CN114685921A - Preparation method of quantum dot resin material - Google Patents
Preparation method of quantum dot resin material Download PDFInfo
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- CN114685921A CN114685921A CN202011641779.7A CN202011641779A CN114685921A CN 114685921 A CN114685921 A CN 114685921A CN 202011641779 A CN202011641779 A CN 202011641779A CN 114685921 A CN114685921 A CN 114685921A
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- 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
- C08K3/02—Elements
- C08K3/04—Carbon
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- 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
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/06—Polystyrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention provides a method for preparing a quantum dot resin material, which specifically comprises the following steps: the method comprises the following steps: preparing quantum dot powder, namely preparing carbon quantum with good stability and no toxicity by using a hydrothermal reaction; step two: compounding ingredients, namely fully mixing the quantum dot powder with a dispersing agent and a resin base material; step three: and (3) extruding and granulating, namely extruding and granulating the fully mixed composite material at a high temperature through a double screw to form the quantum dot resin material. The quantum dot resin obtained by the method has excellent fluorescence, mechanical property and flame retardant property. The method is simple and feasible, is suitable for various resins, and only needs to uniformly disperse a certain proportion of quantum dot powder in the resin base material.
Description
Technical Field
The invention relates to a preparation method of a quantum dot resin material with good fluorescence, mechanical property and flame retardant property, the resin material can be suitable for the display field, injection molding of special products, film materials and the like, and the method is simple and feasible and has innovation.
Background
At present, the use of polyolefin or polyester resin materials has been deeply achieved in the aspects of mass life, but most of the polyolefin or polyester resin materials are applied to the aspects of lower-end injection molding or film material products. How to improve the added value of the alloy to the maximum extent and optimize the mechanical property of the alloy becomes a research hotspot. The carbon quantum dots are fluorescent nanoparticles with the size of 2-4nm in the true sense, the particle size of the carbon quantum dots is adjustable, the raw materials are mild, the synthesis is simple, and the product is non-toxic. Due to the fact that the nano-size effect of the quantum dots can well reinforce the resin base material, the tensile strength and the bending strength of the resin base material are greatly improved, and on the other hand, the device of the quantum dots serving as a backlight source can effectively improve the color gamut level of the display equipment. Meanwhile, the abundant functional groups on the surface of the carbon quantum dots can quickly consume ambient oxygen under high-temperature open fire to form carbon dioxide, water and coke to carry out flame-retardant protection on the base material.
The mixing of the quantum dots and the polymer resin can greatly provide the fluorescence, mechanical property and flame retardant property of the resin material, but at present, the quantum dots and the polymer resin are doped at high temperature to cause quenching inactivation of the quantum dots, such as the fluorescent resin with poor activity described in CN 109790234, and only trace by preserving a small amount of optical property. In addition, the nano size of the quantum dot is easy to generate agglomeration phenomenon, so that the product performance is poor, and the fluorescence disappears. The fluorescent compound and the production method thereof described in CN 103992344 have extremely high production requirements, complex and toxic raw material matching, and are not easy to be popularized in a large area. The invention can make up for the defects to develop the nontoxic quantum dot resin material which has simple process and can be prepared in large quantity.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a quantum dot resin material. The method overcomes the defect that other quantum dots are easy to quench after being mixed at high temperature by a screw at present, endows the material with more excellent mechanical property and better flame retardant property, greatly improves the added value of the material, and can be applied to injection molding of optical devices and special products, film materials and the like.
The technical scheme of the invention is as follows: a preparation method of a quantum dot resin material comprises the following specific steps:
the method comprises the following steps: preparing quantum dot powder; dissolving citric acid and urea serving as raw materials in deionized water to prepare a solution, transferring the solution into a hydrothermal kettle, putting the hydrothermal kettle into a high-temperature oven for reaction, taking out the hydrothermal reaction kettle after the reaction is finished, opening the hydrothermal reaction kettle after the hydrothermal reaction kettle is cooled, taking out a quantum dot solution, and drying the quantum dot solution to obtain quantum dot powder;
step two: compounding ingredients; dispersing agent and quantum dot powder according to the mass ratio of 1: (10-50) mixing to form a component A; and (2) mixing the component A and a resin material according to the mass ratio of 1: (10-100) mixing and stirring in a high-speed mixer to form a composite ingredient;
step three: extruding and granulating; and extruding and granulating the composite ingredients at high temperature through a double screw to form the quantum dot resin material.
Preferably, the molar ratio of citric acid to urea in the first step is 1: (0.5-1) preparing the solution with the mass concentration of 1-2%; the temperature of the high-temperature oven is 180 ℃ and 200 ℃, and the reaction time is 6-10 hours.
Preferably, the rotation speed of the high-speed mixer in the second step is 1000-1400r/min, and the mixing and stirring time is 2-4 minutes.
The parameters of the double-screw extruder in the third step are preferably as follows: the melt temperature is set to be 170-280 ℃ (the temperature is set according to the melting temperature of the selected resin base material), the screw rotation speed is set to be 20-28r/min, and the feeding speed is 10-15 r/min. And (4) after extrusion, bracing and cooling are carried out in a water cooling mode, and the granulation speed is set to be parallel to the rotating speed of the screw rod and the strip is maintained to be continuous.
Preferably, the dispersant is one or more of stearic acid amide, erucic acid amide, ethylene bis-stearic acid amide or paraffin.
Preferably, the resin-based material is a polyester resin or a polyolefin resin. More preferably, the resin-based material is one or more of polyethylene, polypropylene, polymethyl methacrylate, polystyrene, polycarbonate or polyethylene terephthalate.
The emission wavelength of the obtained quantum dot resin material is between 460 and 490 nm.
Has the advantages that:
the invention changes the types of quantum dots, innovatively uses carbon quanta, the carbon quanta have the microscopic size of 2-4nm, and simultaneously can stably keep the fluorescence characteristic of the carbon quanta under the high-temperature environment, thereby greatly improving the yield of products in the processing process
Secondly, the carbon quantum dots are fully dispersed in the resin material by using the dispersing agent, so that the performance reduction caused by agglomeration is reduced.
And thirdly, the carbon quantum dot composite resin material is innovatively used, the mechanical property, the fluorescence property and the flame retardance of the resin material are improved, the application fields of various products are enlarged, and the added value of the product is improved.
And fourthly, the quantum dot resin material can be molded by various methods such as injection molding, film blowing and the like to prepare products. The concentration and the proportion of the carbon quantum dots in the resin base material can be randomly controlled by the quantum dot resin material, and the carbon quantum dot resin material can be customized as required.
Drawings
FIG. 1 is a comparative illustration of fluorescence of a quantum dot resin material in example 1 in a conventional resin;
FIG. 2 is a fluorescence excitation and emission spectrum of the quantum dot resin in example 1;
FIG. 3 is a projection electron micrograph of the carbon synthesized in example 1.
Detailed Description
The technical solutions in the embodiments are clearly and completely described in conjunction with the embodiments of the present invention, and the described embodiments are only some embodiments of the present invention, but not all 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 scope of protection of the present invention.
Example 1:
1. mixing a mixture of 1:1, preparing a solution with the concentration of 1% by citric acid and urea in deionized water, and transferring the prepared solution into a hydrothermal reaction kettle, wherein the liquid level is not more than two thirds of the liquid level of the reaction kettle. Putting the hydrothermal kettle into a high-temperature oven at 200 ℃ for reaction, wherein the reaction duration is 8 hours, finally taking out the hydrothermal kettle, cooling to room temperature, opening the hydrothermal kettle, taking out the quantum dot solution, and drying to obtain quantum dot powder for later use, wherein the optimal emission wavelength of the obtained quantum dot is 460nm as shown in figure 2, and the average particle size of the obtained quantum dot is 2.6nm as shown in figure 3;
2. and (2) mixing stearic acid amide and the carbon quantum dot powder obtained in the step (1) according to the mass ratio of 1:10 to form a component A, and mixing and stirring the component A and polymethyl methacrylate in a high-speed mixer at a mass ratio of 1:100 at a speed of 1200r/min for 3 minutes to form a component B for later use;
3. putting the component B into a double-screw extruder for melting, mixing and granulating, wherein the melt temperature of the double-screw extruder is set to 210 ℃, the screw rotating speed is set to 25r/min, the feeding speed is 12r/min, bracing and cooling are carried out in a water cooling mode after extrusion, and the setting of the granulating speed and the screw rotating speed are kept in parallel and are kept continuously to obtain the flame-retardant fluorescent quantum dot polymethyl methacrylate resin with high strength as shown in figure 1;
example 2:
1. mixing a mixture of 1: 0.9 of citric acid and urea are prepared into a solution with the concentration of 1% in deionized water, and the prepared solution is transferred into a hydrothermal reaction kettle, wherein the liquid level is not more than two thirds of the liquid level of the reaction kettle. Putting the hydrothermal kettle into a high-temperature oven at 180 ℃ for reaction, wherein the reaction duration is 6 hours, finally taking out the hydrothermal kettle, cooling to room temperature, opening the hydrothermal kettle, taking out the quantum dot solution, and drying to obtain quantum dot powder with the average particle size of 3nm for later use;
2. mixing erucamide and the carbon quantum dot powder obtained in the step 1 according to the mass ratio of 1: mixing the component A and polyethylene according to the mass ratio of 1:80 for 3 minutes in a high-speed mixer at the speed of 1200r/min to form a component B for standby;
3. putting the component B into a double-screw extruder for melting, mixing and granulating, wherein the melt temperature of the double-screw extruder is set to 180 ℃, the screw rotating speed is set to 20r/min, the feeding speed is 13r/min, bracing and cooling are carried out in a water cooling mode after extrusion, and the grain cutting speed is set to be parallel to the screw rotating speed and is kept continuously to obtain the flame-retardant fluorescent quantum dot polyethylene particles with high strength;
example 3:
1. mixing a mixture of 1: 0.8 of citric acid and urea are prepared into a solution with the concentration of 1% in deionized water, and the prepared solution is transferred into a hydrothermal reaction kettle, wherein the liquid level is not more than two thirds of the liquid level of the reaction kettle. Putting the hydrothermal kettle into a high-temperature oven at 200 ℃ for reaction, wherein the reaction duration is 9 hours, finally taking out the hydrothermal kettle, cooling to room temperature, opening the hydrothermal kettle, taking out the quantum dot solution, and drying to obtain quantum dot powder with the average particle size of 2.5nm for later use;
2. and (2) mixing ethylene bis stearamide and the carbon quantum dot powder obtained in the step (1) according to the mass ratio of 1:30 to form a component A, and mixing and stirring the component A and polypropylene in a high-speed mixer at a speed of 1000r/min for 3 minutes according to the mass ratio of 1:60 to form a component B for later use;
3. putting the component B into a double-screw extruder for melting, mixing and granulating, wherein the melt temperature of the double-screw extruder is set to 190 ℃, the screw rotating speed is set to 28r/min, the feeding speed is 15r/min, bracing and cooling are carried out in a water cooling mode after extrusion, and the granulation speed is set to be parallel to the screw rotating speed and is maintained to be continuous, so that the flame-retardant fluorescent quantum dot polyethylene particles with high strength are obtained;
example 4:
1. mixing a mixture of 1: 0.7 of citric acid and urea are prepared into a solution with the concentration of 1% in deionized water, and the prepared solution is transferred into a hydrothermal reaction kettle, wherein the liquid level is not more than two thirds of the liquid level of the reaction kettle. Putting the hydrothermal kettle into a high-temperature oven at 200 ℃ for reaction, wherein the reaction duration is 10 hours, finally taking out the hydrothermal kettle, cooling to room temperature, opening the hydrothermal kettle, taking out the quantum dot solution, and drying to obtain quantum dot powder with the average particle size of 2.8nm for later use;
2. and (3) mixing paraffin and the carbon quantum dot powder obtained in the step (1) according to a mass ratio of 1:10 to form a component A, and mixing and stirring the component A and polystyrene in a high-speed mixer at a speed of 1400r/min for 3 minutes to form a component B for later use according to the mass ratio of 1: 40;
3. putting the component B into a double-screw extruder for melting, mixing and granulating, wherein the melt temperature of the double-screw extruder is set to 280 ℃, the screw rotating speed is set to 22r/min, the feeding speed is 15r/min, bracing and cooling are carried out in a water cooling mode after extrusion, and the granulation speed is set to be parallel to the screw rotating speed and maintain continuous strip, so that the flame-retardant fluorescent quantum dot polystyrene particles with high strength are obtained;
example 5:
1. mixing a mixture of 1: 0.6 of citric acid and urea are prepared into a solution with the concentration of 1% in deionized water, and the prepared solution is transferred into a hydrothermal reaction kettle, wherein the liquid level is not more than two thirds of the liquid level of the reaction kettle. Putting the hydrothermal kettle into a high-temperature oven at 200 ℃ for reaction, wherein the reaction duration is 7 hours, finally taking out the hydrothermal kettle, cooling to room temperature, opening the hydrothermal kettle, taking out the quantum dot solution, and drying to obtain quantum dot powder with the average particle size of 2.6nm for later use;
2. and (2) mixing ethylene bis stearamide and the carbon quantum dot powder obtained in the step (1) according to the mass ratio of 1: 20 to form a component A, and mixing and stirring the component A and polycarbonate in a high-speed mixer at a speed of 1200r/min for 3 minutes to form a component B for later use according to the mass ratio of 1: 30;
3. putting the component B into a double-screw extruder for melting, mixing and granulating, wherein the melt temperature of the double-screw extruder is set to 250 ℃, the screw rotating speed is set to 21r/min, the feeding speed is 10r/min, bracing and cooling are carried out in a water cooling mode after extrusion, and the granulation speed is set to be parallel to the screw rotating speed and maintain continuous strip, so that the flame-retardant fluorescent quantum dot polycarbonate particles with high strength are obtained;
example 6:
1. mixing a mixture of 1: 0.5 of citric acid and urea are prepared into a solution with the concentration of 2% in deionized water, and the prepared solution is transferred into a hydrothermal reaction kettle, wherein the liquid level is not more than two thirds of the liquid level of the reaction kettle. Putting the hydrothermal kettle into a high-temperature oven at 200 ℃ for reaction, wherein the reaction duration is 6 hours, finally taking out the hydrothermal kettle, cooling to room temperature, opening the hydrothermal kettle, taking out the quantum dot solution, and drying to obtain quantum dot powder with the average particle size of 2.6nm for later use;
2. and (2) mixing ethylene bis stearamide and the carbon quantum dot powder obtained in the step (1) according to the mass ratio of 1:10 to form a component A, and mixing and stirring the component A and polyethylene glycol terephthalate in a high-speed mixer at a speed of 1400r/min for 4 minutes according to the mass ratio of 1:10 to form a component B for later use;
3. putting the component B into a double-screw extruder for melting, mixing and granulating, wherein the melt temperature of the double-screw extruder is set to 220 ℃, the screw rotating speed is set to 23r/min, the feeding speed is 11r/min, bracing and cooling are carried out in a water cooling mode after extrusion, and the granulation speed is set to be parallel to the screw rotating speed and maintain continuous strip, so that the flame-retardant fluorescent quantum dot polyethylene terephthalate particles with high strength are obtained;
Claims (8)
1. a preparation method of a quantum dot resin material comprises the following specific steps:
the method comprises the following steps: preparing quantum dot powder; dissolving citric acid and urea serving as raw materials in deionized water to prepare a solution, transferring the solution into a hydrothermal kettle, putting the hydrothermal kettle into a high-temperature oven for reaction, taking out the hydrothermal reaction kettle after the reaction is finished, opening the hydrothermal reaction kettle after the hydrothermal reaction kettle is cooled, taking out a quantum dot solution, and drying the quantum dot solution to obtain quantum dot powder;
step two: compounding ingredients; dispersing agent and quantum dot powder according to the mass ratio of 1: (10-50) and mixing to form a component A; and (2) mixing the component A and a resin material according to the mass ratio of 1: (10-100) mixing and stirring in a high-speed mixer to form a composite ingredient;
step three: extruding and granulating; and extruding and granulating the composite ingredients at high temperature through a double screw to form the quantum dot resin material.
2. The method of claim 1, wherein the molar ratio of citric acid to urea in step one is 1: (0.5-1) preparing the solution with the mass concentration of 1-2%; the temperature of the high-temperature oven is 180 ℃ and 200 ℃, and the reaction time is 6-10 hours.
3. The method as claimed in claim 1, wherein the rotation speed of the high-speed mixer in step two is 1000-1400r/min, and the mixing time is 2-4 minutes.
4. The process according to claim 1, wherein the parameters of the twin-screw extruder in step three are: the melt temperature is set to be 170-280 ℃, the screw rotating speed is set to be 20-28r/min, and the feeding speed is 10-15 r/min.
5. The method of claim 1, wherein the dispersant is one or more of stearic acid amide, erucic acid amide, ethylene bis stearic acid amide, and paraffin wax.
6. The method according to claim 1, wherein the resin-based material is a polyester resin or a polyolefin resin.
7. The method according to claim 1, wherein the resin-based material is one or more of polyethylene, polypropylene, polymethyl methacrylate, polystyrene, polycarbonate, and polyethylene terephthalate.
8. The method according to claim 1, wherein the emission wavelength of the obtained quantum dot resin material is between 460 and 490 nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115651291A (en) * | 2022-07-13 | 2023-01-31 | 北京化工大学 | In-situ growth multicolor fluorescent carbon dot resin material and preparation method and application thereof |
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