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.
The invention provides a preparation method of light diffusion particles, which comprises the following steps:
(1) adding an acidic solution into diatomite, filtering after soaking, leaching for 2-3 times by using deionized water, and then drying, grinding and refining the diatomite to obtain diatomite particles;
(2) adding an organic solvent into the diatomite particles prepared in the step (1), adding glass micropowder while stirring, and then performing ultrasonic dispersion treatment for 30-60 min; obtaining a mixture A;
(3) and blowing the mixture A by adopting flame in a spheroidizing furnace to obtain the light diffusion particles.
The diatomite is a biogenic siliceous sedimentary rock which mainly comprises remains of ancient diatoms and mainly comprises SiO as a chemical component2Mainly contains a small amount of Al2O3、Fe2O3CaO, MgO and organic matter. According to the method, the acidic solution is added into the diatomite for soaking treatment, so that most of impurities such as iron, aluminum and the like in the diatomite can be removed, the specific surface area of the diatomite is greatly improved, and meanwhile, the pore structure of the diatomite can be modified in the acid washing process; leaching with deionized water, removing redundant acid liquor on the diatomite, drying the diatomite, and grinding and refining to obtain diatomite particles;
adding glass micropowder into the diatomite particles, wherein the glass micropowder penetrates into the pore structures of the diatomite particles under the action of ultrasound, and is melted and attached to the inner pore structures of the diatomite particles in situ in a flame blowing process in a spheroidizing furnace; compared with the traditional inorganic particles, the diatomite particles loaded with the molten glass micropowder provided by the invention can reflect and refract light randomly, and ensure the transmittance of the light while ensuring the excellent covering effect.
The preparation method of the glass micro powder is not specially limited, and the particle size of the glass micro powder can be satisfied and can penetrate into a pore structure of the diatomite. The preparation method of the glass micropowder comprises the steps of firstly feeding glass into a press machine for high-pressure crushing to obtain glass cullet with the particle size of 3-8 cm, then transferring the glass cullet into a tungsten carbide high-speed ball mill, setting the rotating speed of the tungsten carbide high-speed ball mill to be 600-800 r/min by taking stainless steel balls with the particle size of 1-2 cm as grinding balls, and carrying out ball milling on the glass cullet to obtain the glass micropowder.
In the present invention, the acidic solution is used for pickling diatomaceous earth, and the kind of the acidic solution is not particularly limited and may be any one commonly known to those skilled in the art, and for example, the acidic solution may be at least one of hydrochloric acid, nitric acid, sulfuric acid, boric acid, perchloric acid, thiocyanic acid, sulfurous acid, phosphoric acid, phosphorous acid, hypochloric acid, formic acid, acetic acid, benzoic acid, benzenesulfonic acid, and the like.
In the present invention, the organic solvent serves as a carrier for the fine diatomite particles and the fine glass powder, which is not particularly required by the present invention and known to those skilled in the art, and is preferably at least one of acetone, N-dimethylformamide, N-methylpyrrolidone, N-dimethylacetamide, dichloromethane, triethyl phosphate, chloroform, toluene, ethanol, acetic acid, ethyl acetate, formic acid, chloroform, tetrahydrofuran, and dimethylsulfoxide.
Further, according to the present invention, the particle size of the diatomaceous earth particles is 5 to 10 μm; the particle size of the glass micro powder is 1-3 mu m.
Furthermore, according to the present invention, in the step (2), the weight ratio of the diatomite particles to the glass fine powder affects the reflection and refraction effects of the diatomite particles obtained by the subsequent preparation on the light, if the addition amount of the glass fine powder is too small, the glass fine powder cannot be sufficiently filled in the pore structure of the diatomite particles, such that the light diffusion effect of the light diffusion particles formed by the diatomite particles is not good, and the filling amount of the glass fine powder is too large, such that not only waste is caused, but also the subsequent burning and melting of the glass fine powder is affected. In the invention, the weight ratio of the diatomite particles to the glass micro powder is 1: (0.3-0.6).
In the step (3), the vacuum degree of the spheroidizing furnace is controlled to be 0.10-0.45 Mpa, and the glass micropowder is ensured to be in-situ fused in the pore structure of the diatomite particles and attached to the pore structure by blowing the mixture A under the vacuum condition.
The invention provides light diffusion particles prepared by the preparation method.
The invention provides an application of the light diffusion particles in an optical diffusion film, which comprises the following steps:
mixing the light diffusion particle nylon particles, adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Nippon paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for the lower coating of the optical diffusion film;
mixing the light diffusion particles with polymethyl methacrylate (PMMA) particles (provided by Nippon Hydrocarbon chemical industry Co., Ltd.), adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Ribang paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for coating on an optical diffusion film;
the lower coating composition and the upper coating composition were coated on both sides of a PET substrate (manufactured by Ningbo Yang science and technology Co., Ltd.) in sequence, and the coating process of the substrate was as follows: unreeling the substrate by an unreeling machine, then automatically reeling, coating the composition on the substrate, and baking by a five-section baking oven at the temperature of 90 ℃, 100 ℃, 110 ℃, 120 ℃ and 105 ℃; the length of the oven is 20m, the retention time of the substrate in the oven is 1min, and finally the substrate is wound by a winding machine to obtain the optical diffusion film.
In the invention, the particle size of the nylon particles is 3-8 μm.
The particle size of the PMMA particles is 10-20 mu m.
The thickness of the PET base material is not specially limited, and the PET base material can be a PET base material commonly used in the prior art, and the thickness of the PET base material is 100-250 mu m;
the thickness of the lower coating composition coated on the surface of the PET substrate is 5-15 mu m;
the thickness of the coating layer composition coated on the surface of the PET substrate is 10-35 μm.
In the invention, by applying the light diffusion particles provided by the invention in the optical diffusion film, the covering performance of the optical diffusion film can be obviously improved, and the light transmittance of the optical diffusion film can also be obviously improved.
The advantages of the light diffusing particles provided by the present invention are further illustrated by the following specific examples.
Example 1
A method for preparing light diffusion particles:
(1) adding a hydrochloric acid solution (1mol/L) into diatomite, filtering after soaking treatment, leaching for 2 times by using deionized water, and then drying, grinding and refining at the temperature of 60 ℃ to obtain diatomite particles with the particle size of 8 mu m;
(2) adding acetone into the diatomite particles prepared in the step (1), adding glass micro powder with the particle size of 2 mu m while stirring, and then performing ultrasonic dispersion treatment for 40 min; obtaining a mixture A; the weight ratio of the diatomite particles to the glass micro powder is 1: 0.5;
(3) controlling the vacuum degree of the spheroidizing furnace to be 0.30Mpa, and blowing the mixture A by adopting flame to obtain the light diffusion particles;
mixing the light diffusion particles with nylon particles with the particle size of 5 mu m, then adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Libang paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for the lower coating of the optical diffusion film;
mixing the light diffusion particles with polymethyl methacrylate (PMMA) particles (Nippon Hydrochemical industries Co.) with the particle size of 15 μm, adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Nippon paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for coating on an optical diffusion film;
the lower coating composition and the upper coating composition were applied to both sides of a 150 μm PET substrate (produced by ningbo yang technologies, inc.) in sequence, and the substrate coating process was as follows: unreeling the substrate by an unreeling machine, then automatically reeling, coating the composition on the substrate, and baking by a five-section baking oven at the temperature of 90 ℃, 100 ℃, 110 ℃, 120 ℃ and 105 ℃; the length of the oven is 20m, the retention time of the substrate in the oven is 1min, and finally the substrate is wound by a winding machine to obtain the optical diffusion film;
the substrate winding speed, i.e. the distance between the drawdown plate and the substrate, was controlled such that the upper coating thickness of the PET substrate was 20 μm and the lower coating thickness was 10 μm.
Example 2
A method for preparing light diffusion particles:
(1) adding a hydrochloric acid solution (1mol/L) into diatomite, filtering after soaking treatment, leaching for 3 times by using deionized water, and then drying, grinding and refining at the temperature of 60 ℃ to obtain diatomite particles with the particle size of 7 mu m;
(2) adding acetone into the diatomite particles prepared in the step (1), adding glass micro powder with the particle size of 2 mu m while stirring, and then carrying out ultrasonic dispersion treatment for 50 min; obtaining a mixture A; the weight ratio of the diatomite particles to the glass micro powder is 1: 0.4;
(3) controlling the vacuum degree of the spheroidizing furnace to be 0.30Mpa, and blowing the mixture A by adopting flame to obtain the light diffusion particles;
mixing the light diffusion particles with nylon particles with the particle size of 5 mu m, then adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Libang paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for the lower coating of the optical diffusion film;
mixing the light diffusion particles with polymethyl methacrylate (PMMA) particles (Nippon Hydrochemical industries Co.) with the particle size of 15 μm, adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Nippon paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for coating on an optical diffusion film;
the lower coating composition and the upper coating composition were applied to both sides of a 150 μm PET substrate (produced by ningbo yang technologies, inc.) in sequence, and the substrate coating process was as follows: unreeling the substrate by an unreeling machine, then automatically reeling, coating the composition on the substrate, and baking by a five-section baking oven at the temperature of 90 ℃, 100 ℃, 110 ℃, 120 ℃ and 105 ℃; the length of the oven is 20m, the retention time of the substrate in the oven is 1min, and finally the substrate is wound by a winding machine to obtain the optical diffusion film;
the substrate winding speed, i.e. the distance between the drawdown plate and the substrate, was controlled such that the upper coating thickness of the PET substrate was 20 μm and the lower coating thickness was 10 μm.
Example 3
A method for preparing light diffusion particles:
(1) adding a hydrochloric acid solution (1mol/L) into diatomite, filtering after soaking treatment, leaching for 2 times by using deionized water, and then drying, grinding and refining at 60 ℃ to obtain diatomite particles with the particle size of 5 mu m;
(2) adding acetone into the diatomite particles prepared in the step (1), adding glass micro powder with the particle size of 2 mu m while stirring, and then performing ultrasonic dispersion treatment for 30 min; obtaining a mixture A; the weight ratio of the diatomite particles to the glass micro powder is 1: 0.5;
(3) controlling the vacuum degree of the spheroidizing furnace to be 0.30Mpa, and blowing the mixture A by adopting flame to obtain the light diffusion particles;
mixing the light diffusion particles with nylon particles with the particle size of 5 mu m, then adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Libang paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for the lower coating of the optical diffusion film;
mixing the light diffusion particles with polymethyl methacrylate (PMMA) particles (Nippon Hydrochemical industries Co.) with the particle size of 15 μm, adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Nippon paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for coating on an optical diffusion film;
the lower coating composition and the upper coating composition were applied to both sides of a 150 μm PET substrate (produced by ningbo yang technologies, inc.) in sequence, and the substrate coating process was as follows: unreeling the substrate by an unreeling machine, then automatically reeling, coating the composition on the substrate, and baking by a five-section baking oven at the temperature of 90 ℃, 100 ℃, 110 ℃, 120 ℃ and 105 ℃; the length of the oven is 20m, the retention time of the substrate in the oven is 1min, and finally the substrate is wound by a winding machine to obtain the optical diffusion film;
the substrate winding speed, i.e. the distance between the drawdown plate and the substrate, was controlled such that the upper coating thickness of the PET substrate was 20 μm and the lower coating thickness was 10 μm.
Example 4
A method for preparing light diffusion particles:
(1) adding a hydrochloric acid solution (1mol/L) into diatomite, filtering after soaking treatment, leaching for 3 times by using deionized water, and then drying, grinding and refining at the temperature of 60 ℃ to obtain diatomite particles with the particle size of 10 mu m;
(2) adding acetone into the diatomite particles prepared in the step (1), adding glass micro powder with the particle size of 2 mu m while stirring, and then performing ultrasonic dispersion treatment for 60 min; obtaining a mixture A; the weight ratio of the diatomite particles to the glass micro powder is 1: 0.5;
(3) controlling the vacuum degree of the spheroidizing furnace to be 0.3Mpa, and blowing the mixture A by adopting flame to obtain the light diffusion particles;
mixing the light diffusion particles with nylon particles with the particle size of 5 mu m, then adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Libang paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for the lower coating of the optical diffusion film;
mixing the light diffusion particles with polymethyl methacrylate (PMMA) particles (Nippon Hydrochemical industries Co.) with the particle size of 15 μm, adding polyester polyol, adding a curing agent (PC2000, produced by Kyowa Nippon paint Co., Ltd.), and uniformly stirring and mixing to obtain a composition for coating on an optical diffusion film;
the lower coating composition and the upper coating composition were applied to both sides of a 150 μm PET substrate (produced by ningbo yang technologies, inc.) in sequence, and the substrate coating process was as follows: unreeling the substrate by an unreeling machine, then automatically reeling, coating the composition on the substrate, and baking by a five-section baking oven at the temperature of 90 ℃, 100 ℃, 110 ℃, 120 ℃ and 105 ℃; the length of the oven is 20m, the retention time of the substrate in the oven is 1min, and finally the substrate is wound by a winding machine to obtain the optical diffusion film;
the substrate winding speed, i.e. the distance between the drawdown plate and the substrate, was controlled such that the upper coating thickness of the PET substrate was 20 μm and the lower coating thickness was 10 μm.
Example 5
This example was carried out by the same procedure as in example 1 except that in step (2), the fine glass powder having a particle size of 1 μm was used without changing the particle size, to prepare the light-diffusing particles, and then the subsequent treatment as in example 1 was carried out to prepare an optical diffusion film.
Example 6
This example was carried out by the same procedure as in example 1 except that in the step (2), the fine glass powder having a particle size of 3 μm was used without changing the particle size, to prepare the light-diffusing particles, and then the subsequent treatment as in example 1 was carried out to prepare an optical diffusion film.
Example 7
This example prepared light diffusing particles according to the method of example 1, except that in step (1.2), the weight ratio of the diatomaceous earth particles to the glass fine powder was 1: 0.3, and the remainder was unchanged, to prepare the light diffusion particles, followed by the subsequent treatment of example 1 to prepare an optical diffusion film.
Example 8
This example prepared light diffusing particles according to the method of example 1, except that in step (1.2), the weight ratio of the diatomaceous earth particles to the glass fine powder was 1: 0.6, and the remainder was unchanged, to prepare the light diffusion particles, followed by the subsequent treatment of example 1 to prepare an optical diffusion film.
Example 9
This example was conducted in the same manner as in example 1 except that in the step (1.3), the degree of vacuum of the spheroidizing furnace was controlled to 0.10MPa, and the remainder was kept constant, to thereby prepare the light diffusing particles, followed by conducting the subsequent processes of example 1 to thereby prepare an optical diffusion film.
Example 10
This example was carried out to prepare light-diffusing particles in the same manner as in example 1, except that in the step (1.3), the degree of vacuum of the spheroidizing furnace was controlled to 0.45MPa, and the remainder was kept constant, to prepare the light-diffusing particles, followed by the subsequent treatment of example 1 to prepare an optical diffusion film.
Example 11
This example prepares light diffusion particles by the method of example 1, except that nylon particles having a particle size of 3 μm were used and the remainder were unchanged, to prepare the optical diffusion film.
Example 12
This example prepares light diffusion particles by the method of example 1, except that nylon particles having a particle size of 8 μm were used and the remainder was unchanged, to prepare the optical diffusion film.
Example 13
This example prepared light diffusion particles according to the method of example 1, except that polymethyl methacrylate (PMMA) particles having a particle size of 10 μm were used, and the rest were unchanged, to prepare the optical diffusion film.
Example 14
This example prepared light diffusion particles according to the method of example 1, except that polymethyl methacrylate (PMMA) particles having a particle size of 20 μm were used, and the rest was unchanged, to prepare the optical diffusion film.
Comparative example 1
Comparative example light-diffusing particles were prepared as in example 1, except that the weight ratio of the diatomite particles to the glass micropowder was 1: 0.1. the light diffusion particles were prepared while the rest were unchanged, and then an optical diffusion film was prepared according to the subsequent treatment of example 1.
Comparative example 2
Comparative example light-diffusing particles were prepared as in example 1, except that the weight ratio of the diatomite particles to the glass micropowder was 1: 0.8. the light diffusion particles were prepared while the rest were unchanged, and then an optical diffusion film was prepared according to the subsequent treatment of example 1.
Comparative example 3
This comparative example prepared light-diffusing particles in the same manner as in example 1, except that in the step (1), diatomaceous earth was ground and refined to give diatomaceous earth fine particles having a particle size of 15 μm, and the remainder was unchanged to prepare the light-diffusing particles, followed by the subsequent treatment of example 1 to prepare an optical diffusion film.
Comparative example 4
This comparative example prepared light diffusion particles in the same manner as in example 1 except that in the step (1), diatomaceous earth was ground and refined to give diatomaceous earth fine particles having a particle size of 3 μm, and the remainder was unchanged, to prepare the light diffusion particles, followed by the subsequent treatment of example 1 to prepare an optical diffusion film.
Comparative example 5
This comparative example prepared light-diffusing particles in the same manner as in example 1 except that in step (2), fine glass powder having a particle size of 5 μm was added and the remainder was unchanged to prepare the light-diffusing particles, followed by the subsequent treatment of example 1 to prepare an optical diffusion film.
Comparative example 6
This comparative example prepared light diffusion particles according to the method of example 1, except that in the step (3), the degree of vacuum of the spheroidizing furnace was controlled to 0.80Mpa, and the remainder was constant, to prepare the light diffusion particles, followed by the subsequent treatment of example 1 to prepare an optical diffusion film.
Comparative example 7
This example prepares light diffusion particles by the method of example 1, except that nylon particles having a particle size of 10 μm were used and the remainder was unchanged to prepare the optical diffusion film.
Comparative example 8
This example prepared light diffusion particles according to the method of example 1, except that polymethyl methacrylate (PMMA) particles having a particle size of 7 μm were used, and the rest were unchanged, to prepare the optical diffusion film.
Comparative example 9
This example prepared light diffusion particles according to the method of example 1, except that polymethyl methacrylate (PMMA) particles having a particle size of 30 μm were used, and the rest was unchanged, to prepare the optical diffusion film.
The optical diffusion film prepared in the above example was tested by the following test method:
1. light transmittance and haze
The test was carried out using a WGT-S light transmittance/haze meter manufactured by Shanghai precision scientific instruments, Inc.
2. Adhesion force
The test was carried out according to GB/T9286 "test for marking paint, varnish and lacquer film".
3. Influence of brightness
The light-emitting surface of the backlight unit was divided into 4 areas of 2X 2, and the front luminance after lighting for 1 hour was measured using a Foshda BM-7A luminance meter. The measurement angle was 1 °, and the distance between the luminance meter and the single-sided light emitting surface of the backlight was 50 cm. The luminance was obtained as an arithmetic average of the luminances of 4 portions in the single-sided light emitting surface of the backlight.
The optical diffusion film prepared in the example was placed in a backlight unit to be used as an upper diffusion film, and compared with the luminance value when the upper diffusion film was removed (the luminance of the backlight unit when the upper diffusion film was removed was 100%).
Table 1:
|
light transmittance (%)
|
Haze (%)
|
Adhesion of upper coating
|
Lower coating adhesion
|
Brightness of light
|
Example 1
|
91.54
|
94.52
|
5B
|
5B
|
99.5%
|
Example 2
|
91.31
|
94.64
|
5B
|
5B
|
99.2%
|
Example 3
|
91.23
|
94.23
|
5B
|
5B
|
99.1%
|
Example 4
|
90.55
|
94.02
|
5B
|
5B
|
98.4%
|
Example 5
|
91.62
|
94.35
|
5B
|
5B
|
99.7%
|
Example 6
|
90.84
|
94.25
|
5B
|
5B
|
98.9%
|
Example 7
|
90.25
|
94.62
|
5B
|
5B
|
98.2%
|
Example 8
|
91.35
|
94.25
|
5B
|
5B
|
99.3%
|
Example 9
|
91.62
|
94.36
|
5B
|
5B
|
99.7%
|
Example 10
|
90.15
|
94.53
|
5B
|
5B
|
98.1%
|
Example 11
|
91.26
|
94.26
|
5B
|
5B
|
99.1%
|
Example 12
|
90.34
|
94.23
|
5B
|
5B
|
98.3%
|
Example 13
|
90.17
|
94.21
|
5B
|
5B
|
98.1%
|
Example 14
|
91.23
|
94.28
|
5B
|
5B
|
99.1%
|
Comparative example 1
|
83.74
|
93.45
|
5B
|
5B
|
90.4%
|
Comparative example 2
|
88.56
|
95.83
|
5B
|
5B
|
95.8%
|
Comparative example 3
|
87.43
|
96.22
|
5B
|
5B
|
95.7%
|
Comparative example 4
|
78.42
|
95.44
|
5B
|
5B
|
87.5%
|
Comparative example 5
|
82.64
|
94.52
|
5B
|
5B
|
89.4%
|
Comparative example 6
|
75.46
|
93.48
|
5B
|
5B
|
85.5%
|
Comparative example 7
|
89.38
|
94.63
|
5B
|
4B
|
95.9%
|
Comparative example 8
|
83.41
|
94.15
|
5B
|
5B
|
90.2%
|
Comparative example 9
|
87.82
|
94.08
|
3B
|
5B
|
95.8% |
The test data show that the light diffusion particles provided by the invention have excellent light diffusion performance, are suitable for optical diffusion films, and have excellent light transmission performance while having excellent covering performance (high haze); in addition, the optical diffusion film provided by the invention has small influence on the brightness.
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.