CN115139605A - Synthesis method and material using cyclic block copolymer and quantum dots - Google Patents

Synthesis method and material using cyclic block copolymer and quantum dots Download PDF

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CN115139605A
CN115139605A CN202210678348.0A CN202210678348A CN115139605A CN 115139605 A CN115139605 A CN 115139605A CN 202210678348 A CN202210678348 A CN 202210678348A CN 115139605 A CN115139605 A CN 115139605A
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block copolymer
copolymer
layer
quantum dots
annular block
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许铭富
许书元
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Wanxing Intelligent Nantong Technology Co ltd
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Wanxing Intelligent Nantong Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/306—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl acetate or vinyl alcohol (co)polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29B9/00—Making granules
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29B9/00—Making granules
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B32B27/00—Layered products comprising a layer of synthetic resin
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    • B32—LAYERED PRODUCTS
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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    • B32—LAYERED PRODUCTS
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    • B32B2255/00—Coating on the layer surface
    • B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/26—Polymeric coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/412—Transparent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/71—Resistive to light or to UV
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/72—Density
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/726—Permeability to liquids, absorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/726—Permeability to liquids, absorption
    • B32B2307/7265—Non-permeable
    • C—CHEMISTRY; METALLURGY
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/08—Copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica

Abstract

The invention discloses a synthetic method and a material using a cyclic block copolymer and quantum dots, and relates to the field of optical materials. When the material using the annular block copolymer and the quantum dots is prepared, firstly, the annular block copolymer, the cadmium selenide quantum dots and mercaptan are reacted to obtain a composite copolymer, the composite copolymer and the annular block copolymer are mixed, melted, pulled, cooled, cut and then cast and rolled to prepare a core layer, the ethylene-vinyl alcohol copolymer is cast and rolled to prepare a light transmitting layer, the ethylene-vinyl alcohol copolymer, titanium dioxide and silicon dioxide are mixed, cast and rolled to prepare a light control layer, the light transmitting layer and the light control layer are rolled and pressed on the two side surfaces of the core layer with equal area, and then surface protection treatment is carried out to prepare the material of the annular block copolymer and the quantum dots. The material of the prepared annular segmented copolymer and quantum dots has good waterproof performance and optical performance.

Description

Synthetic method and material using cyclic block copolymer and quantum dots
Technical Field
The invention relates to the technical field of optical materials, in particular to a synthetic method and a material using a cyclic block copolymer and quantum dots.
Background
The quantum dot material has the characteristics of wide excitation spectrum, narrow emission spectrum, high color purity and good light stability, and is applied to the fields of display and illumination.
At present, an optical plate using a quantum dot material uses polymethyl methacrylate or glass and polyethylene glycol terephthalate as main carrier materials, and the polymethyl methacrylate and the quantum dot material are synthesized to form a quantum dot-polymethyl methacrylate copolymer and make the copolymer into an optical material structure. However, the saturated water absorption of polymethyl methacrylate is 0.3%, when the polymethyl methacrylate absorbs moisture and expands in a high-temperature and high-humidity environment, the material is easily deformed, and the requirements of the gap and the flatness of the display structure combination are difficult to meet, and meanwhile, the water vapor transmission rate and the oxygen transmission rate of the polymethyl methacrylate are higher than the requirements of a photoelectric display product, so that the current optical material structure adopts a multilayer protection structure design, and therefore, how to effectively reduce the overlapping or the bonding of multilayer optical substrates, and the reduction of the light transmittance are problems which need to be solved urgently.
Disclosure of Invention
The invention aims to provide a synthetic method and a material using a cyclic block copolymer and quantum dots, so as to solve the problems in the prior art.
The material using the annular block copolymer and the quantum dots is characterized by mainly comprising a core layer, a light transmitting layer and a light control layer which are adjacent to two sides of the core layer, and an outer protective layer on the outermost side.
Optimally, the core layer is prepared by reacting a cyclic block copolymer, cadmium selenide quantum dots and mercaptan to obtain a composite copolymer, and mixing, melting and pulling the composite copolymer and the cyclic block copolymer.
Preferably, the component of the light-transmitting layer is ethylene-vinyl alcohol copolymer; the light control layer is prepared by mixing, tape casting and rolling ethylene-vinyl alcohol copolymer, titanium dioxide and silicon dioxide.
Preferably, the outer protective layer is prepared by spraying polyvinylidene fluoride resin on the surfaces of both sides of the semi-finished product.
As optimization, a synthesis mode using a cyclic block copolymer and quantum dots mainly comprises the following preparation steps:
(1) The cyclic block copolymer and toluene are mixed in a mass ratio of 1:4 to 1:6, uniformly mixing, adding cadmium selenide quantum dots with the mass of the annular block copolymer being 0.8-1 time of that of the annular block copolymer and mercaptan with the mass of the annular block copolymer being 0.3-0.5 time of that of the annular block copolymer, stirring and reacting for 1-2 h at the temperature of 90-100 ℃ and at the speed of 800-1000 r/min, and standing for 6-8 h at the temperature of 20-30 ℃ and 1-2 kPa to prepare a composite copolymer;
(2) Grinding the composite copolymer to a particle size of 1-5 μm, and mixing the ground composite copolymer and the annular block copolymer according to a mass ratio of 1: 8-1: 20, uniformly mixing, melting, pulling, cooling and cutting through a granulator to obtain modified resin;
(3) Preparing a film with the thickness of 0.03-0.06 mm from the modified resin as a core layer by a tape casting rolling mode, preparing a film with the thickness of 0.025-0.25 mm from the ethylene-vinyl alcohol copolymer as a light transmission layer, and preparing the ethylene-vinyl alcohol copolymer, titanium dioxide and silicon dioxide into a film with the thickness of 4:0.1:1 to 5:0.3:1, uniformly mixing to prepare a film with the thickness of 0.05-1.7 mm as an optical control layer for thickness adjustment, rolling and pressing a light transmitting layer and the optical control layer on the surfaces of the two sides of a core layer with the same area to prepare a semi-finished product, and finally performing surface protection treatment on the two sides of the semi-finished product to prepare the material using the annular block copolymer and the quantum dots.
As optimization, the melting temperature in the step (2) is 200-220 ℃, and the cooling temperature is 20-30 ℃.
Preferably, the purities of the titanium dioxide and the silicon dioxide in the step (3) are both 99.9%, and the particle diameters are both 1-5 μm.
As optimization, the technological parameters of the rolling and pressing in the step (3) are as follows: the temperature is 160-190 ℃, and the pressure is 1.3-1.5 MPa.
As optimization, the surface protection treatment method in the step (3) comprises the following steps: spraying a layer of polyvinylidene fluoride resin with the viscosity of about 100-120 cps, and naturally drying to form an external protective layer with the thickness of 3-6 microns.
Compared with the prior art, the invention has the following beneficial effects:
when the material using the annular block copolymer and the quantum dots is prepared, firstly, the annular block copolymer, the cadmium selenide quantum dots and mercaptan react to obtain a composite copolymer, the composite copolymer and the annular block copolymer are mixed, melted and pulled to prepare a core layer, the ethylene-vinyl alcohol copolymer is cast and rolled to prepare a light transmitting layer, the ethylene-vinyl alcohol copolymer, titanium dioxide and silicon dioxide are mixed, cast and rolled to prepare a light control layer, the light transmitting layer and the light control layer are rolled and pressed on the two side surfaces of the core layer with equal area, and then surface protection treatment is carried out to prepare the material of the annular block copolymer and the quantum dots.
First, the cyclic block copolymer has high light transmittance, ultraviolet light resistance, high ultraviolet light transmittance, low water absorption, and high fluidity. The density is lower than that of the existing optical material, so that the material is very suitable to be used as a carrier material of a quantum dot optical material, and meanwhile, the integration of an optical film of a backlight module can be accelerated, and the reduction of light transmittance caused by the superposition or lamination of multilayer optical substrates is reduced.
Secondly, mercaptan is added in the preparation process of the composite copolymer, and the mercaptan reacts with the surface of the cadmium selenide quantum dot to be connected, so that the cadmium selenide quantum is easily coated and loaded by the annular block copolymer, the dispersity of the cadmium selenide quantum is improved, and the optical performance of the material of the annular block copolymer and the quantum dot is improved; the light control layer can effectively regulate and control the light transmittance and haze of the optical material, and the light transmittance and haze are reduced along with the increase of the thickness of the light control layer, so that the material of the annular block copolymer and the quantum dot with required performance can be obtained easily; an external protective layer formed by spraying polyvinylidene fluoride resin on the surface can effectively protect the material, thereby improving the waterproof performance of the material of the annular block copolymer and the quantum dots.
Drawings
FIG. 1 shows a process for preparing a complex copolymer;
FIG. 2 shows the overall structure of a material using cyclic block copolymers with quantum dots;
FIG. 3 shows a process for preparing a semi-finished product;
FIG. 4 shows a fitted curve of light transmittance versus thickness;
fig. 5 shows the optical color gamut values of the core layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 5 and the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method of the present invention, the following examples are given, and the methods for measuring the indices of the materials of the cyclic block copolymer and the quantum dot prepared in the following examples are as follows:
waterproof performance: the material using the cyclic block copolymer and the quantum dot obtained in each example and the comparative example material were placed in a wet environment with the same size, shape and area and the same humidity for the same time, and then the surface was dried and weighed, and the water absorption = weight gain/original weight was calculated.
Optical properties: the materials using the cyclic block copolymer and the quantum dot obtained in each example were shaped into the same size and area as those of the comparative example material, and the light transmittance was measured.
Example 1
A synthetic method using a cyclic block copolymer and quantum dots mainly comprises the following preparation steps:
(1) The cyclic block copolymer and toluene are mixed in a mass ratio of 1:4, uniformly mixing, adding cadmium selenide quantum dots with the mass of 0.8 time of that of the annular block copolymer and mercaptan with the mass of 0.3 time of that of the annular block copolymer, stirring and reacting for 1 hour at 90 ℃,800r/min, and standing for 8 hours at 20 ℃ under 1kPa to prepare a composite copolymer;
(2) Grinding the composite copolymer to a particle size of 1 μm, and mixing the ground composite copolymer and the annular block copolymer according to a mass ratio of 1:8, uniformly mixing, mixing by a granulator, heating to 200 ℃, melting, pulling, cooling to 10 ℃, and cutting to obtain modified resin;
(3) Preparing a film with the thickness of 0.03mm from the modified resin as a core layer, preparing a film with the thickness of 0.025mm from the ethylene-vinyl alcohol copolymer as a light transmission layer, and preparing the ethylene-vinyl alcohol copolymer, titanium dioxide with the particle size of 1 mu m and silicon dioxide with the particle size of 1 mu m according to a mass ratio of 4:0.1:1, uniformly mixing the two materials to prepare a film with the thickness of 0.05mm as a light control layer for thickness adjustment, rolling and pressing a light transmitting layer and the light control layer on the two side surfaces of a core layer with the same area at 160 ℃ and 1.3MPa to prepare a semi-finished product, finally spraying a layer of polyvinylidene fluoride resin with the viscosity of about 100cps on the two side surfaces of the semi-finished product, naturally drying to form an external protective layer with the thickness of 3 mu m, and preparing the material using the annular block copolymer and the quantum dots.
Example 2
A synthetic method using a cyclic block copolymer and quantum dots mainly comprises the following preparation steps:
(1) The cyclic block copolymer and toluene are mixed in a mass ratio of 1:5, uniformly mixing, adding cadmium selenide quantum dots with the mass of 0.9 time that of the annular block copolymer and mercaptan with the mass of 0.4 time that of the annular block copolymer, stirring and reacting for 1.5h at 95 ℃ and 900r/min, and standing for 7h at 25 ℃ and 1.5kPa to prepare a composite copolymer;
(2) Grinding the composite copolymer to a particle size of 3 μm, and mixing the ground composite copolymer and the annular block copolymer according to a mass ratio of 1:8, uniformly mixing, mixing by a granulator, heating to 210 ℃, melting, pulling, cooling to 20 ℃, and cutting to obtain modified resin;
(3) Preparing a film with the thickness of 0.045mm from the modified resin as a core layer, preparing a film with the thickness of 0.1mm from the ethylene-vinyl alcohol copolymer as a light transmission layer, and preparing the modified resin into the film with the thickness of 0.045mm and the film with the thickness of 0.1mm from the ethylene-vinyl alcohol copolymer as the light transmission layer by a casting rolling mode, wherein the modified resin is prepared from the ethylene-vinyl alcohol copolymer, titanium dioxide with the particle size of 3 mu m and silicon dioxide with the particle size of 3 mu m according to the mass ratio of 4.5:0.2:1, uniformly mixing the two materials to prepare a film with the thickness of 1mm, using the film as a light control layer to adjust the thickness, rolling and pressing a light transmitting layer and the light control layer on the surfaces of the two sides of a core layer with the same area at 170 ℃ and 1.4MPa to prepare a semi-finished product, finally spraying a layer of polyvinylidene fluoride resin with the viscosity of about 110cps on the surfaces of the two sides of the semi-finished product, naturally drying to form an external protective layer with the thickness of 4 mu m, and preparing the material using the annular block copolymer and the quantum dots.
Example 3
A synthetic method using a cyclic block copolymer and quantum dots mainly comprises the following preparation steps:
(1) The cyclic block copolymer and toluene are mixed in a mass ratio of 1:6, uniformly mixing, adding cadmium selenide quantum dots with the mass of 1 time of that of the annular block copolymer and mercaptan with the mass of 0.5 time of that of the annular block copolymer, stirring and reacting for 1 hour at 100 ℃ and 1000r/min, and standing for 6 hours at 30 ℃ and 2kPa to prepare a composite copolymer;
(2) Grinding the composite copolymer to a particle size of 5 μm, and mixing the ground composite copolymer and the annular block copolymer according to a mass ratio of 1:20, uniformly mixing, mixing by a granulator, heating to 220 ℃, melting, pulling, cooling to 30 ℃, and cutting to obtain modified resin;
(3) Preparing a film with the thickness of 0.6mm from the modified resin as a core layer, preparing a film with the thickness of 0.25mm from the ethylene-vinyl alcohol copolymer as a light transmission layer, and preparing the ethylene-vinyl alcohol copolymer, titanium dioxide with the particle size of 5 mu m and silicon dioxide with the particle size of 5 mu m into a film by a casting rolling mode according to the mass ratio of 5:0.3:1, uniformly mixing the two materials to prepare a film with the thickness of 1.7mm, using the film as a light control layer to adjust the thickness, rolling and pressing a light transmitting layer and the light control layer on the two side surfaces of a core layer with the same area at 190 ℃ and 1.5MPa to prepare a semi-finished product, finally spraying a layer of polyvinylidene fluoride resin with the viscosity of about 120cps on the two side surfaces of the semi-finished product, naturally drying to form an external protective layer with the thickness of 6 mu m, and preparing the material using the annular block copolymer and the quantum dots.
Comparative example 1
A synthetic method using a cyclic block copolymer and quantum dots mainly comprises the following preparation steps:
(1) The cyclic block copolymer and toluene are mixed in a mass ratio of 1:5, uniformly mixing, adding cadmium selenide quantum dots with the mass of 0.9 time that of the annular block copolymer, stirring and reacting for 1.5 hours at 95 ℃ and 900r/min, and standing for 7 hours at 25 ℃ and 1.5kPa to prepare a composite copolymer;
(2) Grinding the composite copolymer to a particle size of 3 μm, and mixing the ground composite copolymer and the annular block copolymer according to a mass ratio of 1:8, uniformly mixing, mixing by a granulator, heating to 210 ℃, melting, pulling, cooling to 20 ℃, and cutting to obtain modified resin;
(3) Preparing a film with the thickness of 0.045mm from the modified resin as a core layer, preparing a film with the thickness of 0.025mm from the ethylene-vinyl alcohol copolymer as a light transmission layer, and preparing the ethylene-vinyl alcohol copolymer, titanium dioxide with the particle size of 3 mu m and silicon dioxide with the particle size of 3 mu m according to a mass ratio of 4.5:0.2:1, uniformly mixing the two materials to prepare a film with the thickness of 0.05mm, using the film as a light control layer to adjust the thickness, rolling and pressing a light transmitting layer and the light control layer on the two side surfaces of a core layer with the same area at 170 ℃ and 1.4MPa to prepare a semi-finished product, finally spraying a layer of polyvinylidene fluoride resin with the viscosity of about 110cps on the two side surfaces of the semi-finished product, naturally drying to form an external protective layer with the thickness of 4 mu m, and preparing the material using the annular block copolymer and the quantum dots.
Comparative example 2
A synthetic method using a cyclic block copolymer and quantum dots mainly comprises the following preparation steps:
(1) The cyclic block copolymer and toluene are mixed in a mass ratio of 1:5, uniformly mixing, adding cadmium selenide quantum dots with the mass of 0.9 time that of the annular block copolymer and mercaptan with the mass of 0.4 time that of the annular block copolymer, stirring and reacting for 1.5h at 95 ℃ and 900r/min, and standing for 7h at 25 ℃ and 1.5kPa to prepare a composite copolymer;
(2) Grinding the composite copolymer to a particle size of 3 μm, and mixing the ground composite copolymer and the annular block copolymer according to a mass ratio of 1:8, uniformly mixing, mixing by a granulator, heating to 210 ℃, melting, pulling, cooling to 20 ℃, and cutting to obtain modified resin;
(3) Preparing a film with the thickness of 45 mu m from the modified resin as a core layer by a tape casting rolling mode, preparing a film with the thickness of 0.1mm from the ethylene-vinyl alcohol copolymer as a light transmitting layer, performing rolling and pressing on two light transmitting layers on the two side surfaces of the core layer with the same area at 170 ℃ and 1.4MPa to prepare a semi-finished product, finally spraying a layer of polyvinylidene fluoride resin with the viscosity of about 110cps on the two side surfaces of the semi-finished product, forming an external protective layer with the thickness of 4 mu m after natural drying, and preparing the material using the annular block copolymer and the quantum dots.
Comparative example 3
A synthetic method using a cyclic block copolymer and quantum dots mainly comprises the following preparation steps:
(1) The cyclic block copolymer and toluene are mixed in a mass ratio of 1:5, uniformly mixing, adding cadmium selenide quantum dots with the mass of 0.9 time that of the annular block copolymer and mercaptan with the mass of 0.4 time that of the annular block copolymer, stirring and reacting for 1.5h at 95 ℃ and 900r/min, and standing for 7h at 25 ℃ and 1.5kPa to prepare a composite copolymer;
(2) Grinding the composite copolymer to a particle size of 3 μm, and mixing the ground composite copolymer and the annular block copolymer in a mass ratio of 1:20, uniformly mixing, mixing by a granulator, heating to 210 ℃, melting, pulling, cooling to 20 ℃, and cutting to obtain modified resin;
(3) Preparing a film with the thickness of 45 mu m from the modified resin as a core layer, preparing a film with the thickness of 0.25mm from the ethylene-vinyl alcohol copolymer as a light transmission layer, and preparing the ethylene-vinyl alcohol copolymer, titanium dioxide with the particle size of 3 mu m and silicon dioxide with the particle size of 3 mu m into a film by a casting rolling mode according to the mass ratio of 4.5:0.2:1, uniformly mixing to prepare a film with the thickness of 1.5mm as an optical control layer, and rolling and pressing the light transmitting layer and the optical control layer on the two side surfaces of the core layer with the same area at 170 ℃ and 1.4MPa to prepare the material using the annular block copolymer and the quantum dots.
Examples of effects
Table 1 below gives the analysis results of the water-repellent property and the optical property of the materials using the cyclic block copolymer and the quantum dot according to examples 1 to 3 and comparative examples 1 to 3 of the present invention.
TABLE 1
Water Vapor Transmission Rate (WVTR) Light transmittance Water Vapor Transmission Rate (WVTR) Light transmittance
Example 1 0.32g/m 2 ·24hour 58％ Comparative example 1 0.33g/m 2 ·24hour 42％
Example 2 0.25g/m 2 ·24hour 49％ Comparative example 2 0.19g/m 2 ·24hour 84％
Example 3 0.25g/m 2 ·24hour 41％ Comparative example 3 0.45g/m 2 ·24hour 48％
From the comparison of experimental data of examples 1 to 3 and comparative examples 1 to 3 in table 1, it can be found that the materials of the cyclic block copolymer and the quantum dot prepared by the present invention have good water resistance and optical properties.
Compared with experimental data of the example 2 and the comparative example 1 in the table 1, the light transmittance of the example 2 is higher than that of the comparative example 1, which shows that the mercaptan is added in the preparation process of the composite copolymer, and the mercaptan reacts with the surface of the cadmium selenide quantum dot to connect, so that the cadmium selenide quantum is easily coated and loaded by the annular block copolymer, the dispersibility of the cadmium selenide quantum is improved, and the optical performance of the material of the annular block copolymer and the quantum dot is improved; compared with the experimental data of examples 1, 2 and 3 and comparative example 2, the experimental data of examples 1, 2 and 3 and comparative example 2 show that the light transmittance of examples 1, 2 and 3 is small and monotonous, which shows that the light control layer can effectively regulate and control the light transmittance and haze of the optical material, and the light transmittance and haze are reduced along with the increase of the thickness of the light control layer, so that the materials of the cyclic block copolymer and the quantum dot with required performance can be easily prepared; from the comparison of experimental data of examples 1, 2 and 3 with comparative example 3, it can be seen that the water vapor transmission rate of examples 1, 2 and 3 with comparative example 3 is increased, which indicates that the external protective layer formed by spraying polyvinylidene fluoride resin on the surface can effectively protect the material, thereby improving the waterproof performance of the material of the cyclic block copolymer and the quantum dot.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (9)

1. The material using the annular block copolymer and the quantum dots is characterized by mainly comprising a core layer, a light transmitting layer and a light control layer which are adjacent to two sides of the core layer, and an outer protective layer on the outermost side.
2. The material using the cyclic block copolymer and the quantum dot as claimed in claim 1, wherein the core layer is prepared by reacting the cyclic block copolymer, the cadmium selenide quantum dot and the thiol to obtain a composite copolymer, and mixing, melting, drawing, cooling and rolling the composite copolymer and the cyclic block copolymer.
3. The material using the cyclic block copolymer and the quantum dot as claimed in claim 1, wherein the light-transmitting layer is composed of an ethylene-vinyl alcohol copolymer; the light control layer is prepared by mixing, casting and rolling ethylene-vinyl alcohol copolymer, titanium dioxide and silicon dioxide.
4. The material using the cyclic block copolymer and the quantum dot as claimed in claim 1, wherein the outer protective layer is formed by spraying polyvinylidene fluoride resin on both surfaces of the semi-finished product.
5. A synthetic method using a cyclic block copolymer and quantum dots is characterized by mainly comprising the following preparation steps:
(1) The cyclic block copolymer and toluene are mixed in a mass ratio of 1:4 to 1:6, uniformly mixing, adding cadmium selenide quantum dots with the mass of the annular block copolymer being 0.8-1 time of that of the annular block copolymer and mercaptan with the mass of the annular block copolymer being 0.3-0.5 time of that of the annular block copolymer, stirring and reacting for 1-2 h at the temperature of 90-100 ℃ and at the speed of 800-1000 r/min, and standing for 6-8 h at the temperature of 20-30 ℃ and 1-2 kPa to prepare a composite copolymer;
(2) Grinding the composite copolymer to a particle size of 1-5 μm, and mixing the ground composite copolymer and the annular block copolymer according to a mass ratio of 1: 8-1: 20, uniformly mixing, melting, pulling, cooling and cutting through a granulator to obtain modified resin;
(3) Preparing a film with the thickness of 0.03-0.06 mm from the modified resin as a core layer by a tape casting rolling mode, preparing a film with the thickness of 0.025-0.25 mm from the ethylene-vinyl alcohol copolymer as a light transmission layer, and mixing the ethylene-vinyl alcohol copolymer, titanium dioxide and silicon dioxide according to a mass ratio of 4:0.1:1 to 5:0.3:1, uniformly mixing to prepare a film with the thickness of 0.05-1.7 mm as an optical control layer for thickness adjustment, rolling and pressing a light transmitting layer and the optical control layer on the surfaces of the two sides of a core layer with the same area to prepare a semi-finished product, and finally performing surface protection treatment on the two sides of the semi-finished product to prepare the material using the annular block copolymer and the quantum dots.
6. The method as claimed in claim 5, wherein the melting temperature in step (2) is 200-220 ℃ and the cooling temperature is 20-30 ℃.
7. The method of claim 5, wherein the purity of the titanium dioxide and the purity of the silicon dioxide in the step (3) are both 99.9%, and the particle diameter is 1-5 μm.
8. The method as claimed in claim 5, wherein the rolling and pressing process parameters in step (3) are as follows: the temperature is 160-190 ℃, and the pressure is 1.3-1.5 MPa.
9. The method of claim 5, wherein the surface protection treatment in step (3) is performed by: spraying a layer of polyvinylidene fluoride resin with the viscosity of about 100-120 cps, and naturally drying to form an external protective layer with the thickness of 3-6 microns.
CN202210678348.0A 2022-06-16 2022-06-16 Synthesis method and material using cyclic block copolymer and quantum dots Pending CN115139605A (en)

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