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Photo-curable nano-zirconia dispersion liquid, preparation method thereof and optical film

A technology of nano-zirconia and dispersion liquid, applied in the direction of coating, etc., can solve the problems of low refractive index of dispersion liquid, ignoring hardness performance, low hardness of coating layer, etc., and achieve the effect of high process efficiency, high hardness and increased refractive index

Active Publication Date: 2022-07-12
SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Patent CN 112499678B discloses a nano-zirconia powder, its preparation method and the resulting dispersion, and an optical film. The modified zirconia is not purified during the preparation of the resin dispersion, and the dispersion components are The resin part in the solution has not been selected and optimized, resulting in a relatively low refractive index of the dispersion, and the entire dispersion preparation process has ignored the hardness performance of the dispersion after coating the light film, resulting in the late coating layer of the prepared dispersion relatively low hardness

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  • Photo-curable nano-zirconia dispersion liquid, preparation method thereof and optical film
  • Photo-curable nano-zirconia dispersion liquid, preparation method thereof and optical film

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preparation example Construction

[0047] In the present invention, the preparation method of surface-modified zirconia comprises the following steps:

[0048] (A) providing the zirconia solution of the organic solvent phase;

[0049] Alternatively, the zirconia aqueous solution and the organic solvent can be concentrated and replaced to obtain a zirconia solution in the organic solvent phase;

[0050] Wherein, the zirconia mass concentration of the zirconia solution in the organic solvent phase is below 50%;

[0051] (B) adding the surface modifier to the zirconia solution of the above-mentioned organic solvent phase to modify the zirconia to obtain the modified mixed solution;

[0052] (C) the modified mixed solution obtained in step (B) removes the solvent to obtain surface-coated zirconia powder;

[0053] (D) The surface-coated zirconia powder obtained in step (C) is washed alternately with the first polar solvent and the second polar solvent, and then dried to obtain surface-modified zirconia;

[0054] ...

Embodiment 1

[0078] A preparation method of a photocurable nano-zirconia dispersion, comprising the following steps:

[0079] S1: take 400 g of a zirconia aqueous solution with a mass concentration of 20% (the particle size of zirconia is 5 nm), use a rotary evaporator to concentrate and remove water until the mass concentration of zirconia is above 30%, then add 240 g of propylene glycol methyl ether, and then concentrate Until the mass concentration of zirconia is more than 30%, repeat the procedure to replace water with propylene glycol methyl ether to obtain a zirconia solution with a mass concentration of 30% propylene glycol methyl ether phase;

[0080] S2: adding 6g isooctanoic acid and 6g silane KBM-503 to the zirconium oxide solution of the propylene glycol methyl ether phase obtained in step S1, and then refluxing and stirring at 120°C for 4 hours for surface modification to obtain a modified mixed solution;

[0081] S3: the modified mixed solution obtained in step S2 is subjecte...

Embodiment 2

[0085] The difference between this embodiment and Embodiment 1 is that the particle size of zirconia in this embodiment is 8 nm, and step S5 in this embodiment:

[0086] Weigh 30 g of purified surface-modified zirconia powder and surface-treated silicon oxide powder (the average particle size of silicon oxide is 3 nm, and the maximum particle size is less than 5 nm; the surface treatment method of silicon oxide is the same as in Example 1) 1.5g was dissolved in 150g butanone, and then 1.5g of BYK-111 dispersant was added to assist ultrasonic or grinding to fully dissolve and disperse the powder, and then 17g of o-phenylphenoxyethyl acrylate was added and evaporated under reduced pressure. After butanone, a zirconia dispersion liquid with a mass concentration of 60% is obtained, which is a photocurable nano-zirconia dispersion liquid;

[0087] Other steps are the same as in Example 1.

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Abstract

The invention provides a photocurable nano-zirconia dispersion liquid and a preparation method thereof, and an optical film, and relates to the technical field of fine chemical engineering, the organic solvent type dispersion liquid comprises zirconia, silicon oxide and an optical acrylic resin monomer; wherein the zirconium oxide is surface-modified zirconium oxide, the mass concentration of the zirconium oxide in the dispersion liquid is more than 50%, the content of the silicon oxide is 0.1-5% of the mass of the zirconium oxide, the average particle size of the silicon oxide is 2-3nm, and the maximum particle size of the silicon oxide is less than 5nm; wherein the particle size of the silicon oxide is smaller than that of the zirconium oxide. The technical problems that the refractive index of the dispersion liquid is low and the hardness of a later coating layer is low are solved, and the technical effect of improving the refractive index of the dispersion liquid and the hardness of the later coating layer is achieved.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a photocurable nano-zirconia dispersion liquid, a preparation method thereof, and an optical film. Background technique [0002] Nano zirconia has high refractive index, light transmittance in the visible light region, and strong corrosion resistance. In recent years, it has been widely used in the optical field as a material for adjusting the refractive index, such as camera lenses, car windows, photovoltaic glass, various types of Display, optical filter and LED packaging resin and other fields. [0003] When nano-zirconia is directly added without treatment, on the one hand, due to the large surface active energy of nanoparticles, agglomeration will occur, and on the other hand, the dispersion and combination of nanoparticles in organic media are not sufficient, which will directly affect. Post-use effects. Therefore, various methods have been proposed to compound nan...

Claims

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Application Information

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IPC IPC(8): C09D4/02C09D7/62
CPCC09D4/00C09D7/62C09D7/67
Inventor 朱恒张栋艾辽东奚洪亮
Owner SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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