, sensitivity to gaps, organic chemical resistance, poor scratch resistance and poor ultraviolet resistance, and yellowing can occur after long-term exposure to ultraviolet rays. Like other resins, PC is susceptible to attack by certain organic solvents.
The PC lens is formed by melting and injection molding of PC granules, and the molding temperature is as high as above 320 ℃. Therefore, the organic additive is easy to be pyrolyzed, aged, denatured, etc. during high temperature processing. For example, conventional ultraviolet absorbers are susceptible to failure at such high temperatures. At present, the PC granules in China mainly depend on imported products. The product is added with a high-temperature resistant ultraviolet absorbent, has a cutoff wavelength of 390 nm for ultraviolet rays, and can bear the high-temperature processing process of the PC lens without failure.
At present, the development of electronic products such as mobile phones and the like is creating new market demands, such as blue-light-proof lens products and the like. In the past spectacle market, lenses with 390 nm ultraviolet protection function can be sold as ultraviolet protection lenses. Now, with the change of policy, the basic requirement for acceptable lenses is to be able to block uv light below 390 nm. CR39, however, requires a high technical threshold in terms of uv protection for its early products due to material properties and processing requirements. The demand for new blue blocking further raises this technical threshold, and thus, the CR39 lens raw material product as a whole is still not mature enough in blue blocking performance. Companies that produce CR39 lens stock that provides excellent uv and blue protection may change the market for this lens stock. From this point, it can be seen that if the CR39 can be functionalized to meet new market needs following market changes, it is possible to make breakthrough progress on this traditional product. The ultraviolet-proof and blue-proof products can be functionally subdivided by protecting 400 nm, 410 nm, 420 nm, 430 nm and 450nm, and meet different customer requirements.
In view of the above-mentioned drawbacks, the present designer actively makes research and innovation to create a PC blue-light-proof lens with refractive index of 1.591 and a preparation method thereof, so that the lens has industrial application value.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a PC blue light prevention lens with the refractive index of 1.591 and a preparation method thereof.
The invention designs a PC blue light prevention coating material which is coated on the surface of a PC lens to realize the blue light prevention effect of a film layer. The test result shows that the visible light transmittance of the PC lens exceeds 92 percent. The firmness of the film layer is not reduced after film coating, hardening and film coating. The cut-off wavelength of the UV-visible light reaches 410 nm, which exceeds that of the UV-proof PC lens.
The invention discloses a 1.591 refractive index PC blue light prevention lens, which comprises a polycarbonate lens, a blue light prevention coating surface layer coated on the front surface of the polycarbonate lens and a blue light prevention coating back layer coated on the back surface of the polycarbonate lens;
the blue-light-proof coating surface layer is formed by ultraviolet curing of a blue-light-proof coating fabric;
the back layer of the blue-light-proof coating is formed by ultraviolet curing of a blue-light-proof coating back material;
the blue-light-proof coating fabric is prepared from a photocuring organic silicon coating base material, a nano-silver concentrated solution and dichloromethane;
the back layer of the blue-light-proof coating is prepared from a photocuring organic silicon coating base material, zinc oxide sol and dichloromethane;
the photocuring organic silicon coating base material is prepared from gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, methacrylic acid, triethylamine, p-hydroxyanisole, phenyl trimethoxy silane, deionized water, trimethyl ethoxy silane, polyurethane acrylate and a photoinitiator 1173D;
the zinc oxide sol is prepared from zinc acetate, isopropanol and monoethanolamine;
the nano silver concentrated solution is prepared from silver nitrate solution, absolute ethyl alcohol, chitosan and hydrazine hydrate.
A preparation method of a 1.591 refractive index PC blue light prevention lens comprises the following specific preparation steps:
(1) preparation of the prereactate: mixing gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and methacrylic acid, putting into a three-neck flask, stirring and mixing to obtain a mixture, adding triethylamine and p-hydroxyanisole into the three-neck flask, heating, raising the temperature, and stirring for reaction to obtain a pre-reactant;
(2) preparation of the organic silicon hybrid acrylic prepolymer: after the stirring reaction is finished, continuously adding phenyltrimethoxysilane and deionized water into the three-neck flask, after the stirring reaction is continued, adding trimethylethoxysilane into the three-neck flask, and after the stirring reaction, performing reduced pressure distillation to remove water to obtain an organic silicon hybrid acrylic prepolymer;
(3) preparation of photocuring organic silicon coating base material: weighing the organic silicon hybrid acrylic prepolymer, polyurethane acrylate and a photoinitiator 1173D, putting into a stirrer, and uniformly stirring to obtain a photocuring organic silicon coating base material;
(4) preparation of zinc oxide sol: mixing zinc acetate and isopropanol, then putting into a reaction kettle, adding monoethanolamine into the reaction kettle, heating, stirring, standing and aging to form zinc oxide sol;
(5) preparing a nano silver concentrated solution: mixing a silver nitrate solution, absolute ethyl alcohol and chitosan to obtain a base solution, mixing hydrazine hydrate and absolute ethyl alcohol to obtain a dropping liquid, adding the dropping liquid into the base solution at room temperature, and performing rotary evaporation and concentration after shaking table oscillation reaction to obtain a nano-silver concentrated solution;
(6)1.591 preparation of PC blue light prevention lens with refractive index: uniformly mixing the photocuring organic silicon coating base material, the nano-silver concentrated solution and dichloromethane to prepare a blue-light-proof coating fabric, uniformly mixing the photocuring organic silicon coating base material, the zinc oxide sol and the dichloromethane to obtain a blue-light-proof coating back material, respectively coating the blue-light-proof coating fabric and the blue-light-proof coating back material on the front surface and the back surface of a polycarbonate lens, drying after coating, and curing under ultraviolet light to obtain the PC blue-light-proof lens with the refractive index of 1.591.
Further, the preparation method comprises the following specific steps:
(1) mixing gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and methacrylic acid according to the mass ratio of 7:3, putting the mixture into a three-neck flask, stirring and mixing for 10-15 min to obtain a mixture, adding triethylamine accounting for 1% of the mass of the mixture and p-hydroxyanisole accounting for 0.1% of the mass of the mixture into the three-neck flask, heating to 95-105 ℃, stirring and reacting for 30-40 min to obtain a pre-reactant;
(2) after the stirring reaction is finished, continuously adding phenyltrimethoxysilane with the same mass as that of the pre-reactant and deionized water with 80% of the mass of the pre-reactant into the three-neck flask, continuously stirring for reaction for 30-40 min, then adding trimethylethoxysilane with 1% of the mass of the pre-reactant into the three-neck flask, stirring for reaction for 30-40 min, and then carrying out reduced pressure distillation to remove water to obtain the organosilicon hybrid acrylic prepolymer;
(3) weighing 60-70 parts by weight of the organic silicon hybrid acrylic prepolymer, 30-40 parts by weight of polyurethane acrylate and 3-5 parts by weight of photoinitiator 1173D, putting into a stirrer, and uniformly stirring to obtain a photocuring organic silicon coating base material;
(4) mixing zinc acetate and isopropanol according to the mass ratio of 1:6, then putting the mixture into a reaction kettle, adding monoethanolamine with the same mass as zinc acetate into the reaction kettle, heating to 50-60 ℃, stirring at a constant temperature for 2-3 h, standing and aging for 48-50 h to form zinc oxide sol;
(5) mixing a silver nitrate solution with a concentration of 0.2mol/L, absolute ethyl alcohol and chitosan according to a mass ratio of 10:10:1 to obtain a base solution, mixing hydrazine hydrate and absolute ethyl alcohol according to a solid-to-liquid ratio of 1:1 to obtain a dropping liquid, adding the dropping liquid into the base solution according to a volume ratio of 2:1 at room temperature, carrying out shaking reaction on a table for 50-60 min, and then carrying out rotary evaporation concentration for 20-30 min at 70-80 ℃ to obtain a nano-silver concentrated solution;
(6) uniformly mixing the photocuring organic silicon coating base material, the nano-silver concentrated solution and dichloromethane in a mass ratio of 10:2:1 to obtain a blue-light-proof coating fabric, uniformly mixing the photocuring organic silicon coating base material, the zinc oxide sol and the dichloromethane in a mass ratio of 10:1:1 to obtain a blue-light-proof coating back material, respectively coating the blue-light-proof coating fabric and the blue-light-proof coating back material on the front surface and the back surface of a polycarbonate lens, controlling the thickness of a coating film to be 20-30 mu m, drying at 50-60 ℃ for 20-30 min after the coating is finished, and curing under ultraviolet light for 30-40 s to obtain the PC blue-light-proof lens with the refractive index of 1.591.
By the scheme, the invention at least has the following advantages:
the invention firstly introduces photosensitive acrylate group into organic silicon resin to prepare hybrid organic silicon resin, realizes the photocuring of the organic silicon resin, introduces phenyl group into the hybrid organic silicon resin, utilizes the excellent ultraviolet absorption property of the phenyl group to improve the ultraviolet resistance of the coating, simultaneously takes the organic silicon resin as a coating base material, has excellent mechanical property and can play the effects of wear resistance and impact resistance, then methylene dichloride, zinc oxide and nano silver are added into the organic silicon resin, on one hand, the methylene dichloride and the polycarbonate resin have better miscibility, the addition of the nano silver can combine the coating and a PC lens through the mutual dissolution, winding and other effects to improve the adhesive force of the coating, and the nano silver surface layer is coated on the surface of the lens, wherein Ag nano particles are dispersed and embedded in the structure of the surface layer, the blue-light-resistant PC lens can effectively absorb 380-450 nm short-wave blue light, the blocking rate of zinc oxide of the back layer to ultraviolet light below 380nm is 98.83%, the scattering effect of zinc oxide films and Ag nano particles in the back layer and the surface layer is utilized to achieve effective blocking of ultraviolet light and short-wave blue light, and therefore the blue-light-resistant PC lens with the refractive index of 1.591 is obtained, and the test result shows that the visible light transmission rate of the PC lens exceeds 92%. The firmness of the film layer is not reduced after film coating, hardening and film coating. The cut-off wavelength of the UV-visible light reaches 410 nm, which exceeds that of the UV-proof PC lens.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
(1) Preparation of the prereactate: mixing gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and methacrylic acid according to the mass ratio of 7:3, putting the mixture into a three-neck flask, stirring and mixing for 10-15 min to obtain a mixture, adding triethylamine accounting for 1% of the mass of the mixture and p-hydroxyanisole accounting for 0.1% of the mass of the mixture into the three-neck flask, heating to 95-105 ℃, stirring and reacting for 30-40 min to obtain a pre-reactant;
(2) preparation of the organic silicon hybrid acrylic prepolymer: after the stirring reaction is finished, continuously adding phenyltrimethoxysilane with the same mass as that of the pre-reactant and deionized water with 80% of the mass of the pre-reactant into the three-neck flask, continuously stirring for reacting for 30-40 min, then adding trimethylethoxysilane with 1% of the mass of the pre-reactant into the three-neck flask, stirring for reacting for 30-40 min, and then carrying out reduced pressure distillation to remove water to obtain an organosilicon hybrid acrylic prepolymer;
(3) preparation of photocuring organic silicon coating base material: weighing 60-70 parts by weight of the organic silicon hybrid acrylic prepolymer, 30-40 parts by weight of polyurethane acrylate and 3-5 parts by weight of a photoinitiator 1173D, putting into a stirrer, and uniformly stirring to obtain a photocuring organic silicon coating base material;
(4) preparation of zinc oxide sol: mixing zinc acetate and isopropanol according to the mass ratio of 1:6, then putting the mixture into a reaction kettle, adding monoethanolamine with the same mass as zinc acetate into the reaction kettle, heating to 50-60 ℃, stirring at a constant temperature for 2-3 h, standing and aging for 48-50 h to form zinc oxide sol;
(5) preparing a nano silver concentrated solution: mixing a silver nitrate solution with a concentration of 0.2mol/L, absolute ethyl alcohol and chitosan according to a mass ratio of 10:10:1 to obtain a base solution, mixing hydrazine hydrate and absolute ethyl alcohol according to a solid-to-liquid ratio of 1:1 to obtain dropping liquid, adding the dropping liquid into the base solution according to a volume ratio of 2:1 at room temperature, carrying out shaking reaction on a table for 50-60 min, and then carrying out rotary evaporation concentration for 20-30 min at 70-80 ℃ to obtain a nano-silver concentrated solution;
(6)1.591 preparation of PC blue light prevention lens with refractive index: uniformly mixing the photocuring organic silicon coating base material, the nano-silver concentrated solution and dichloromethane in a mass ratio of 10:2:1 to obtain a blue-light-proof coating fabric, uniformly mixing the photocuring organic silicon coating base material, the zinc oxide sol and the dichloromethane in a mass ratio of 10:1:1 to obtain a blue-light-proof coating back material, respectively coating the blue-light-proof coating fabric and the blue-light-proof coating back material on the front surface and the back surface of a polycarbonate lens, controlling the thickness of a coating film to be 20-30 mu m, drying at 50-60 ℃ for 20-30 min after the coating is finished, and curing under ultraviolet light for 30-40 s to obtain the PC blue-light-proof lens with the refractive index of 1.591.
Example 1
(1) Preparation of the prereactate: mixing gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and methacrylic acid according to the mass ratio of 7:3, putting the mixture into a three-neck flask, stirring and mixing for 10min to obtain a mixture, adding triethylamine accounting for 1% of the mass of the mixture and p-hydroxyanisole accounting for 0.1% of the mass of the mixture into the three-neck flask, heating to 95 ℃, stirring and reacting for 30min to obtain a pre-reactant;
(2) preparation of the organic silicon hybrid acrylic prepolymer: after the stirring reaction is finished, continuously adding phenyltrimethoxysilane with the same mass as that of the pre-reactant and deionized water with the mass of 80% of that of the pre-reactant into the three-neck flask, continuously stirring for reacting for 30min, then adding trimethylethoxysilane with the mass of 1% of that of the pre-reactant into the three-neck flask, stirring for reacting for 30min, and then carrying out reduced pressure distillation to remove water to obtain the organic silicon hybrid acrylic prepolymer;
(3) preparation of photocuring organic silicon coating base material: weighing 60 parts by weight of the organic silicon hybrid acrylic prepolymer, 30 parts by weight of urethane acrylate and 3 parts by weight of photoinitiator 1173D, putting the mixture into a stirrer, and uniformly stirring to obtain a photocuring organic silicon coating base material;
(4) preparation of zinc oxide sol: mixing zinc acetate and isopropanol according to the mass ratio of 1:6, then putting into a reaction kettle, adding monoethanolamine with the same mass as zinc acetate into the reaction kettle, heating to 50 ℃, stirring at constant temperature for 2h, standing and aging for 48h to form zinc oxide sol;
(5) preparing a nano silver concentrated solution: mixing a silver nitrate solution with a concentration of 0.2mol/L, absolute ethyl alcohol and chitosan according to a mass ratio of 10:10:1 to obtain a base solution, mixing hydrazine hydrate and absolute ethyl alcohol according to a solid-to-liquid ratio of 1:1 to obtain dropping liquid, adding the dropping liquid into the base solution according to a volume ratio of 2:1 at room temperature, carrying out shaking reaction on a table concentrator for 50min, and then carrying out rotary evaporation concentration at 70 ℃ for 20min to obtain a nano-silver concentrated solution;
(6)1.591 preparation of PC blue light prevention lens with refractive index: uniformly mixing the photocuring organic silicon coating base material, the nano-silver concentrated solution and dichloromethane in a mass ratio of 10:2:1 to obtain a blue-light-proof coating fabric, uniformly mixing the photocuring organic silicon coating base material, the zinc oxide sol and the dichloromethane in a mass ratio of 10:1:1 to obtain a blue-light-proof coating back material, respectively coating the blue-light-proof coating fabric and the blue-light-proof coating back material on the front surface and the back surface of the polycarbonate lens, controlling the thickness of a coating film to be 20 mu m, drying at 50 ℃ for 20min after the coating is finished, and curing under ultraviolet light for 30s to obtain the PC blue-light-proof lens with the refractive index of 1.591.
Example 2
(1) Preparation of the prereactate: mixing gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and methacrylic acid according to the mass ratio of 7:3, putting the mixture into a three-neck flask, stirring and mixing for 13min to obtain a mixture, adding triethylamine accounting for 1% of the mass of the mixture and p-hydroxyanisole accounting for 0.1% of the mass of the mixture into the three-neck flask, heating to 100 ℃, and stirring and reacting for 35min to obtain a pre-reactant;
(2) preparation of the organic silicon hybrid acrylic prepolymer: after the stirring reaction is finished, continuously adding phenyltrimethoxysilane with the same mass as that of the pre-reactant and deionized water with the mass of 80% of that of the pre-reactant into the three-neck flask, continuously stirring for reacting for 35min, then adding trimethylethoxysilane with the mass of 1% of that of the pre-reactant into the three-neck flask, stirring for reacting for 35min, and then carrying out reduced pressure distillation to remove water to obtain the organic silicon hybrid acrylic prepolymer;
(3) preparation of photocuring organic silicon coating base material: weighing 65 parts by weight of the organic silicon hybrid acrylic prepolymer, 35 parts by weight of urethane acrylate and 4 parts by weight of photoinitiator 1173D, putting the mixture into a stirrer, and uniformly stirring to obtain a photocuring organic silicon coating base material;
(4) preparation of zinc oxide sol: mixing zinc acetate and isopropanol according to the mass ratio of 1:6, then putting into a reaction kettle, adding monoethanolamine with the same mass as zinc acetate into the reaction kettle, heating to 55 ℃, stirring at constant temperature for 3h, standing and aging for 49h to form zinc oxide sol;
(5) preparing a nano silver concentrated solution: mixing a silver nitrate solution with a concentration of 0.2mol/L, absolute ethyl alcohol and chitosan according to a mass ratio of 10:10:1 to obtain a base solution, mixing hydrazine hydrate and absolute ethyl alcohol according to a solid-to-liquid ratio of 1:1 to obtain dropping liquid, adding the dropping liquid into the base solution according to a volume ratio of 2:1 at room temperature, carrying out shaking reaction on a table concentrator for 55min, and then carrying out rotary evaporation concentration for 25min at 75 ℃ to obtain a nano-silver concentrated solution;
(6)1.591 preparation of PC blue light prevention lens with refractive index: uniformly mixing the photocuring organic silicon coating base material, the nano-silver concentrated solution and dichloromethane in a mass ratio of 10:2:1 to obtain a blue-light-proof coating fabric, uniformly mixing the photocuring organic silicon coating base material, the zinc oxide sol and the dichloromethane in a mass ratio of 10:1:1 to obtain a blue-light-proof coating back material, respectively coating the blue-light-proof coating fabric and the blue-light-proof coating back material on the front surface and the back surface of a polycarbonate lens, controlling the thickness of a coating film to be 25 mu m, drying at 55 ℃ for 25min after the coating is finished, and curing under ultraviolet light for 35s to obtain the PC blue-light-proof lens with the refractive index of 1.591.
Example 3
(1) Preparation of the prereactate: mixing gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and methacrylic acid according to the mass ratio of 7:3, putting the mixture into a three-neck flask, stirring and mixing for 15min to obtain a mixture, adding triethylamine accounting for 1% of the mass of the mixture and p-hydroxyanisole accounting for 0.1% of the mass of the mixture into the three-neck flask, heating to 105 ℃, stirring and reacting for 40min to obtain a pre-reactant;
(2) preparation of the organic silicon hybrid acrylic prepolymer: after the stirring reaction is finished, continuously adding phenyltrimethoxysilane with the same mass as that of the pre-reactant and deionized water with the mass of 80% of that of the pre-reactant into the three-neck flask, continuously stirring for reacting for 40min, then adding trimethylethoxysilane with the mass of 1% of that of the pre-reactant into the three-neck flask, stirring for reacting for 40min, and then carrying out reduced pressure distillation to remove water to obtain the organic silicon hybrid acrylic prepolymer;
(3) preparation of photocuring organic silicon coating base material: weighing 70 parts by weight of the organic silicon hybrid acrylic prepolymer, 40 parts by weight of urethane acrylate and 5 parts by weight of photoinitiator 1173D, putting the mixture into a stirrer, and uniformly stirring to obtain a photocuring organic silicon coating base material;
(4) preparation of zinc oxide sol: mixing zinc acetate and isopropanol according to the mass ratio of 1:6, then putting into a reaction kettle, adding monoethanolamine with the same mass as zinc acetate into the reaction kettle, heating to 60 ℃, stirring for 3h at constant temperature, standing and aging for 50h to form zinc oxide sol;
(5) preparing a nano silver concentrated solution: mixing a silver nitrate solution with a concentration of 0.2mol/L, absolute ethyl alcohol and chitosan according to a mass ratio of 10:10:1 to obtain a base solution, mixing hydrazine hydrate and absolute ethyl alcohol according to a solid-to-liquid ratio of 1:1 to obtain dropping liquid, adding the dropping liquid into the base solution according to a volume ratio of 2:1 at room temperature, carrying out shaking reaction on a table concentrator for 60min, and then carrying out rotary evaporation concentration at 80 ℃ for 30min to obtain a nano-silver concentrated solution;
(6)1.591 preparation of PC blue light prevention lens with refractive index: uniformly mixing the photocuring organic silicon coating base material, the nano-silver concentrated solution and dichloromethane in a mass ratio of 10:2:1 to obtain a blue-light-proof coating fabric, uniformly mixing the photocuring organic silicon coating base material, the zinc oxide sol and the dichloromethane in a mass ratio of 10:1:1 to obtain a blue-light-proof coating back material, respectively coating the blue-light-proof coating fabric and the blue-light-proof coating back material on the front surface and the back surface of a polycarbonate lens, controlling the thickness of a coating film to be 30 mu m, drying at 60 ℃ for 30min after the coating is finished, and curing under ultraviolet light for 40s to obtain the PC blue-light-proof lens with the refractive index of 1.591.
Comparative example 1: the preparation method is similar to that of example 1 of the invention, except that the common polyalkyl silicone resin is used to replace the photocuring silicone coating base material of the invention to prepare the blue-light-proof lens;
comparative example 2: the preparation method is similar to that of inventive example 1, except that no dichloromethane is added to prepare a blue light-blocking lens;
comparative example 3: the preparation method is similar to that of the inventive example 1, except that no zinc oxide sol and nano silver concentrate are added to prepare the blue light prevention lens.
The performance of the blue light-proof lenses of the invention and comparative examples 1-3 was tested, and the test results are shown in table 1:
the detection method comprises the following steps:
and (3) detecting the wear resistance: testing by adopting a step of a grid cutting method GB/T9286-98, and detecting the proportion of the affected area at the cross cutting part to the total area of the lens after grid cutting, wherein the smaller the proportion is, the higher the wear resistance is;
and (3) blue light prevention performance detection: detecting the blocking rate of blue light and ultraviolet light and the natural light transmittance by using a light transmittance tester, and evaluating the blue light prevention and ultraviolet light prevention effects of the lens by using the blocking rate of the blue light and the ultraviolet light and the natural light transmittance as indexes;
TABLE 1 Performance test results
Figure RE-GDA0002489806650000091
As can be seen from the detection data in the above table, in the comparative example 1, because the photo-cured silicone coating base material of the present invention is not used, the affected area ratio of the cross-cut part after the grid cutting is obviously increased, it can be seen that the wear resistance and the adhesion firmness of the blue light prevention coating are improved by the photo-cured silicone coating base material of the present invention, in the comparative example 2, because dichloromethane is not added, the affected area ratio of the cross-cut part after the grid cutting is obviously increased, it can be seen that the wear resistance and the adhesion firmness of the blue light prevention coating are improved by the dichloromethane of the present invention, in the comparative example 3, because zinc oxide sol and nano silver concentrated solution are not added, the blue light blocking rate and the ultraviolet light blocking rate are both obviously reduced, and it can be seen that after the zinc oxide sol and the nano silver concentrated solution are added, the blue light blocking rate and the ultraviolet light blocking rate of the.

Claims (3)

1. A1.591 refractive index PC blue light-proof lens comprises a polycarbonate lens, a blue light-proof coating surface layer coated on the front surface of the polycarbonate lens and a blue light-proof coating back layer coated on the back surface of the polycarbonate lens; the method is characterized in that:
the blue-light-proof coating surface layer is formed by ultraviolet curing of a blue-light-proof coating fabric;
the back layer of the blue-light-proof coating is formed by ultraviolet curing of a blue-light-proof coating back material;
the blue-light-proof coating fabric is prepared from a photocuring organic silicon coating base material, a nano-silver concentrated solution and dichloromethane;
the back layer of the blue-light-proof coating is prepared from a photocuring organic silicon coating base material, zinc oxide sol and dichloromethane;
the photocuring organic silicon coating base material is prepared from gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, methacrylic acid, triethylamine, p-hydroxyanisole, phenyl trimethoxy silane, deionized water, trimethyl ethoxy silane, polyurethane acrylate and a photoinitiator 1173D;
the zinc oxide sol is prepared from zinc acetate, isopropanol and monoethanolamine;
the nano silver concentrated solution is prepared from silver nitrate solution, absolute ethyl alcohol, chitosan and hydrazine hydrate.
2. A preparation method of a 1.591 refractive index PC blue-light-proof lens is characterized by comprising the following specific preparation steps:
(1) preparation of the prereactate: mixing gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and methacrylic acid, putting into a three-neck flask, stirring and mixing to obtain a mixture, adding triethylamine and p-hydroxyanisole into the three-neck flask, heating, raising the temperature, and stirring for reaction to obtain a pre-reactant;
(2) preparation of the organic silicon hybrid acrylic prepolymer: after the stirring reaction is finished, continuously adding phenyltrimethoxysilane and deionized water into the three-neck flask, after the stirring reaction is continued, adding trimethylethoxysilane into the three-neck flask, and after the stirring reaction, performing reduced pressure distillation to remove water to obtain an organic silicon hybrid acrylic prepolymer;
(3) preparation of photocuring organic silicon coating base material: weighing the organic silicon hybrid acrylic prepolymer, polyurethane acrylate and a photoinitiator 1173D, putting into a stirrer, and uniformly stirring to obtain a photocuring organic silicon coating base material;
(4) preparation of zinc oxide sol: mixing zinc acetate and isopropanol, then putting into a reaction kettle, adding monoethanolamine into the reaction kettle, heating, stirring, standing and aging to form zinc oxide sol;
(5) preparing a nano silver concentrated solution: mixing a silver nitrate solution, absolute ethyl alcohol and chitosan to obtain a base solution, mixing hydrazine hydrate and absolute ethyl alcohol to obtain a dropping liquid, adding the dropping liquid into the base solution at room temperature, and performing rotary evaporation and concentration after shaking table oscillation reaction to obtain a nano-silver concentrated solution;
(6)1.591 preparation of PC blue light prevention lens with refractive index: uniformly mixing the photocuring organic silicon coating base material, the nano-silver concentrated solution and dichloromethane to prepare a blue-light-proof coating fabric, uniformly mixing the photocuring organic silicon coating base material, the zinc oxide sol and the dichloromethane to obtain a blue-light-proof coating back material, respectively coating the blue-light-proof coating fabric and the blue-light-proof coating back material on the front surface and the back surface of a polycarbonate lens, drying after coating, and curing under ultraviolet light to obtain the PC blue-light-proof lens with the refractive index of 1.591.
3. The method for preparing the 1.591 refractive index PC blue-light-proof lens as claimed in claim 2, wherein the specific preparation steps are as follows:
(1) preparation of the prereactate: mixing gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and methacrylic acid according to the mass ratio of 7:3, putting the mixture into a three-neck flask, stirring and mixing for 10-15 min to obtain a mixture, adding triethylamine accounting for 1% of the mass of the mixture and p-hydroxyanisole accounting for 0.1% of the mass of the mixture into the three-neck flask, heating to 95-105 ℃, stirring and reacting for 30-40 min to obtain a pre-reactant;
(2) preparation of the organic silicon hybrid acrylic prepolymer: after the stirring reaction is finished, continuously adding phenyltrimethoxysilane with the same mass as that of the pre-reactant and deionized water with 80% of the mass of the pre-reactant into the three-neck flask, continuously stirring for reacting for 30-40 min, then adding trimethylethoxysilane with 1% of the mass of the pre-reactant into the three-neck flask, stirring for reacting for 30-40 min, and then carrying out reduced pressure distillation to remove water to obtain an organosilicon hybrid acrylic prepolymer;
(3) preparation of photocuring organic silicon coating base material: weighing 60-70 parts by weight of the organic silicon hybrid acrylic prepolymer, 30-40 parts by weight of polyurethane acrylate and 3-5 parts by weight of a photoinitiator 1173D, putting into a stirrer, and uniformly stirring to obtain a photocuring organic silicon coating base material;
(4) preparation of zinc oxide sol: mixing zinc acetate and isopropanol according to the mass ratio of 1:6, then putting the mixture into a reaction kettle, adding monoethanolamine with the same mass as zinc acetate into the reaction kettle, heating to 50-60 ℃, stirring at a constant temperature for 2-3 h, standing and aging for 48-50 h to form zinc oxide sol;
(5) preparing a nano silver concentrated solution: mixing a silver nitrate solution with a concentration of 0.2mol/L, absolute ethyl alcohol and chitosan according to a mass ratio of 10:10:1 to obtain a base solution, mixing hydrazine hydrate and absolute ethyl alcohol according to a solid-to-liquid ratio of 1:1 to obtain a dropping liquid, adding the dropping liquid into the base solution according to a volume ratio of 2:1 at room temperature, carrying out shaking reaction on a table for 50-60 min, and then carrying out rotary evaporation concentration for 20-30 min at 70-80 ℃ to obtain a nano-silver concentrated solution;
(6)1.591 preparation of PC blue light prevention lens with refractive index: uniformly mixing the photocuring organic silicon coating base material, the nano-silver concentrated solution and dichloromethane in a mass ratio of 10:2:1 to obtain a blue-light-proof coating fabric, uniformly mixing the photocuring organic silicon coating base material, the zinc oxide sol and the dichloromethane in a mass ratio of 10:1:1 to obtain a blue-light-proof coating back material, respectively coating the blue-light-proof coating fabric and the blue-light-proof coating back material on the front surface and the back surface of a polycarbonate lens, controlling the thickness of a coating film to be 20-30 mu m, drying at 50-60 ℃ for 20-30 min after the coating is finished, and curing under ultraviolet light for 30-40 s to obtain the PC blue-light-proof lens with the refractive index of 1.591.
CN202010189760.7A 2020-03-18 2020-03-18 1.591 refractive index PC blue light prevention lens and preparation method thereof Pending CN111352253A (en)

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