CN112080055B - Luminescent material color master batch particle and preparation method and application thereof - Google Patents
Luminescent material color master batch particle and preparation method and application thereof Download PDFInfo
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- CN112080055B CN112080055B CN202010861526.4A CN202010861526A CN112080055B CN 112080055 B CN112080055 B CN 112080055B CN 202010861526 A CN202010861526 A CN 202010861526A CN 112080055 B CN112080055 B CN 112080055B
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- 239000000463 material Substances 0.000 title claims abstract description 125
- 239000002245 particle Substances 0.000 title claims abstract description 93
- 239000004595 color masterbatch Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 229920001169 thermoplastic Polymers 0.000 claims abstract description 59
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 46
- -1 polypropylene Polymers 0.000 claims abstract description 36
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 33
- 125000002723 alicyclic group Chemical group 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 27
- 239000004743 Polypropylene Substances 0.000 claims abstract description 25
- 229920001155 polypropylene Polymers 0.000 claims abstract description 25
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 24
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000002861 polymer material Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 239000004416 thermosoftening plastic Substances 0.000 claims description 44
- 239000002096 quantum dot Substances 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 28
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 22
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 claims description 19
- 239000004952 Polyamide Substances 0.000 claims description 19
- 239000004698 Polyethylene Substances 0.000 claims description 19
- 229920002647 polyamide Polymers 0.000 claims description 19
- 229920000573 polyethylene Polymers 0.000 claims description 19
- 239000013081 microcrystal Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- 238000001125 extrusion Methods 0.000 claims description 8
- 239000008346 aqueous phase Substances 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 4
- 125000003700 epoxy group Chemical group 0.000 claims description 3
- 125000004185 ester group Chemical group 0.000 claims description 3
- 230000005284 excitation Effects 0.000 claims description 3
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 claims description 3
- 230000032683 aging Effects 0.000 abstract description 23
- 230000003287 optical effect Effects 0.000 abstract description 9
- 230000001681 protective effect Effects 0.000 abstract description 6
- 238000013461 design Methods 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 239000008204 material by function Substances 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 description 39
- 239000004033 plastic Substances 0.000 description 39
- 239000004715 ethylene vinyl alcohol Substances 0.000 description 14
- 238000001228 spectrum Methods 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000012071 phase Substances 0.000 description 9
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical group [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 8
- 230000001795 light effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 239000004721 Polyphenylene oxide Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 229930040373 Paraformaldehyde Natural products 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000001506 calcium phosphate Substances 0.000 description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N coumarin Chemical compound C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229920002098 polyfluorene Polymers 0.000 description 2
- 229920006324 polyoxymethylene Polymers 0.000 description 2
- 229920006380 polyphenylene oxide Polymers 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- CFNMUZCFSDMZPQ-GHXNOFRVSA-N 7-[(z)-3-methyl-4-(4-methyl-5-oxo-2h-furan-2-yl)but-2-enoxy]chromen-2-one Chemical compound C=1C=C2C=CC(=O)OC2=CC=1OC/C=C(/C)CC1OC(=O)C(C)=C1 CFNMUZCFSDMZPQ-GHXNOFRVSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229960000956 coumarin Drugs 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001940 europium oxide Inorganic materials 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910003451 terbium oxide Inorganic materials 0.000 description 1
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—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
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—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
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5425—Silicon-containing compounds containing oxygen containing at least one C=C bond
Abstract
The invention provides a luminescent material color master batch particle, a preparation method and application thereof, and belongs to the technical field of functional materials. The invention provides a luminescent material color master batch particle, which comprises the following preparation raw materials in parts by mass: 15-25 parts of luminescent material; 45-55 parts of thermoplastic polymer material; 10-20 parts of ethylene-vinyl acetate copolymer; 1-2 parts of dibutyl phthalate; 3-5 parts of polypropylene wax powder; 5-10 parts of silane coupling agent; 8-15 parts of polyfunctional alicyclic resin. The invention takes the thermoplastic polymer material as the protective material, has better protective effect on the luminescent material under the action of the ethylene-vinyl acetate copolymer, the dibutyl phthalate, the silane coupling agent, the polyfunctional alicyclic resin and the polypropylene wax powder, ensures that the luminescent material has excellent optical stability and ageing resistance, is very convenient to use, greatly improves the degree of freedom of product design, and can be widely applied to lighting devices, display devices or decorative devices.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a luminescent material color master batch particle and a preparation method and application thereof.
Background
Solid light emission is a very rapidly developing field in recent years, and various light emitting devices made of semiconductor Light Emitting Diodes (LEDs) and photoluminescent materials have been widely used in the fields of illumination, display, and the like.
In order to meet the lighting requirements of different purposes, the service life is prolonged, the degree of freedom of product design is expanded, and the further improvement of the stability of the luminescent material is a current research hot spot. For quantum dot luminescent materials, in the prior art, solid powder form quantum dot microcrystals are generally adopted to replace a quantum dot solution when the luminescent materials are prepared, but the luminescent materials based on the quantum dot microcrystals have poor ageing resistance and optical stability and narrow application range of products, so that market demands cannot be met.
Disclosure of Invention
The invention aims to provide a luminescent material color master batch particle, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a luminescent material color master batch particle, which comprises the following preparation raw materials in parts by mass:
15-25 parts of a luminescent material;
45-55 parts of thermoplastic polymer material;
10-20 parts of ethylene-vinyl acetate copolymer;
1-2 parts of dibutyl phthalate;
3-5 parts of polypropylene wax powder;
5-10 parts of a silane coupling agent;
8-15 parts of a polyfunctional alicyclic resin.
Preferably, the wavelength band of the luminescent material comprises 480-4815 nm, 490-495 nm, 500-515 nm, 520-525 nm, 530-535 nm, 540-560 nm, 565-580 nm, 585-595 nm, 600-620 nm, 625-635 nm, 640-65 nm, 660-665 nm or 670-6755 nm.
Preferably, the luminescent material comprises quantum dot microcrystals, rare earth oxide luminescent material, organic micromolecular luminescent material, organic macromolecule luminescent material, calcium phosphate luminescent material, calcium halophosphate luminescent material, nitride luminescent material or perovskite luminescent material.
Preferably, the thermoplastic polymer material includes at least one of ethylene-vinyl alcohol copolymer, polyamide, polyethylene, polypropylene, polyvinyl chloride, polyoxymethylene, polycarbonate, polyphenylene oxide, and chlorinated polyether.
Preferably, the multifunctional alicyclic resin contains both alicyclic epoxy groups and glycidyl ester groups in its molecular structure.
Preferably, the granularity of the luminescent material color master batch particles is 2-5 mm.
The invention provides a preparation method of luminescent material color master batch particles, which comprises the following steps:
first mixing a thermoplastic high polymer material, a silane coupling agent, dibutyl phthalate and a multifunctional alicyclic resin to obtain a first mixture;
performing second mixing on the first mixture and the luminescent material to obtain a second mixture;
and thirdly mixing the second mixture, the ethylene-vinyl acetate copolymer and the polypropylene wax powder, and granulating to obtain the luminescent material color master batch particles.
Preferably, the granulation comprises extrusion and cutting performed sequentially; the extrusion temperature is 145-175 ℃.
The invention provides the application of the luminescent material color master batch particles in lighting devices, display devices or decorative devices, wherein the luminescent material color master batch particles are prepared by the technical scheme or the preparation method.
Preferably, the excitation light source of the luminescent material color master batch is a blue light LED chip or an ultraviolet LED chip.
The invention provides a luminescent material color master batch particle, which comprises the following preparation raw materials in parts by mass: 15-25 parts of a luminescent material; 45-55 parts of thermoplastic polymer material; 10-20 parts of ethylene-vinyl acetate copolymer; 1-2 parts of dibutyl phthalate; 3-5 parts of polypropylene wax powder; 5-10 parts of a silane coupling agent; 8-15 parts of a polyfunctional alicyclic resin. The invention takes thermoplastic polymer material as protective material, which is resistant to almost all chemical solvents and has good chemical stability, under the action of ethylene-vinyl acetate copolymer, dibutyl phthalate, silane coupling agent, polyfunctional alicyclic resin and polypropylene wax powder, the invention has better protective effect on luminescent material, so that the luminescent material has excellent optical stability, good oxidation resistance and attenuation resistance, is not easy to age, is environment-friendly, has good processing performance, low production cost and long service life, is very convenient to use, greatly improves the degree of freedom of product design, and can be widely applied to lighting devices, display devices or decorative devices.
Drawings
FIG. 1 is a spectrum of a color master batch having a wavelength of 520nm prepared in example 1;
FIG. 2 is a graph showing the results of an aging resistance test of the color master batch having a wavelength of 520nm prepared in example 1;
FIG. 3 is a spectrum of the color master batch having a wavelength of 540nm prepared in example 2;
FIG. 4 is a graph showing the results of an aging resistance test of the color master batch having a wavelength of 540nm prepared in example 2;
FIG. 5 is a spectrum of 570nm color master batch prepared in example 3;
FIG. 6 is a graph showing the results of an aging resistance test of the 570nm color master batch prepared in example 3;
FIG. 7 is a spectrum of 605nm color master batch prepared in example 4;
FIG. 8 is a graph showing the results of an aging resistance test of the color master batch having a wavelength of 605nm prepared in example 4;
FIG. 9 is a spectrum of 635nm wavelength masterbatch prepared in example 5;
FIG. 10 is a graph showing the results of an aging resistance test of 635nm wavelength color master batch prepared in example 5;
FIG. 11 is a spectrum of 660 nm-wavelength color master batch prepared in example 6;
FIG. 12 is a graph showing the results of the aging resistance test of the color master batch having a wavelength of 660nm prepared in example 6.
Description of the embodiments
The invention provides a luminescent material color master batch particle, which comprises the following preparation raw materials in parts by mass:
15-25 parts of a luminescent material;
45-55 parts of thermoplastic polymer material;
10-20 parts of ethylene-vinyl acetate copolymer;
1-2 parts of dibutyl phthalate;
3-5 parts of polypropylene wax powder;
5-10 parts of a silane coupling agent;
8-15 parts of a polyfunctional alicyclic resin.
The preparation raw materials of the luminescent material color master batch comprise 15-25 parts by weight of luminescent material, preferably 15-20 parts by weight. In the invention, the wavelength band of the luminescent material preferably comprises 480-4815 nm, 490-495 nm, 500-515 nm, 520-525 nm, 530-535 nm, 540-560 nm, 565-580 nm, 585-595 nm, 600-620 nm, 625-425 nm, 640-65 nm, 660-6615 nm or 670-675 nm. In the present invention, the luminescent material preferably includes a quantum dot crystallite, a rare earth oxide luminescent material, an organic small molecule luminescent material, an organic high molecule luminescent material, a calcium phosphate luminescent material, a calcium halophosphate luminescent material, a nitride luminescent material or a perovskite luminescent material, wherein the quantum dot crystallite preferably includes a CT-G series aqueous phase quantum dot crystallite and/or a TG-R series aqueous phase quantum dot crystallite, more preferably a CT-G series aqueous phase quantum dot crystallite or a TG-R series aqueous phase quantum dot crystallite, and in the embodiment of the present invention, a quantum dot crystallite product manufactured by Xiamen far-tech limited is specifically adopted. The invention preferably adopts CT-G series water phase quantum dot microcrystals and/or TG-R series water phase quantum dot microcrystals, which is beneficial to ensuring that the finally obtained luminescent material color master batch particles have better optical stability and ageing resistance. In the present invention, the rare earth oxide luminescent material preferably includes yttrium oxide, europium oxide or terbium oxide, the organic small molecule luminescent material preferably includes coumarin or a coumarin derivative, the organic high molecule luminescent material preferably includes polyparaphenylene vinylene, polyparaphenylene vinylene derivative, polythiophene derivative, polyoxazole, polyoxadiazole derivative, polyfluorene or polyfluorene derivative, and the perovskite luminescent material preferably includes lead cesium halide, lead methylammonium halide or lead-free perovskite. In the present invention, the particle size of the luminescent material is preferably 0.5 to 18 μm.
Based on the mass parts of the luminescent material, the preparation raw materials of the luminescent material masterbatch comprise 45-55 parts of thermoplastic polymer material, preferably 50-55 parts. In the present invention, the thermoplastic polymer material preferably includes at least one of ethylene-vinyl alcohol copolymer (EVOH), polyamide (PA), polyethylene (PE), polypropylene, polyvinyl chloride, polyoxymethylene, polycarbonate, polyphenylene oxide, and chlorinated polyether, more preferably a mixture of ethylene-vinyl alcohol copolymer, polyamide, and polyethylene, and the mass ratio of the ethylene-vinyl alcohol copolymer, polyamide, and polyethylene in the mixture is preferably (10 to 20): 15: (20-30), specifically, 20:15:20 or 10:15:30. in the present invention, the particle size of the thermoplastic polymer material is preferably 1 to 5mm. The invention takes thermoplastic polymer material as protective material, which is resistant to almost all chemical solvents and has good chemical stability, under the action of ethylene-vinyl acetate copolymer, dibutyl phthalate, silane coupling agent, polyfunctional alicyclic resin and polypropylene wax powder, the invention has better protective effect on luminescent material, so that the luminescent material has high optical stability, good oxidation resistance and attenuation resistance, is not easy to age, is environment-friendly, has good processing performance, low production cost, long service life, convenient use and greatly improves the degree of freedom of product design, and can be widely applied to lighting devices, display devices or decorative devices.
Based on the mass parts of the luminescent material, the preparation raw materials of the luminescent material color master batch particles comprise 10-20 parts of ethylene-vinyl acetate copolymer, preferably 10-15 parts. The invention uses the ethylene-vinyl acetate copolymer to match with the thermoplastic polymer material, and the ethylene-vinyl acetate copolymer has good chemical stability, aging resistance, no water absorption, higher light transmittance, good film forming property, better barrier property, and favorable package protection for the luminescent material, so that the luminescent material has excellent optical stability and ageing resistance.
Based on the mass parts of the luminescent material, the preparation raw materials of the luminescent material color master batch particles comprise 1-2 parts of dibutyl phthalate, and preferably 1-1.5 parts. The dibutyl phthalate disclosed by the invention can play a plasticizing role in the granulating process, so that the obtained luminescent material masterbatch has excellent processing performance, and a product obtained by processing the luminescent material masterbatch has better flex resistance.
Based on the mass parts of the luminescent material, the preparation raw materials of the luminescent material color master batch comprise 3-5 parts of polypropylene wax powder, preferably 3.5-4.5 parts, and more preferably 4 parts. The invention utilizes the strong dispersibility and hydrophobicity of the polypropylene wax powder, is favorable for fully dispersing all preparation raw materials in the granulating process, and ensures that the finally obtained luminescent material masterbatch has strong hydrophobicity.
Based on the mass parts of the luminescent material, the preparation raw materials of the luminescent material color master batch particles comprise 5-10 parts of silane coupling agent, preferably 8-10 parts. In the present invention, the silane coupling agent is preferably a vinyl silane coupling agent, more preferably vinyl trimethoxy silane (i.e., silane coupling agent A-171). The silane coupling agent is added when the luminescent material color master batch particles are prepared, and is a difunctional compound, so that the silane coupling agent can react with inorganic luminescent materials or organic luminescent materials and organic polymer materials, and the preparation raw materials can be fully crosslinked in the granulating process, so that the finally obtained luminescent material color master batch particles have better mechanical properties and stable luminescent quality.
Based on the mass parts of the luminescent material, the preparation raw materials of the luminescent material color master batch comprise 8-15 parts of multifunctional alicyclic resin, preferably 9-13 parts, and more preferably 10-11 parts. In the present invention, the polyfunctional alicyclic resin preferably contains both an alicyclic epoxy group and a glycidyl ester group in its molecular structure; in an embodiment of the present invention, the multifunctional cycloaliphatic resin used is of the type MF-3286. The multifunctional alicyclic resin can play a role in gluing, and is favorable for uniformly bonding the luminescent material and other components together.
In the invention, the granularity of the luminescent material color master batch particles is preferably 2-5 mm.
The invention provides a preparation method of luminescent material color master batch particles, which comprises the following steps:
first mixing a thermoplastic high polymer material, a silane coupling agent, dibutyl phthalate and a multifunctional alicyclic resin to obtain a first mixture;
performing second mixing on the first mixture and the luminescent material to obtain a second mixture;
and thirdly mixing the second mixture, the ethylene-vinyl acetate copolymer and the polypropylene wax powder, and granulating to obtain the luminescent material color master batch particles.
The invention carries out first mixing on a thermoplastic polymer material, a silane coupling agent, dibutyl phthalate and a polyfunctional alicyclic resin to obtain a first mixture. The first mixing is preferably performed in a three-dimensional mixer, specifically, the thermoplastic polymer material is placed in the three-dimensional mixer, the mixer is started, and the silane coupling agent, the dibutyl phthalate and the polyfunctional alicyclic resin are added for first mixing. The invention is not particularly limited in the time and the rotation speed of the first mixing, and the components can be fully and uniformly mixed.
After the first mixture is obtained, the first mixture and the luminescent material are subjected to second mixing to obtain a second mixture. The second mixing is preferably carried out in a three-dimensional mixer, in particular by adding the luminescent material directly to the first mixture placed in the three-dimensional mixer after the first mixing. The time and the rotation speed of the second mixing are not particularly limited, and the components can be fully and uniformly mixed.
After the second mixture is obtained, the second mixture, the ethylene-vinyl acetate copolymer and the polypropylene wax powder are subjected to third mixing, and then are subjected to granulation to obtain the luminescent material color master batch particles. The third mixing is preferably performed in a three-dimensional mixer, specifically, after the second mixing, the ethylene-vinyl acetate copolymer and the polypropylene wax powder are directly added into the second mixture placed in the three-dimensional mixer to perform the third mixing. The invention has no special limitation on the third mixing time and the rotating speed, and can fully and uniformly mix the components to discharge. In the present invention, the granulation preferably includes extrusion and cutting performed sequentially; in the invention, the extrusion temperature is preferably 145-175 ℃, more preferably 150-170 ℃, and even more preferably 155-165 ℃; the invention is not particularly limited to the cutting, and the luminescent material color master batch particles with the granularity meeting the requirements can be obtained. In the present invention, the method further preferably includes: cooling the extruded material obtained after extrusion; the cooling is preferably to cool the extrudate to below 35 ℃, in particular to room temperature; the cooling mode is preferably air cooling. The invention preferably carries out extrusion in a double-screw extruder, cools the obtained extrusion material, and then carries out segmentation in a hob type slitter to obtain the luminescent material masterbatch.
The invention provides the application of the luminescent material color master batch particles in lighting devices, display devices or decorative devices, wherein the luminescent material color master batch particles are prepared by the technical scheme or the preparation method. In the present invention, the display device preferably includes a diffusion plate for display or a QLED optical substrate for display, the illumination device preferably includes an optical panel for illumination or a bead optical cover, and the decoration device preferably includes a decoration plate or an engraved mold having a backlight.
In the present invention, the excitation light source of the luminescent material color master batch is preferably a blue LED chip or an ultraviolet LED chip.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
The preparation raw materials of the luminescent material color master batch particles comprise the following components in parts by weight: 30 parts of thermoplastic PE plastic particles, 15 parts of thermoplastic PA plastic particles, 10 parts of thermoplastic EVOH plastic particles, 15 parts of CT-G series water phase quantum dot microcrystals (model QG 520) with the wavelength of 520nm, 10 parts of ethylene-vinyl acetate copolymer, 1 part of dibutyl phthalate, 4 parts of polypropylene wax powder, 10 parts of multifunctional alicyclic resin (model MF-3286) and 5 parts of vinyl silane coupling agent (silane coupling agent A-171); the particle sizes of the thermoplastic PE plastic particles, the thermoplastic PA plastic particles and the thermoplastic EVOH plastic particles are independently 1-5 mm.
Placing thermoplastic PE plastic particles, thermoplastic PA plastic particles and thermoplastic EVOH plastic particles in a three-dimensional stirrer, starting the stirrer, adding a vinyl silane coupling agent, dibutyl phthalate and a multifunctional alicyclic resin, uniformly mixing, then adding CT-G series water phase quantum dot microcrystals, uniformly mixing, and then adding an ethylene-vinyl acetate copolymer and polypropylene wax powder, and uniformly mixing; the resulting mixture was extruded (temperature: 165 ℃) in a twin-screw granulator and cut to obtain phosphor masterbatch particles having a particle size of 3 mm.
FIG. 1 is a spectrum of the 520nm color master batch prepared in example 1, and Table 1 shows index parameters of the 520nm color master batch prepared in example 1. As can be seen from fig. 1 and table 1, the wavelength of the finally obtained color master batch particles was 520nm by using the quantum dot microcrystalline luminescent material having a wavelength of 520nm.
TABLE 1 index parameters of 520nm color masterbatch particles prepared in example 1
| CIE-x | CIE-y | Half width/nm | Wavelength/nm | Light intensity/% | Light effect |
| 0.1459 | 0.5294 | 28 | 520 | 117 | 86.0 |
The color master batch particles having a wavelength of 520nm prepared in example 1 were subjected to an aging test, specifically, an aging test conducted under a condition of normal temperature (25 ℃) for 2000 hours, and the results are shown in FIG. 2. The results show that the color master batch particles with the wavelength of 520nm prepared in the example 1 have better ageing resistance.
Examples
The luminescent material masterbatch is prepared according to the method of example 1, wherein the preparation raw materials in this example include, in parts by weight: 20 parts of thermoplastic PE plastic particles, 15 parts of thermoplastic PA plastic particles, 20 parts of thermoplastic EVOH plastic particles, 15 parts of CT-G series water phase quantum dot microcrystals (model QG 540) with the wavelength of 540nm, 10 parts of ethylene-vinyl acetate copolymer, 1 part of dibutyl phthalate, 4 parts of polypropylene wax powder, 10 parts of multifunctional alicyclic resin (model MF-3286) and 5 parts of vinyl silane coupling agent (silane coupling agent A-171); the particle sizes of the thermoplastic PE plastic particles, the thermoplastic PA plastic particles and the thermoplastic EVOH plastic particles are independently 1-5 mm.
FIG. 3 is a spectrum of the 540nm color master batch prepared in example 2, and Table 2 shows index parameters of the 540nm color master batch prepared in example 2. As can be seen from fig. 3 and table 2, the wavelength of the prepared color master batch particles is 540nm by using the quantum dot microcrystalline luminescent material with the wavelength of 540nm.
TABLE 2 index parameters of color master batch particles with wavelength of 540nm prepared in example 2
| CIE-x | CIE-y | Half width/nm | Wavelength/nm | Light intensity/% | Light effect |
| 0.2211 | 0.4885 | 27 | 540 | 123 | 84.3 |
The aging resistance of the 540nm color master batch prepared in example 2 was measured in the same manner as in example 1, and the results are shown in FIG. 4. The results show that the color master batch particles with the wavelength of 540nm prepared in example 2 have better ageing resistance.
Examples
The luminescent material masterbatch is prepared according to the method of example 1, wherein the preparation raw materials in this example include, in parts by weight: 20 parts of thermoplastic PE plastic particles, 15 parts of thermoplastic PA plastic particles, 20 parts of thermoplastic EVOH plastic particles, 15 parts of CT-G series water phase quantum dot microcrystals (model QG 570) with the wavelength of 570nm, 10 parts of ethylene-vinyl acetate copolymer, 1 part of dibutyl phthalate, 4 parts of polypropylene wax powder, 10 parts of multifunctional alicyclic resin (model MF-3286) and 5 parts of vinyl silane coupling agent (silane coupling agent A-171); the particle sizes of the thermoplastic PE plastic particles, the thermoplastic PA plastic particles and the thermoplastic EVOH plastic particles are independently 1-5 mm.
FIG. 5 is a spectrum of 570nm color master batch prepared in example 3, and Table 3 shows index parameters of 570nm color master batch prepared in example 3. As can be seen from fig. 5 and table 3, the wavelength of the prepared color master batch particles was 570nm by using the quantum dot microcrystalline luminescent material with a wavelength of 570nm.
TABLE 3 index parameters of 570nm color master batch particles prepared in example 3
| CIE-x | CIE-y | Half width/nm | Wavelength/nm | Light intensity/% | Light effect |
| 0.4187 | 0.5252 | 29 | 570 | 162 | 88.7 |
The aging resistance of the 570nm color master batch prepared in example 3 was measured in the same manner as in example 1, and the results are shown in FIG. 6. The results show that the 570nm color master batch prepared in example 3 has better ageing resistance.
Examples
The luminescent material masterbatch is prepared according to the method of example 1, wherein the preparation raw materials in this example include, in parts by weight: 20 parts of thermoplastic PE plastic particles, 15 parts of thermoplastic PA plastic particles, 20 parts of thermoplastic EVOH plastic particles, 15 parts of TG-R series water phase quantum dot microcrystals with the wavelength of 605nm (model number QR 605), 10 parts of ethylene-vinyl acetate copolymer, 1 part of dibutyl phthalate, 4 parts of polypropylene wax powder, 10 parts of multifunctional alicyclic resin (model number MF-3286) and 5 parts of vinyl silane coupling agent (silane coupling agent A-171); the particle sizes of the thermoplastic PE plastic particles, the thermoplastic PA plastic particles and the thermoplastic EVOH plastic particles are independently 1-5 mm.
FIG. 7 is a spectrum of 605nm color master batch prepared in example 4, and Table 4 shows index parameters of 605nm color master batch prepared in example 4. As can be seen from fig. 7 and table 4, the wavelength of the prepared color master particles was 605nm by using the quantum dot microcrystalline luminescent material having a wavelength of 605nm.
TABLE 4 index parameters of the 605nm wavelength masterbatch prepared in example 4
| CIE-x | CIE-y | Half width/nm | Wavelength/nm | Light intensity/% | Light effect |
| 0.5838 | 0.3648 | 33 | 605 | 163 | 78.6 |
The aging resistance of the 605nm color master batch prepared in example 4 was measured in the same manner as in example 1, and the results are shown in FIG. 8. The results show that the 605nm color master batch prepared in example 4 has better ageing resistance.
Examples
The luminescent material masterbatch is prepared according to the method of example 1, wherein the preparation raw materials in this example include, in parts by weight: 20 parts of thermoplastic PE plastic particles, 15 parts of thermoplastic PA plastic particles, 20 parts of thermoplastic EVOH plastic particles, 15 parts of TG-R series water phase quantum dot microcrystals with the wavelength of 635nm (model number QR 635), 10 parts of ethylene-vinyl acetate copolymer, 1 part of dibutyl phthalate, 4 parts of polypropylene wax powder, 10 parts of multifunctional alicyclic resin (model number MF-3286) and 5 parts of vinyl silane coupling agent (silane coupling agent A-171); the particle sizes of the thermoplastic PE plastic particles, the thermoplastic PA plastic particles and the thermoplastic EVOH plastic particles are independently 1-5 mm.
FIG. 9 is a spectrum of 635nm wavelength masterbatch prepared in example 5, and Table 5 shows index parameters of 635nm wavelength masterbatch prepared in example 5. As can be seen from fig. 9 and table 5, the wavelength of the prepared color master batch particles was 635nm using the quantum dot microcrystalline luminescent material having a wavelength of 635nm.
TABLE 5 index parameters of 635nm wavelength masterbatch prepared in example 5
| CIE-x | CIE-y | Half width/nm | Wavelength/nm | Light intensity/% | Light effect |
| 0.5693 | 0.2693 | 55 | 635 | 121 | 68.1 |
The anti-aging property of the 635nm wavelength color master batch prepared in example 5 was measured in the same manner as in example 1, and the results are shown in FIG. 10. The result shows that the 635nm wavelength color master batch prepared in example 5 has better ageing resistance.
Examples
The luminescent material masterbatch is prepared according to the method of example 1, wherein the preparation raw materials in this example include, in parts by weight: 20 parts of thermoplastic PE plastic particles, 15 parts of thermoplastic PA plastic particles, 20 parts of thermoplastic EVOH plastic particles, 15 parts of TG-R series water phase quantum dot microcrystals with the wavelength of 660nm (model number QR 660), 10 parts of ethylene-vinyl acetate copolymer, 1 part of dibutyl phthalate, 4 parts of polypropylene wax powder, 10 parts of multifunctional alicyclic resin (model number MF-3286) and 5 parts of vinyl silane coupling agent (silane coupling agent A-171); the particle sizes of the thermoplastic PE plastic particles, the thermoplastic PA plastic particles and the thermoplastic EVOH plastic particles are independently 1-5 mm.
FIG. 11 is a spectrum of 660 nm-wavelength color master batch prepared in example 6, and Table 6 shows index parameters of 660 nm-wavelength color master batch prepared in example 6. As can be seen from fig. 11 and table 6, the wavelength of the prepared color master particles was 660nm by using the quantum dot microcrystalline luminescent material having a wavelength of 660nm.
TABLE 6 index parameters of color masterbatch having a wavelength of 660nm prepared in example 6
| CIE-x | CIE-y | Half width/nm | Wavelength/nm | Light intensity/% | Light effect |
| 0.40901 | 0.1921 | 57 | 660 | 93 | 46.8 |
The aging resistance of the 660nm wavelength masterbatch prepared in example 6 was measured in the same manner as in example 1, and the results are shown in FIG. 12. The results show that the 660 nm-wavelength masterbatch prepared in example 6 has better ageing resistance.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. The luminescent material color master batch comprises the following preparation raw materials in parts by mass:
15-25 parts of luminescent material; the luminescent material is a quantum dot microcrystal, and the quantum dot microcrystal is CT-G series aqueous phase quantum dot microcrystal or TG-R series aqueous phase quantum dot microcrystal;
45-55 parts of thermoplastic polymer material; the thermoplastic high polymer material is a mixture of ethylene-vinyl alcohol copolymer, polyamide and polyethylene;
10-20 parts of ethylene-vinyl acetate copolymer;
1-2 parts of dibutyl phthalate;
3-5 parts of polypropylene wax powder;
5-10 parts of silane coupling agent;
8-15 parts of polyfunctional alicyclic resin;
the preparation method of the luminescent material color master batch comprises the following steps:
first mixing a thermoplastic high polymer material, a silane coupling agent, dibutyl phthalate and a multifunctional alicyclic resin to obtain a first mixture;
performing second mixing on the first mixture and the luminescent material to obtain a second mixture;
and thirdly mixing the second mixture, the ethylene-vinyl acetate copolymer and the polypropylene wax powder, and granulating to obtain the luminescent material color master batch particles.
2. The luminescent material color master batch of claim 1, wherein the wavelength band of the luminescent material comprises 480-485 nm, 490-495 nm, 500-515 nm, 520-525 nm, 530-535 nm, 540-560 nm, 565-580 nm, 585-595 nm, 600-620 nm, 625-635 nm, 640-655 nm, 660-665 nm, or 670-675 nm.
3. The luminescent material color master batch according to claim 1, wherein the multifunctional alicyclic resin contains both alicyclic epoxy groups and glycidyl ester groups in its molecular structure.
4. A luminescent material masterbatch according to any one of claims 1-3, characterized in that the luminescent material masterbatch has a particle size of 2-5 mm.
5. The method for preparing the luminescent material color master batch according to any one of claims 1 to 4, comprising the steps of:
first mixing a thermoplastic high polymer material, a silane coupling agent, dibutyl phthalate and a multifunctional alicyclic resin to obtain a first mixture;
performing second mixing on the first mixture and the luminescent material to obtain a second mixture;
and thirdly mixing the second mixture, the ethylene-vinyl acetate copolymer and the polypropylene wax powder, and granulating to obtain the luminescent material color master batch particles.
6. The method of claim 5, wherein the granulating comprises sequentially extruding and cutting; the extrusion temperature is 145-175 ℃.
7. Use of the luminescent material masterbatch according to any one of claims 1 to 4 or the luminescent material masterbatch according to any one of claims 5 to 6 in lighting devices, display devices or decorative devices.
8. The use according to claim 7, wherein the excitation light source of the luminescent material color master particles is a blue LED chip or an ultraviolet LED chip.
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