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CN-121991751-A - Nano metal oxide perfluoropolyether oil phase dispersion and supergravity synthesis method thereof

CN121991751ACN 121991751 ACN121991751 ACN 121991751ACN-121991751-A

Abstract

The invention discloses a nano metal oxide perfluoropolyether oil phase dispersion and a supergravity synthesis method thereof, belonging to the technical field of material preparation. The dispersion consists of surfactant modified nano metal oxide particles and perfluoropolyether base oil in a mass ratio of 1:5-1:100. The synthesis method is completed through the steps of metal salt dissolution, hypergravity reaction for preparing metal hydroxide, oxidation conversion, in-situ surface modification and ultrasonic dispersion, and the hypergravity field-enhanced mass transfer is performed to precisely control the particle size of particles. The dispersion is transparent or semitransparent, the average particle diameter of the nano particles is 3-15nm, the dispersion is stable in an acid-base environment with the pH value of 1-14 and a temperature range of minus 40-200 ℃, and the dispersion is suitable for extreme working conditions such as aerospace, military industry and the like and has wide application prospect.

Inventors

  • ZENG XIAOFEI
  • HUANG CONGJUN
  • CHEN JIANFENG
  • MAO WEI
  • WANG JIEXIN

Assignees

  • 北京化工大学
  • 衢州化工新材料创新研究院

Dates

Publication Date
20260508
Application Date
20260128

Claims (10)

  1. 1. A nano metal oxide perfluoropolyether oil phase dispersion is characterized in that the dispersion comprises surfactant modified nano metal oxide particles and perfluoropolyether base oil in a mass ratio of 1:5-1:100.
  2. 2. The nano metal oxide perfluoropolyether oil phase dispersion of claim 1, wherein the nano metal oxide particles are one or more of cerium oxide, zinc oxide, and titanium oxide.
  3. 3. The nano metal oxide perfluoro polyether oil phase dispersion of claim 1, wherein the surfactant is one or more of perfluoro polyether carboxylic acid, perfluoro alkyl amine, perfluoro suberic acid, perfluoro dodecanoic acid, 1H, 2H-perfluoro decyl amine and perfluoro polyether silane coupling agent.
  4. 4. A process for the preparation of a nano metal oxide perfluoropolyether oil phase dispersion as claimed in any one of claims 1 to 3, comprising the steps of: s1, dissolving metal salt in methanol, and stirring and dissolving to obtain a metal salt solution; s2, feeding methanol into a hypergravity reactor, and after a flow field is stable, sequentially adding an alkali source solution and the metal salt solution in the step S1, and carrying out a cyclic mixing reaction to obtain a metal hydroxide solution; S3, introducing oxygen or adding an oxidant into the hypergravity reactor to oxidize the metal hydroxide solution into a metal oxide solution; S4, adding a surfactant into the hypergravity reactor for cyclic modification, washing, centrifuging and drying to obtain the oil-soluble modified nano metal oxide; S5, ultrasonically dispersing the oil-soluble modified nano metal oxide in the step S4 into the perfluoropolyether base oil to form uniform and stable transparent or semitransparent oil phase dispersion.
  5. 5. The method for preparing a nano metal oxide perfluoropolyether oil phase dispersion according to claim 4, wherein in step S1, the metal salt is one or more of cerium nitrate, cerium chloride, cerium sulfate, cerium perchlorate, zinc sulfate, zinc nitrate, zinc chloride, titanium tetrachloride, titanyl sulfate, and titanyl nitrate; The concentration of the metal salt solution is 0.2M-0.25M.
  6. 6. The method of claim 4, wherein in the step S2, the volume ratio of the metal salt solution, the methanol solution and the alkali source solution is 50:20:4.1.
  7. 7. The method of claim 4, wherein in step S2, the alkali source solution is one or more of sodium hydroxide solution, potassium hydroxide solution, sodium carbonate solution, and ammonia solution.
  8. 8. The method of claim 4, wherein in step S3, the oxidizing agent is one or both of hydrogen peroxide and sodium hypochlorite.
  9. 9. The method for preparing a nano metal oxide perfluoropolyether oil phase dispersion according to claim 4, wherein in step S4, the cyclic modification time is 1-20min; The polar organic solvent used in washing and centrifuging is one or more of methanol, tetrahydrofuran and acetone.
  10. 10. The method for preparing a nano metal oxide perfluoropolyether oil phase dispersion according to claim 4, wherein the temperature of the reaction system of the supergravity reactor is 40-100 ℃.

Description

Nano metal oxide perfluoropolyether oil phase dispersion and supergravity synthesis method thereof Technical Field The invention relates to the technical field of material preparation, in particular to a nano metal oxide perfluoropolyether oil phase dispersion and a supergravity synthesis method thereof. Background Nanoparticles exhibit broad application potential due to their unique small-size effects, surface effects, quantum size effects, interface effects, and macroscopic quantum tunneling effects. The nano metal oxide as one new kind of functional material is used widely as catalyst material, ultraviolet absorber, polishing powder, antiwear and antifriction material and luminescent material. The performance of nano metal oxide is closely related to the structure, morphology, size and size distribution of the nano metal oxide and the chemical and physical environment of the nano metal oxide, and the properties can be regulated and controlled by adopting different synthesis methods. In the lubrication field, tribological mechanisms of nano particles used as a lubricating additive mainly include a deposited film mechanism, an ultra-smooth rolling friction mechanism, a penetration and tribochemical reaction film mechanism, a ball mechanism and a composite mechanism. Therefore, the research on controllable preparation technology of nano metal oxide and the exploration of proper reaction conditions enable the nano metal oxide to be stably dispersed in the perfluoropolyether base lubricating oil have important significance for improving the oil performance. In the prior art, chinese patent CN117551492A discloses a method for improving antifriction, wear resistance and self-repairing performance of lubricating oil by adding an attapulgite/nano cerium oxide composite material, and the method can improve the performance of the lubricating oil, but the adopted plant-mediated synthesis method is complex in flow, harsh in condition and high in energy consumption, the prepared nano cerium oxide still has agglomeration risk on the surface of the attapulgite, the composite material is hydrophilic, and the composite material must rely on subsequent long-time sanding modification to be stably dispersed in the oil, so that the process is complicated, the cost is high, and the large-scale application of the composite material is restricted. Disclosure of Invention The invention aims to provide a nano metal oxide perfluoropolyether oil phase dispersion and a supergravity synthesis method thereof, wherein the supergravity method is combined with modification of a perfluorinated surfactant to realize high-stability dispersion of nano particles in fluorine oil, and the prepared oil phase dispersion can be applied to acid-alkali environments and has a wide working temperature range. To achieve the above object, the present invention provides a nano metal oxide perfluoropolyether oil phase dispersion comprising surfactant-modified nano metal oxide particles and perfluoropolyether base oil in a mass ratio of 1:5 to 1:100. Preferably, the nano metal oxide particles are one or more of cerium oxide, zinc oxide and titanium oxide. Preferably, the surfactant is one or more of perfluoropolyether carboxylic acid, perfluoroalkyl amine, perfluorosuberic acid, perfluorododecanoic acid, 1H, 2H-perfluorodecylamine, and perfluoropolyether silane coupling agent. The invention also provides a preparation method of the nano metal oxide perfluoropolyether oil phase dispersion, which comprises the following steps: s1, dissolving metal salt in methanol, and stirring and dissolving to obtain a metal salt solution; s2, feeding methanol into a hypergravity reactor, and after a flow field is stable, sequentially adding an alkali source solution and the metal salt solution in the step S1, and carrying out a cyclic mixing reaction to obtain a metal hydroxide solution; S3, introducing oxygen or adding an oxidant into the hypergravity reactor to oxidize the metal hydroxide solution into a metal oxide solution; S4, adding a surfactant into the hypergravity reactor for cyclic modification, washing, centrifuging and drying to obtain the oil-soluble modified nano metal oxide; S5, ultrasonically dispersing the oil-soluble modified nano metal oxide in the step S4 into the perfluoropolyether base oil to form uniform and stable transparent or semitransparent oil phase dispersion. Preferably, in step S1, the metal salt is one or more of cerium nitrate, cerium chloride, cerium sulfate, cerium perchlorate, zinc sulfate, zinc nitrate, zinc chloride, titanium tetrachloride, titanyl sulfate, and titanyl nitrate; The concentration of the metal salt solution is 0.2M-0.25M. Preferably, in step S2, the volume ratio of the metal salt solution, the methanol solution and the alkali source solution is 50:20:4.1. Preferably, in step S2, the alkaline source solution is one or more of sodium hydroxide solution, potassium hydroxide solution, sodium carbonate solution, and ammonia