CN111257973A - Anti-infrared spectacle lens and preparation method thereof - Google Patents
Anti-infrared spectacle lens and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 239000002105 nanoparticle Substances 0.000 claims abstract description 89
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 48
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 37
- 239000011258 core-shell material Substances 0.000 claims abstract description 36
- 239000000178 monomer Substances 0.000 claims abstract description 27
- 239000012074 organic phase Substances 0.000 claims abstract description 27
- 229920002261 Corn starch Polymers 0.000 claims abstract description 13
- 239000008120 corn starch Substances 0.000 claims abstract description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 12
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 72
- 238000006243 chemical reaction Methods 0.000 claims description 66
- 238000003756 stirring Methods 0.000 claims description 48
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 40
- 229910052757 nitrogen Inorganic materials 0.000 claims description 36
- 238000001914 filtration Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000006185 dispersion Substances 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 239000007822 coupling agent Substances 0.000 claims description 12
- 239000003999 initiator Substances 0.000 claims description 12
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 10
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 10
- 239000006082 mold release agent Substances 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 8
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 8
- 238000012719 thermal polymerization Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 7
- 239000011347 resin Substances 0.000 abstract description 7
- 239000004094 surface-active agent Substances 0.000 abstract description 5
- 239000002250 absorbent Substances 0.000 abstract description 3
- 230000002745 absorbent Effects 0.000 abstract description 3
- 239000002270 dispersing agent Substances 0.000 abstract description 2
- 238000010556 emulsion polymerization method Methods 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- 239000012716 precipitator Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 description 10
- 239000011521 glass Substances 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 210000004087 cornea Anatomy 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 230000001684 chronic effect Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229910001448 ferrous ion Inorganic materials 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 210000001525 retina Anatomy 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 208000002177 Cataract Diseases 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 206010015911 Eye burns Diseases 0.000 description 1
- 208000019462 Occupational injury Diseases 0.000 description 1
- BEMTYRFDNZGZQX-UHFFFAOYSA-N [Zn].[Cs] Chemical compound [Zn].[Cs] BEMTYRFDNZGZQX-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 210000001742 aqueous humor Anatomy 0.000 description 1
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 1
- 229910001632 barium fluoride Inorganic materials 0.000 description 1
- 208000010217 blepharitis Diseases 0.000 description 1
- 230000009693 chronic damage Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000005865 ionizing radiation Effects 0.000 description 1
- 208000002741 leukoplakia Diseases 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
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Classifications
-
- 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
- G02B1/041—Lenses
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/22—Absorbing filters
- G02B5/223—Absorbing filters containing organic substances, e.g. dyes, inks or pigments
-
- 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
Abstract
The invention relates to an anti-infrared spectacle lens and a preparation method thereof, belonging to the technical field of optical lens preparation. The invention firstly uses corn starch with a spherical structure as a template, urea as an organic phase dispersant and ferrous chloride as raw materials, ammonia water as a precipitator, prepares ferrite nanoparticles by a solution method, modifies a surfactant on the surface of the ferrite, wraps the nanoparticles modified by the surfactant by a high molecular resin through a soap-free emulsion polymerization method to form a core-shell structure, and adds the core-shell structure as a red light (infrared ray) absorbent into a conventional lens monomer to process into the anti-red light lens. The addition of the core-shell type ferrous salt nano-particles obviously improves the infrared ray resistance of the lens, has small influence on the mechanical strength of the original lens and has wide application prospect.
Description
Technical Field
The invention relates to an anti-infrared spectacle lens and a preparation method thereof, belonging to the technical field of optical lens preparation.
Background
Infrared radiation is infrared radiation (also known as heat rays). They can be classified into long-wave infrared rays (far infrared rays), medium-wave infrared rays and short-wave infrared rays (near infrared rays). The long-wave infrared ray has a wavelength of 25-40 μm-l mm, and can be absorbed by skin to generate heat sensation. The wavelength of the medium-wave infrared ray is 3-25 microns, and the medium-wave infrared ray can be absorbed by cornea and skin. The wavelength of the short wave infrared ray is 750 nanometers to 3 micrometers, and the burn can be caused after the short wave infrared ray is absorbed by tissues. The infrared radiation source in nature is the strongest by the sun. In a production environment, the primary sources of infrared radiation include furnaces, molten metals and glass, intense infrared light sources, and baking and heating equipment, among others. Occupational injuries often occur to operators using arc lamps, electric welding, or oxyacetylene welding.
Infrared, also known as infrared radiation, thermal radiation or heat rays, is a component of non-ionizing radiation and affects the body primarily on the skin and eyes. When infrared rays irradiate the skin, most of the infrared rays can be absorbed, and only about 1.4 percent of the infrared rays are reflected. Chronic injury to the eye, often chronic congestive blepharitis, can result from chronic exposure to low-energy infrared radiation. The damage of infrared rays to eyes has several different conditions, and the infrared rays with the wavelength of 750-1300 nm have higher transmittance to eye corneas and can cause the damage of eye fundus retinas. Especially infrared rays near 1100 nm, can enable anterior media (corneal lens and the like) of the eye not to be damaged and directly cause fundus retina burn. Infrared rays having a wavelength of 1900 nm or more are almost completely absorbed by the cornea, and cause corneal burn (cloudiness, leukoplakia). The energy of infrared rays with wavelength more than 1400 nm is mostly absorbed by cornea and intraocular fluid and cannot penetrate iris. Only infrared rays below 1300 nm can penetrate through the iris, and the iris is damaged. The human eye may cause cataracts if exposed to infrared light for a long period of time.
Currently, there are two methods for protecting glasses against infrared rays. 1) The reflection of infrared rays is realized by evaporating metal or metal compound on the surface of the lens or glass. Such as vapor-deposited gold, copper, barium fluoride, zinc cesium, and the like. 2) The infrared ray is absorbed by doping metal ions, such as ferrous ions or copper ions, in the glass, so that the infrared ray is protected. Both of these approaches, while effective in protecting against infrared radiation, have their own drawbacks. For example, the coating easily causes the reduction of the visible light transmittance of the lens, which is lower than the standard of 80% of the lowest visible light transmittance of the lens, and the visible light transmittance of various resin lens products at present exceeds 90%; the film firmness of other original coating materials of the lens can be influenced; it may not be possible to successfully coat the film due to the difference in the raw material of the substrate. The metal ions are easily doped into inorganic glass, but are difficult to dope into organic resin materials widely used in the lens industry at present. Even if the resin is doped into the resin, the color, the visible light transmittance and the mechanical property of the resin lens are easily influenced. In addition, the oxidation resistance of ferrous ions is poor, and the oxidation phenomenon is easy to occur, so that the lens is discolored.
In view of the above-mentioned drawbacks, the designer actively makes research and innovation to create an anti-infrared spectacle lens and a preparation method thereof, so that the anti-infrared spectacle lens has industrial value.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides an anti-infrared spectacle lens and a method for manufacturing the same.
The invention relates to an infrared-resistant spectacle lens which is prepared from the following raw materials in parts by weight:
60-70 parts of styrene, 10-15 parts of trimethylolpropane triacrylate, 10-15 parts of core-shell type ferrous salt nanoparticles, 5-7 parts of an initiator, 3-5 parts of a coupling agent and 0.3-0.5 part of an internal mold release agent;
the core-shell type ferrous salt nano-particles are prepared from the following raw materials:
corn starch, urea, deionized water, ferrous chloride, ammonia water, sodium dodecyl benzene sulfonate, distilled water, sodium bicarbonate, nitrogen, styrene and potassium persulfate.
Further, the initiator is prepared by mixing sodium bisulfite and ammonium persulfate according to equal mass ratio.
Further, the coupling agent is a silane coupling agent.
Further, the internal release agent is one of silicone oil, silicone resin methyl branched silicone oil, methyl silicone oil and emulsified methyl silicone oil.
A preparation method of an anti-infrared spectacle lens comprises the following specific preparation steps:
(1) preparation of organic phase dispersion: under the anaerobic condition, putting corn starch, urea and deionized water into a reaction kettle, mixing and stirring for reaction to obtain an organic phase dispersion liquid;
(2) preparing ferrite nano particles: adding ferrous chloride into the organic phase dispersion liquid, stirring and dispersing uniformly, then dropwise adding ammonia water, adjusting pH, continuously stirring and reacting, filtering to obtain filter residue, and calcining in an oxygen-free environment to obtain ferrous salt nanoparticles;
(3) preparation of pretreated ferrous salt nanoparticles: under the anaerobic condition, mixing the ferrous salt nano-particles with a sodium dodecyl benzene sulfonate solution, stirring for reaction, filtering and separating to obtain a filter cake, and drying without oxygen to obtain pretreated ferrous salt nano-particles;
(4) preparing core-shell ferrite nanoparticles: adding distilled water and sodium bicarbonate into a three-neck round-bottom flask, continuously introducing nitrogen, stirring, adding styrene and pretreated ferrite nanoparticles into the three-neck round-bottom flask, heating, adding potassium persulfate, carrying out thermal polymerization reaction, filtering and separating after the reaction is finished to obtain reaction filter residues, and drying to obtain core-shell ferrite nanoparticles;
(5) preparation of lens monomer: weighing styrene, trimethylolpropane triacrylate, core-shell ferrite nanoparticles, an initiator, a coupling agent and an internal release agent, adding the weighed materials into a reaction kettle, heating and raising the temperature under the protection of nitrogen, stirring for reaction to obtain a mixture, and filtering and separating to obtain a reaction filtrate, namely a lens monomer;
(6) preparing the anti-infrared spectacle lens: injecting the obtained lens monomer into a lens mold, performing primary curing molding, opening the mold, slicing and cleaning, soaking in a sodium hydroxide solution with the mass fraction of 30% for secondary curing, ultrasonically cleaning with deionized water, and drying to obtain the anti-infrared spectacle lens.
Further, the preparation method comprises the following specific steps:
(1) preparation of organic phase dispersion: mixing corn starch, urea and deionized water according to a mass ratio of 1:1:10 under an anaerobic condition, then filling the mixture into a reaction kettle filled with nitrogen, starting a stirrer, and stirring and mixing the mixture at a rotating speed of 500-600 r/min for 30-40 min to obtain an organic phase dispersion liquid;
(2) preparing ferrite nano particles: adding ferrous chloride accounting for 10% of the mass of the organic phase dispersion liquid into the reaction kettle, stirring and dispersing uniformly, then dropwise adding ammonia water with the concentration of 10mol/L into the reaction kettle, adjusting the pH to 8-9, starting a stirrer after the adjustment is finished, stirring and reacting for 1-2 h at the rotating speed of 200-300 r/min, filtering and separating to obtain filter residues, and calcining for 30-40 min at the temperature of 200-300 ℃ in an oxygen-free environment to obtain ferrous salt nanoparticles;
(3) preparation of pretreated ferrous salt nanoparticles: mixing the obtained ferrous salt nano particles and a sodium dodecyl benzene sulfonate solution with the mass fraction of 10% according to the mass ratio of 1:10 under an anaerobic condition, stirring and reacting for 40-60 min at the rotating speed of 100-200 r/min by using a stirrer, filtering, separating to obtain a filter cake, and drying without oxygen to obtain pretreated ferrous salt nano particles;
(4) preparing core-shell ferrite nanoparticles: adding 250-300 parts of distilled water and 10-15 parts of sodium bicarbonate into a three-neck round-bottom flask with a stirrer, a reflux condenser tube and a nitrogen guide tube in parts by weight, continuously introducing nitrogen into the three-neck round-bottom flask, stirring at a rotating speed of 300-400 r/min for 15-20 min, adding 50-60 parts of styrene and 20-30 parts of pretreated ferrite nanoparticles into the three-neck round-bottom flask, heating to 70-80 ℃, adding 3-5 parts of potassium persulfate, carrying out thermal polymerization reaction for 12-14 h under the protection of nitrogen, filtering and separating after the reaction is finished to obtain reaction filter residues, and drying to obtain core-shell ferrite nanoparticles;
(5) preparation of lens monomer: weighing 60-70 parts of styrene, 10-15 parts of trimethylolpropane triacrylate, 10-15 parts of the core-shell type ferrous salt nanoparticles, 5-7 parts of an initiator, 3-5 parts of a coupling agent and 0.3-0.5 part of an internal mold release agent, adding the materials into a reaction kettle, heating to 100-120 ℃ under the protection of nitrogen, stirring and reacting at a rotating speed of 200-300 r/min for 60-90 min to obtain a mixture, and filtering and separating to obtain a reaction filtrate, namely a lens monomer;
(6) preparing the anti-infrared spectacle lens: injecting the obtained lens monomer into a lens mold, performing primary curing molding, opening the mold, slicing and cleaning, soaking in a sodium hydroxide solution with the mass fraction of 30% for secondary curing, ultrasonically cleaning with deionized water, and drying to obtain the anti-infrared spectacle lens.
By the scheme, the invention at least has the following advantages:
the invention firstly uses corn starch with a spherical structure as a template, urea as an organic phase dispersant and ferrous chloride as raw materials, ammonia water as a precipitator, prepares ferrite nanoparticles by a solution method, modifies a surfactant on the surface of the ferrite, wraps the nanoparticles modified by the surfactant by a high molecular resin through a soap-free emulsion polymerization method to form a core-shell structure, and adds the core-shell structure as a red light (infrared ray) absorbent into a conventional lens monomer to process into the anti-red light lens. In addition, the metal ion nanoparticles are protected by modification of a surfactant and coating of a polymer, so that oxidation reaction of metal ions can be avoided, further discoloration of the lens is avoided, and the compatibility of the nanoparticles and the monomer can be increased by coating of the core-shell type ferrite nanoparticles with the polymer, so that the nanoparticles are uniformly dispersed in the lens; because the nano particles exist in the lens material as a disperse phase, the influence on the mechanical property of the lens can be reduced, the lens product produced by the technical scheme shows good infrared absorption performance in the wavelength range of 750 nanometers to 1 millimeter, and simultaneously, the impact resistance of the lens is reduced by less than 10 percent.
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 organic phase dispersion: mixing corn starch, urea and deionized water according to a mass ratio of 1:1:10 under an anaerobic condition, then filling the mixture into a reaction kettle filled with nitrogen, starting a stirrer, and stirring and mixing the mixture at a rotating speed of 500-600 r/min for 30-40 min to obtain an organic phase dispersion liquid;
(2) preparing ferrite nano particles: adding ferrous chloride accounting for 10% of the mass of the organic phase dispersion liquid into the reaction kettle, stirring and dispersing uniformly, then dropwise adding ammonia water with the concentration of 10mol/L into the reaction kettle, adjusting the pH to 8-9, starting a stirrer after the adjustment is finished, stirring and reacting for 1-2 h at the rotating speed of 200-300 r/min, filtering and separating to obtain filter residues, and calcining for 30-40 min at the temperature of 200-300 ℃ in an oxygen-free environment to obtain ferrous salt nanoparticles;
(3) preparation of pretreated ferrous salt nanoparticles: mixing the obtained ferrous salt nano particles and a sodium dodecyl benzene sulfonate solution with the mass fraction of 10% according to the mass ratio of 1:10 under an anaerobic condition, stirring and reacting for 40-60 min at the rotating speed of 100-200 r/min by using a stirrer, filtering, separating to obtain a filter cake, and drying without oxygen to obtain pretreated ferrous salt nano particles;
(4) preparing core-shell ferrite nanoparticles: adding 250-300 parts of distilled water and 10-15 parts of sodium bicarbonate into a three-neck round-bottom flask with a stirrer, a reflux condenser tube and a nitrogen guide tube in parts by weight, continuously introducing nitrogen into the three-neck round-bottom flask, stirring at a rotating speed of 300-400 r/min for 15-20 min, adding 50-60 parts of styrene and 20-30 parts of pretreated ferrite nanoparticles into the three-neck round-bottom flask, heating to 70-80 ℃, adding 3-5 parts of potassium persulfate, carrying out thermal polymerization reaction for 12-14 h under the protection of nitrogen, filtering and separating after the reaction is finished to obtain reaction filter residues, and drying to obtain core-shell ferrite nanoparticles;
(5) preparation of lens monomer: weighing 60-70 parts of styrene, 10-15 parts of trimethylolpropane triacrylate, 10-15 parts of the core-shell type ferrous salt nanoparticles, 5-7 parts of an initiator, 3-5 parts of a coupling agent and 0.3-0.5 part of an internal mold release agent, adding the materials into a reaction kettle, heating to 100-120 ℃ under the protection of nitrogen, stirring and reacting at a rotating speed of 200-300 r/min for 60-90 min to obtain a mixture, and filtering and separating to obtain a reaction filtrate, namely a lens monomer;
(6) preparing the anti-infrared spectacle lens: injecting the obtained lens monomer into a lens mold, performing primary curing molding, opening the mold, slicing and cleaning, soaking in a sodium hydroxide solution with the mass fraction of 30% for secondary curing, ultrasonically cleaning with deionized water, and drying to obtain the anti-infrared spectacle lens.
Example 1
(1) Preparation of organic phase dispersion: mixing corn starch, urea and deionized water according to a mass ratio of 1:1:10 under an anaerobic condition, then filling the mixture into a reaction kettle filled with nitrogen, starting a stirrer to stir and mix for 30min at a rotating speed of 500r/min, and obtaining an organic phase dispersion liquid;
(2) preparing ferrite nano particles: adding ferrous chloride accounting for 10% of the mass of the organic phase dispersion liquid into the reaction kettle, stirring and dispersing uniformly, then dropwise adding ammonia water with the concentration of 10mol/L into the reaction kettle, adjusting the pH to 8, starting a stirrer after the adjustment is finished, stirring and reacting at the rotating speed of 200r/min for 1 hour, filtering and separating to obtain filter residue, and calcining at the temperature of 200 ℃ for 30 minutes in an anaerobic environment to obtain ferrous salt nano particles;
(3) preparation of pretreated ferrous salt nanoparticles: mixing the obtained ferrite nanoparticles with a sodium dodecyl benzene sulfonate solution with the mass fraction of 10% in an oxygen-free condition according to the mass ratio of 1:10, stirring and reacting for 40min at the rotating speed of 100r/min by using a stirrer, filtering, separating to obtain a filter cake, and drying without oxygen to obtain pretreated ferrite nanoparticles;
(4) preparing core-shell ferrite nanoparticles: adding 250 parts by weight of distilled water and 10 parts by weight of sodium bicarbonate into a three-neck round-bottom flask with a stirrer, a reflux condenser tube and a nitrogen guide tube, continuously introducing nitrogen into the three-neck round-bottom flask, stirring at the rotating speed of 300r/min for 15min, adding 50 parts by weight of styrene and 20 parts by weight of pretreated ferrite nanoparticles into the three-neck round-bottom flask, heating to 70 ℃, adding 3 parts by weight of potassium persulfate, carrying out thermal polymerization reaction for 12h under the protection of nitrogen, filtering and separating after the reaction is finished to obtain reaction filter residues, and drying to obtain core-shell ferrite nanoparticles;
(5) preparation of lens monomer: weighing 60 parts of styrene, 10 parts of trimethylolpropane triacrylate, 10 parts of the core-shell type ferrous salt nano particles, 5 parts of an initiator, 3 parts of a coupling agent and 0.3 part of an internal mold release agent, adding into a reaction kettle, heating to 100 ℃ under the protection of nitrogen, stirring at a rotating speed of 200r/min for reacting for 60min to obtain a mixture, and filtering and separating to obtain a reaction filtrate, namely a lens monomer;
(6) preparing the anti-infrared spectacle lens: injecting the obtained lens monomer into a lens mold, performing primary curing molding, opening the mold, slicing and cleaning, soaking in a sodium hydroxide solution with the mass fraction of 30% for secondary curing, ultrasonically cleaning with deionized water, and drying to obtain the anti-infrared spectacle lens.
Example 2
(1) Preparation of organic phase dispersion: mixing corn starch, urea and deionized water according to a mass ratio of 1:1:10 under an anaerobic condition, then filling the mixture into a reaction kettle filled with nitrogen, starting a stirrer to stir and mix for 35min at a rotating speed of 550r/min to obtain an organic phase dispersion liquid;
(2) preparing ferrite nano particles: adding ferrous chloride accounting for 10% of the mass of the organic phase dispersion liquid into the reaction kettle, stirring and dispersing uniformly, then dropwise adding ammonia water with the concentration of 10mol/L into the reaction kettle, adjusting the pH to 9, starting a stirrer after the adjustment is finished, stirring and reacting at the rotating speed of 250r/min for 2 hours, filtering and separating to obtain filter residue, and calcining at the temperature of 250 ℃ for 35 minutes in an anaerobic environment to obtain ferrous salt nano particles;
(3) preparation of pretreated ferrous salt nanoparticles: mixing the obtained ferrite nanoparticles with a sodium dodecyl benzene sulfonate solution with the mass fraction of 10% in an anaerobic condition according to the mass ratio of 1:10, stirring and reacting for 45min at the rotating speed of 150r/min by using a stirrer, filtering, separating to obtain a filter cake, and drying without oxygen to obtain pretreated ferrite nanoparticles;
(4) preparing core-shell ferrite nanoparticles: adding 280 parts of distilled water and 13 parts of sodium bicarbonate into a three-neck round-bottom flask with a stirrer, a reflux condenser tube and a nitrogen guide tube, continuously introducing nitrogen into the three-neck round-bottom flask, stirring at the rotating speed of 350r/min for 18min, adding 55 parts of styrene and 25 parts of pretreated ferrite nanoparticles into the three-neck round-bottom flask, heating to 75 ℃, adding 4 parts of potassium persulfate, carrying out thermal polymerization reaction for 13h under the protection of nitrogen, filtering and separating after the reaction is finished to obtain reaction filter residues, and drying to obtain core-shell ferrite nanoparticles;
(5) preparation of lens monomer: weighing 65 parts of styrene, 13 parts of trimethylolpropane triacrylate, 13 parts of the core-shell type ferrous salt nanoparticles, 6 parts of an initiator, 4 parts of a coupling agent and 0.4 part of an internal mold release agent, adding into a reaction kettle, heating to 110 ℃ under the protection of nitrogen, stirring at a rotating speed of 250r/min for 75min to react to obtain a mixture, and filtering and separating to obtain a reaction filtrate, namely a lens monomer;
(6) preparing the anti-infrared spectacle lens: injecting the obtained lens monomer into a lens mold, performing primary curing molding, opening the mold, slicing and cleaning, soaking in a sodium hydroxide solution with the mass fraction of 30% for secondary curing, ultrasonically cleaning with deionized water, and drying to obtain the anti-infrared spectacle lens.
Example 3
(1) Preparation of organic phase dispersion: mixing corn starch, urea and deionized water according to a mass ratio of 1:1:10 under an anaerobic condition, then filling the mixture into a reaction kettle filled with nitrogen, starting a stirrer to stir and mix for 40min at a rotating speed of 600r/min, and obtaining an organic phase dispersion liquid;
(2) preparing ferrite nano particles: adding ferrous chloride accounting for 10% of the mass of the organic phase dispersion liquid into the reaction kettle, stirring and dispersing uniformly, then dropwise adding ammonia water with the concentration of 10mol/L into the reaction kettle, adjusting the pH to 9, starting a stirrer after the adjustment is finished, stirring and reacting at the rotating speed of 300r/min for 2 hours, filtering and separating to obtain filter residues, and calcining at the temperature of 300 ℃ for 40 minutes in an anaerobic environment to obtain ferrous salt nano particles;
(3) preparation of pretreated ferrous salt nanoparticles: mixing the obtained ferrite nanoparticles with a sodium dodecyl benzene sulfonate solution with the mass fraction of 10% in an anaerobic condition according to the mass ratio of 1:10, stirring and reacting for 60min by using a stirrer at the rotating speed of 200r/min, filtering, separating to obtain a filter cake, and drying without oxygen to obtain pretreated ferrite nanoparticles;
(4) preparing core-shell ferrite nanoparticles: adding 300 parts of distilled water and 15 parts of sodium bicarbonate into a three-neck round-bottom flask with a stirrer, a reflux condenser tube and a nitrogen guide tube, continuously introducing nitrogen into the three-neck round-bottom flask, stirring at a rotating speed of 400r/min for 20min, adding 60 parts of styrene and 30 parts of pretreated ferrite nanoparticles into the three-neck round-bottom flask, heating to 80 ℃, adding 5 parts of potassium persulfate, carrying out thermal polymerization reaction for 14h under the protection of nitrogen, filtering and separating after the reaction is finished to obtain reaction filter residues, and drying to obtain core-shell ferrite nanoparticles;
(5) preparation of lens monomer: weighing 70 parts of styrene, 15 parts of trimethylolpropane triacrylate, 15 parts of the core-shell type ferrous salt nanoparticles, 7 parts of an initiator, 5 parts of a coupling agent and 0.5 part of an internal mold release agent, adding into a reaction kettle, heating to 120 ℃ under the protection of nitrogen, stirring at a rotating speed of 300r/min for 90min to obtain a mixture, and filtering and separating to obtain a reaction filtrate, namely a lens monomer;
(6) preparing the anti-infrared spectacle lens: injecting the obtained lens monomer into a lens mold, performing primary curing molding, opening the mold, slicing and cleaning, soaking in a sodium hydroxide solution with the mass fraction of 30% for secondary curing, ultrasonically cleaning with deionized water, and drying to obtain the anti-infrared spectacle lens.
Comparative example 1: the preparation method is basically the same as that of the example 1 of the present invention, except that the core-shell type ferrite nanoparticles of the present invention are replaced with ferrite nanoparticles;
comparative example 2: the preparation was essentially the same as in example 1 of the present invention, except that no corn starch was added when preparing the organic phase dispersion;
the present invention was tested for performance in examples 1-3 and comparative examples 1 and 2, respectively, and the test results are shown in table 1:
the detection method comprises the following steps:
and (3) detecting the infrared light absorption rate: and (3) testing the ratio of the absorbed thermal radiation energy projected onto the lens to the total thermal radiation energy projected onto the lens by using an infrared temperature tester, namely the infrared light absorption rate.
Reduction rate of impact resistance: testing the impact strength D1 of the lens to be tested and the impact strength D2 of the lens without the infrared absorbent, wherein the impact resistance reduction rate is (D2-D1)/D2.
TABLE 1 Performance test results
As can be seen from the detection data in the table above, the addition of the core-shell type ferrite nanoparticles of the invention significantly improves the infrared ray resistance of the lens, has little influence on the mechanical strength of the original lens, and has wide application prospects.
Claims (6)
1. An infrared-resistant spectacle lens is characterized by being prepared from the following raw materials in parts by weight:
60-70 parts of styrene, 10-15 parts of trimethylolpropane triacrylate, 10-15 parts of core-shell type ferrous salt nanoparticles, 5-7 parts of an initiator, 3-5 parts of a coupling agent and 0.3-0.5 part of an internal mold release agent;
the core-shell type ferrous salt nano-particles are prepared from the following raw materials:
corn starch, urea, deionized water, ferrous chloride, ammonia water, sodium dodecyl benzene sulfonate, distilled water, sodium bicarbonate, nitrogen, styrene and potassium persulfate.
2. The ir-resistant spectacle lens according to claim 1, wherein the initiator is a mixture of sodium bisulfite and ammonium persulfate at an equal mass ratio.
3. The ir-resistant ophthalmic lens of claim 1, wherein the coupling agent is a silane coupling agent.
4. The ir-resistant spectacle lens according to claim 1, wherein the internal mold release agent is one of silicone oil, silicone methyl branched silicone oil, methyl silicone oil, and emulsified methyl silicone oil.
5. The preparation method of the infrared-resistant spectacle lens is characterized by comprising the following specific preparation steps:
(1) preparation of organic phase dispersion: under the anaerobic condition, putting corn starch, urea and deionized water into a reaction kettle, mixing and stirring for reaction to obtain an organic phase dispersion liquid;
(2) preparing ferrite nano particles: adding ferrous chloride into the organic phase dispersion liquid, stirring and dispersing uniformly, then dropwise adding ammonia water, adjusting pH, continuously stirring and reacting, filtering to obtain filter residue, and calcining in an oxygen-free environment to obtain ferrous salt nanoparticles;
(3) preparation of pretreated ferrous salt nanoparticles: under the anaerobic condition, mixing the ferrous salt nano-particles with a sodium dodecyl benzene sulfonate solution, stirring for reaction, filtering and separating to obtain a filter cake, and drying without oxygen to obtain pretreated ferrous salt nano-particles;
(4) preparing core-shell ferrite nanoparticles: adding distilled water and sodium bicarbonate into a three-neck round-bottom flask, continuously introducing nitrogen, stirring, adding styrene and pretreated ferrite nanoparticles into the three-neck round-bottom flask, heating, adding potassium persulfate, carrying out thermal polymerization reaction, filtering and separating after the reaction is finished to obtain reaction filter residues, and drying to obtain core-shell ferrite nanoparticles;
(5) preparation of lens monomer: weighing styrene, trimethylolpropane triacrylate, core-shell ferrite nanoparticles, an initiator, a coupling agent and an internal release agent, adding the weighed materials into a reaction kettle, heating and raising the temperature under the protection of nitrogen, stirring for reaction to obtain a mixture, and filtering and separating to obtain a reaction filtrate, namely a lens monomer;
(6) preparing the anti-infrared spectacle lens: injecting the obtained lens monomer into a lens mold, performing primary curing molding, opening the mold, slicing and cleaning, soaking in a sodium hydroxide solution with the mass fraction of 30% for secondary curing, ultrasonically cleaning with deionized water, and drying to obtain the anti-infrared spectacle lens.
6. The method for preparing an infrared-resistant spectacle lens according to claim 5, comprising the following steps:
(1) preparation of organic phase dispersion: mixing corn starch, urea and deionized water according to a mass ratio of 1:1:10 under an anaerobic condition, then filling the mixture into a reaction kettle filled with nitrogen, starting a stirrer, and stirring and mixing the mixture at a rotating speed of 500-600 r/min for 30-40 min to obtain an organic phase dispersion liquid;
(2) preparing ferrite nano particles: adding ferrous chloride accounting for 10% of the mass of the organic phase dispersion liquid into the reaction kettle, stirring and dispersing uniformly, then dropwise adding ammonia water with the concentration of 10mol/L into the reaction kettle, adjusting the pH to 8-9, starting a stirrer after the adjustment is finished, stirring and reacting for 1-2 h at the rotating speed of 200-300 r/min, filtering and separating to obtain filter residues, and calcining for 30-40 min at the temperature of 200-300 ℃ in an oxygen-free environment to obtain ferrous salt nanoparticles;
(3) preparation of pretreated ferrous salt nanoparticles: mixing the obtained ferrous salt nano particles and a sodium dodecyl benzene sulfonate solution with the mass fraction of 10% according to the mass ratio of 1:10 under an anaerobic condition, stirring and reacting for 40-60 min at the rotating speed of 100-200 r/min by using a stirrer, filtering, separating to obtain a filter cake, and drying without oxygen to obtain pretreated ferrous salt nano particles;
(4) preparing core-shell ferrite nanoparticles: adding 250-300 parts of distilled water and 10-15 parts of sodium bicarbonate into a three-neck round-bottom flask with a stirrer, a reflux condenser tube and a nitrogen guide tube in parts by weight, continuously introducing nitrogen into the three-neck round-bottom flask, stirring at a rotating speed of 300-400 r/min for 15-20 min, adding 50-60 parts of styrene and 20-30 parts of pretreated ferrite nanoparticles into the three-neck round-bottom flask, heating to 70-80 ℃, adding 3-5 parts of potassium persulfate, carrying out thermal polymerization reaction for 12-14 h under the protection of nitrogen, filtering and separating after the reaction is finished to obtain reaction filter residues, and drying to obtain core-shell ferrite nanoparticles;
(5) preparation of lens monomer: weighing 60-70 parts of styrene, 10-15 parts of trimethylolpropane triacrylate, 10-15 parts of the core-shell type ferrous salt nanoparticles, 5-7 parts of an initiator, 3-5 parts of a coupling agent and 0.3-0.5 part of an internal mold release agent, adding the materials into a reaction kettle, heating to 100-120 ℃ under the protection of nitrogen, stirring and reacting at a rotating speed of 200-300 r/min for 60-90 min to obtain a mixture, and filtering and separating to obtain a reaction filtrate, namely a lens monomer;
(6) preparing the anti-infrared spectacle lens: injecting the obtained lens monomer into a lens mold, performing primary curing molding, opening the mold, slicing and cleaning, soaking in a sodium hydroxide solution with the mass fraction of 30% for secondary curing, ultrasonically cleaning with deionized water, and drying to obtain the anti-infrared spectacle lens.
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