CN109679007B - High-dispersity quantum dot injection plastic rice and preparation method thereof - Google Patents

High-dispersity quantum dot injection plastic rice and preparation method thereof Download PDF

Info

Publication number
CN109679007B
CN109679007B CN201811637323.6A CN201811637323A CN109679007B CN 109679007 B CN109679007 B CN 109679007B CN 201811637323 A CN201811637323 A CN 201811637323A CN 109679007 B CN109679007 B CN 109679007B
Authority
CN
China
Prior art keywords
quantum dots
dispersity
rice
quantum dot
injection molding
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201811637323.6A
Other languages
Chinese (zh)
Other versions
CN109679007A (en
Inventor
吴敬伟
黄明鹭
王翔
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xiamen Migong Technology Co ltd
Original Assignee
Xiamen Migong Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xiamen Migong Technology Co ltd filed Critical Xiamen Migong Technology Co ltd
Priority to CN201811637323.6A priority Critical patent/CN109679007B/en
Publication of CN109679007A publication Critical patent/CN109679007A/en
Application granted granted Critical
Publication of CN109679007B publication Critical patent/CN109679007B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F120/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/10Esters
    • C08F120/12Esters of monohydric alcohols or phenols
    • C08F120/14Methyl esters, e.g. methyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F120/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/10Esters
    • C08F120/12Esters of monohydric alcohols or phenols
    • C08F120/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F120/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16Dicarboxylic acids and dihydroxy compounds
    • C08G63/18Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/19Hydroxy compounds containing aromatic rings
    • C08G63/193Hydroxy compounds containing aromatic rings containing two or more aromatic rings
    • C08G63/195Bisphenol A
    • 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
    • C08K9/02Ingredients treated with inorganic substances
    • 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

Abstract

The invention relates to a high-dispersity quantum dot injection molding rice and a preparation method thereof, wherein the injection molding rice prepared by the method takes a high-molecular polymer as a base material, and is formed by uniformly dispersing and compounding quantum dots in a certain proportion and concentration, and curing; the material rice with the quantum dots uniformly dispersed can be used for injection molding into quantum dot light conversion devices with various forms. The high-dispersity quantum dot injection molding plastic rice comprises a high polymer base material, and quantum dots and a dispersing agent which are uniformly dispersed in the high polymer base material. The preparation method comprises the following steps: the method comprises the following steps: surface modification of the quantum dots, namely performing high-temperature resistant treatment on the quantum dots; step two: compounding ingredients, namely fully mixing the surface-modified quantum dots and a dispersing agent, and then adding the mixture into a high polymer monomer for prepolymerization; step three: and (4) extrusion molding, namely extruding and cutting the prepolymerized material into the injection molding rice containing the high-dispersity quantum dots.

Description

High-dispersity quantum dot injection plastic rice and preparation method thereof
Technical Field
The invention relates to the field of display and illumination, in particular to high-dispersity quantum dot injection plastic rice and a preparation method thereof.
Background
Nowadays, display and lighting devices using LEDs as light sources have become widespread. The traditional white light LED adopts a mode of adding yellow fluorescent powder outside a blue light LED, and in spectral distribution, a blue light part is relatively pure, while green light and red light parts have no obvious peak value, and the saturation of red and green is not high on an imaging spectrum. The peak value of red, green and blue light is obvious when the quantum dot backlight is used, and the saturation of the color is higher after imaging. Furthermore, quantum dots have size adjustability. The quantum dots with different particle diameters correspond to light with different emission wavelengths. Therefore, the quantum dot based device can effectively improve the color gamut level of the display device as a backlight source. Meanwhile, the required spectrum can be more effectively fitted in the application of the lighting equipment. Has wide application prospect in the fields of health illumination and plant illumination.
At present, in display or lighting devices, quantum dots and polymer composites are often fabricated into structures such as light guide plates, rods, or films. As a device for converting blue light excitation fitting into white light, the product form is restricted by the technology and is not flexible. For some light guide devices with special structures, the product size can be effectively controlled, the yield and the production efficiency are improved, and the application forms and the fields of the light guide devices are further expanded.
It is a common technical means to mix quantum dots with high polymer resin meeting optical requirements to prepare light conversion devices with various forms. However, quantum dots and various high polymer doping processes suffer from a number of problems. For example, the process of compounding quantum dots with some high polymers requires a high-temperature environment, and is easy to quench and inactivate fluorescence. In addition, the quantum dot and the high polymer are easy to agglomerate in the compounding process, the dispersibility in the base material is poor, and the integral optical effect is influenced. The original quantum dot optical device needs to process and allocate quantum dots in the production process, the production threshold is too high, the raw materials are complex, the requirement on the storage environment is high, and the like.
Disclosure of Invention
The invention relates to a high-dispersity quantum dot injection molding rice and a preparation method thereof, wherein the injection molding rice prepared by the method takes a high-molecular polymer as a base material, and is formed by uniformly dispersing and compounding quantum dots in a certain proportion and concentration, and curing; the material rice with the quantum dots uniformly dispersed can be used for injection molding into quantum dot light conversion devices with various forms.
The technical scheme of the invention is realized as follows:
a high-dispersity quantum dot injection molding plastic rice is characterized in that: comprises a high polymer base material, and quantum dots and a dispersing agent which are uniformly dispersed in the high polymer base material.
Furthermore, the quantum dots are coated by high-temperature-resistant ligands.
Furthermore, the high-temperature-resistant ligand is formed by compounding an organic matter and an inorganic matter. Wherein the organic substances are stearic acid, palmitic acid, oleic acid and oliveOne or more of elemene oil, 1-octadecene and 1-octadecylamine; the inorganic substance is Al2O3、ZrO2、SiC、Si3N4、SiO2、TiO2One or more of them.
Further, the dispersant is one or more of stearic acid amide, erucic acid amide, oleic acid amide, ethylene bis-stearic acid amide, ethylene bis-oleic acid amide, stearyl erucic acid amide, pentaerythritol stearate, oleic acid palmitamide and paraffin.
Further, the polymer monomer is one or more of methyl methacrylate, butyl methacrylate, diphenyl ester, bisphenol A, styrene, acrylic acid, acrylonitrile, vinyl acetate and silica gel.
Furthermore, the quantum dots are formed by mixing quantum dots with single color or multiple colors, and the emission wavelength of the quantum dots is between 350 and 900 nm.
A preparation method of high-dispersity quantum dot injection molding rice comprises the following steps:
the method comprises the following steps: surface modification of the quantum dots, namely performing high-temperature resistant treatment on the quantum dots;
step two: compounding ingredients, namely fully mixing the surface-modified quantum dots and a dispersing agent, and then adding the mixture into a high polymer monomer for prepolymerization;
step three: and (4) extrusion molding, namely extruding and cutting the prepolymerized material into the injection molding rice containing the high-dispersity quantum dots.
Further, the specific method of the first step includes:
mixing the quantum dots and the high-temperature-resistant ligand, stirring the mixed solution, and then placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution; then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
Further, the specific method in the second step comprises:
adding the dried quantum dot powder into a dispersing agent, and mechanically stirring and uniformly mixing;
and (3) adding a high polymer monomer into the reaction kettle in advance, quickly injecting the mixture of the quantum dots and the dispersing agent into the reaction kettle, stirring and heating for prepolymerization.
Further, the specific method in the third step includes:
and transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
Further, the mass ratio of the quantum dots to the dispersing agent is 1: 10-1: 100; the mass ratio of the quantum dots to the polymer monomers is 1: 100-1: 100000.
As can be seen from the above description of the present invention, compared with the prior art, the present invention has the following advantages:
the invention changes the original method for preparing the quantum dot optical device, the quantum dots are prepared in the injection molding material rice, and the injection molding material rice is only required to be selected for direct processing and molding when the quantum dot optical device is prepared, thereby omitting the complex steps of quantum dot allocation, high polymer and quantum dot polymerization and the like in the production of the original optical device, and reducing the production threshold of the quantum dot optical device; meanwhile, the quantum dots are uniformly dispersed in the material rice in advance, so that the quantum dots in the prepared optical device are uniformly dispersed, and the yield of the prepared optical device is improved.
The injection molding material rice produced by the invention has good stability and is convenient to store, and compared with the prior method of respectively storing the quantum dots, the high polymer, the dispersing agent and the like, the method greatly reduces the raw material storage requirement and difficulty in the production process.
The quantum dots are uniformly and stably dispersed in the high polymer base material meeting the optical requirements and used as the precursor material for injection molding, so that the quantum dots can be promoted to be widely applied to backlight display and lighting devices.
In the invention, the optical device made of the injection molding material can be directly matched with a required spectrum under the excitation of a blue lamp, so that the production steps of fluorescent light splitting, blending, curing and the like are reduced, the production steps are simplified, and the process requirement is reduced.
The modified quantum dots are stable in high-temperature environment, do not have structural and photochemical property changes, and have higher thermal stability compared with the traditional quantum dots.
The use of the dispersing agent in the invention enables the quantum dots in the injection molding material rice prepared by compounding the quantum dots and the high polymer to have good dispersibility, can effectively avoid the phenomenon of agglomeration in the doping process of the quantum dots and the high polymer material, and improves the light conversion efficiency on the basis of meeting the optical performance index.
And the injection molding material rice provided by the invention is used as a raw material for injection molding, has strong plasticity, and can be applied to quantum dot light conversion devices in various forms.
The quantum dot injection molding rice can effectively fit a required spectrum under the excitation of a blue lamp according to the concentration and proportion of the quantum dots in the material rice, so that the color gamut level of a display device can be remarkably improved, and the equipment requirement meeting the requirements of healthy illumination and plant illumination can be prepared.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a schematic view of the structure of the injection molding compound of the present invention;
FIG. 2 is a flow chart of the process for preparing the injection molding material rice of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
Referring to fig. 1, the high-dispersity quantum dot injection molding plastic rice is characterized in that: comprises a high polymer substrate 1, and quantum dots 2 and a dispersing agent 3 which are uniformly dispersed in the high polymer substrate.
The quantum dots 2 are quantum dots 2 coated by high-temperature-resistant ligands.
The high-temperature resistant ligand is compounded by organic matters and inorganic matters. Wherein the organic matter is one or more of stearic acid, palmitic acid, oleic acid, olive oil, 1-octadecene and 1-octadecylamine; the inorganic substance is Al2O3、ZrO2、SiC、Si3N4、SiO2、TiO2One or more of them.
The dispersant 3 is composed of one or more of stearic acid amide, erucic acid amide, oleic acid amide, ethylene bis-stearic acid amide, ethylene bis-oleic acid amide, stearyl erucic acid amide, pentaerythritol stearate, oleic acid palmitamide and paraffin.
The polymer monomer is one or more of methyl methacrylate, butyl methacrylate, diphenyl ester, bisphenol A, styrene, acrylic acid, acrylonitrile, vinyl acetate and silica gel.
The quantum dots 2 are formed by mixing quantum dots 2 with single colors or multiple colors, and the emission wavelength of the quantum dots 2 is between 350 and 900 nm.
A preparation method of high-dispersity quantum dot 2 injection molding material rice comprises the following steps:
the method comprises the following steps: surface modification of the quantum dots 2, namely performing high-temperature resistant treatment on the quantum dots 2;
step two: compounding ingredients, namely fully mixing the surface-modified quantum dots 2 with a dispersant 3, and then adding the mixture into a high polymer monomer for prepolymerization;
step three: and (3) extrusion molding, namely extruding and cutting the prepolymerized material into the 2-injection molding material containing the high-dispersity quantum dots.
The specific method of the first step comprises the following steps:
mixing the quantum dots 2 with a high-temperature-resistant ligand, stirring the mixed solution, and then placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
The specific method of the second step comprises the following steps:
adding the dried quantum dot 2 powder into a dispersing agent 3, and mechanically stirring and uniformly mixing;
and (3) adding a high polymer monomer into the reaction kettle in advance, quickly injecting the mixture of the quantum dots 2 and the dispersing agent 3 into the reaction kettle, stirring and heating for prepolymerization.
The third specific method comprises the following steps:
and transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
The mass ratio of the quantum dots 2 to the dispersing agent 3 is 1: 10-1: 100; the mass ratio of the quantum dots 2 to the polymer monomers is 1: 100-1: 100000.
The specific embodiment is as follows:
example 1:
1. mixing stearic acid and Al in equal molar ratio2O3Adding into a high-pressure reaction kettle, and stirring and reacting for 12 hours at the temperature of 200 ℃. Stopping the reaction after 12h, cooling to normal temperature, transferring to a 60 ℃ oven, and devolatilizing to remove part of unreacted solvent to obtain the high-temperature-resistant ligand.
Adding quantum dots with the mass ratio of 20% into a certain amount of high-temperature-resistant ligand, mixing, stirring the mixed solution, and placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
2. Adding 100mg of dried quantum dot powder into 1g of stearic acid amide, and mechanically stirring and uniformly mixing;
10kg of methyl methacrylate is added into the reaction kettle in advance, the mixture of the quantum dots and the stearic acid amide is quickly injected into the reaction kettle, stirred and heated for prepolymerization.
3. And transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
Example 2:
1. adding stearic acid and SiC in equal molar ratio into a high-pressure reaction kettle, and controlling the temperature to be 200 ℃ to stir and react for 12 hours. Stopping the reaction after 12h, cooling to normal temperature, transferring to a 60 ℃ oven, and devolatilizing to remove part of unreacted solvent to obtain the high-temperature-resistant ligand.
Adding quantum dots with the mass ratio of 20% into a certain amount of high-temperature-resistant ligand, mixing, stirring the mixed solution, and placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
2. Adding 250mg of dried quantum dot powder into 25g of erucamide, and mechanically stirring and uniformly mixing;
10kg of methyl methacrylate is added into the reaction kettle in advance, the mixture of the quantum dots and the erucamide is quickly injected into the reaction kettle, stirred and heated for prepolymerization.
3. And transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
Example 3:
1. mixing stearic acid and SiO in equal molar ratio2Adding into a high-pressure reaction kettle, and stirring and reacting for 12 hours at the temperature of 200 ℃. Stopping the reaction after 12h, cooling to normal temperature, transferring to a 60 ℃ oven, and devolatilizing to remove part of unreacted solvent to obtain the high-temperature-resistant ligand.
Adding quantum dots with the mass ratio of 20% into a certain amount of high-temperature-resistant ligand, mixing, stirring the mixed solution, and placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
2. Adding 500mg of dried quantum dot powder into 100g of oleamide, and mechanically stirring and uniformly mixing;
10kg of methyl methacrylate is added into the reaction kettle in advance, the mixture of the quantum dots and the oleamide is quickly injected into the reaction kettle, stirred and heated for prepolymerization.
3. And transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
Example 4:
1. mixing palmitic acid and Al in equal molar ratio2O3Adding into a high-pressure reaction kettle, and stirring and reacting for 12 hours at the temperature of 200 ℃. Stopping the reaction after 12h, cooling to normal temperature, transferring to a 60 ℃ oven, and devolatilizing to remove part of unreacted solvent to obtain the high-temperature-resistant ligand.
Adding quantum dots with the mass ratio of 20% into a certain amount of high-temperature-resistant ligand, mixing, stirring the mixed solution, and placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
2. Adding 1g of dried quantum dot powder into 100g of ethylene bis stearamide, and mechanically stirring and uniformly mixing;
20kg of butyl methacrylate is added into the reaction kettle in advance, the mixture of the quantum dots and the ethylene bis stearamide is quickly injected into the reaction kettle, stirred and heated for prepolymerization.
3. And transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
Example 5:
1. mixing palmitic acid and SiO in equal molar ratio2Adding into a high-pressure reaction kettle, and stirring and reacting for 12 hours at the temperature of 200 ℃. Stopping the reaction after 12h, and cooling to normal temperatureTransferring the mixture to a 60 ℃ oven for devolatilization to remove part of unreacted solvent, and obtaining the high-temperature-resistant ligand.
Adding quantum dots with the mass ratio of 20% into a certain amount of high-temperature-resistant ligand, mixing, stirring the mixed solution, and placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
2. Adding 2.5g of dried quantum dot powder into 250g of stearic acid amide, and mechanically stirring and uniformly mixing;
20kg of butyl methacrylate is added into the reaction kettle in advance, the mixture of the quantum dots and the stearic acid amide is quickly injected into the reaction kettle, stirred and heated for prepolymerization.
3. And transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
Example 6:
1. mixing stearic acid and TiO in equal molar ratio2Adding into a high-pressure reaction kettle, and stirring and reacting for 12 hours at the temperature of 200 ℃. Stopping the reaction after 12h, cooling to normal temperature, transferring to a 60 ℃ oven, and devolatilizing to remove part of unreacted solvent to obtain the high-temperature-resistant ligand.
Adding quantum dots with the mass ratio of 20% into a certain amount of high-temperature-resistant ligand, mixing, stirring the mixed solution, and placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
2. Adding 5g of dried quantum dot powder into 500g of erucamide, and mechanically stirring and uniformly mixing;
20kg of methyl methacrylate is added into the reaction kettle in advance, the mixture of the quantum dots and the erucamide is quickly injected into the reaction kettle, stirred and heated for prepolymerization.
3. And transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
Example 7:
1. mixing oleic acid and Al in equal molar ratio2O3Adding into a high-pressure reaction kettle, and stirring and reacting for 12 hours at the temperature of 200 ℃. Stopping the reaction after 12h, cooling to normal temperature, transferring to a 60 ℃ oven, and devolatilizing to remove part of unreacted solvent to obtain the high-temperature-resistant ligand.
Adding quantum dots with the mass ratio of 20% into a certain amount of high-temperature-resistant ligand, mixing, stirring the mixed solution, and placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
2. Adding 50g of dried quantum dot powder into 500g of oleamide, and mechanically stirring and uniformly mixing;
30kg of methyl methacrylate is added into the reaction kettle in advance, the mixture of the quantum dots and the oleamide is quickly injected into the reaction kettle, stirred and heated for prepolymerization.
3. And transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
Example 8:
1. adding palmitic acid and SiC in equal molar ratio into a high-pressure reaction kettle, and controlling the temperature to be 200 ℃ to stir and react for 12 hours. Stopping the reaction after 12h, cooling to normal temperature, transferring to a 60 ℃ oven, and devolatilizing to remove part of unreacted solvent to obtain the high-temperature-resistant ligand.
Adding quantum dots with the mass ratio of 20% into a certain amount of high-temperature-resistant ligand, mixing, stirring the mixed solution, and placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
2. Adding 100g of dried quantum dot powder into 1kg of paraffin, and mechanically stirring and uniformly mixing;
30kg of butyl methacrylate is added into the reaction kettle in advance, the mixture of the quantum dots and the paraffin is quickly injected into the reaction kettle, and the mixture is stirred and heated for prepolymerization.
3. And transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
Example 9:
1. mixing oleic acid and SiO in equal molar ratio2Adding into a high-pressure reaction kettle, and stirring and reacting for 12 hours at the temperature of 200 ℃. Stopping the reaction after 12h, cooling to normal temperature, transferring to a 60 ℃ oven, and devolatilizing to remove part of unreacted solvent to obtain the high-temperature-resistant ligand.
Adding quantum dots with the mass ratio of 20% into a certain amount of high-temperature-resistant ligand, mixing, stirring the mixed solution, and placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
2. Adding 300g of dried quantum dot powder into 3kg of erucamide, and mechanically stirring and uniformly mixing;
30kg of diphenyl ester and bisphenol A mixed monomer is added into a reaction kettle in advance, the mixture of the quantum dots and the erucamide is quickly injected into the reaction kettle, stirred and heated for prepolymerization.
3. And transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
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. High-dispersity quantum dot injection molding plasticRice, which is characterized in that: the quantum dot/dispersant composite material comprises a high polymer base material, and quantum dots and a dispersant which are uniformly dispersed in the high polymer base material; the quantum dots are quantum dots coated by high-temperature-resistant ligands; the high-temperature resistant ligand is formed by compounding an organic matter and an inorganic matter; wherein the organic matter is one or more of stearic acid, palmitic acid, oleic acid, olive oil, 1-octadecene and 1-octadecylamine; the inorganic substance is Al2O3、ZrO2、SiC、Si3N4、SiO2、TiO2One or more of them.
2. The high-dispersity quantum dot injection-molded plastic rice as claimed in claim 1, wherein the high-dispersity quantum dot injection-molded plastic rice is characterized in that: the dispersant is one or more of stearic acid amide, erucic acid amide, oleic acid amide, ethylene bis-stearic acid amide, ethylene bis-oleic acid amide, stearyl erucic acid amide, pentaerythritol stearate, oleic acid palmitamide and paraffin.
3. The high-dispersity quantum dot injection-molded plastic rice as claimed in any one of claims 1-2, wherein: the polymer monomer is one or more of methyl methacrylate, butyl methacrylate, diphenyl ester, bisphenol A, styrene, acrylic acid, acrylonitrile, vinyl acetate and silica gel.
4. The high-dispersity quantum dot injection-molded plastic rice as claimed in claim 3, wherein the high-dispersity quantum dot injection-molded plastic rice is characterized in that: the quantum dots are formed by mixing quantum dots with single color or multiple colors, and the emission wavelength of the quantum dots is between 350-900 nm.
5. A preparation method of high-dispersity quantum dot injection molding rice is characterized by comprising the following steps:
the method comprises the following steps: surface modification of the quantum dots, namely performing high-temperature resistant treatment on the quantum dots;
step two: compounding ingredients, namely fully mixing the surface-modified quantum dots and a dispersing agent, and then adding the mixture into a high polymer monomer for prepolymerization;
step three: extruding and molding, namely extruding and cutting the prepolymerized material into the injection molding rice containing the high-dispersity quantum dots;
the specific method of the first step comprises the following steps:
mixing the quantum dots and the high-temperature-resistant ligand, stirring the mixed solution, and then placing the mixed solution in an ultrasonic instrument to fully disperse the mixed solution;
then transferring the mixed liquid into a flask for continuous stirring until the reaction is stopped;
and finally transferring the mixed solution to a watch glass to volatilize the redundant solvent, and baking to obtain dry powder.
6. The preparation method of the high-dispersity quantum dot injection molding rice as claimed in claim 5, wherein the specific method in the second step comprises the following steps:
adding the dried quantum dot powder into a dispersing agent, and mechanically stirring and uniformly mixing;
and (3) adding a high polymer monomer into the reaction kettle in advance, quickly injecting the mixture of the quantum dots and the dispersing agent into the reaction kettle, stirring and heating for prepolymerization.
7. The preparation method of the high-dispersity quantum dot injection molding rice as claimed in claim 5, wherein the specific method of the third step comprises the following steps:
and transferring the pre-polymerized material to a feeding groove, extruding the material, cooling and solidifying the extruded material, and cutting the material into particles to form the material rice.
8. The preparation method of the high-dispersity quantum dot injection molding rice as claimed in any one of claims 5-7, wherein the method comprises the following steps: the mass ratio of the quantum dots to the dispersing agent is 1: 10-1: 100; the mass ratio of the quantum dots to the polymer monomers is 1: 100-1: 100000.
CN201811637323.6A 2018-12-29 2018-12-29 High-dispersity quantum dot injection plastic rice and preparation method thereof Active CN109679007B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811637323.6A CN109679007B (en) 2018-12-29 2018-12-29 High-dispersity quantum dot injection plastic rice and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811637323.6A CN109679007B (en) 2018-12-29 2018-12-29 High-dispersity quantum dot injection plastic rice and preparation method thereof

Publications (2)

Publication Number Publication Date
CN109679007A CN109679007A (en) 2019-04-26
CN109679007B true CN109679007B (en) 2021-07-09

Family

ID=66190238

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811637323.6A Active CN109679007B (en) 2018-12-29 2018-12-29 High-dispersity quantum dot injection plastic rice and preparation method thereof

Country Status (1)

Country Link
CN (1) CN109679007B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112649409A (en) * 2020-12-24 2021-04-13 北京北达聚邦科技有限公司 Method for detecting quantum dot light stability
CN114685921B (en) * 2020-12-31 2023-09-26 苏州国纳思新材料科技有限公司 Preparation method of quantum dot resin material

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BR112014018744B1 (en) * 2012-02-03 2020-12-15 Lumileds Holding B.V PROCESS FOR THE PRODUCTION OF A SOLID POLYMER WITH THE LUMINESCENT NANOPARTICLES INCORPORATED IN THE POLYMER, LUMINESCENT POLYMERIC ARTICLE, LIGHTING UNIT AND LUMINESCENT MATERIAL
CN102690658A (en) * 2012-05-28 2012-09-26 广东普加福光电科技有限公司 Quantum dot-embedded porous silicon dioxide composite material, and preparation method and application thereof
CN105778887B (en) * 2014-12-22 2018-10-26 Tcl集团股份有限公司 A kind of method, quantum dot complex particle and the application of sealing quantum dot
CN104516039B (en) * 2014-12-23 2018-04-27 深圳市华星光电技术有限公司 The production method and liquid crystal display device of quantum dot color filter
WO2018095442A1 (en) * 2016-11-22 2018-05-31 华南农业大学 Quantum dot and use of composite material thereof in preparing ultraviolet resistant products

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
All-Inorganic Perovskite Nanocrystals with a Stellar Set of Stabilities and Their Use in White Light-Emitting Diodes;Chang Yajing等;《ACS APPLIED MATERIALS & INTERFACES》;20181010;第10卷(第43期);第37267-37276页 *

Also Published As

Publication number Publication date
CN109679007A (en) 2019-04-26

Similar Documents

Publication Publication Date Title
CN106957645B (en) Quantum dot photoresist and preparation method thereof
CN109679007B (en) High-dispersity quantum dot injection plastic rice and preparation method thereof
WO2011032358A1 (en) Plastic light-converting fluorescent granules and use thereof
CN102532857A (en) Polycarbonate composite material suitable for LED (light-emitting diode) lamp cover and preparation method thereof
WO2018056632A1 (en) Hybrid organic/inorganic quantum dot composite and method for preparing the same
TW201643527A (en) Backlight unit and display apparatus comprising the same
CN108467552A (en) Light diffusion master batch and preparation method thereof
CN103937158A (en) Quantum dot with high transparency and high fluorescence efficiency/epoxy resin nano composite material, preparation and applications thereof
CN106098952A (en) A kind of HONGGUANG carbon quantum dot of organosilicon functionalization and its preparation method and application
CN110114440A (en) Wavelength convert photism resin combination and its manufacturing method and wavelength convert component and light-emitting component
CN111363385B (en) Preparation method of organic modified barium titanate nanoparticles and preparation method of quantum dot optical film
CN102702637A (en) High light-transmittance and high light-shielding polystyrene composition and preparation method of composition
CN110114701A (en) Wavelength convert photism resin combination and its manufacturing method and wavelength convert component and light-emitting component
CN113861970A (en) Preparation method of cellulose-based carbon dots and application of cellulose-based carbon dots in blue light resistant field
CN107177167B (en) Heat-dissipating resin composition for LED substrate and preparation method thereof
CN107501578B (en) A kind of high temperature resistant, organic smooth opening agent of low migration and master batch that thus opening agent is prepared
TWI719300B (en) Nitrogen-containing cyclic compound, color conversion film, backlight unit, and display apparatus comprising the same
CN109608758B (en) Photodiffusion PP material and preparation method thereof
CN102376847B (en) Composite optical device, mold, preparation method and optical system
CN105419135A (en) Diffusion plate master batch, preparation method thereof and preparation method of diffusion plate
CN104004126B (en) The preparation method of organic fluorescence light-emitting film
CN102337016A (en) Preparation method of light-diffusion master batch
CN111378444A (en) Quantum dot film and preparation method thereof
TWI570187B (en) Optical solid state prepolymer and molding composition
KR20170037499A (en) Compound containing nitrogen and color conversion film comprising the same

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant