CN111440402A - Nano composite infrared-resistant lens monomer with refractive index of 1.60 - Google Patents

Nano composite infrared-resistant lens monomer with refractive index of 1.60 Download PDF

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Publication number
CN111440402A
CN111440402A CN202010391623.1A CN202010391623A CN111440402A CN 111440402 A CN111440402 A CN 111440402A CN 202010391623 A CN202010391623 A CN 202010391623A CN 111440402 A CN111440402 A CN 111440402A
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China
Prior art keywords
refractive index
infrared
matrix polymer
lens monomer
monomer
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Pending
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CN202010391623.1A
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Chinese (zh)
Inventor
钱军
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 CN202010391623.1A priority Critical patent/CN111440402A/en
Publication of CN111440402A publication Critical patent/CN111440402A/en
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    • 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
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • 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
    • C08K5/0008Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/005Stabilisers against oxidation, heat, light, ozone
    • 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

A nano composite anti-infrared lens monomer with refractive index of 1.60 contains a matrix polymer, a near-infrared absorbent and an ultraviolet absorbent; the matrix polymer was prepared according to the following procedure: adding a silane coupling agent into a reaction kettle, adding a proper amount of a curing agent and a solvent under the stirring condition, and adjusting the pH value to 5.5-6.5, wherein n (the silane coupling agent): n (curing agent) is 1: 1.5-2.8; then adding tetrabutyl titanate into the reaction kettle, and reacting for 8-12h at 100-130 ℃ to obtain a pre-reactant; adding PMMA into the pre-reactant, stirring uniformly, removing the solvent by spinning, and adding a proper amount of curing agent to obtain the matrix polymer; the nano titanium dioxide with higher refractive index is introduced into a PMMA system, the surface of a titanium dioxide precursor n-butyl titanate is modified, and then PMMA is added, so that the good dispersion of titanium dioxide nano particles in a polymer system can be fully promoted, the agglomeration of the nano particles is reduced, the high transparency of the lens is ensured, and the lens has higher refractive index.

Description

Nano composite infrared-resistant lens monomer with refractive index of 1.60
Technical Field
The invention relates to a nano composite anti-infrared lens monomer with a refractive index of 1.60.
Background
Compared with optical glass, the optical resin has the advantages of light weight, easy dyeing, difficult breakage and the like, and is widely used in the fields of spectacle lenses, optical disk substrates, optical lenses, prisms and the like; in recent years, the lenses made of glass materials have been replaced by resin lenses because the safety and comfort of wearing glasses by myopes are greatly affected due to the defects of fragility, heavy weight and the like. Among them, the medium and high refractive index optical resin lens is more favored by users by the special advantages of high light transmittance, ultraviolet resistance, ultra-thin property and the like; generally, in the lens industry, the refractive index is higher than 1.60, the refractive index is medium, and the refractive index is low below 1.56, under the same precondition, the higher the refractive index of the lens is, the thinner the lens is, the lighter the lens is; at present, most of optical resins in domestic markets have refractive indexes below 1.60, and less optical materials with refractive indexes higher than 1.6 are available; with the development of the times, the varieties and functions of the lenses are enriched, and particularly, the daily protection lenses are distinguished to prevent ultraviolet rays, blue light and the like; generally, the effect of protecting human eyes by using ultraviolet-proof lenses and blue-proof lenses is acknowledged, but besides common harmful light rays such as ultraviolet rays and blue light rays, light rays also harm the health of eyes anytime and anywhere, and near infrared rays are one of the chief causes of threatening the health of eyes; the near infrared band is 780 nm-1400 nm, which is a thermal radiation with longer wavelength, and the penetration force is stronger than that of the ultraviolet ray, which is more harmful to human eyes. Therefore, there is a need for an optical resin monomer material for producing a resin lens having a high refractive index and an anti-infrared function.
Disclosure of Invention
The invention aims to solve the defects of the prior art, and provides a nano composite anti-infrared lens monomer with the refractive index of 1.60, wherein the lens monomer contains a matrix polymer, a near-infrared absorbent and an ultraviolet absorbent;
the matrix polymer is prepared according to the following steps: weighing a certain amount of silane coupling agent, adding the silane coupling agent into a reaction kettle, adding a proper amount of curing agent and solvent under the stirring condition, and adjusting the pH value to be 5.5-6.5, wherein n (silane coupling agent): n (curing agent) is 1: 1.5-2.8; then adding tetrabutyl titanate into the reaction kettle, and reacting for 8-12h at 100-130 ℃ to obtain a pre-reactant; adding PMMA into the pre-reactant, stirring uniformly, removing the solvent by spinning, and adding a proper amount of curing agent to obtain the matrix polymer; wherein the mass ratio of PMMA, n-butyl titanate and curing agent is 8-10: 2-4: 6-9: 2-4.
Preferably, the near infrared absorbent is selected from any one of cyanine pigments, phthalocyanine pigments, azo dyes and diimine salt dyes.
Preferably, the addition amount of the near infrared absorbent is 1-2.5% of the mass of the matrix polymer.
Preferably, the ultraviolet absorbent is one or more selected from benzotriazole, benzophenone and benzotriazole.
Preferably, the addition amount of the ultraviolet absorbent is 0.8-1.5% of the mass of the matrix polymer.
Preferably, the solvent is any one of isopropyl alcohol and acetone.
Preferably, the silane coupling agent is one of KH550, KH560 and KH 570.
A preparation method of a nano composite infrared-resistant lens monomer with a refractive index of 1.60 comprises the following steps: mixing the matrix polymer, the near-infrared absorbent and the ultraviolet absorbent according to the mass ratio, and extruding and granulating at 180-220 ℃ to obtain the nano composite infrared resistant lens monomer.
The invention has the following beneficial effects:
(1) according to the invention, nano titanium dioxide with higher refractive index is introduced into a PMMA system, the surface of titanium dioxide precursor n-butyl titanate is modified, and then PMMA is added, so that good dispersion of titanium dioxide nano particles in a polymer system can be fully promoted, the agglomeration of the nano particles is reduced, the high transparency of the lens is ensured, and the lens has higher refractive index;
(2) the preparation method disclosed by the invention is simple in preparation process and mild in condition, and can ensure that the infrared-proof absorbent can fully exert the characteristic of absorbing infrared wavelength of the infrared-proof absorbent and ensure that the resin has higher refractive index.
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.
Example 1
A nano composite anti-infrared lens monomer with a refractive index of 1.60 comprises a matrix polymer, a near-infrared absorbent and an ultraviolet absorbent;
a preparation method of a nano composite infrared-resistant lens monomer with a refractive index of 1.60 comprises the following steps:
(1) the matrix polymer is prepared according to the following steps: weighing a certain amount of silane coupling agent, adding the silane coupling agent into a reaction kettle, adding a proper amount of curing agent and isopropanol under the stirring condition, and adjusting the pH value to be 5.5-6.5, wherein n (silane coupling agent): n (curing agent) ═ 1: 2.5; then adding tetrabutyl titanate into the reaction kettle, and reacting for 10 hours at the temperature of 100-130 ℃ to obtain a pre-reactant; adding PMMA into the pre-reactant, stirring uniformly, removing isopropanol by spinning, and adding a proper amount of curing agent to obtain the matrix polymer; wherein the mass ratio of PMMA to n-butyl titanate to the curing agent is 10:2:7: 3;
(2) mixing the matrix polymer, the near-infrared absorbent and the ultraviolet absorbent according to the mass ratio of 100:2:1, and extruding and granulating at 180-220 ℃ to obtain a nano composite infrared resistant lens monomer;
the near-infrared absorbent is cyanine pigment, and the ultraviolet absorbent is benzotriazole.
When the resin lens is used for producing the resin lens, the refractive index of the resin lens is 1.60, the average transmittance of the resin lens in visible light (400-700nnm) is more than 98%, and the average transmittance of the resin lens in a near-infrared band of 800-1400 nm is less than 35%.
Example 2
A nano composite anti-infrared lens monomer with a refractive index of 1.60 comprises a matrix polymer, a near-infrared absorbent and an ultraviolet absorbent;
a preparation method of a nano composite infrared-resistant lens monomer with a refractive index of 1.60 comprises the following steps:
(1) the matrix polymer is prepared according to the following steps: weighing a certain amount of silane coupling agent, adding the silane coupling agent into a reaction kettle, adding a proper amount of curing agent and isopropanol under the stirring condition, and adjusting the pH value to be 5.5-6.5, wherein n (silane coupling agent): n (curing agent) ═ 1: 2; then adding tetrabutyl titanate into the reaction kettle, and reacting for 12 hours at the temperature of 100-130 ℃ to obtain a pre-reactant; adding PMMA into the pre-reactant, stirring uniformly, removing isopropanol by spinning, and adding a proper amount of curing agent to obtain the matrix polymer; wherein the mass ratio of PMMA to n-butyl titanate to the curing agent is 9:4:9: 2.5;
(2) mixing the matrix polymer, the near-infrared absorbent and the ultraviolet absorbent according to the mass ratio of 100:2.5:1.2, and extruding and granulating at 180-220 ℃ to obtain a nano composite infrared resistant lens monomer;
the near-infrared absorbent is a diimine salt dye, and the ultraviolet absorbent is benzotriazole.
When the resin lens is used for producing the resin lens, the refractive index of the resin lens is 1.65, the average transmittance of the resin lens in visible light (400-700nnm) is more than 98%, and the average transmittance of the resin lens in a near-infrared band of 800-1400 nm is less than 32%.
Example 3
A nano composite anti-infrared lens monomer with a refractive index of 1.60 comprises a matrix polymer, a near-infrared absorbent and an ultraviolet absorbent;
a preparation method of a nano composite infrared-resistant lens monomer with a refractive index of 1.60 comprises the following steps:
(1) the matrix polymer is prepared according to the following steps: weighing a certain amount of silane coupling agent, adding the silane coupling agent into a reaction kettle, adding a proper amount of curing agent and isopropanol under the stirring condition, and adjusting the pH value to be 5.5-6.5, wherein n (silane coupling agent): n (curing agent) ═ 1: 1.8; then adding tetrabutyl titanate into the reaction kettle, and reacting for 11 hours at the temperature of 100-130 ℃ to obtain a pre-reactant; adding PMMA into the pre-reactant, stirring uniformly, removing isopropanol by spinning, and adding a proper amount of curing agent to obtain the matrix polymer; wherein the mass ratio of PMMA to n-butyl titanate to the curing agent is 9:3:7: 2;
(2) mixing the matrix polymer, the near-infrared absorbent and the ultraviolet absorbent according to the mass ratio of 100:2.2:1.2, and extruding and granulating at 180-220 ℃ to obtain a nano composite infrared resistant lens monomer;
the near-infrared absorbent is phthalocyanine pigment, and the ultraviolet absorbent is benzotriazole.
When the resin lens is used for producing the resin lens, the refractive index of the resin lens is 1.62, the average transmittance in visible light (400-700nnm) is more than 98%, and the average transmittance in the near infrared band of 800-1400 nm is less than 34%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (8)

1. A nano composite anti-infrared lens monomer with a refractive index of 1.60 is characterized in that the lens monomer contains a matrix polymer, a near-infrared absorbent and an ultraviolet absorbent;
the matrix polymer is prepared according to the following steps: weighing a certain amount of silane coupling agent, adding the silane coupling agent into a reaction kettle, adding a proper amount of curing agent and solvent under the stirring condition, and adjusting the pH value to be 5.5-6.5, wherein n (silane coupling agent): n (curing agent) is 1: 1.5-2.8; then adding tetrabutyl titanate into the reaction kettle, and reacting for 8-12h at 100-130 ℃ to obtain a pre-reactant; adding PMMA into the pre-reactant, stirring uniformly, removing the solvent by spinning, and adding a proper amount of curing agent to obtain the matrix polymer; wherein the mass ratio of PMMA, n-butyl titanate and curing agent is 8-10: 2-4: 6-9: 2-4.
2. The nanocomposite infrared-resistant lens monomer with refractive index of 1.60 according to claim 1, wherein the near infrared absorbent is selected from any one of cyanine pigments, phthalocyanine pigments, azo dyes and diimine salt dyes.
3. The nanocomposite IR-resistant lens monomer according to claim 1, wherein the amount of the near-IR absorber added is 1-2.5% of the mass of the matrix polymer.
4. The nanocomposite infrared-resistant lens monomer with refractive index of 1.60 as claimed in claim 1, wherein the ultraviolet absorber is one or more selected from benzotriazole, benzophenone and benzotriazole.
5. The nanocomposite, ir-resistant lens monomer according to claim 1, wherein the refractive index is 1.60, and the monomer is: the addition amount of the ultraviolet absorbent is 0.8-1.5% of the mass of the matrix polymer.
6. The nanocomposite, ir-resistant lens monomer according to claim 1, wherein the refractive index is 1.60, and the monomer is: the solvent is any one of isopropanol and acetone.
7. The nanocomposite, ir-resistant lens monomer according to claim 1, wherein the refractive index is 1.60, and the monomer is: the silane coupling agent is one of KH550, KH560 and KH 570.
8. The method for preparing a nanocomposite anti-infrared lens monomer with refractive index of 1.60 according to claim 1, wherein the method comprises the following steps: the method comprises the following steps: mixing the matrix polymer, the near-infrared absorbent and the ultraviolet absorbent according to the mass ratio, and extruding and granulating at 180-220 ℃ to obtain the nano composite infrared resistant lens monomer.
CN202010391623.1A 2020-05-11 2020-05-11 Nano composite infrared-resistant lens monomer with refractive index of 1.60 Pending CN111440402A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106366533A (en) * 2016-08-30 2017-02-01 东兴华鸿光学科技有限公司 Optical lens with low thermal conductivity

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102031022A (en) * 2010-10-27 2011-04-27 华南理工大学 Method for modifying nano titanium dioxide sol by utilizing silane coupling agent
CN102604135A (en) * 2012-03-02 2012-07-25 上海交通大学 Preparation method of polymethyl methacrylate/titanium dioxide nano-grade composite material
CN103980643A (en) * 2014-06-04 2014-08-13 江苏华天通纳米科技有限公司 Blue light cut nano compound resin material, lens and preparation method thereof
CN104478231A (en) * 2014-11-20 2015-04-01 南阳理工学院 Method for preparing ultraviolet-resistant TiO2 film
CN110698861A (en) * 2019-11-15 2020-01-17 江南大学 Preparation method of organic-inorganic nano hybrid high-refractive-index optical material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102031022A (en) * 2010-10-27 2011-04-27 华南理工大学 Method for modifying nano titanium dioxide sol by utilizing silane coupling agent
CN102604135A (en) * 2012-03-02 2012-07-25 上海交通大学 Preparation method of polymethyl methacrylate/titanium dioxide nano-grade composite material
CN103980643A (en) * 2014-06-04 2014-08-13 江苏华天通纳米科技有限公司 Blue light cut nano compound resin material, lens and preparation method thereof
CN104478231A (en) * 2014-11-20 2015-04-01 南阳理工学院 Method for preparing ultraviolet-resistant TiO2 film
CN110698861A (en) * 2019-11-15 2020-01-17 江南大学 Preparation method of organic-inorganic nano hybrid high-refractive-index optical material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106366533A (en) * 2016-08-30 2017-02-01 东兴华鸿光学科技有限公司 Optical lens with low thermal conductivity

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