CN117362727A - Composite color-changing high-definition spectacle lens and preparation method thereof - Google Patents
Composite color-changing high-definition spectacle lens and preparation method thereof Download PDFInfo
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- CN117362727A CN117362727A CN202311304194.XA CN202311304194A CN117362727A CN 117362727 A CN117362727 A CN 117362727A CN 202311304194 A CN202311304194 A CN 202311304194A CN 117362727 A CN117362727 A CN 117362727A
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- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 130
- 239000013310 covalent-organic framework Substances 0.000 claims abstract description 45
- 239000000758 substrate Substances 0.000 claims abstract description 34
- 238000004528 spin coating Methods 0.000 claims abstract description 30
- 229910000314 transition metal oxide Inorganic materials 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 6
- 238000001907 polarising light microscopy Methods 0.000 claims abstract 4
- 239000010410 layer Substances 0.000 claims description 66
- 238000000034 method Methods 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 11
- 239000000080 wetting agent Substances 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 9
- 239000004925 Acrylic resin Substances 0.000 claims description 8
- 229920000178 Acrylic resin Polymers 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- -1 acrylic ester Chemical class 0.000 claims description 6
- 239000011268 mixed slurry Substances 0.000 claims description 6
- 239000003607 modifier Substances 0.000 claims description 6
- 239000013530 defoamer Substances 0.000 claims description 5
- 125000006617 triphenylamine group Chemical group 0.000 claims description 5
- 239000002518 antifoaming agent Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 238000009966 trimming Methods 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000011247 coating layer Substances 0.000 claims 4
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
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- 238000013329 compounding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 230000008859 change Effects 0.000 description 9
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- 238000010521 absorption reaction Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 4
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 4
- 239000013460 polyoxometalate Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- MTZQAGJQAFMTAQ-UHFFFAOYSA-N ethyl benzoate Chemical group CCOC(=O)C1=CC=CC=C1 MTZQAGJQAFMTAQ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- DLKQHBOKULLWDQ-UHFFFAOYSA-N 1-bromonaphthalene Chemical compound C1=CC=C2C(Br)=CC=CC2=C1 DLKQHBOKULLWDQ-UHFFFAOYSA-N 0.000 description 1
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical group [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000013080 microcrystalline material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G02—OPTICS
- G02C—SPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
- G02C7/00—Optical parts
- G02C7/10—Filters, e.g. for facilitating adaptation of the eyes to the dark; Sunglasses
- G02C7/102—Photochromic filters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0218—Pretreatment, e.g. heating the substrate
- B05D3/0227—Pretreatment, e.g. heating the substrate with IR heaters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
- B05D5/065—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects having colour interferences or colour shifts or opalescent looking, flip-flop, two tones
- B05D5/066—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects having colour interferences or colour shifts or opalescent looking, flip-flop, two tones achieved by multilayers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D11/00—Producing optical elements, e.g. lenses or prisms
- B29D11/00865—Applying coatings; tinting; colouring
- B29D11/00884—Spin coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D11/00—Producing optical elements, e.g. lenses or prisms
- B29D11/00865—Applying coatings; tinting; colouring
- B29D11/00894—Applying coatings; tinting; colouring colouring or tinting
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2502/00—Acrylic polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2601/00—Inorganic fillers
- B05D2601/02—Inorganic fillers used for pigmentation effect, e.g. metallic effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2602/00—Organic fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ophthalmology & Optometry (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Eyeglasses (AREA)
Abstract
The invention relates to a composite color-changing high-definition spectacle lens and a preparation method thereof, wherein the lens comprises an antireflection film layer, a rear surface protection film layer, a substrate, a photochromic layer, a front surface protection film layer and an antireflection film layer which are sequentially arranged from a human eye side to a light incidence side; the photochromic layer is a photochromic material formed by compounding a powdery covalent organic framework material COFs, a transition metal oxide photochromic material and a polyoxometallate photochromic material POMs; the preparation method comprises the steps of substrate preparation, photochromic layer spin coating liquid preparation, substrate pretreatment and film spin coating. The invention combines the organic frame material and the inorganic photochromic material, so that the photochromic sheet has the characteristics of high response speed of the organic photochromic material and the characteristics of good reversibility and strong fatigue resistance of the inorganic photochromic material.
Description
Technical Field
The invention relates to the technical field of photochromism of high-definition spectacle lenses, in particular to a composite color-changing high-definition spectacle lens and a preparation method thereof.
Background
In the resin lens manufacturing industry, to obtain high quality photochromic lenses, it is necessary to use appropriate optical resin monomers and photochromic materials. At present, photochromic lenses are mainly divided into film-layer photochromic lenses and substrate-photochromic lenses.
The film layer color change is to spin-coat a color-changing film layer containing a photochromic material on the surface of a substrate, wherein the color-changing film layer contains an organic photochromic material or an inorganic photochromic material. The organic photochromic material realizes the color change through the process of realizing the configuration transformation or cyclization of molecules under the illumination condition, has high response speed but poor fatigue resistance, and has the performance attenuation after multiple photochromic fading cycles, and the materials of spiropyrans and rhodamine are commonly used; inorganic photochromic materials have the advantages of good fatigue resistance, good reversibility and the like, but besides Polyoxometallates (POMs), the solubility is generally poor, the color change is single, the color change efficiency is different from that of organic materials, and silver halide, transition metal oxides and the like are commonly used. From the above discussion, it is known that each of the organic photochromic material and the inorganic photochromic material has advantages and disadvantages, if different organic/inorganic photochromic materials can be compounded by chemical bond connection or doping blending, and the adhesiveness between the photochromic film layer and the substrate can be improved by the preparation process, or the optical performance of the film layer photochromic lens can be systematically improved.
Disclosure of Invention
In order to solve the technical problems, the invention provides a color-changing high-definition spectacle lens which has the advantages of high response speed of an organic photochromic material, good reversibility of an inorganic photochromic material, strong fatigue resistance and the like, and the invention provides the following technical scheme:
a composite color-changing high-definition spectacle lens comprises an antireflection film layer, a rear surface protection film layer, a substrate, a photochromic layer, a front surface protection film layer and an antireflection film layer which are sequentially arranged from the eye side to the light incidence side;
the substrate is prepared from acrylic materials; the spectacle lens prepared from the acrylic acid ester material has the advantages of high Abbe number and slight dispersion, but has poor cohesiveness with the common photochromic material, and the common photochromic film layer is coated on the surface of the spectacle lens in a spin-coating way, so that the film layer is easy to fall off after a long time; the composite photochromic material of the present invention can improve the adhesion with a substrate in addition to the optical performance.
The photochromic layer comprises the following components in parts by mass: 50-100 parts of acrylic resin, 20-30 parts of composite photochromic material, 20-30 parts of wetting agent, 5-8 parts of dispersing agent, 1-3 parts of surfactant, 1-3 parts of defoamer and 0.5-0.8 part of modifier;
the composite photochromic material comprises the following components: powdered covalent organic framework materials COFs, transition metal oxide photochromic materials, polyoxometallate photochromic materials POMs.
Covalent organic framework material COFs are currently applied to the field of photocatalysis, and are porous microcrystalline materials which can be connected with transition metal oxide photochromic materials in a chemical bond mode after being blended, a plurality of absorption peaks are formed on a spectrum after the transition metal oxide photochromic materials are discolored, and absorption peaks are formed at blue-green junctions, green-red junctions, yellow-red junctions and red-black junctions, so that the contrast of lenses is improved, and object images are clearer; meanwhile, the covalent organic framework material COFs is compounded with the polyoxometallate photochromic material, the problem of poor powder solubility of the COFs can be solved through the matching, and the covalent organic framework material COFs has a larger pi conjugated framework and a regular pi-pi stacking structure, so that the layer or interlayer charge transfer is facilitated, and the compound speed of the POMs electron-hole pair of the polyoxometallate photochromic material can be improved due to the existence of the covalent organic framework material COFs, so that the response speed is further improved; and the bonding force between the photochromic layer and the substrate can be remarkably improved by adding the covalent organic framework material COFs.
Further, the composite photochromic material comprises the following components in parts by weight: 2-5 parts of powdery covalent organic frame material COFs, 5-8 parts of transition metal oxide photochromic material and 10-15 parts of polyoxometallate photochromic material POMs. The ratio of each component in the composite photochromic material directly determines the color changing efficiency and the process feasibility, wherein the powdery covalent organic framework material COFs is used as a framework-type auxiliary color changing material without excessive, and the cost is high, so the powdery covalent organic framework material COFs occupies less space; the transition metal oxide photochromic material and the polyoxometallate photochromic material POMs are used as main photochromic materials, the POMs occupy relatively more proportion, and the POMs occupy the largest proportion relatively due to solubility.
Furthermore, the powdery covalent organic framework material is a triphenylamine group COFs material, and has the advantages of high transparency, high thermal stability and the like. The triphenylamine-based COFs material is used as an electrochromic material at present, and the triphenylamine-based COFs material is applied to the field of photochromism in a breakthrough manner, and the solubility of the triphenylamine-based COFs material in the composite photochromism material is improved due to the special molecular structure of triphenylamine, so that the processability of the photochromism layer is improved.
Further, the transition metal oxide photochromic material is TiO 2 ,TiO 2 The transparent oxide semiconductor material is a typical transparent oxide semiconductor material, and can effectively promote carrier separation and inhibit recombination in a composite photochromic material, thereby effectively improving the photochromic efficiency.
Further, the mass ratio of the powdery covalent organic framework material COFs, the transition metal oxide photochromic material and the polyoxometallate photochromic material POMs in the composite photochromic material is 1:2:4.
Furthermore, the thickness of the photochromic layer is 3-5 mu m, if the photochromic layer is too thin, on one hand, the color changing depth cannot meet the requirement, and on the other hand, the existence of the covalent organic framework material COFs is too thin, so that the grinding period is greatly improved, and the process difficulty is increased; meanwhile, the thickness of the photochromic layer cannot be too thick, otherwise, the cost is increased and the uniformity of the film layer is easily affected.
The preparation method of the composite color-changing high-definition spectacle lens comprises the following steps:
s1, preparing a substrate: filling the mixed acrylic ester base material into a mold, placing the filled mold into a curing furnace, and performing primary curing, standing and cooling, demolding, trimming and cleaning to form a substrate;
s2, preparing a photochromic layer spin coating liquid: weighing a sufficient amount of each component material of the composite photochromic material, adding the materials into a grinder for blending and fine grinding, and then adding a wetting agent for stirring and dispersing grinding to obtain mixed slurry; adding acrylic resin, a dispersing agent, a surfactant, a defoaming agent and a modifying agent into the mixed slurry, and blending to form photochromic spin-coating liquid;
the compound photochromic material is grinded to a specific particle size and stirred uniformly, then wetting agent can be added for dispersion, otherwise, the compound photochromic material is easy to agglomerate, and the problem of uneven color change and the like is caused.
S3, spin coating of a photochromic layer: fixing the substrate on a spin coater, performing low-frequency short-wave infrared irradiation pretreatment on one side of the substrate to be spin-coated with the photochromic layer for 10-15min, and immediately spin-coating the photochromic layer spin-coating liquid on the substrate;
before spin coating of the photochromic layer, the lens is pretreated, and the main purpose is to slightly soften the shallow surface layer of the substrate by utilizing the thermal effect of infrared rays, so that the bonding strength of the substrate and the photochromic layer is increased on the premise of not influencing the spin coating process.
S4, spin coating of other film layers: and after the photochromic layer is cured, sequentially spin-coating the rest film layer.
Further, the grain diameter range after the fine grinding process of the composite photochromic material in the step S2 is 1-2 mu m.
Further, in step S3, the wavelength of the low-frequency short-wave infrared rays is 1.5-3 μm.
The invention has the beneficial effects that:
1. the organic and inorganic photochromic materials are compounded, so that the organic photochromic material has the characteristics of high response speed, good reversibility and strong fatigue resistance.
2. The composite material of the COFs material and the inorganic material has good uniformity, and the bonding strength of the photochromic layer and the substrate can be improved.
3. The COFs composite transition metal oxide photochromic material is connected in a chemical bond mode, and has a plurality of absorption peaks in spectrum, namely absorption peaks at blue-green junctions, green-red junctions, yellow-red junctions and red-black junctions, and the transmittance is low, so that the contrast ratio is improved, and the object image is clearer.
4. The COFs composite polyoxometallate photochromic material POMs has good solubility and reversibility, the problem of poor solubility of COFs powder can be solved through the proportion, and the COFs has a larger pi conjugated framework and a regular pi-pi stacking structure, so that the charge transfer between layers or layers of the COFs composite polyoxometallate photochromic material POMs is facilitated, the composite speed of POM electron-hole pairs can be improved, and the color change response speed is further improved.
Detailed Description
Example 1,
A composite color-changing high-definition spectacle lens comprises an antireflection film layer, a rear surface protection film layer, a substrate, a photochromic layer, a front surface protection film layer and an antireflection film layer which are sequentially arranged from the eye side to the light incidence side; in this embodiment, the rear surface protective film layer and the front surface protective film layer are all hardened layers.
The substrate is made of acrylic materials.
The photochromic layer comprises the following components in parts by mass: 75 parts of acrylic resin, 21 parts of composite photochromic material, 25 parts of wetting agent, 6 parts of dispersing agent, 2 parts of surfactant, 2 parts of defoamer and 0.6 part of modifier; in this embodiment, the composite photochromic material includes 3 parts of powdery triphenylamine group COFs material and TiO 2 6 parts of polyoxometalate photochromic material POMs (pre-oriented metal oxide) 12 parts. In the embodiment, the polyoxometallate photochromic material POMs can be selected from ammonium molybdate [ (NH) with low price and wide application 4 ) 6 Mo 7 O 24 ](Mo 7); the wetting agent is ethyl benzoate, the dispersing agent is sodium dodecyl sulfate, the surfactant is dodecyl trimethyl ammonium chloride, the defoaming agent is dimethyl silicone oil, and the modifier is isooctyl acrylate.
The preparation method of the composite color-changing high-definition spectacle lens comprises the following steps:
s1, preparing a substrate: filling the mixed acrylic ester base material into a mold, placing the filled mold into a curing furnace, and performing primary curing, standing and cooling, demolding, trimming and cleaning to form a substrate;
s2, preparing a photochromic layer spin coating liquid: weighing a sufficient amount of each component material of the composite photochromic material, adding the materials into a grinder, blending, fine grinding and fine grinding until the particle size of the mixture is smaller than 2 mu m, and then adding a wetting agent for stirring and dispersing grinding to obtain mixed slurry; adding acrylic resin, a dispersing agent, a surfactant, a defoaming agent and a modifying agent into the mixed slurry, and blending to form photochromic spin-coating liquid; the spin-coating thickness was 4. Mu.m.
S3, spin coating of a photochromic layer: fixing the substrate on a spin coater, performing low-frequency short-wave infrared (wavelength 2 μm) irradiation pretreatment on one side of the substrate to be spin-coated with the photochromic layer for 12min, and immediately spin-coating the photochromic layer spin-coating liquid on the substrate;
s4, spin coating of other film layers: and after the photochromic layer is cured, sequentially spin-coating the rest film layer.
EXAMPLE 2,
The photochromic layer of the embodiment comprises the following components in parts by mass: 100 parts of acrylic resin, 28 parts of composite photochromic material, 30 parts of wetting agent, 8 parts of dispersing agent, 3 parts of surfactant, 3 parts of defoamer and 0.8 part of modifier; in this embodiment, the composite photochromic material includes 4 parts of powdery triphenylamine group COFs material and TiO 2 8 parts of polyoxometalate photochromic material POMs (polyoxymethylene) 16 parts.
The other components, proportions and preparation process are the same as in example 1.
EXAMPLE 3,
The implementation isThe photochromic layer of the example comprises the following components in parts by mass: 50 parts of acrylic resin, 20 parts of composite photochromic material, 20 parts of wetting agent, 5 parts of dispersing agent, 1 part of surfactant, 1 part of defoamer and 0.5 part of modifier; in this embodiment, the composite photochromic material includes 3 parts of powdery triphenylamine group COFs material and TiO 2 6 parts of polyoxometalate photochromic material POMs11 parts.
The other components, proportions and preparation process are the same as in example 1.
Comparative example 1,
The photochromic material in the photochromic layer of this comparative example was 21 parts of a single spiropyran-based photochromic material, and the remaining components were the same as in example 1.
The preparation method of the comparative example comprises the following steps:
s1, preparing a substrate: filling the mixed acrylic ester base material into a mold, placing the filled mold into a curing furnace, and performing primary curing, standing and cooling, demolding, trimming and cleaning to form a substrate;
s2, spin coating of a film layer: and fixing the substrate on a spin coater, spin-coating the photochromic layer, and then sequentially spin-coating the rest film layer.
Comparative example 2,
The photochromic material in the photochromic layer of this comparative example was a single polyoxometallate photochromic material POMs material, and the remainder was the same as in example 1. The preparation method of this comparative example was the same as that of comparative example 1.
The optical performance test was performed for each of examples 1 to 3 and comparative examples 1 to 2, using lenses having refractive indices of 1.50 and lens luminosity of 300 degrees, and mainly comprising: measuring a dispersion value, detecting a color-changing and fading speed and detecting fatigue resistance. Wherein:
the refractive index and dispersion value are measured by grinding the prepared lens into rectangular slices, dripping alpha-bromonaphthalene contact liquid on the Abbe refractometer, and reading out the refractive index and dispersion value by adjusting the upper knob and the lower knob on one side of the refractometer.
The method comprises the steps of detecting the color-changing and fading speed, manufacturing a lens into a strip shape with a certain specification, placing an ultraviolet light source in a test bin of an ultraviolet-visible spectrophotometer, setting a scanning point to 565nm, turning on the ultraviolet light source, detecting the transmittance change of a material in the color-changing process by the ultraviolet-visible spectrophotometer, recording the time when the color-changing rate reaches 80%, turning off the ultraviolet light source after the transmittance is not changed any more, and continuously detecting the transmittance change of the material in the color-changing process by the ultraviolet-visible spectrophotometer, recording the time when the color-changing rate is reduced to 10%, thereby obtaining the color-changing and fading rate of the color-changing lens.
The anti-fatigue performance is that the lens is made into a strip shape with certain specification, an ultraviolet light source is placed in a test bin of an ultraviolet-visible spectrophotometer, a scanning point is set to 565nm, the ultraviolet light source is turned on, after 3000 times of color-changing and fading experiments are carried out, the color-changing rate of each lens after the 3001 st time of ultraviolet light source irradiation is recorded.
The detection data are shown in the following table:
as can be seen from the comparison analysis of the table, the embodiments 1-3 of the invention have the advantages of small chromatic dispersion, high response speed of color change and high fatigue resistance; compared with the comparative example 1, the composite photochromic material of the invention has slightly better color-changing and fading speed than the organic photochromic material, obviously improves the fatigue resistance and greatly prolongs the service life of the color-changing sheet compared with the single organic photochromic material; as can be seen from comparative example 1 and comparative example 2, the present invention not only has superior fatigue resistance but also significantly increases the rate of discoloration and fading as compared to the single inorganic photochromic material.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. The utility model provides a compound high definition spectacle lens that discolours which characterized in that: the anti-reflection coating comprises an anti-reflection coating layer, a rear surface protection coating layer, a substrate, a photochromic layer, a front surface protection coating layer and an anti-reflection coating layer which are sequentially arranged from the human eye side to the light incidence side;
the substrate is prepared from acrylic materials;
the photochromic layer comprises the following components in parts by mass: 50-100 parts of acrylic resin, 20-30 parts of composite photochromic material, 20-30 parts of wetting agent, 5-8 parts of dispersing agent, 1-3 parts of surfactant, 1-3 parts of defoamer and 0.5-0.8 part of modifier;
the composite photochromic material comprises the following components: powdered covalent organic framework materials COFs, transition metal oxide photochromic materials, polyoxometallate photochromic materials POMs.
2. The composite color-changing high-definition spectacle lens according to claim 1, wherein the composite photochromic material comprises the following components in parts by mass: 2-5 parts of powdery covalent organic frame material COFs, 5-8 parts of transition metal oxide photochromic material and 10-15 parts of polyoxometallate photochromic material POMs.
3. A composite color-changing high definition ophthalmic lens according to claim 2, characterized in that: the powdery covalent organic framework material is a triphenylamine group COFs material.
4. A composite color shifting high definition ophthalmic lens according to claim 3, characterized in that: the transition metal oxide photochromic material is TiO 2 。
5. The composite color-changing high definition ophthalmic lens of claim 4, wherein: the mass ratio of the powdery covalent organic framework material COFs to the transition metal oxide photochromic material to the polyoxometallate photochromic material POMs in the composite photochromic material is 1:2:4.
6. The composite color-changing high definition ophthalmic lens of claim 1, wherein: the thickness of the photochromic layer is 3-5 mu m.
7. A method of producing a composite color-changing high definition spectacle lens according to any one of claims 1 to 6, comprising the steps of:
s1, preparing a substrate: filling the mixed acrylic ester base material into a mold, placing the filled mold into a curing furnace, and performing primary curing, standing and cooling, demolding, trimming and cleaning to form a substrate;
s2, preparing a photochromic layer spin coating liquid: weighing a sufficient amount of each component material of the composite photochromic material, adding the materials into a grinder for blending and fine grinding, and then adding a wetting agent for stirring and dispersing grinding to obtain mixed slurry; adding acrylic resin, a dispersing agent, a surfactant, a defoaming agent and a modifying agent into the mixed slurry, and blending to form photochromic spin-coating liquid;
s3, spin coating of a photochromic layer: fixing the substrate on a spin coater, performing low-frequency short-wave infrared irradiation pretreatment on one side of the substrate to be spin-coated with the photochromic layer for 10-15min, and immediately spin-coating the photochromic layer spin-coating liquid on the substrate;
s4, spin coating of other film layers: and after the photochromic layer is cured, sequentially spin-coating the rest film layer.
8. The method for preparing the composite color-changing high-definition spectacle lens according to claim 6, which is characterized in that: the grain diameter range of the composite photochromic material after the fine grinding process in the step S2 is 1-2 mu m.
9. The method for preparing the composite color-changing high-definition spectacle lens according to claim 6, which is characterized in that: the wavelength of the low-frequency short-wave infrared rays in the step S3 is 1.5-3 mu m.
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