WO2023173712A1 - 氧化锆单体型分散液及其制备方法、光学膜和显示屏 - Google Patents

氧化锆单体型分散液及其制备方法、光学膜和显示屏 Download PDF

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WO2023173712A1
WO2023173712A1 PCT/CN2022/119288 CN2022119288W WO2023173712A1 WO 2023173712 A1 WO2023173712 A1 WO 2023173712A1 CN 2022119288 W CN2022119288 W CN 2022119288W WO 2023173712 A1 WO2023173712 A1 WO 2023173712A1
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zirconium oxide
dispersion
zirconia
oxide monomer
nano
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PCT/CN2022/119288
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English (en)
French (fr)
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宋锡滨
马海洋
吕玉兴
艾辽东
奚洪亮
张艳
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山东国瓷功能材料股份有限公司
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Priority to JP2023524450A priority Critical patent/JP2024517039A/ja
Priority to US18/332,941 priority patent/US20230323139A1/en
Publication of WO2023173712A1 publication Critical patent/WO2023173712A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
    • C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
    • C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/45—Anti-settling agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/67—Particle size smaller than 100 nm
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/80—Processes for incorporating ingredients

Definitions

  • the present disclosure relates to the technical field of zirconia, and in particular to a zirconia monomer dispersion liquid and its preparation method, optical film and display screen.
  • zirconium oxide monomer dispersion is used to prepare optical films such as brightness enhancement films, which can be used on LCD displays to increase the brightness and clarity of the screen.
  • patent CN 106268394 B discloses a method for preparing zirconium oxide particles or its dispersion.
  • the transmittance at a wavelength of 400nm is more than 35%
  • the transmittance at a wavelength of 800nm is more than 35%.
  • the transmittance is above 95%, and the viscosity at 25°C is below 20mPa ⁇ s.
  • the patent does not cover the transmittance of the zirconia monomer dispersion.
  • the zirconia monomer dispersion is an organic-inorganic composite system, and the components interact with each other and the influencing factors are complex, especially
  • the refractive index of each component in the system, the stability of the zirconia particles in the system, and the transmittance of the system are difficult to balance with each other. If you blindly pursue high indicators in one aspect, it will inevitably lead to a decrease in the indicators on the other side. Therefore, it is of great significance to develop a monomer dispersion with high light transmittance that has a simple process, coordinated indicators in the system, and is suitable for practical applications.
  • the purpose of the present disclosure includes providing a zirconium oxide monomer dispersion and a preparation method thereof to alleviate at least one technical problem existing in the prior art.
  • the present disclosure provides a zirconia monomer dispersion liquid, including the following raw materials:
  • Nano-zirconia, monomer resin, stabilizer and refractive index adjuster
  • the mass fraction of the nano-zirconia in the zirconium oxide monomer dispersion is 50-75%;
  • the mass of the stabilizer is 1-10% of the mass of the nano-zirconia
  • the mass of the refractive index modifier is 1-10% of the mass of the nano-zirconia
  • the monomer resin includes any one or a combination of at least two of phenoxybenzyl acrylate, biphenyl carbinyl acrylate, benzyl acrylate or o-phenyl phenoxyethyl acrylate.
  • the average particle size of the nano-zirconia is 1-20 nm.
  • the structure of the stabilizer is RX n ;
  • R is selected from any one or a combination of at least two of alkyl groups, sulfonate groups, phosphate groups, amide groups, carboxyl groups, hydroxyl groups, aromatic rings or substituted aromatic rings;
  • X is selected from any one or a combination of at least two of polyether chains, acrylate chains, polyester chains or alkyl chains;
  • n is an integer between 1-3.
  • the stabilizer includes any one or a combination of at least two of octylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, triethylhexyl phosphate, stearamide or hydroxypropyl acrylate.
  • the structure of the refractive index modifier is AB m ;
  • A is selected from any one or a combination of at least two substituted or unsubstituted acryloyloxy groups, methylene groups, alkoxy groups, carbon-carbon double bonds, silicon-carbon groups or alkyl groups;
  • B is selected from any one or a combination of at least two of hydroxyl, carbonyl, ester, siloxy, alkoxy, carboxyl, substituted or unsubstituted aromatic rings;
  • n is an integer between 1-3.
  • the refractive index modifier includes ethylene glycol ether, 4-(4-acryloyloxybutoxy)-benzoic acid or tris(methoxyethoxy)propyloxysilane. Any one or a combination of at least two.
  • the present disclosure also provides a method for preparing a zirconium oxide monomer dispersion, which includes the following steps:
  • the nano-zirconia is mixed with a monomer resin for primary dispersion, and then mixed with the stabilizer and refractive index adjuster for secondary dispersion to obtain a zirconium oxide monomer dispersion.
  • the time of one dispersion is 30-90 minutes;
  • the secondary dispersion time is 30-60 minutes;
  • both the primary dispersion and the secondary dispersion are carried out using dispersing equipment.
  • the present disclosure also provides an optical film made of the above-mentioned zirconium oxide monomer dispersion.
  • the present disclosure provides a zirconia monomer dispersion, which is mainly made of nano zirconia, monomer resin, stabilizer, refractive index adjuster and other raw materials, wherein nano zirconia is used as inorganic dispersed particles, It can reduce the scattering of light by particles, thereby improving the transmittance of the system; the addition of stabilizers can improve the dispersion and uniformity of the zirconia monomer dispersion.
  • the addition of refractive index adjusters can make the entire system The refractive index of each raw material is more matched, thereby improving the transmittance of the system.
  • the present disclosure provides a method for preparing a zirconia monomer dispersion.
  • nano zirconia is mixed with a monomer resin for primary dispersion, and then mixed with a stabilizer and a refractive index adjuster for a secondary dispersion.
  • Disperse to obtain a zirconium oxide monomer dispersion the preparation method is simple and does not require the participation of an intermediate phase in the entire dispersion process, which can greatly reduce process steps and reduce costs.
  • the present disclosure provides an optical film made of the above-mentioned zirconium oxide monomer dispersion liquid.
  • the optical film produced has good optical properties.
  • the present disclosure also provides a display screen including the above-mentioned optical film.
  • the display screen has good brightness and clarity.
  • a zirconium oxide monomer dispersion including the following raw materials:
  • Nano-zirconia, monomer resin, stabilizer and refractive index adjuster
  • the mass fraction of nano-zirconia in the zirconia monomer dispersion is 50-75%;
  • the mass of the stabilizer is 1-10% of the mass of nano-zirconia
  • the mass of the refractive index modifier is 1-10% of the mass of nano-zirconia
  • the monomer resin includes any one or a combination of at least two of phenoxybenzyl acrylate, biphenyl carbinyl acrylate, benzyl acrylate or o-phenyl phenoxyethyl acrylate.
  • the source of nano-zirconia is not limited and can be commercially available or can be prepared by oneself using conventional preparation methods in the field.
  • Nano-zirconia is selected as the inorganic dispersed particle in this zirconium oxide monomer dispersion. On the one hand, due to its smaller particle size, it can reduce the scattering effect of particles on light, thereby improving the transmittance of the system. On the other hand, nano-zirconia The refractive index of zirconia also has a good degree of matching with the refractive index of the specific type of monomer resin of the present disclosure, which can greatly reduce the degree of light scattering by the system, thereby improving the transmittance of the system.
  • stabilizer can make nano-zirconia less likely to agglomerate and have better stability, thereby maintaining a higher transmittance of the system.
  • the refractive index adjuster can make the refractive index matching between nano-zirconia and monomer resin higher, so that the entire system has higher transmittance.
  • Typical but non-limiting mass fractions of nano-zirconia are 50%, 52%, 54%, 56%, 58%, 60%, 62%, 64%, 65%, 66%, 68%, 70%, 72 %, 74% or 75%.
  • the monomer resin mainly disperses nano-zirconia, its dosage only needs to ensure that the mass fraction of nano-zirconia in the zirconium oxide monomer dispersion reaches 50-75%.
  • the added amounts of stabilizers and refractive index modifiers are calculated based on the mass of nano-zirconia.
  • the typical but non-limiting mass fraction of the stabilizer in nano-zirconia is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%. If the mass fraction of the stabilizer in the nano-zirconia is too low (less than 1%), it will not be able to stabilize the system and improve the transmittance of the system; the stabilizer in the nano-zirconia mass fraction is too high (higher than 10%) , it will have an impact on the refractive index matching of each component of the entire system, resulting in failure to achieve the expected results and increased costs.
  • the typical but non-limiting mass fraction of the refractive index modifier in the nano-zirconia is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%. If the mass fraction of the refractive index modifier in nano-zirconia is too low (less than 1%), it will not be able to adjust the refractive index matching of the system; if the mass fraction of the refractive index modifier in nano-zirconia is too high (higher than 10%), it will easily lead to failure to achieve the expected results and increase costs.
  • the present disclosure provides a zirconia monomer dispersion liquid, which is mainly made of nano zirconia, monomer resin, stabilizer, refractive index adjuster and other raw materials.
  • nano zirconia is used as inorganic dispersed particles, which can reduce particulate matter. Scattering of light, thereby improving the transmittance of the system; the addition of stabilizers can improve the dispersion and uniformity of the zirconia monomer dispersion.
  • the addition of refractive index adjusters can make each raw material in the entire system The refractive index is more closely matched, thereby improving the transmittance of the system.
  • the zirconium oxide monomer dispersion has high stability and transmittance.
  • the average particle size of nano-zirconia is 1-20 nm.
  • Typical but non-limiting particle sizes of nano-zirconia are, for example, 1 nm, 2 nm, 4 nm, 5 nm, 6 nm, 8 nm, 10 nm, 12 nm, 14 nm, 15 nm, 16 nm, 18 nm or 20 nm.
  • the structure of the stabilizer is RX n , where R is an anchoring group that can anchor with nano-zirconia, and X is a solvating group that can interact with monomer resin. take effect.
  • R is selected from any one or a combination of at least two of alkyl groups, sulfonic acid groups, phosphate groups, amide groups, carboxyl groups, hydroxyl groups, aromatic rings or substituted aromatic rings.
  • X is selected from any one or a combination of at least two of polyether chains, acrylate chains, polyester chains or alkyl chains.
  • n is an integer from 1 to 3, for example, it can be 1, 2 or 3.
  • the stabilizer includes any one or at least of octylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, triethylhexyl phosphate, stearamide or hydroxypropyl acrylate. A combination of both.
  • the structure of the refractive index modifier is AB m ;
  • A is selected from any one or a combination of at least two substituted or unsubstituted acryloxy groups, alkoxy groups, carbon-carbon double bonds, alkyl groups or siloxy groups.
  • B is selected from any one or a combination of at least two of hydroxyl group, carbonyl group, ester group, silicon carbon group, carboxyl group, substituted or unsubstituted aromatic ring.
  • n is an integer from 1 to 3, for example, it can be 1, 2 or 3.
  • the refractive index modifier includes ethylene glycol ether, 4-(4-acryloyloxybutoxy)-benzoic acid or tris(methoxyethoxy)propyl acyl Any one or a combination of at least two of the oxysilanes.
  • the refractive index adjuster can be matched with the entire organic and inorganic system, thereby better adjusting the refractive index of the system and reducing the light intensity of the system. Scattering improves the transmittance of the system.
  • a method for preparing a zirconium oxide monomer dispersion including the following steps:
  • Nano-zirconia is mixed with a monomer resin for primary dispersion, and then mixed with a stabilizer and a refractive index adjuster for secondary dispersion to obtain a zirconium oxide monomer dispersion.
  • nanometer zirconia is first mixed with monomer resin for primary dispersion, and then mixed with stabilizer and refractive index adjuster for secondary dispersion.
  • This preparation method has a simple process and does not require an intermediate phase in the entire dispersion process. Participation can greatly reduce process steps and reduce costs.
  • the time for one dispersion is 30-90 minutes.
  • Typical but non-limiting time for a dispersion is 30min, 40min, 50min, 60min, 70min, 80min or 90min.
  • the time of secondary dispersion is 30-60 minutes. Typical but non-limiting secondary dispersion times are 30 min, 40 min, 50 min or 60 min.
  • both primary dispersion and secondary dispersion are carried out using dispersing equipment.
  • the dispersing equipment described here can be understood as any equipment or technical means in the field that can disperse materials in the form of smaller droplets in the corresponding medium, including but not limited to mechanical stirring, magnetic stirring, ultrasound, and homogenizers. , colloid mill, etc.
  • an optical film is also provided, which is made of the above-mentioned zirconium oxide monomer dispersion.
  • the optical film produced has good optical properties.
  • a display screen including the above-mentioned optical film.
  • the display screen has good brightness and clarity.
  • This embodiment provides a zirconium oxide monomer dispersion, including the following raw materials:
  • Nano-zirconia, monomer resin, stabilizer and refractive index adjuster
  • the average particle size of nano-zirconia is 10nm
  • the mass fractions of nano-zirconia in the zirconia monomer dispersion are 50%, 60% and 75% respectively
  • the monomer resin is phenoxybenzyl acrylate
  • the stabilizer is Octylphenol polyoxyethylene ether is added in an amount of 5% of the mass of nano-zirconia
  • the refractive index modifier is ethylene glycol ether, and its amount is added in an amount of 5% of the mass of nano-zirconia.
  • a stabilizer and a refractive index adjuster are added to the above monomer pre-dispersion liquid, and the dispersion is continued for 30 minutes to obtain a zirconium oxide monomer dispersion liquid.
  • Examples 2 to 14 respectively provide a zirconium oxide monomer dispersion, the specific composition of which is shown in Table 1.
  • the preparation method of the zirconium oxide monomer dispersion provided in Example 2 to Example 14 is the same as that in Example 1.
  • Comparative Example 1 to Comparative Example 7 respectively provide a zirconium oxide monomer dispersion, and the specific composition is as shown in Table 1.
  • the preparation method of the zirconium oxide monomer dispersion provided in Comparative Example 1 to Comparative Example 7 is the same as that in Example 1.
  • the amount of stabilizer added in Table 1 refers to the mass percentage of stabilizer in nano-zirconia
  • the amount of refractive index modifier added refers to the mass percentage of refractive index modifier in nano-zirconia
  • the mass fraction of nano-zirconia is Refers to the mass fraction of nano-zirconia in the zirconia monomer dispersion.
  • the refractive index matching between the monomer resin and nano-zirconia When the refractive index matching between the monomer resin and nano-zirconia is high, it will have a positive effect on improving the transmittance of the system.
  • the refractive index matching degree of nanometer zirconia and the monomer resins PBA, BPMA, BZA and OPPEA in the present disclosure is higher than the refractive index matching degree of 2-EHA in Comparative Example 7. Therefore, the zirconia prepared in Examples 1-4 The transmittance of the monomer dispersion is significantly higher than that of Comparative Example 7.
  • Example 5 the added amount of stabilizer and refractive index adjuster is 1wt%, which is lower than 5wt% in Example 1. Its dispersion effect and refractive index adjustment effect are lower than those in Example 1. Therefore, in Example 5, the monomer The transmittance of the dispersion was lower than that of Example 1.
  • Example 6 the added amount of stabilizer and refractive index adjuster is 10wt%, which is higher than the 5wt% in Example 1.
  • the addition of high content of stabilizer and refractive index adjuster will affect the refractive index matching of each component of the entire system. This affects the transmittance of the system, resulting in the transmittance of the monomer dispersion of Example 6 being lower than that of Example 1.
  • the dosage of stabilizer and refractive index adjuster should be controlled within a reasonable range, otherwise it will not only have the opposite effect, but also increase the cost. Comparative Examples 5 and 6 can also illustrate this point.
  • the zirconia monomer dispersion provided by the present disclosure is mainly made of nano zirconia, monomer resin, stabilizer, refractive index adjuster and other raw materials.
  • nano zirconia is used as inorganic dispersed particles, which can reduce the light sensitivity of the particles.
  • the scattering effect increases the transmittance of the system;
  • stabilizers can improve the dispersion and uniformity of the zirconia monomer dispersion.
  • the addition of refractive index adjusters can improve the refraction of each raw material in the entire system. The rate is more matched, thereby improving the transmittance of the system.
  • the optical film produced by using it has good optical properties.

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Abstract

本公开提供了一种氧化锆单体型分散液及其制备方法、光学膜和显示屏，涉及氧化锆技术领域。该氧化锆单体型分散液主要由纳米氧化锆、单体树脂、稳定剂和折射率调节剂等原料制成，其中，采用纳米氧化锆作为无机分散粒子，可以降低微粒对光的散射作用，从而提高体系的透射率；稳定剂的加入可提高氧化锆单体型分散液的分散性及均一性；此外，折射率调节剂的加入，可使整个体系中的各原料的折射率更加匹配，从而提高体系的透射率。本公开还提供了上述氧化锆单体型分散液的制备方法，工艺简单，整个分散过程中无需中间相的参与，可大大缩减工艺步骤，降低成本。

Description

氧化锆单体型分散液及其制备方法、光学膜和显示屏
相关申请的交叉引用
本申请要求于2022年03月18日提交中国专利局的申请号为202210271565.8、名称为“氧化锆单体型分散液及其制备方法、光学膜和显示屏”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本公开涉及氧化锆技术领域，尤其是涉及一种氧化锆单体型分散液及其制备方法、光学膜和显示屏。
背景技术
近年来，通过氧化锆颗粒分散体与透明树脂或薄膜结合得到单体型氧化锆分散液在光学领域中得到很好的应用。例如，利用氧化锆单体型分散液制备增亮膜等光学膜，可用在LCD显示器上，增加屏幕的亮度和清晰度。
上述的用途中，氧化锆的一次粒径和单体树脂中氧化锆的二次聚集粒径与可见光线的波长(380～800nm)相近时，由于氧化锆颗粒带来的散射的影响，会导致单体树脂或膜体系出现白浊，无法得到所需的透明性。因此，亟待开发一种将氧化锆颗粒以微粒的形式分散于树脂中的透明性高的氧化锆分散液。
尽管现今已有一些单体型分散液被成功制备，但是其大多存在透射率差的问题，以至于在应用到下游显示领域中时影响效果的发挥。例如，专利CN 106268394 B公开了一种氧化锆微粒或其分散液的制备方法，其氧化锆水分散液含量为20％重量以上时，在波长400nm下的透射率为35％以上，波长800nm下的透射率为95％以上，温度25℃下的粘度为20mPa·s以下。但是，该专利中并未涉及有关氧化锆单体型分散液透射率的内容，氧化锆单体型分散液是一个有机-无机复合体系，各组分之间相互影响且影响因素复杂，特别是体系中各组分的折射率，体系中氧化锆粒子的稳定性以及体系的透射率之间难以相互平衡，若一味地追求某一方面的高指标，必然会带来另一方面指标的降低。因此，开发一种工艺简单、体系中各项指标协调、符合实际应用的具备较高透光率的单体型分散液具有重要意义。
有鉴于此，特提出本公开。
公开内容
本公开的目的包括提供一种氧化锆单体型分散液及其制备方法，以缓解现有技术中存在的至少一个技术问题。
为了实现上述目的，本公开的技术方案如下：
本公开提供了一种氧化锆单体型分散液，包括以下原料：
纳米氧化锆、单体树脂、稳定剂和折射率调节剂；
其中，所述纳米氧化锆占所述氧化锆单体型分散液的质量分数为50-75％；
所述稳定剂的质量为所述纳米氧化锆质量的1-10％；
所述折射率调节剂的质量为所述纳米氧化锆质量的1-10％；
所述单体树脂包括苯氧苄丙烯酸酯、联苯甲醇丙烯酸酯、苄基丙烯酸酯或邻苯基苯氧乙基丙烯酸酯中的任意一种或至少两种的组合。
可选的，所述纳米氧化锆的平均粒径为1-20nm。
可选的，所述稳定剂的结构为R-X n；
其中，R选自烷基、磺酸基、磷酸基、酰胺基、羧基、羟基、芳环或取代型芳环中的任意一种或至少两种的组合；
X选自聚醚链、丙烯酸酯链、聚酯链或烷基链中的任意一种或至少两种的组合；
n为1-3之间的整数。
可选的，所述稳定剂包括辛基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、三乙基己基磷酸、硬脂酰胺或丙烯酸羟丙酯中的任意一种或至少两种的组合。
可选的，所述折射率调节剂的结构为A-B m；
其中，A选自取代或未取代的丙烯酰氧基、亚甲基、烷氧基、碳碳双键、硅碳基或烷基中的任意一种或至少两种的组合；
B选自羟基、羰基、酯基、硅氧基、烷氧基、羧基、取代或未取代芳环中的任意一种或至少两种的组合；
m为1-3之间的整数。
可选的，所述折射率调节剂包括乙二醇乙醚、4-(4-丙烯酰氧基丁氧基)-苯甲酸或三(甲氧基乙氧基)丙基酰氧基硅烷中的任意一种或至少两种的组合。
本公开还提供了一种氧化锆单体型分散液的制备方法，包括以下步骤：
将所述纳米氧化锆与单体树脂混合后进行一次分散，然后再与所述稳定剂和折射率调节剂混合后进行二次分散，得到氧化锆单体型分散液。
可选的，所述一次分散的时间为30-90min；
优选的，所述二次分散的时间为30-60min；
优选的，所述一次分散和二次分散均采用分散设备进行分散。
本公开还提供了一种光学膜，采用上述的氧化锆单体型分散液制成。
与现有技术相比，本公开具有如下有益效果：
(1)本公开提供了一种氧化锆单体型分散液，主要由纳米氧化锆、单体树脂、稳定剂和折射率调节剂等原料制成，其中，采用纳米氧化锆作为无机分散粒子，可以降低微粒对光的散射作用，从而提高体系的透射率；稳定剂的加入可提高氧化锆单体型分散液的分散性及均一性，此外，折射率调节剂的加入，可使整个体系中的各原料的折射率更加匹配，从而提高体系的透射率。
(2)本公开提供了一种氧化锆单体型分散液的制备方法，先将纳米氧化锆与单体树脂混合后进行一次分散，然后再与稳定剂和折射率调节剂混合后进行二次分散，得到氧化锆单体型分散液；该制备方法工艺简单，整个分散过程中无需中间相的参与，可大大缩减工艺步骤，降低成本。
(3)本公开提供了一种光学膜，采用上述的氧化锆单体型分散液制成。鉴于上述氧化锆单体型分散液所具有的优势，使得所制得的光学膜具有良好的光学性能。
(4)本公开还提供了一种显示屏，包含上述光学膜。鉴于上述光学膜所具有的优势，使得显示屏具有良好的亮度和清晰度。
具体实施方式
下面将结合实施方式和实施例对本公开的实施方案进行详细描述，但是本领域技术人员将会理解，下列实施方式和实施例仅用于说明本公开，而不应视为限制本公开的范围。未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
根据本公开的第一个方面，提供了一种氧化锆单体型分散液，包括以下原料：
纳米氧化锆、单体树脂、稳定剂和折射率调节剂；
其中，纳米氧化锆占氧化锆单体型分散液的质量分数为50-75％；
稳定剂的质量为纳米氧化锆质量的1-10％；
折射率调节剂的质量为纳米氧化锆质量的1-10％；
单体树脂包括苯氧苄丙烯酸酯、联苯甲醇丙烯酸酯、苄基丙烯酸酯或邻苯基苯氧乙基丙烯酸酯中的任意一种或至少两种的组合。
在本公开中，纳米氧化锆的来源不作限定，可市售得到，也可采用本领域常规的制备方法自行制备得到。
对于单体树脂的种类有一定的限定，使其对于纳米氧化锆具有良好的分散能力，且无需中间相的参与，同时还具有与纳米氧化锆相匹配的折射率。
该氧化锆单体型分散液中选用纳米氧化锆作为无机分散粒子，一方面由于其具有较小的粒径，可以降低微粒对光的散射作用，从而提高体系的透射率，另一方面，纳米氧化锆的折射率还与本公开特定种类的单体树脂的折射率具有良好的匹配程度，这可大大降低体系对光的散射程度，从而提高体系的透射率。
稳定剂的加入可使得纳米氧化锆不易团聚，具有较好的稳定性，从而保持体系具有较高的透射率。
折射率调节剂可使纳米氧化锆与单体树脂的折射率匹配度更高，从而使得整个体系具有较高的透射率。
对于氧化锆单体型分散液中各原料的用量有一定的限定。
纳米氧化锆占典型但非限制性的质量分数为50％、52％、54％、56％、58％、60％、62％、64％、65％、66％、68％、70％、72％、74％或75％。
由于单体树脂主要是分散纳米氧化锆，其用量只要确保纳米氧化锆在氧化锆单体型分散液中的质量分数达到50-75％即可。
稳定剂和折射率调节剂的加入量以纳米氧化锆的质量进行计算。
稳定剂占纳米氧化锆典型但非限制性的质量分数为1％、2％、3％、4％、5％、6％、7％、8％、9％或10％。若稳定剂占纳米氧化锆的质量分数过低(低于1％)，则起不到稳定体系、提高体系透射率的作用；稳定剂占纳米氧化锆的质量分数过高(高于10％)，则会对整个体系各组分的折射率匹配度产生影响，导致达不到预期效果，且会增加成本。
折射率调节剂占纳米氧化锆典型但非限制性的质量分数为1％、2％、3％、4％、5％、6％、7％、8％、9％或10％。若折射率调节剂占纳米氧化锆的质量分数过低(低于1％)，则起不到调节体系折射率匹配度的作用；折射率调节剂占纳米氧化锆的质量分数过高(高于10％)，则容易导致达不到预期效果，且会增加成本。
本公开提供了一种氧化锆单体型分散液，主要由纳米氧化锆、单体树脂、稳定剂和折射率调节剂等原料制成，其中，采用纳米氧化锆作为无机分散粒子，可以降低微粒对光的散射作用，从而提高体系的透射率；稳定剂的加入可提高氧化锆单体型分散液的分散性及均一性，此外，折射率调节剂的加入，可使整个体系中的各原料的折射率更加匹配，从而 提高体系的透射率。通过上述各原料之间的配合作用，使得该氧化锆单体型分散液具有较高的稳定性和透射率。
作为本公开的一种可选实施方式，纳米氧化锆的平均粒径为1-20nm。纳米氧化锆典型但非限制性的粒径例如为1nm、2nm、4nm、5nm、6nm、8nm、10nm、12nm、14nm、15nm、16nm、18nm或20nm。
通过对纳米氧化锆的平均粒径的限定，有利于提高体系的折射率。
作为本公开的一种可选实施方式，稳定剂的结构为R-X n，其中，R为锚定基团，可以与纳米氧化锆发生锚定作用，X为溶剂化基团，可以与单体树脂发生作用。
其中，R选自烷基、磺酸基、磷酸基、酰胺基、羧基、羟基、芳环或取代型芳环中的任意一种或至少两种的组合。
X选自聚醚链、丙烯酸酯链、聚酯链或烷基链中的任意一种或至少两种的组合。
n为1-3的整数，例如可为1、2或3。
作为本公开的一种可选实施方式，稳定剂包括辛基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、三乙基己基磷酸、硬脂酰胺或丙烯酸羟丙酯中的任意一种或至少两种的组合。
通过对稳定剂结构中R和X基团种类以及稳定剂种类的具体限定，使得稳定剂能够更好地与氧化锆粒子及单体树脂进行作用，以提高体系透射率。
作为本公开的一种可选实施方式，折射率调节剂的结构为A-B m；
其中，A选自取代或未取代的丙烯酰氧基、烷氧基、碳碳双键、烷基或硅氧基中的任意一种或至少两种的组合。
B选自羟基、羰基、酯基、硅碳基、羧基、取代或未取代芳环中的任意一种或至少两种的组合。
m为1-3的整数，例如可为1、2或3。
作为本公开的一种可选实施方式，折射率调节剂包括乙二醇乙醚、4-(4-丙烯酰氧基丁氧基)-苯甲酸或三(甲氧基乙氧基)丙基酰氧基硅烷中的任意一种或至少两种的组合。
通过对折射率调节剂结构中A基团和B基团种类以及折射率调节剂种类的具体限定，使得折射率调节剂与整个有机无机体系匹配，从而更好的调节体系折射率，降低体系光散射，提高体系透射率。
根据本公开的第二个方面，还提供了一种氧化锆单体型分散液的制备方法，包括以下步骤：
将纳米氧化锆与单体树脂混合后进行一次分散，然后再与稳定剂和折射率调节剂混合后进行二次分散，得到氧化锆单体型分散液。
该制备方法中先将纳米氧化锆与单体树脂混合后进行一次分散，然后再与稳定剂和折射率调节剂混合后进行二次分散，该制备方法工艺简单，整个分散过程中无需中间相的参与，可大大缩减工艺步骤，降低成本。
作为本公开的一种可选实施方式，一次分散的时间为30-90min。典型但非限制性的一次分散的时间为30min、40min、50min、60min、70min、80min或90min。
作为本公开的一种可选实施方式，二次分散的时间为30-60min。典型但非限制性的二次分散的时间为30min、40min、50min或60min。
作为本公开的一种可选实施方式，一次分散和二次分散均采用分散设备进行分散。
此处所述的分散设备可以理解为该领域任何一种可以使物料以较小液滴形式分散于相应介质中的设备或技术手段，包括但不限于机械搅拌、磁力搅拌、超声、均质机、胶体磨等。
根据本公开的第三个方面，还提供了一种光学膜，采用上述的氧化锆单体型分散液制成。
鉴于上述氧化锆单体型分散液所具有的优势，使得所制得的光学膜具有良好的光学性能。
根据本公开的第四个方面，还提供了一种显示屏，包含上述光学膜。
鉴于上述光学膜所具有的优势，使得显示屏具有良好的亮度和清晰度。
下面结合实施例和对比例对本公开提供的技术方案做进一步的描述。
实施例1
本实施例提供了一种氧化锆单体型分散液，包括以下原料：
纳米氧化锆、单体树脂、稳定剂和折射率调节剂；
其中，纳米氧化锆的平均粒径为10nm，纳米氧化锆占氧化锆单体型分散液的质量分数分别为50％、60％和75％，单体树脂为苯氧苄丙烯酸酯，稳定剂为辛基酚聚氧乙烯醚，其添加量为纳米氧化锆质量的5％；折射率调节剂为乙二醇乙醚，其添加量为纳米氧化锆质量的5％。
本实施例提供的氧化锆单体型分散液的制备方法包括以下步骤：
将纳米氧化锆在分散设备辅助下分散于单体树脂中，并持续分散30min，得到单体型预分散液；
然后向上述单体型预分散液中添加稳定剂和折射率调节剂，并持续分散30min，得到氧化锆单体型分散液。
实施例2-实施例14
实施例2-实施例14分别提供了一种氧化锆单体型分散液，具体组成如表1所示。
实施例2-实施例14提供的氧化锆单体型分散液的制备方法与实施例1相同。
对比例1-对比例7
对比例1-对比例7分别提供了一种氧化锆单体型分散液，具体组成如表1所示。
对比例1-对比例7提供的氧化锆单体型分散液的制备方法与实施例1相同。
需要说明的是，表1中稳定剂添加量是指稳定剂占纳米氧化锆的质量百分数，折射率调节剂添加量是指折射率调节剂占纳米氧化锆的质量百分数，纳米氧化锆质量分数是指纳米氧化锆占氧化锆单体型分散液的质量分数。
同时，对各实施例和对比例所制得的氧化锆单体型分散液在650nm波长下的透射率进行检测，通过紫外可见分光光度计(青岛蓝特思科教仪器公司制造的C-7100)进行测定。具体结果如表1所示。
表1
Figure PCTCN2022119288-appb-000001
Figure PCTCN2022119288-appb-000002
Figure PCTCN2022119288-appb-000003
从表1中数据可以看到，与对比例1-4相比，由于实施例中既添加了稳定剂又添加了折射率调节剂，氧化锆单体型分散液的分散效果及折射率调节效果均好于对比例1-4，所以实施例中单体型分散液的透射率明显高于对比例。
当单体树脂与纳米氧化锆折射率匹配度较高时，对提高体系的透射率具有积极作用。本公开中纳米氧化锆与单体树脂PBA、BPMA、BZA和OPPEA的折射率匹配度高于对比例7中2-EHA的折射率匹配度，因此，实施例1-4中所制备的氧化锆单体分散液的透射率明显高于对比例7。
实施例5中稳定剂及折射率调节剂添加量为1wt％，低于实施例1中的5wt％，其分散效果及折射率调节效果低于实施例1，因此，实施例5中单体型分散液的透射率低于实施例1。实施例6中稳定剂及折射率调节剂添加量为10wt％，高于实施例1中的5wt％，高含量稳定剂及折射率调节剂的添加会对整个体系各组分的折射率匹配度产生影响，进而影响体系的透射率，导致实施例6单体型分散液的透射率低于实施例1。以上说明，稳定剂及折射率调节剂用量应控制在合理范围，否则不但会起到相反效果，而且会造成成本的升高。对比例5、6也能说明这一点。
尽管已用具体实施例来说明和描述了本公开，然而应意识到，在不背离本公开的精神和范围的情况下可以作出许多其它的更改和修改。因此，这意味着在所附权利要求中包括属于本公开范围内的所有这些变化和修改。
工业实用性
本公开提供的氧化锆单体型分散液，主要由纳米氧化锆、单体树脂、稳定剂和折射率调节剂等原料制成，其中，采用纳米氧化锆作为无机分散粒子，可以降低微粒对光的散射作用，从而提高体系的透射率；稳定剂的加入可提高氧化锆单体型分散液的分散性及均一性，此外，折射率调节剂的加入，可使整个体系中的各原料的折射率更加匹配，从而提高 体系的透射率。鉴于氧化锆单体型分散液所具有的优势，使得应用其所制得的光学膜具有良好的光学性能。

Claims (12)

  1. 一种氧化锆单体型分散液，其特征在于，包括以下原料：
    纳米氧化锆、单体树脂、稳定剂和折射率调节剂；
    其中，所述纳米氧化锆占所述氧化锆单体型分散液的质量分数为50-75％；
    所述稳定剂的质量为所述纳米氧化锆质量的1-10％；
    所述折射率调节剂的质量为所述纳米氧化锆质量的1-10％；
    所述单体树脂包括苯氧苄丙烯酸酯、联苯甲醇丙烯酸酯、苄基丙烯酸酯或邻苯基苯氧乙基丙烯酸酯中的任意一种或至少两种的组合。
  2. 根据权利要求1所述的氧化锆单体型分散液，其特征在于，所述纳米氧化锆的平均粒径为1-20nm。
  3. 根据权利要求1所述的氧化锆单体型分散液，其特征在于，所述稳定剂的结构为R-X n；
    其中，R选自烷基、磺酸基、磷酸基、酰胺基、羧基、羟基、芳环或取代型芳环中的任意一种或至少两种的组合；
    X选自聚醚链、丙烯酸酯链、聚酯链或烷基链中的任意一种或至少两种的组合；
    n为1-3之间的整数。
  4. 根据权利要求3所述的氧化锆单体型分散液，其特征在于，所述稳定剂包括辛基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、三乙基己基磷酸、硬脂酰胺或丙烯酸羟丙酯中的任意一种或至少两种的组合。
  5. 根据权利要求1所述的氧化锆单体型分散液，其特征在于，所述折射率调节剂的结构为A-B m；
    其中，A选自取代或未取代的丙烯酰氧基、亚甲基、烷氧基、碳碳双键、硅碳基或烷基中的任意一种或至少两种的组合；
    B选自羟基、羰基、酯基、硅氧基、烷氧基、羧基、取代或未取代芳环中的任意一种或至少两种的组合；
    m为1-3之间的整数。
  6. 根据权利要求5所述的氧化锆单体型分散液，其特征在于，所述折射率调节剂包括乙二醇乙醚、4-(4-丙烯酰氧基丁氧基)-苯甲酸或三(甲氧基乙氧基)丙基酰氧基硅烷中的任意一种或至少两种的组合。
  7. 一种氧化锆单体型分散液的制备方法，其特征在于，包括以下步骤：
    将所述纳米氧化锆与单体树脂混合后进行一次分散，然后再与所述稳定剂和折射率调节剂混合后进行二次分散，得到氧化锆单体型分散液。
  8. 根据权利要求7所述的氧化锆单体型分散液的制备方法，其特征在于，所述一次分散的时间为30-90min。
  9. 根据权利要求7所述的氧化锆单体型分散液的制备方法，其特征在于，所述二次分散的时间为30-60min。
  10. 根据权利要求7所述的氧化锆单体型分散液的制备方法，其特征在于，所述一次分散和二次分散均采用分散设备进行分散。
  11. 一种光学膜，其特征在于，采用权利要求1-6任一项所述的氧化锆单体型分散液制成。
  12. 一种显示屏，其特征在于，包含权利要求11所述的光学膜。
PCT/CN2022/119288 2022-03-18 2022-09-16 氧化锆单体型分散液及其制备方法、光学膜和显示屏 WO2023173712A1 (zh)

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