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CN-121991532-A - Nano metal oxide modification method, modified nano titanium dioxide particles and application thereof

CN121991532ACN 121991532 ACN121991532 ACN 121991532ACN-121991532-A

Abstract

The invention belongs to the technical field of materials, and particularly relates to a nano metal oxide modification method, modified nano titanium dioxide particles and application thereof. The method comprises the following steps of S1, preparing nano titanium dioxide particles by a hydrothermal method, S2, dispersing the nano titanium dioxide particles in a solvent to prepare nano titanium dioxide particle dispersion liquid, S3, adjusting the nano titanium dioxide particle dispersion liquid to an acidic or neutral condition, dropwise adding a metal modifier into the nano titanium dioxide particle dispersion liquid, stirring for reaction, and vacuum drying to obtain modified nano titanium dioxide particles, wherein the metal modifier is a zirconate coupling agent. The modified nano titanium dioxide particles provided by the invention are applied to optical cement, so that the modified nano titanium dioxide particles not only have good optical performance, but also have outstanding light resistance.

Inventors

  • MU GUANGYUAN
  • JIN JIANGJIANG
  • HUANG JING
  • YAO KUN

Assignees

  • 武汉尚赛光电科技有限公司

Dates

Publication Date
20260508
Application Date
20251231

Claims (10)

  1. 1. The nano metal oxide modification method is characterized by comprising the following steps of: s1, preparing nano titanium dioxide particles by a hydrothermal method; S2, dispersing nano titanium dioxide particles in a solvent to prepare nano titanium dioxide particle dispersion liquid; s3, regulating the nano titanium dioxide particle dispersion liquid to an acidic or neutral condition, dropwise adding a metal modifier into the nano titanium dioxide particle dispersion liquid, stirring for reaction, and vacuum drying to obtain modified nano titanium dioxide particles; the metal modifier is a zirconate coupling agent.
  2. 2. A method for modifying a nano metal oxide according to claim 1, wherein the central metal atom of the zirconate coupling agent is Zr and comprises at least one saturated or unsaturated alkoxy hydrolysis group.
  3. 3. The method for modifying nano metal oxide according to claim 2, wherein: The structural formula of the zirconate coupling agent is Zr (OR 1 )p(R 2 ) q, p+q=4, and p >0; R 1 is saturated or unsaturated alkyl of C 1-20 , R 2 is one of saturated or unsaturated alkyl of C 1-20 and alkyl substituted phenyl of C 1-20 , the alkylene part of the substituent of the alkyl substituted phenyl of C 1-20 is interrupted by N atom, O atom, ester bond, acyl, sulfonate bond, phosphate bond, pyrophosphate bond, sulfonate group and sulfonate group, and H at the terminal position of R 2 is substituted or unsubstituted by a reactive group.
  4. 4. A method of modifying a nano-metal oxide according to claim 3, wherein the saturated or unsaturated alkyl group of C 1-20 is selected from the group consisting of saturated alkyl groups of C 1-6 which are substituted or unsubstituted at the end with alkenyl groups, the reactive group is selected from the group consisting of amine groups, hydroxyl groups, (meth) acrylate groups, carboxyl groups, epoxy groups, vinyl groups and mercapto groups, p is 1 and q is 3.
  5. 5. The method for modifying nano metal oxide according to claim 1, wherein the nano titanium dioxide particles have a size of 10-1000 nm.
  6. 6. The method for modifying nano metal oxide according to claim 1, wherein the weight ratio of the nano titanium dioxide particles to the metal modifier is 1 (0.01-0.2).
  7. 7. The modification method of the nano metal oxide according to claim 1, wherein the hydrothermal method is characterized in that a titanium source is taken as a precursor, water, an organic solvent or a mixed solution of the titanium source and the organic solvent is taken as a reaction medium, the mixture is stirred uniformly to obtain a precursor solution, an acidic solution is added to adjust the pH value, the mixture is put into a polytetrafluoroethylene high-pressure reaction kettle to react for 18-24 hours at 120-240 ℃, and a precipitate obtained after the suspension is centrifuged is washed, dried and ground to obtain crystalline nano titanium dioxide.
  8. 8. The method for modifying nano metal oxide according to claim 7, wherein: The titanium source is selected from one or more of titanate, titanium tetrachloride and titanium sulfate; the organic solvent is selected from any one or more of ethanol, chloroform, ethyl acetate, isopropanol, ethylene glycol, cyclohexane and acetone; The solvent in the nano titanium dioxide particle dispersion liquid is selected from any one or a combination of more of ethanol, chloroform, ethyl acetate, isopropanol, glycol, cyclohexane and acetone, and the mass fraction of titanium dioxide in the nano titanium dioxide particle dispersion liquid is 15-40%.
  9. 9. Modified nano-titania particles prepared by the method according to any one of claims 1 to 8.
  10. 10. Use of modified nano-titania particles according to claim 9 for the preparation of ink materials or gels in display devices.

Description

Nano metal oxide modification method, modified nano titanium dioxide particles and application thereof Technical Field The invention belongs to the technical field of materials, and particularly relates to a nano metal oxide modification method, modified nano titanium dioxide particles and application thereof. Background In the field of development of optical resin compositions, in order to achieve a high refractive index of a material, it is generally adopted in the prior art to add high refractive index nanoparticles (such as ZrO 2,TiO2) into an organic material, so that the refractive index of the material can be effectively increased to 1.66, or even more than 1.70. However, in the actual industrialized application process, the technical means has obvious technical defects that Van der Waals force among hydroxyl groups on the surfaces of TiO 2 particles is generated, the repulsive force among powder is changed into attractive force by hydrogen bond generation, and the agglomeration phenomenon among TiO 2 particles is enhanced. In addition, since titanium dioxide itself has strong photochemical activity, when TiO 2 is irradiated by light (especially ultraviolet light), valence band electrons are excited to conduction bands to form electron-hole pairs, and these high-activity electrons and holes can react with water or oxygen to generate hydroxyl free radicals and superoxide anions with strong oxidizing ability, so that problems of yellowing, aging and the like are caused, and key service properties such as light transmittance, mechanical properties, weather resistance and the like of the optical resin composition are directly reduced. These technical drawbacks severely restrict the quality improvement and application expansion of the high refractive index optical resin composition in the high-end optical field (such as optical lenses, display devices, etc.). Based on this, titanium dioxide is surface-modified prior to use. At present, the common modification means is surface modification of a coupling agent, wherein one part of functional groups in molecules can react with active groups on the surface of nano TiO 2 powder to form strong chemical bonding, so that the surface of titanium dioxide is coated by the coupling agent, a modified product of TiO 2 has good dispersion performance in an organic matter, and the other part of functional groups can perform certain chemical reaction or physical winding with an organic polymer to enable nano TiO 2 and an organic medium to generate a special functional 'molecular bridge', so that the comprehensive performance of the nano composite material is improved. However, it should be noted that the existing coupling agent surface modification technology can only solve the agglomeration problem and interface combination problem of the TiO 2 nano particles, and can not effectively regulate and control the photochemical activity of the TiO 2 nano particles, so that the problems of yellowing, aging and the like of the organic polymer caused by the photocatalytic activity can not be solved. Therefore, development of a surface modification means for TiO 2 nanoparticles is needed, and on the basis of ensuring the dispersibility and refractive index improvement effect of TiO 2 nanoparticles, the problem of yellowing of organic polymers caused by photocatalytic activity is effectively solved, so as to meet the performance requirements of high-end optical resin compositions. Disclosure of Invention In order to solve the defects in the prior art, the invention provides a nano metal oxide modification method, modified nano titanium dioxide particles and application thereof. The technical scheme provided by the invention is as follows: A method for modifying nano metal oxide, comprising the following steps: s1, preparing nano titanium dioxide particles by a hydrothermal method; S2, dispersing nano titanium dioxide particles in a solvent to prepare nano titanium dioxide particle dispersion liquid; s3, regulating the nano titanium dioxide particle dispersion liquid to an acidic or neutral condition, dropwise adding a metal modifier into the nano titanium dioxide particle dispersion liquid, stirring for reaction, and vacuum drying to obtain modified nano titanium dioxide particles; the central metal atom of the metal modifier is a zirconate coupling agent. Further, the central metal atom of the metal modifier is Zr and at least contains one saturated or unsaturated alkoxy hydrolysis group. Further, the metal modifier is selected from the group consisting of saturated OR unsaturated alkyl groups of the structural formula Zr (OR 1)p(R2)q,p+q=4,p＞0;R1 is C 1-20, R 2 is C 1-20, saturated OR unsaturated alkyl, C 1-20 and phenyl substituted by alkyl, the alkylene portion of the substituent represented by R 2 may be interrupted by N atom, O atom, ester bond, acyl, sulfonate bond, phosphate bond, pyrophosphate bond, sulfonate acyloxy, and H at the terminal position on R 2 may be substitute