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CN115215976A - Weather-resistant and aging-resistant lens and preparation method thereof - Google Patents

Weather-resistant and aging-resistant lens and preparation method thereof Download PDF

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Publication number
CN115215976A
CN115215976A CN202210950747.8A CN202210950747A CN115215976A CN 115215976 A CN115215976 A CN 115215976A CN 202210950747 A CN202210950747 A CN 202210950747A CN 115215976 A CN115215976 A CN 115215976A
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China
Prior art keywords
curing
lens
aluminum powder
powder
resistant
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Pending
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CN202210950747.8A
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Chinese (zh)
Inventor
唐伟明
戴双汉
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JIANGSU KEAOXI OPTICAL MATERIAL TECHNOLOGY CO LTD
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JIANGSU KEAOXI OPTICAL MATERIAL TECHNOLOGY CO LTD
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Priority to CN202210950747.8A priority Critical patent/CN115215976A/en
Publication of CN115215976A publication Critical patent/CN115215976A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/10Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
    • C08F283/105Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule on to unsaturated polymers containing more than one epoxy radical per molecule
    • 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
    • C08K3/02Elements
    • C08K3/08Metals
    • 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
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
    • C08K5/52Phosphorus bound to oxygen only
    • C08K5/524Esters of phosphorous acids, e.g. of H3PO3
    • 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
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/04Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
    • G02B1/041Lenses
    • 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
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0812Aluminium

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Polymerisation Methods In General (AREA)

Abstract

The invention provides a weather-resistant and aging-resistant lens and a preparation method thereof, wherein a lens monomer comprises the following components in percentage by weight: 90-95% of matrix polymer; UV powder 0.1-0.2%; 0.15 to 0.35 percent of pigment powder; 0.01 to 0.035 percent of initiator; 0.02 to 0.1 percent of parting agent; 5 to 7 percent of modified aluminum powder; according to the invention, 5-7% of modified aluminum powder by mass fraction is added into the lens monomer, the aluminum powder is modified by a silane coupling agent to improve the compatibility of the aluminum powder and resin, and the weather resistance and aging resistance of the lens finished product are improved to the greatest extent through the synergistic effect of the components.

Description

Weather-resistant and aging-resistant lens and preparation method thereof
Technical Field
The invention relates to a preparation method of a weather-resistant and aging-resistant lens, and particularly relates to optimization of monomer components.
Background
At present, glasses are closely related to the life of people, the utilization rate of the glasses is higher and higher, the range can be extended from myopia glasses, presbyopia glasses and corrective glasses to sunglasses and the like, on one hand, along with the improvement of the use frequency of the glasses, the wear rate of the glasses is increased, after the surface of optical resin is worn, the precision and the light transmittance of optical elements are influenced, and the service life of the glasses is also influenced. There is therefore a need to improve the weathering resistance of the lenses.
Disclosure of Invention
In order to slow down the abrasion of the lens and further improve the weather-resistant and aging-resistant capability of the lens, the preparation method of the weather-resistant and aging-resistant lens is provided.
The specific scheme is as follows:
a weather-resistant and aging-resistant lens comprises the following components:
matrix polymer, UV powder, pigment powder, initiator, parting agent and modified aluminum powder;
the matrix polymer comprises epoxy acrylic resin, dibenzyl maleate, dibenzyl phosphite and styrene;
the mass percentage of the modified aluminum powder is 5-7%, the metal aluminum powder is modified by a silane coupling agent to greatly improve the compatibility of the lens resin, and the metal aluminum has a shielding effect on water molecules, so that the barrier property of the lens resin on the water molecules can be enhanced, the absorption of hydrophilic groups in the molecules on the water molecules can be reduced, and when the aluminum powder is in contact with water or air, cracks can be blocked and repaired due to expansion, so that the wet-heat aging resistance of the resin lens can be improved; the aluminum has stronger reflection function to ultraviolet rays, and the absorption of the resin lens to ultraviolet rays is greatly reduced.
Preferably, the specific preparation method of the modified aluminum powder comprises the following steps: washing the metal aluminum powder by using a solvent, filtering and drying at normal temperature; preparing a silane coupling agent, water and ethanol into a solution according to a certain mass ratio, standing for hydrolysis, adding metal aluminum powder, stirring for reaction at normal temperature, washing with ethanol, filtering, and drying to obtain modified metal aluminum powder, wherein the preferred solvent is acetone; the surface of the metal aluminum powder is treated before modification, and organic impurities remained on the surface of the metal aluminum powder can influence the dispersion of the modified metal aluminum powder in a monomer, and finally influence the qualification rate of finished lens products.
Preferably, the silane coupling agent is gamma-APS, and the ratio of the silane coupling agent to water to ethanol is as follows: (0.08-3): (1-5): (20-50); by controlling the addition amount of the silane coupling agent, the condition of agglomeration caused by excessive addition of the coupling agent during subsequent high-temperature treatment is avoided;
preferably, the ratio of the silane coupling agent to the water to the ethanol is: 1.5:3:35, when the silane coupling agent: water: the mass ratio of ethanol is 1.5:3: at 35 hours, the electrostatic repulsion among the aluminum powder is maximized, and meanwhile, the silane coupling agent is subjected to polycondensation reaction to form an oligomer, so that a certain three-dimensional barrier is formed, the interaction among particles is favorably reduced, and the aluminum powder pigment is stably dispersed in the aqueous solution;
preferably, the mass percent of the matrix polymer is 90-95%; the mass percent of the UV powder is 0.1-0.2%; the mass percentage of the pigment powder is 0.15-0.35%; the mass percent of the initiator is 0.01-0.035%; the mass percentage of the release agent is 0.02-0.1%.
Preferably, the solvent for washing the metal aluminum powder is acetone.
A preparation method of a weather-resistant and aging-resistant lens comprises the following steps:
s1: weighing the matrix polymer, the pigment powder, the initiator, the release agent and the modified aluminum powder according to the proportion, stirring at normal pressure, continuously adding the UV powder, stirring, and stirring in a pump for 3-6 hours after stirring at normal pressure is finished;
s2: after stirring, adding the materials into a reaction kettle, vacuumizing and removing bubbles;
s3: filling by using a glass mold after vacuumizing and defoaming are finished;
s4: putting the mould into a curing oven for primary curing;
s5: carrying out operations of releasing, trimming and cleaning the substrate molded in the mold;
s6: and putting the substrate into a curing furnace for secondary curing.
Preferably, the specific process of primary curing in S4 is as follows:
setting the temperature at 30 ℃ and curing for 0.01h; gradually heating to 50 ℃, and curing for 0.15h; keeping the temperature at 50 ℃ for 9h; continuously heating to 55 ℃, and curing for 8h; gradually heating to 110 ℃, and curing for 2h; keeping the temperature at 110 ℃ for 2h, gradually cooling to 60 ℃, and curing for 1h.
Preferably, the specific process of the secondary curing in S5 is as follows:
gradually heating to 110 ℃ at 30 ℃, curing for 1h, and keeping the temperature at 110 ℃ for 4h; gradually cooling to 30 deg.C, and curing for 0.1h.
S6: and putting the substrate into a curing furnace for secondary curing and sectional control, and finally curing and forming.
Preferably, the specific process of primary curing is as follows: setting the temperature at 30 ℃, and curing for 0.01h; gradually heating to 50 ℃, and curing for 0.15h; keeping the temperature at 50 ℃ for 9h; continuously heating to 55 ℃, and curing for 8h; gradually heating to 110 ℃, and curing for 2h; keeping the temperature at 110 ℃ for 2h, gradually cooling to 60 ℃, and curing for 1h.
Preferably, the secondary curing process comprises the following steps: gradually heating to 110 ℃ at 30 ℃, curing for 1h, and keeping the temperature at 110 ℃ for 4h; gradually cooling to 30 deg.C, and curing for 0.1h.
Has the advantages that:
(1) The invention provides a monomer suitable for a lens with a refractive index of 1.60 and a preparation method thereof, on one hand, 5-7% of silane coupling agent modified aluminum powder by mass is added into the monomer components of the lens, and the metal aluminum powder is modified, so that the compatibility between the metal aluminum powder and resin is greatly improved, and the metal aluminum has a shielding effect on water molecules, so that the barrier property of the lens resin on the water molecules can be enhanced, the absorption of hydrophilic groups in the molecules on the water molecules is reduced, and the aluminum powder can expand to block and repair micro cracks when contacting with water or air, so that the moisture-heat aging resistance of the resin lens is improved; in addition, aluminum has strong reflection effect on ultraviolet rays, so that the absorption of the resin lens on ultraviolet rays can be reduced by adding aluminum powder, and the weather resistance and aging resistance of a finished lens product can be effectively improved after the modified aluminum powder is doped into the formula of the conventional resin lens.
(2) The silane coupling agent used for modifying the aluminum powder is gamma-APS,
the silane coupling agent is gamma-APS, and the proportion of the silane coupling agent to water to ethanol is as follows: (0.08-3): (1-5): (20-50); by controlling the addition amount of the silane coupling agent, the condition of agglomeration during subsequent high-temperature treatment caused by excessive addition of the coupling agent is avoided; when the silane coupling agent: water: the mass ratio of ethanol is 1.5:3: and 35 hours, the electrostatic repulsion among the aluminum powder is maximized, and meanwhile, the silane coupling agent is subjected to polycondensation reaction to form an oligomer, so that a certain three-dimensional barrier is formed, the interaction among particles is favorably reduced, and the aluminum powder pigment is stably dispersed in the aqueous solution.
(3) The preparation method enables the lens to achieve the optimal curing effect in the preparation process through the sectional curing control.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
The first embodiment is as follows:
(1) Weighing the following materials in percentage by weight:
99.76% of a matrix polymer; 0.15% of UV powder; 0.02% of pigment powder; initiator HILCATDB0.02%; 680.05 percent of mold release agent HILUB;
(2) Connecting a filter to fill a mold;
(3) Putting the mould into a curing oven for primary curing:
heating is carried out through a curing curve and a control program, and the specific technological parameters are as follows: setting the temperature at 30 ℃ and curing for 0.01h; gradually heating to 50 ℃, and curing for 0.15h; keeping the temperature at 50 ℃ for 9h; continuously heating to 55 ℃, and curing for 8h; gradually heating to 110 ℃, and curing for 2h; keeping the temperature at 110 ℃ for 2h, gradually cooling to 60 ℃, and curing for 1h.
(4) Carrying out releasing, trimming and substrate cleaning operations on the substrate molded in the mold: conveying the once-cured semi-finished product to a release table for release operation, separating the lens from the mold, respectively taking out the lens and the mold for trimming and cleaning, and trimming the lens by using a trimmer; carrying out ultrasonic cleaning on the lens by using a cleaning solution;
(5) Putting the substrate into a curing furnace for secondary curing: carrying out secondary curing to further eliminate internal stress, wherein the specific process parameters are as follows: gradually heating to 110 ℃ at 30 ℃, curing for 1h, and keeping the temperature at 110 ℃ for 4h; gradually cooling to 30 deg.C, and curing for 0.1h;
(6) And inspecting the substrate.
The test results are shown below:
example two:
(1) Weighing the following materials in percentage by weight:
94% of a matrix polymer; 0.15% of UV powder; 0.02 percent of pigment powder; initiator HILCATDB0.02%; 680.05 percent of mold release agent HILUB; 5.76 percent of aluminum powder;
(2) Filling a mould by connecting a filter;
(3) Putting the mould into a curing oven for primary curing: heating is carried out through a curing curve and a control program, and the specific technological parameters are as follows: setting the temperature at 30 ℃ and curing for 0.01h; gradually heating to 50 ℃, and curing for 0.15h; keeping the temperature at 50 ℃ for 9h; continuously heating to 55 ℃, and curing for 8h; gradually heating to 110 ℃, and curing for 2h; keeping the temperature at 110 ℃ for 2h, gradually cooling to 60 ℃, and curing for 1h.
(4) Carrying out releasing, trimming and substrate cleaning operations on the substrate molded in the mold: conveying the once-cured semi-finished product to a release table for release operation, separating the lens from the mold, respectively taking out the lens and the mold for trimming and cleaning, and trimming the lens by using a trimmer; carrying out ultrasonic cleaning on the lens by using a cleaning solution;
(5) Putting the substrate into a curing furnace for secondary curing: carrying out secondary curing to further eliminate internal stress, wherein the specific process parameters are as follows: gradually heating to 110 ℃ at 30 ℃, curing for 1h, and keeping the temperature at 110 ℃ for 4h; gradually cooling to 30 deg.C, and curing for 0.1h;
(6) And inspecting the substrate.
Example three:
(1) Weighing the following materials in percentage by weight:
94% of a matrix polymer; 0.15 percent of UV powder; 0.02 percent of pigment powder; initiator HILCATDB0.02%; 680.05 percent of mold release agent HILUB; 5.76 percent of modified aluminum powder; the preparation method of the modified aluminum powder comprises the following steps: wherein, the metal aluminum powder is washed by acetone, filtered and dried at normal temperature; silane coupling agent, water and ethanol are mixed according to a ratio of 1.5:3:35, standing for hydrolysis, adding metal aluminum powder, stirring at normal temperature for reaction, washing with ethanol, filtering, and drying to obtain the modified metal aluminum powder.
(2) Filling a mould by connecting a filter;
(3) Putting the mould into a curing oven for primary curing: heating is carried out through a curing curve and a control program, and the specific process parameters are as follows: setting the temperature at 30 ℃, and curing for 0.01h; gradually heating to 50 ℃, and curing for 0.15h; keeping the temperature at 50 ℃ for 9h; continuously heating to 55 ℃, and curing for 8h; gradually heating to 110 ℃, and curing for 2h; keeping the temperature at 110 ℃ for 2h, gradually cooling to 60 ℃, and curing for 1h.
(4) Carrying out releasing, trimming and substrate cleaning operations on the substrate molded in the mold: conveying the once-cured semi-finished product to a release table for release operation, separating the lens from the mold, respectively taking out the lens and the mold for trimming and cleaning, and trimming the lens by using a trimmer; carrying out ultrasonic cleaning on the lens by using a cleaning solution;
(5) Putting the substrate into a curing furnace for secondary curing: carrying out secondary curing to further eliminate internal stress, wherein the specific process parameters are as follows: gradually heating to 110 ℃ at 30 ℃, curing for 1h, and keeping the temperature at 110 ℃ for 4h; gradually cooling to 30 deg.C, and curing for 0.1h.
(6) And inspecting the substrate.
Impact testing was performed on the lenses obtained in examples 1 to 3: the lens made in example three did not crack when a steel ball with a diameter of 16mm was used to impact the convex surface of the lens by free fall from a height of 1.27 m.
As a further improvement, the above-mentioned is only a preferred embodiment of the present invention, and should not be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. The weather-resistant and aging-resistant lens is characterized in that a lens monomer comprises the following components:
matrix polymer, UV powder, pigment powder, initiator, mold release agent and modified aluminum powder;
the matrix polymer comprises epoxy acrylic resin, dibenzyl maleate, dibenzyl phosphite and styrene;
the mass percentage of the modified aluminum powder is 5-7%.
2. The weather-resistant and aging-resistant lens according to claim 1, wherein the specific preparation method of the modified aluminum powder comprises: washing the metal aluminum powder by using a solvent, filtering and drying at normal temperature; preparing a silane coupling agent, water and ethanol into a solution according to a certain mass ratio, standing for hydrolysis, adding metal aluminum powder, stirring for reaction at normal temperature, washing with ethanol, filtering, and drying to obtain the modified metal aluminum powder.
3. The lens of claim 2, wherein the silane coupling agent is γ -APS, and the ratio of the silane coupling agent to water to ethanol is: (0.08-3): (1-5): (20 to 50).
4. The lens of claim 3, wherein the ratio of the silane coupling agent to the water to the ethanol is: 1.5:3:35.
5. the lens of claim 1, wherein the matrix polymer is 90-95% by weight; the mass percent of the UV powder is 0.1-0.2%; the mass percentage of the pigment powder is 0.15-0.35%; the mass percent of the initiator is 0.01-0.035%; the mass percentage of the release agent is 0.02-0.1%.
6. The lens of claim 2, wherein the solvent for washing the metal aluminum powder is acetone.
7. The method for preparing a weathering resistant and weathering resistant lens according to any of claims 1 to 6, comprising the steps of:
s1: weighing the matrix polymer, the pigment powder, the initiator, the release agent and the modified aluminum powder according to the proportion, stirring at normal pressure, continuously adding the UV powder, stirring, and stirring in a pump for 3-6 hours after normal-pressure stirring is finished;
s2: after stirring, adding the materials into a reaction kettle, vacuumizing and removing bubbles;
s3: filling by using a glass mold after vacuumizing and defoaming are finished;
s4: putting the mould into a curing oven for primary curing;
s5: carrying out operations of releasing, trimming and cleaning the substrate molded in the mold;
s6: and putting the substrate into a curing furnace for secondary curing.
8. The method for preparing the lens with weather resistance and aging resistance as claimed in claim 7, wherein the specific process of the primary curing in S4 is as follows:
setting the temperature at 30 ℃, and curing for 0.01h; gradually heating to 50 ℃, and curing for 0.15h; keeping the temperature at 50 ℃ for 9h; continuously heating to 55 ℃, and curing for 8h; gradually heating to 110 ℃, and curing for 2h; keeping the temperature at 110 ℃ for 2h, gradually cooling to 60 ℃, and curing for 1h.
9. The method for preparing the lens with weather resistance and aging resistance as claimed in claim 7, wherein the secondary curing in S5 comprises the following specific processes:
gradually heating to 110 ℃ at 30 ℃, curing for 1h, and keeping the temperature at 110 ℃ for 4h; gradually cooling to 30 deg.C, and curing for 0.1h.
CN202210950747.8A 2022-08-09 2022-08-09 Weather-resistant and aging-resistant lens and preparation method thereof Pending CN115215976A (en)

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CN115215976A true CN115215976A (en) 2022-10-21

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0725920A (en) * 1993-07-15 1995-01-27 Mitsubishi Chem Corp Composition for polymerization and resin material
JP2012092185A (en) * 2010-10-26 2012-05-17 Mitsubishi Engineering Plastics Corp Polyacetal resin composition and molding composed of the same
CN104583251A (en) * 2012-08-28 2015-04-29 可奥熙搜路司有限公司 Method for manufacturing epoxy acrylic optical material
CN110256640A (en) * 2019-06-12 2019-09-20 江苏韩创新材料有限公司 A kind of optical mirror slip and manufacturing method
CN110637040A (en) * 2017-05-25 2019-12-31 可奥熙搜路司有限公司 Resin composition for epoxy acrylic medium refractive optical lens and preparation method thereof
JP2020007416A (en) * 2018-07-04 2020-01-16 株式会社クラレ Lens made of methacrylic resin
CN111308584A (en) * 2019-12-06 2020-06-19 江苏康耐特光学有限公司 Blue-light-proof and infrared-proof resin lens with refractive index of 1.50 and preparation method thereof
CN113703084A (en) * 2021-08-30 2021-11-26 江苏韩创新材料有限公司 Transparent blue-light-proof lens and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0725920A (en) * 1993-07-15 1995-01-27 Mitsubishi Chem Corp Composition for polymerization and resin material
JP2012092185A (en) * 2010-10-26 2012-05-17 Mitsubishi Engineering Plastics Corp Polyacetal resin composition and molding composed of the same
CN104583251A (en) * 2012-08-28 2015-04-29 可奥熙搜路司有限公司 Method for manufacturing epoxy acrylic optical material
CN110637040A (en) * 2017-05-25 2019-12-31 可奥熙搜路司有限公司 Resin composition for epoxy acrylic medium refractive optical lens and preparation method thereof
JP2020007416A (en) * 2018-07-04 2020-01-16 株式会社クラレ Lens made of methacrylic resin
CN110256640A (en) * 2019-06-12 2019-09-20 江苏韩创新材料有限公司 A kind of optical mirror slip and manufacturing method
CN111308584A (en) * 2019-12-06 2020-06-19 江苏康耐特光学有限公司 Blue-light-proof and infrared-proof resin lens with refractive index of 1.50 and preparation method thereof
CN113703084A (en) * 2021-08-30 2021-11-26 江苏韩创新材料有限公司 Transparent blue-light-proof lens and preparation method thereof

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* Cited by examiner, † Cited by third party
Title
杨美丽: "铝粉末/环氧树脂复合材料制备与性能研究", 中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑, pages 295 - 297 *

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Application publication date: 20221021