阅读说明：本技术 一种qd色母粒及其制备方法 (QD color master batch and preparation method thereof ) 是由 王晓 谢婷 张子宾 于 2021-02-03 设计创作，主要内容包括：本发明提供了一种QD色母粒,由以下重量份的组分制备而成：塑胶粒子97.6～99.1份,QD-PMMA粉末0.5～2份,光稳定剂0.4份,抗氧化剂5～10份；所述塑胶粒子为PS、PC、COC或者PMMA中的任意一种。本发明还提供了一种QD色母粒的制备方法,包括以下步骤：S1、根据所需配置的QD色母粒称取塑胶粒子、QD-PMMA粉末、光稳定剂和抗氧化剂；S2、将称取好的塑胶粒子、QD-PMMA粉末、光稳定剂和抗氧化剂,置入搅拌装置中混合均匀；S3、将S2中混合均匀的原料置入双螺杆挤出机挤出造粒机制造成特定形状；S4、将S3中挤出的湿润塑料圆条冷却,通过干燥设备充分干燥后切粒得到产品。本发明制备的一种QD色母粒纯正的高品质色彩,更广色域显示,精准的色彩控制,更长寿,更节能。(The invention provides a QD color master batch which is prepared from the following components in parts by weight: 97.6-99.1 parts of plastic particles, 0.5-2 parts of QD-PMMA powder, 0.4 part of light stabilizer and 5-10 parts of antioxidant; the plastic particle is any one of PS, PC, COC or PMMA. The invention also provides a preparation method of the QD color master batch, which comprises the following steps: s1, weighing plastic particles, QD-PMMA powder, a light stabilizer and an antioxidant according to the QD color master batch required to be prepared; s2, placing the weighed plastic particles, QD-PMMA powder, light stabilizer and antioxidant into a stirring device for uniformly mixing; s3, putting the uniformly mixed raw materials in the S2 into a double-screw extruder, extruding and granulating to manufacture into a specific shape; and S4, cooling the wet plastic round strip extruded in the step S3, fully drying the round strip by drying equipment, and then cutting into granules to obtain the product. The QD color master batch prepared by the invention has pure high-quality color, wider color gamut display, accurate color control, longer service life and more energy conservation.)

1. The QD color master batch is characterized by being prepared from the following components in parts by weight: 97.6-99.1 parts of plastic particles, 0.5-2 parts of QD-PMMA powder, 0.4 part of light stabilizer and 5-10 parts of antioxidant; the plastic particle is any one of PS, PC, COC or PMMA.

2. The QD color masterbatch of claim 1, wherein the QD-PMMA powder is a green QD-PMMA powder, the green QD-PMMA powder comprises 20% QD by weight, and the emission spectrum of the green QD-PMMA is at a wavelength of 533 ± 2 nm.

3. The QD color masterbatch of claim 1, wherein the QD-PMMA powder is red QD-PMMA powder, the weight percentage of QDs in the red QD-PMMA powder is 20%, and the emission spectrum of the red QD-PMMA is at 626 ± 2 nm.

4. The QD color master batch preparation method according to any one of claims 1 to 3, comprising the following steps:

s1, weighing the required plastic particles, QD-PMMA powder, light stabilizer and antioxidant according to the mass of the color master batch required to be prepared;

s2, placing the weighed plastic particles, QD-PMMA powder, light stabilizer and antioxidant into a stirring device for uniformly mixing;

s3, putting the uniformly mixed raw materials in the S2 into a double-screw extruder, extruding and granulating to manufacture into a specific shape;

and S4, cooling the wet plastic round strip extruded in the S3, fully drying the round strip by drying equipment, and then cutting the round strip into particles to obtain the color master batch particles.

5. The QD masterbatch preparation method of claim 4, wherein the rotation speed of the main machine of the stirring device in S2 is 250rpm/min, the mixing time of the raw materials is 20-45 minutes, and the temperatures of the extruder zones are: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 200 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 210 ℃ and the temperature of the die head is 210 ℃.

6. The QD color master batch preparation method according to claim 4, wherein a mini-type twin-screw extrusion granulator is selected from S3, the extrusion molding temperature is 230-240 ℃, and the feeding speed is 15 rpm/min.

7. The QD masterbatch preparation method of claim 6, wherein the S3 is fed under semi-starvation condition.

8. The QD color master batch preparation method according to claim 4, wherein the drying equipment in the S4 has a temperature of 50-70 ℃ and a drying time of 1-2 hours.

9. The QD color master batch preparation method according to claim 4, wherein the cooling temperature of the plastic raw material is 0-10 ℃ during the cutting in the S4 process.

Technical Field

The invention relates to the field of plastic plates used in the industries of TV backlight modules and display devices, in particular to QD color master batch and a preparation method thereof.

Background

In the prior art, both a TV backlight module and a display device are made of materials such as acrylic (PMMA for short in the present invention), polycarbonate (PC for short in the present invention), polystyrene (PS for short in the present invention), and the like, and the materials have optical characteristics of a plastic plate such as a certain haze, a certain light transmittance, a certain refractive index, and the like, or RG fluorescent powder is coated or printed or sprayed on the plastic plate to realize a color gamut and energy consumption higher than those in the prior art. However, with the improvement of living standard of people, the color quality is not high, the color gamut display is not wide enough, the color is not easy to control, the service life is short, the energy is not saved enough, and the existing plastic plate and the technology containing RG fluorescent powder can not meet the requirements of people. Therefore, the problem of raw materials of plastic plates is urgently needed to be solved, so that people can pursue pure high-quality colors, display in a wider color gamut, control colors accurately, prolong the service life and save more energy.

Disclosure of Invention

The invention aims to provide a QD color master batch and a preparation method thereof aiming at overcoming the defects of the prior art. The invention is manufactured into the plastic plate raw material through the unique nanometer characteristic of the QD material, and meets the requirements of high-quality color, wider color gamut display, accurate color control, longer service life and more energy conservation of TV backlight modules and display devices.

The technical scheme of the invention is realized as follows:

the QD color master batch is prepared from the following components in parts by weight: 97.6-99.8 parts of plastic particles, 0.5-2 parts of QD-PMMA powder, 0.4 part of light stabilizer and 5-10 parts of antioxidant.

Preferably, the plastic particle is any one of PS, PC, COC (cyclic olefin copolymer, herein abbreviated as COC), or PMMA.

Preferably, the QD-PMMA powder is green QD-PMMA powder, the weight percentage of QDs in the green QD-PMMA powder is 20%, and the emission spectrum of the green QD-PMMA powder is at a wavelength of 533 ± 2 nm. More preferably, the weight part of the green QD-PMMA powder is 2 parts.

Preferably, the QD-PMMA powder is red QD-PMMA powder, the weight percentage of QDs in the red QD-PMMA powder is 20%, and the emission spectrum of the red QD-PMMA powder is at the wavelength of 626 ± 2 nm. More preferably, the weight part of the red QD-PMMA powder is 0.5 part.

Preferably, the light stabilizer is the ultraviolet light absorber RIASTRB UV-326.

Preferably, the antioxidant is antioxidant 0810, comprising a phosphite triester.

Based on the same inventive concept, the invention also provides a preparation method of the QD color master batch, which comprises the following steps:

s1, weighing the required plastic particles, QD-PMMA powder, light stabilizer and antioxidant according to the mass of the color master batch required to be prepared;

s2, placing the weighed plastic particles, QD-PMMA powder, light stabilizer and antioxidant into a stirring device for uniformly mixing;

s3, putting the uniformly mixed raw materials in the S2 into a double-screw extruder, extruding and granulating to manufacture into a specific shape;

and S4, cooling the wet plastic round strip extruded in the S3, fully drying the round strip by drying equipment, and then cutting the round strip into particles to obtain the color master batch particles.

Preferably, the rotation speed of the main machine of the stirring device in the step S2 is 250rpm/min, the mixing time of the raw materials is 20-45 minutes, and the temperature of each zone of the extruder is as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 200 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 210 ℃ and the temperature of the die head is 210 ℃.

Preferably, a small-sized twin-screw extrusion granulator is selected in the S3, the cavity between a main screw and the inner wall of the barrel is small, the heat transfer and dissipation efficiency is high, and the material dispersion is good; the extrusion molding temperature is 230-240 ℃, the feeding speed is 15rpm/min, and semi-starvation feeding is adopted;

preferably, the temperature of the drying equipment in the S4 is 50-70 ℃, and the drying time is 1-2 hours.

Preferably, when the plastic raw material is cut into pellets in S4, the cooling temperature of the plastic raw material is 0-10 ℃.

The invention has the beneficial effects that:

the QD color master batch utilizes the nanometer characteristic of QD-PMMA, and a plastic plate formed by combining the green master batch and the red master batch according to a certain proportion can be extruded, cut, formed and assembled on a corresponding TV backlight module and a display device after a certain time. By adopting a Photoluminescence (PL) principle and being excited by high-energy blue light, the QD color master batch extrusion molding plate just forms an RGB primary color light source, so that the color gamut coverage of a display picture is wider, the color control is more accurate, and the energy is saved. The wavelength of the pure blue, green and red colors of the plate subjected to the blue laser is longer, the purity is higher and the half-peak width is reduced by using an integrating sphere to test the plate. In a CIE 1936 chromatogram, xy coordinates of various chromaticity are respectively tested on high-energy blue light, red light and green light by using a green master batch and a red master batch, and a surrounded triangular area sRGB (red green blue green blue green blue green blue green blue green blue green. Furthermore, the existing common TV color gamut is 72% NTSC, the TV color gamut containing RG fluorescent powder is 85-90% NTSC, and the TV color gamut using QD color master batch in the invention is 110% NTSC; the more the coordinate of the three primary colors of RGB is, the higher the saturation is, but the relative brightness is lost, and the integral brightness is improved by adjusting the transmittance of the PS, PC, COC or PMMA plate.

Drawings

FIG. 1 is a comparison of emission spectra of an extrusion molded plastic panel of a TV containing a QD color master batch according to the present invention and a conventional TV;

fig. 2 is a comparison of color gamut diagrams in CIE 1936 for a TV containing QD color masterbatch according to the present invention and a conventional TV, extrusion molded plastic sheet.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the contents 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.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.

Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.

The QD color master batch is prepared from the following components in parts by weight: 97.6-99.1 parts of plastic particles, 0.5-2 parts of QD-PMMA powder, 0.4 part of light stabilizer and 5-10 parts of antioxidant.

Preferably, the plastic particle is any one of PS, PC, COC, or PMMA.

The QD color master batch is commonly known as Quantum dot (QD for short in the present invention) particles, and is a raw material for storing, transporting and processing plastic plates in a semi-finished product form. QD is a novel nano material, the grain diameter of the QD is between 2 and 10 nanometers, the QD can emit concentrated spectrum after excitation, the main optical properties comprise a wide absorption peak, a narrow emission peak, fluorescence efficiency and adjustable emission wavelength, after the QD is stimulated by light or electricity, quantum dot materials of different materials and different sizes can emit specific light, and the corresponding color is more bright. By utilizing the principle of three primary colors, white light is obtained by combining three basic colors of red, green and blue according to different proportions.

The quantum dots are superior to the fluorescent powder mainly because the quantum dots are nanoscale, most of the fluorescent powder is micron-sized, and the nanoscale in the prior art is only limited to laboratory research; the second is that the quantum dot is semiconductor material, its luminescence is produced by interband transition, RG phosphor powder is luminescent after doping ion in a kind of substrate; thirdly, quantum dots are used in the TV backlight module and the display device to manufacture plastic plates, the color gamut of 110% NTSC, and RG fluorescent powder is used to manufacture the plastic plates, and the color gamut of 85-90% NTSC can only be achieved; and fourthly, under the same color gamut, the quantum dots save 50% of energy consumption compared with RG fluorescent powder.

In the invention, PS, PC, COC or PMMA are respectively transparent plastics and are selected according to different functions to be used as main bodies made of master batches with various colors. For example, PMMA is the best in light transmittance and surface hardness, PC is the best in temperature resistance, and PC is the strongest in impact strength. The quantum dots are oxidized and damp in the air and at high temperature, water and oxygen are blocked, and the QD pure powder is wrapped by PMMA powder to avoid QD oxidation performance efficiency. The QD nano-scale crystal is ground into QD pure powder and is mixed with PMMA powder according to a certain proportion, and the PMMA powder is selected for wrapping, so that the QD nano-scale crystal has the advantages that: compared with other carriers such as PS, COC, PC and the like, PMMA has the advantages that the water absorption rate is low by about 0.04%, the energy efficiency of QD can be protected, the cost is low, and the method belongs to the optimal selection. The auxiliary agent has the effects of preferentially reacting with oxygen in granulation at high temperature, avoiding QD oxidation to reduce performance efficiency, and ensuring optical property light transmittance and haze stability of the manufactured product to be consistent.

Preferably, the QD-PMMA powder is green QD-PMMA powder, the weight percentage of QDs in the green QD-PMMA powder is 20%, and the emission spectrum of the green QD-PMMA powder is at a wavelength of 533 ± 2 nm.

More preferably, the weight part of the green QD-PMMA powder is 2 parts. For example, the mass percent of QD in the taken QD-PMMA powder is 20%, the content of QD needs to be further granulated and diluted, and 2 parts of green QD-PMMA powder is added in the manufacturing process, so that the mass percent of QD in the final product is less than 0.4%, a color master batch with the mass percent of less than 1% is formed, and the product with high uniformity is easy to manufacture.

Preferably, the QD-PMMA powder is red QD-PMMA powder, the weight percentage of QDs in the red QD-PMMA powder is 20%, and the emission spectrum of the red QD-PMMA powder is at the wavelength of 626 ± 2 nm.

More preferably, the weight part of the red QD-PMMA powder is 0.5 part. For example, the mass percent of QD in the taken QD-PMMA powder is 20%, the content of QD needs to be further granulated and diluted, and 0.5 part of red QD-PMMA powder is added in the manufacturing process, so that the mass percent of QD in the final product is less than 0.1%, and a color master batch with the mass percent of less than 1% is formed, and a product with high uniformity is easy to manufacture.

Preferably, the antioxidant is antioxidant 0810, comprising a phosphite triester.

Preferably, the light stabilizer is the ultraviolet light absorber RIASTRB UV-326.

Based on the same inventive concept, the invention also provides a preparation method of the QD color master batch, which comprises the following steps:

s1, weighing the required plastic particles, QD-PMMA powder, light stabilizer and antioxidant according to the mass of the color master batch required to be prepared;

s2, placing the weighed plastic particles, QD-PMMA powder, light stabilizer and antioxidant into a stirring device for uniformly mixing;

s3, putting the uniformly mixed raw materials in the S2 into a double-screw extruder, extruding and granulating to manufacture into a specific shape;

and S4, cooling the wet plastic round strip extruded in the S3, fully drying the round strip by drying equipment, and then cutting the round strip into particles to obtain the color master batch particles.

Preferably, the rotation speed of a main machine of the stirring device in S2 is 250rpm/min, the mixing time of the raw materials is 20-45 minutes, and the temperature of each zone of the extruder is as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 200 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 210 ℃ and the temperature of the die head is 210 ℃. The temperature that sets up each district's section is different, and the purpose is also in order to guarantee that the QD reduces the decay of performance efficiency under high temperature, and is high at the temperature of die head for melt in the short time, evenly stir, then through the cooling of different district, make the better shaping of product.

Preferably, a small-sized twin-screw extrusion granulator is selected in S3, the cavity between a main screw and the inner wall of the barrel is small, the heat transfer and dissipation efficiency is high, the material dispersion is good, the diameter of the screw is preferably 25-40 cm, and the production energy is 20-60 kg/h; the extrusion molding temperature is 230-240 ℃, the feeding speed is 15rpm/min, semi-starvation feeding is adopted, and the mixed materials are stirred more uniformly; in the invention, the semi-starvation feeding means that the capacity of raw material supply is approximately equal to the theoretical capacity of an extruder, and if the raw material is fed in a satiating way, the produced product is provided with wire drawing, black spots and bubbles; the granulator table must have vacuum or nitrogen gas filling conditions to cut off oxygen and ensure the performance efficiency of QD.

Preferably, the temperature of the drying equipment in the step S4 is 50-70 ℃, the drying time is 1-2 hours, and under the condition, the extruded sheet is molded better.

Preferably, when the plastic raw material is cut into pellets in S4, the cooling temperature of the plastic raw material is 0-10 ℃, under the condition, according to the characteristics of QD, when the plastic raw material is extruded and molded again, the plastic raw material is softer at the temperature higher than 10 ℃, the plastic raw material is difficult to mold and cut, and the plastic raw material is cooled to the temperature of 10 ℃ or below for better molding.

For further understanding of the present application, the QD color masterbatch and the preparation method thereof provided by the present invention are specifically described below with reference to examples.

Example 1

The QD color master batch is prepared from the following components in parts by weight: 97.6 parts of PS plastic particles, 2 parts of green QD-PMMA powder, 2 parts of an ultraviolet absorber RIASORB UV-3260.4 parts and 08105 parts of an antioxidant. In this example, the green QD-PMMA powder contains 20 wt% QDs, and the emission spectrum of the green QD-PMMA powder is at a wavelength of 533 ± 2 nm.

The preparation method of the QD color master batch of this embodiment specifically includes the following steps:

s1, weighing 97.6 parts of PS plastic particles, 2 parts of green QD-PMMA powder, 2 parts of an ultraviolet absorber RIASTRB UV-3260.4 parts and 08105 parts of an antioxidant according to the color master batch required to be prepared;

s2, placing the weighed green QD-PMMA powder, PS particles, ultraviolet absorbent RIASTRB UV-326 and antioxidant 0810 into a stirring device, uniformly mixing, wherein the rotating speed of a main machine of the stirring device is 250rpm/min, the mixing time of raw materials is 20 minutes, and the temperature of each area of an extruder is as follows: the temperature of a first area is 170 ℃, the temperature of a second area is 180 ℃, the temperature of a third area is 190 ℃, the temperature of a fourth area is 200 ℃, the temperature of a fifth area is 210 ℃, the temperature of a sixth area is 220 ℃, the temperature of a seventh area is 210 ℃ and the temperature of a die head is 210 ℃;

s3, putting the uniformly mixed raw materials in the step S2 into a double-screw extruder extrusion granulator to be manufactured into a specific shape, and selecting a small-sized double-screw extrusion granulator with the diameter of a screw being 25 cm; the extrusion molding temperature is 230 ℃, the feeding speed is 15rpm/min, and semi-starvation feeding is adopted;

s4, cooling the wet plastic round strip extruded in the S3, fully drying the round strip by drying equipment, and then cutting the round strip into granules to obtain plastic granules, wherein the temperature of the used drying equipment is 50 ℃, and the drying time is 1.5 hours; and (3) during grain cutting, cooling the plastic raw material to 10 ℃, and cutting grains to obtain green color master batch particles.

Example 2:

the QD color master batch comprises, by weight, 99.1 parts of plastic particles PS, 0.5 part of red QD-PMMA powder, 0.78 part of an ultraviolet absorber RIASTRB UV-3260.4 part and 081010 part of an antioxidant. In this example, the percentage by weight of QDs in the red QD-PMMA powder was 20%, and the emission spectrum of the red QD-PMMA was at a wavelength of 626 ± 2 nm.

The preparation method of the QD color master batch of this embodiment specifically includes the following steps:

s1, weighing 99.1 parts of PS plastic particles, 0.5 part of red QD-PMMA powder, RIASORB UV-3260.4 parts of an ultraviolet absorber and 081010 parts of an antioxidant according to the color master batch required to be prepared;

s2, putting the weighed green QD-PMMA powder, PS particles, ultraviolet absorbent RIASTRB UV-326 and antioxidant 0810 into a stirring device, uniformly mixing, wherein the rotating speed of a main machine of the stirring device is 250rpm/min, the mixing time of raw materials is 45 minutes, and the temperature of each zone of an extruder is as follows: the temperature of a first area is 170 ℃, the temperature of a second area is 180 ℃, the temperature of a third area is 190 ℃, the temperature of a fourth area is 200 ℃, the temperature of a fifth area is 210 ℃, the temperature of a sixth area is 220 ℃, the temperature of a seventh area is 210 ℃ and the temperature of a die head is 210 ℃;

s3, putting the uniformly mixed raw materials in the S2 into a double-screw extruder extrusion granulator to manufacture into a specific shape, wherein a small-sized double-screw extrusion granulator is selected from the S3, and the diameter of a screw is 40 cm; the extrusion molding temperature is 240 ℃, the feeding speed is 15rpm/min, and semi-starvation feeding is adopted;

s4, cooling the wet plastic round strip extruded in the S3, fully drying the round strip by drying equipment, and then cutting the round strip into granules to obtain plastic granules, wherein the temperature of the drying equipment is 70 ℃, and the drying time is 2 hours; and when the red color master batch is cut into particles, the cooling temperature of the plastic raw material is 2 ℃, and the red color master batch particles are obtained by cutting into particles.

Then, after the green color master batch of example 1 and the red color master batch of example 2 are mixed, the mass ratio of the red color master batch to the green color master batch in the plastic sheet for extrusion molding is 6: 4. The test results of the prepared panels are shown in fig. 1 and 2. The efficiency of the green quantum dots decays faster than that of the red quantum dots at high temperatures.

FIG. 1 is a comparison of emission spectra of a QD-containing color masterbatch extrusion molded panel of the present invention and a conventional TV panel; as can be seen from fig. 1, the quantum dot color master batch plastic sheet with better performance is successfully prepared by the present invention, and compared with the sheet in the conventional TV, the QD-containing plastic sheet can be better. The wavelength of the pure blue, green and red colors tested by the integrating sphere is longer, the purity is higher, the half-peak width is reduced, and the color is more bright.

Fig. 2 is a comparison of color gamut diagrams in CIE 1936 between a QD color masterbatch extrusion molded plate provided by the present invention and a plate of a conventional TV. In a CIE 1936 chromatogram, a green master batch and a red master batch are respectively used for testing xy coordinates of various chromaticity under high-energy blue light, red light and green light, and a just surrounded triangular area sRGB (red Red Green blue), the area of sRGB formed by the QD-containing master batches is larger than that of sRGB of a traditional TV, the larger the area formed by the sRGB is, the more colors can be displayed, the higher the color gamut NTSC is, and the wider the relative color gamut is, and the purer the color is.

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.