CN108752629B - Preparation method of light scattering particles - Google Patents
Preparation method of light scattering particles Download PDFInfo
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- CN108752629B CN108752629B CN201810573456.5A CN201810573456A CN108752629B CN 108752629 B CN108752629 B CN 108752629B CN 201810573456 A CN201810573456 A CN 201810573456A CN 108752629 B CN108752629 B CN 108752629B
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- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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Abstract
The invention belongs to the technical field of light scattering materials, and particularly relates to a preparation method of light scattering particles, which comprises the steps of adding an acidic solution into a mixture of quartz powder and mica powder, uniformly mixing, adding the mixture into an ejector for accelerating treatment, drying, and irradiating by laser beams to obtain the light scattering particles; the invention forms micropore defects on the surface of the quartz powder by accelerating the jet device, and mica powder is stripped and embedded in micropores on the surface of the quartz powder; and after laser beam irradiation, the mica is welded on the surface of the quartz powder, and the obtained light scattering particles have excellent light scattering effect.
Description
Technical Field
The invention belongs to the technical field of light scattering materials, and particularly relates to a preparation method of light scattering particles.
Background
Scattering of light refers to a phenomenon in which a part of light propagates in a direction away from the original direction when the light passes through an inhomogeneous medium, and light in the direction away from the original direction is referred to as scattered light. Light scattering is widely used, and in order to obtain a uniform surface light source, a point light source or a line light source is diffused into a surface light source by adding particles having light scattering ability to a plastic plate. However, the light scattering particles in the prior art have a limited light scattering ability, and people have to select light scattering particles with different particle sizes to meet the requirement of uniform light.
Disclosure of Invention
The invention aims to provide a preparation method of light scattering particles, and the prepared light scattering particles have excellent light scattering capacity.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of light scattering particles comprises the steps of adding an acidic solution into a mixture of quartz powder and mica powder, uniformly mixing, adding into an ejector for accelerating treatment, drying, and irradiating by laser beams to obtain the light scattering particles.
In the invention, the jet device is accelerated to form micropore defects on the surface of the quartz powder, and meanwhile, the mica powder is stripped and embedded in micropores on the surface of the quartz powder; and after laser beam irradiation, the mica is welded on the surface of the quartz powder, and the light scattering particles with excellent light scattering effect are obtained.
Further, in the invention, the quartz powder is subjected to ball milling treatment to enable the particle size to be 3-8 μm; the particle size of the mica powder is 0.2-0.5 mu m.
According to the invention, the mass ratio of the quartz powder to the mica powder can be selected in a wide range, but in order to ensure that the surface of the quartz powder can be inserted and welded to the mica powder, namely to ensure that the prepared light scattering particles have excellent light scattering effect, the mass ratio of the quartz powder to the mica powder is 1:
(0.3～1)。
in the invention, the laser beam is generated by an ytterbium-doped fiber laser source, and the power of the laser beam is 0.1-25 Kw.
The invention also provides an application of the light scattering particles, wherein the light scattering particles are added into the surface layer of the reflecting film, and further, the reflecting film comprises a core layer and surface layers arranged on one side or two sides of the core layer, and the surface layers comprise the following components: 80-90 parts of polyester resin, 5-15 parts of light scattering particles and 5-8 parts of antistatic agent;
the light scattering particles are filled in the surface layer of the reflecting film, so that the light scattering effect of the reflecting film is realized, the diffuse reflection capability of the reflecting film is improved, the excellent light uniformizing capability in a short OD model is ensured, and the phenomena of light shadows and peripheral shadows are prevented.
The reflecting film provided by the invention is composed of the core layer and the surface layer, wherein the thickness ratio of the core layer to the surface layer has larger influence on the light reflecting capacity of the core layer and the light homogenizing capacity of the surface layer; when the thickness of the core layer is too small, the luminance of the reflective film is deteriorated. Preferably, in the present invention, the ratio of the thicknesses of the core layer and the skin layer is 1: (0.04-0.125).
In the present invention, the polyester resin is one selected from polyesters formed from a dicarboxylic acid component and a diol component. Further, dicarboxylic acid components such as terephthalic acid, isophthalic acid, 2, 6-naphthalenedicarboxylic acid, 4' -biphenyldicarboxylic acid, adipic acid and sebacic acid are exemplified. Examples of the diol component include ethylene glycol, 1, 4-butanediol, 1, 4-cyclohexanedimethanol, and 1, 6-hexanediol. Further, the polyester resin is preferably an aromatic polyester. Further, the polyester resin is preferably one of polyethylene terephthalate (PET), polybutylene terephthalate (PBT) and polyethylene naphthalate (PEN).
The antistatic agent has the effects of reducing the electrostatic adsorption effect on the surface of the reflecting film and reducing the charge accumulation on the surface of the reflecting film, so that the adsorption problem of the reflecting film in the cutting, assembling and using processes is avoided, and the quality of the reflecting film is improved.
In the invention, the acid solution is used for removing impurities contained in the quartz powder and ensuring the cleanness of the quartz powder, the acid solution can be one of hydrochloric acid, dilute sulfuric acid, formic acid or acetic acid, and the concentration of the acid solution is 1-5 mol/L.
In the invention, the ejector consists of a nozzle, a suction chamber and a diffuser pipe, and in the prior art, the ejector is widely applied to the technical field of water treatment, such as ozone dissolving and chlorine dioxide sterilization, oxygenation and iron removal and the like; the specific working principle of the ejector is that under the high-speed rotation of the pump impeller, liquid is sprayed out from the nozzle at a high speed, when the liquid flowing at a high speed passes through the air mixing chamber, vacuum is formed in the air mixing chamber, a large amount of air is sucked by the air duct, after the air enters the air mixing chamber, the air and the liquid are mixed violently at the throat to form an air-liquid mixture, the air-liquid mixture is discharged by the diffuser pipe, the air rises in fine bubbles in a water body, and efficient substance transfer is formed in the whole process. According to the invention, the vacuum condition formed by the high-speed flow is utilized, so that the quartz powder and the mica powder are cut mutually, the micropore defects are formed on the surface of the quartz powder, the mica powder is further stripped and inserted into the micropore defects on the surface of the quartz powder, and then the quartz powder particles loaded with the mica powder are obtained by drying. Specifically, the quartz powder particles loaded with the mica powder are dried in a vacuum drying oven at the temperature of 40-50 ℃ and the vacuum degree of 0.3-0.45 Mpa.
In the invention, the mica powder is a silicate with a layered structure, the structure is a compound silicon-oxygen layer formed by two silicon-oxygen tetrahedrons and one aluminum-oxygen octahedron, and the mica powder can be peeled to 0.001 mu m theoretically when the peeling condition allows. The light diffusion layer is formed by stripping and inserted on the quartz powder, and the diffusion effect is formed at the interface of the quartz powder and the mica powder, so that the excellent light diffusion effect is achieved.
The quartz powder is a hard, wear-resistant and chemically stable silicate mineral called silicon micropowder, and the main component of the quartz powder is SiO2According to the invention, the quartz powder is filled in the surface layer of the reflecting film, so that the light is diffused, and the technical effect of diffuse reflection is achieved; secondly, the filling of the quartz powder can also replace the opening agent in the prior art, actually, in the prior art, an anti-blocking agent for improving the opening performance of the film needs to be added on the surface layer in the preparation process of the optical reflecting film, and the anti-blocking effect can also be achieved by adding the light scattering particles, namely, the addition of the opening agent is omitted by adding the light scattering particles, so that not only is the storage bin saved, but also the cost is effectively reduced.
In the invention, in order to further improve the insertion firmness degree of the mica powder on the surface of the quartz powder, the mica powder is welded on the surface of the quartz powder by a laser beam irradiation method.
In the invention, the core layer of the reflecting film mainly plays a role in reflecting light, and further, the core layer adopts the technical scheme that resin incompatible with polyester resin is added into the polyester resin in the prior art, and inorganic particles with a shading effect are filled in the polyester resin; furthermore, the reflecting film is a three-layer co-extrusion structure of a surface layer/a core layer/a surface layer, and the total thickness of the reflecting film is one of 150 μm, 188 μm, 225 μm, 250 μm and 300 μm.
Further, the polyester resin may be selected from polyethylene terephthalate (PET), and the incompatible resin may be selected from one of polyolefin resins, such as polypropylene resin, or one of poly-4-methylpentene. The incompatible resin and the polyester resin are melted and mixed to form a closed cell structure in the core layer structure under the action of high stretching ratio, and light rays can generate refraction and reflection effects at the interface of the cell structure, so that the reflection effect of the light rays is realized.
Further, in the present invention, the core layer comprises the following components: 80-90 parts of polyester resin, 12-18 parts of incompatible resin and 1-5 parts of inorganic particles.
In the invention, the surface layer can be arranged on one side or both sides of the core layer; that is, the reflective film may have a structure of skin layer/core layer, or skin layer/core layer/skin layer.
The invention also provides a preparation method of the diffuse reflection type reflecting film, which comprises the following steps:
(1) feeding the surface raw materials into an extruder according to a formula, and carrying out melt mixing to obtain a surface raw material mixture;
(2) weighing raw materials of a core layer, mixing the raw materials by a drying and mixing device, then feeding the mixture into an extruder for melting and mixing, carrying out tape casting extrusion on the mixture and a surface layer raw material mixture at a die head, cooling a cast sheet, and carrying out longitudinal stretching, transverse stretching and heat setting treatment to obtain the reflective film.
Further, the extruder in the steps (1) and (2) is a double-screw extruder.
Furthermore, in the invention, the brightness, namely the brightness of the prepared reflecting film is greatly influenced by the stretching ratio, the larger the stretching ratio is, the more the reflecting film is stretched, the more the cell structures formed between the polyester resin and the incompatible resin of the core layer are, the richer the interface is, the more obvious the reflection and refraction effects on light are, thereby being more beneficial to improving the brightness; and the higher the stretching ratio is, the greater the risk of film rupture is, and the greater the influence on the continuity of the production is, in step (2) of the invention, the stretching ratio of the reflective film at the longitudinal stretching position is 3.65-3.8.
Compared with the prior art, the invention has the following technical effects:
the invention forms micropore defects on the surface of the quartz powder by accelerating the jet device, and mica powder is stripped and embedded in micropores on the surface of the quartz powder; and after laser beam irradiation, the mica is welded on the surface of the quartz powder, and the obtained light scattering particles have excellent light scattering effect.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified with the specific embodiments.
Example 1
A diffuse reflection type reflection film includes a core layer and surface layers disposed on both sides of the core layer;
the core layer comprises the following components: 85 parts of polyethylene terephthalate (PET film grade slices produced by China instrumented chemical fiber company Limited, with the trade mark FG620), 15 parts of polypropylene resin (Nordic chemical production, with the product model of WF420HMS) and 3 parts of titanium dioxide (with the particle size of 0.2 mu m);
the surface layer comprises the following components: 85 parts of polyethylene terephthalate (PET film grade slices produced by China instrumented chemical fiber company Limited, the trade mark is FG620), 10 parts of light scattering particles and 6 parts of antistatic agent (plastic antistatic agent 006 produced by Zhongteng chemical industry Co., Ltd.);
the preparation method of the light scattering particles comprises the following steps: ball-milling quartz powder to make the particle size of the quartz powder be 5 microns, adding 500mL of hydrochloric acid solution (2mol/L) into a mixture of 1kg of ball-milled quartz powder and 0.5kg of mica powder (the particle size is 0.4 microns), uniformly mixing, adding into a jet machine for acceleration treatment, drying in a vacuum drying oven at 45 ℃ and the vacuum degree of 0.4Mpa, and irradiating by laser beams to obtain the light scattering particles;
the laser beam is generated by an ytterbium-doped fiber laser source, and the power of the laser beam is 10 Kw;
the preparation method of the diffuse reflection type reflecting film comprises the following steps:
(1) feeding the surface raw materials into a double-screw extruder according to a formula, and carrying out melt mixing to obtain a surface raw material mixture;
(2) weighing raw materials of a core layer, mixing the raw materials through a drying and mixing device, then feeding the mixture into a double-screw extruder for melting and mixing, carrying out tape casting extrusion on the mixture and a surface layer raw material mixture at a die head, cooling a cast sheet, and carrying out longitudinal stretching, transverse stretching and heat setting treatment to obtain the reflective film, wherein the stretching ratio of the longitudinal stretching is 3.72.
Respectively controlling the raw material blanking amount of the surface layer and the core layer and the rotating speed of a corresponding extruder to produce a reflecting film of 188 mu m, wherein the thickness ratio of the core layer to the surface layer of the reflecting film is controlled to be 1: 0.1.
example 2
This example is substantially the same as the diffuse reflection reflective film of example 1 in structure and composition, except that the surface layer includes:
85 parts of polyethylene terephthalate (PET film grade slices produced by China instrumented chemical fiber company Limited, the trade mark is FG620), 5 parts of light scattering particles and 6 parts of antistatic agent (plastic antistatic agent 006 produced by Zhongteng chemical industry Co., Ltd.);
the same procedure as in example 1 was carried out for the preparation of the diffuse reflection type reflective film, except that the other process was not changed.
Example 3
This example is substantially the same as the diffuse reflection reflective film of example 1 in structure and composition, except that the surface layer includes:
85 parts of polyethylene terephthalate (PET film grade slices produced by China instrumented chemical fiber company Limited, the trade mark is FG620), 15 parts of light scattering particles and 6 parts of antistatic agent (plastic antistatic agent 006 produced by Zhongteng chemical industry Co., Ltd.);
the same procedure as in example 1 was carried out for the preparation of the diffuse reflection type reflective film, except that the other process was not changed.
Example 4
This example is substantially the same as the diffuse reflection type reflective film of example 1 in structure and composition, except that the ratio of the thicknesses of the core layer and the surface layer of the reflective film is controlled to be 1: 0.04 and the balance is unchanged to obtain the reflecting film.
Example 5
This example is substantially the same as the diffuse reflection type reflective film of example 1 in structure and composition, except that the ratio of the thicknesses of the core layer and the surface layer of the reflective film is controlled to be 1: 0.125, and the rest is unchanged, so as to obtain the reflecting film.
Example 6
This example is substantially the same as the diffuse reflection type reflective film in example 1 in structure and composition, except that in the preparation process of the light scattering particles, the ball milling of the quartz powder was controlled so that the particle size was 3 μm, and the remainder was unchanged, to prepare the reflective film.
Example 7
This example is substantially the same as the diffuse reflection type reflective film in example 1 in structure and composition, except that in the preparation process of the light scattering particles, the ball milling of the quartz powder was controlled so that the particle size was 8 μm, and the remainder was unchanged, to prepare the reflective film.
Comparative example 1
This example is substantially the same as the diffuse reflection reflective film of example 1 in structure and composition, except that the surface layer includes:
85 parts of polyethylene terephthalate (PET film grade slices produced by China instrumented chemical fiber company Limited, the trade mark is FG620), 2 parts of light scattering particles and 6 parts of antistatic agent (plastic antistatic agent 006 produced by Zhongteng chemical industry Co., Ltd.);
the same procedure as in example 1 was carried out for the preparation of the diffuse reflection type reflective film, except that the other process was not changed.
Comparative example 2
This example is substantially the same as the diffuse reflection reflective film of example 1 in structure and composition, except that the surface layer includes:
85 parts of polyethylene terephthalate (PET film grade slices produced by China instrumented chemical fiber company Limited, the trade mark is FG620), 20 parts of light scattering particles and 6 parts of antistatic agent (plastic antistatic agent 006 produced by Zhongteng chemical industry Co., Ltd.);
the same procedure as in example 1 was carried out for the preparation of the diffuse reflection type reflective film, except that the other process was not changed.
Comparative example 3
This example is substantially the same as the diffuse reflection type reflective film in example 1 in structure and composition, except that in the preparation process of the light scattering particles, the ball milling of the quartz powder was controlled so that the particle size was 12 μm, and the remainder was unchanged, to prepare the reflective film.
Comparative example 4
This example is substantially the same as the diffuse reflection type reflective film of example 1 in structure and composition, except that the ratio of the thicknesses of the core layer and the surface layer of the reflective film is controlled to be 1: 0.02, and the rest is unchanged, so as to obtain the reflecting film. And (3) performance testing:
1. light uniformity of backlight module (OD 18mm)
The reflection film prepared in the embodiment is cut according to the drawing of the backlight module and then placed in the backlight module to form the backlight module, the backlight is lightened, whether the light-emitting surface of the backlight module has light shadows or not and the surrounding shadows are subjectively observed, and the judgment is carried out according to the following standards:
o: the light-emitting surface has no light particle shadow and peripheral shadow, and the light uniformity is best;
and (delta): the light-emitting surface has no light particle shadow, the surrounding shadow phenomenon is slight, and the light uniformity is better;
gamma rays: the light-emitting surface has no light particle shadow, the surrounding shadow phenomenon is serious, and the light uniformity is the worst.
2. Film forming property
The reflective film in the examples was evaluated based on the following points, namely, the longitudinal direction was the continuous film forming direction of the film, and the lateral direction was the direction perpendicular thereto.
A: the membrane can be stably prepared for more than 2 hours;
b: the film can be stably prepared for more than 1 hour and less than 2 hours;
c: when the time is less than 1 hour, film breakage occurs, and stable film formation cannot be achieved.
3. Luminance (also called brightness) of a backlight module (OD ═ 18mm)
The reflection film obtained in the example was cut according to the reflection film drawing of the backlight unit, the light exit surface of the backlight unit was divided into 9 regions of 3 × 3, the front luminance after lighting for 1 hour was measured using a frastk BM-7A luminance meter at a measurement angle of 1 °, the distance between the luminance meter and the light exit surface of the backlight unit was 50cm, and the arithmetic average of the luminances of the 9 regions was determined as the luminance of the reflection film suitable for the backlight unit.
The results of the above tests are summarized in table 1.
Table 1:
in combination with the above test data, it can be seen that the diffuse reflection type reflective film provided by the present invention has an excellent light uniformizing effect.
In the mutual comparison of the respective examples, example 2 (the content of the light scattering particles is reduced), the dodging effect thereof is reduced; example 3 (the content of light scattering particles is increased relative to example 1), the dodging effect meets the requirement, and the brightness is equivalent;
in example 4, the thickness of the surface layer is reduced, the light scattering ability is strong due to the protrusion of a large number of light scattering particles, but a certain film forming property is correspondingly sacrificed, and after the thickness of the core layer is correspondingly increased, the luminance is about 1.1% higher than that of example 1;
in example 5, the thickness of the surface layer was increased, and since a large number of light scattering particles were buried by the polyester of the surface layer, the scattering effect of light was affected to some extent, and the luminance was reduced by 1% as compared to example 1, based on the decrease in the thickness of the core layer which mainly functions to reflect light;
in examples 6 and 7, the particle size of the quartz powder was adjusted, and it can be seen that the performance was not greatly affected;
in comparative example 1, the light uniformity was significantly reduced due to the reduced content of light scattering particles, and the phenomena of a dark image of the lamp particles and a dark image around the lamp particles were significantly observed;
in comparative example 2, the film forming property is deteriorated due to an excessive content of the light scattering particles, and it can be seen that, in combination with comparative example 2, example 3 and example 1, the light emitted from the front surface is decreased due to the scattering effect of the light scattering particles, and the luminance tends to be decreased;
in comparative example 3, the larger particle size of the quartz powder resulted in the larger particle size of the light scattering particles, which gave a general scattering effect, but had a large influence on the film forming property, resulting in more film breakage;
in comparative example 4, the thickness of the surface layer was too thin, the film forming property was poor, and the luminance performance was indeed the best.
In combination with the application of the light scattering particles, the light scattering particles provided by the invention have excellent scattering ability.
The foregoing shows and describes the general principles, essential features, and inventive features of this invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A method for producing a diffuse reflection type reflective film, comprising the steps of:
(1) feeding the surface raw materials into an extruder according to a formula, and carrying out melt mixing to obtain a surface raw material mixture;
(2) weighing raw materials of a core layer, mixing the raw materials by a drying and mixing device, then blanking the mixture into an extruder for melting and mixing, carrying out tape casting extrusion on the mixture and a mixture of raw materials of a surface layer at a die head, cooling a cast sheet, and carrying out longitudinal stretching, transverse stretching and heat setting treatment to obtain a reflecting film;
the surface layer comprises the following components: 80-90 parts of polyester resin, 5-15 parts of light scattering particles and 5-8 parts of antistatic agent;
the preparation method of the light scattering particles comprises the steps of adding an acidic solution into a mixture of quartz powder and mica powder, uniformly mixing, adding into an ejector for accelerating treatment, drying, and irradiating by laser beams to obtain the light scattering particles.
2. The method of claim 1, wherein the quartz powder is ball-milled to have a particle size of 3 to 8 μm;
the particle size of the mica powder is 0.2-0.5 mu m.
3. The method of manufacturing a diffuse reflection reflective film according to claim 1, wherein the ratio of quartz powder to mica powder by mass is 1: (0.3 to 1).
4. The method of claim 1, wherein the laser beam is generated by an ytterbium-doped fiber laser source with a power of 0.1-25 Kw.
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| CN107759932A (en) * | 2017-11-22 | 2018-03-06 | 成都新柯力化工科技有限公司 | A kind of light scattering inorganic microsphere and preparation method for crops plastic greenhouse film |
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| CN107759932A (en) * | 2017-11-22 | 2018-03-06 | 成都新柯力化工科技有限公司 | A kind of light scattering inorganic microsphere and preparation method for crops plastic greenhouse film |
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