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CN-121975190-A - Ionic liquid modified aluminum-doped zinc oxide filler and modified fluororubber

CN121975190ACN 121975190 ACN121975190 ACN 121975190ACN-121975190-A

Abstract

The invention provides an ionic liquid modified aluminum-doped zinc oxide filler and modified fluororubber, which creatively adopts ionic liquid to assist coprecipitation to synthesize a novel core-shell structure composite filler AZO@Ils. The FKM/AZO@ILs composite material is prepared by mechanically blending fluororubber and AZO@ILs, so that the mechanical property, electrical property and thermal property of the composite material are remarkably improved, innovative thought and effective solution are provided for the design and development of high-performance and multifunctional fluororubber composite material, and huge application potential is shown in various fields of aerospace, military, semiconductor manufacturing and the like.

Inventors

  • JIN HUILE
  • CHENG YU
  • LI JUN
  • WU YADONG
  • Peng Xuqiang
  • WANG SHUN

Assignees

  • 温州大学新材料与产业技术研究院
  • 温州大学

Dates

Publication Date
20260505
Application Date
20260202

Claims (9)

  1. 1. The ionic liquid modified aluminum-doped zinc oxide filler is characterized by comprising the following steps of: s1, dissolving soluble zinc salt and soluble aluminum salt in a solvent, and continuously adding 1-ethyl-3-methylimidazolium chloride to obtain solution A; S2, dissolving a precipitator in a solvent, and performing ultrasonic treatment to obtain a solution B; and S3, adding the solution B into the solution A, regulating the pH to 7-8, performing coprecipitation reaction to obtain a precipitate, separating, washing and drying the precipitate, and calcining the precipitate in a protective atmosphere to obtain the ionic liquid modified aluminum-doped zinc oxide filler.
  2. 2. The ionic liquid modified aluminum-doped zinc oxide filler of claim 1, wherein in the step S1, the soluble zinc salt is at least one of zinc acetate, zinc chloride, zinc sulfate and zinc nitrate, and the soluble aluminum salt is at least one of aluminum nitrate, aluminum chloride, aluminum sulfate and aluminum acetate.
  3. 3. The ionic liquid modified aluminum-doped zinc oxide filler according to claim 1, wherein in the step S1, the mole ratio of the soluble zinc salt, the soluble aluminum salt and the 1-ethyl-3-methylimidazolium chloride is (25-35): 1 (8-12).
  4. 4. The ionic liquid modified aluminum-doped zinc oxide filler according to claim 1, wherein in the step S2, the precipitant comprises at least one of sodium hydroxide, sodium carbonate and ammonia water.
  5. 5. The ionic liquid modified aluminum-doped zinc oxide filler according to claim 1, wherein in the step S2, the precipitant comprises sodium hydroxide and sodium carbonate in a molar ratio of (1-3): 1.
  6. 6. The ionic liquid modified aluminum-doped zinc oxide filler according to claim 1, wherein the calcining condition is that the temperature is raised to 800-1000 ℃ and the temperature is kept for 1-3h.
  7. 7. A modified fluororubber is characterized in that the ionic liquid modified aluminum-doped zinc oxide filler is compounded in fluororubber by taking the ionic liquid modified aluminum-doped zinc oxide filler as a filler.
  8. 8. The modified fluororubber as claimed in claim 7, wherein the ratio of the ionic liquid modified aluminum-doped zinc oxide filler to fluororubber is (1-20) 100.
  9. 9. The modified fluororubber as claimed in claim 7, wherein the preparation method comprises the steps of: (A) Fully mixing fluororubber and ionic liquid modified aluminum-doped zinc oxide filler at 40-50 ℃, sequentially adding TAIC and Bifide and fifthly, uniformly mixing, and vulcanizing for 5-15min at 8-12Mpa and 150-190 ℃ to obtain a vulcanized fluororubber; (B) Vulcanizing a section of vulcanized fluororubber at 180-220 ℃ to obtain modified fluororubber, wherein the vulcanized fluororubber is vulcanized at 22-26 h; wherein the parts ratio of the fluororubber to the ionic liquid modified aluminum-doped zinc oxide filler to the TAIC to the Bifide is 100 (1-20): 1-3): 0.5-2.

Description

Ionic liquid modified aluminum-doped zinc oxide filler and modified fluororubber Technical Field The invention relates to the technical field of fluororubber, in particular to an ionic liquid modified aluminum-doped zinc oxide filler and modified fluororubber. Background Fluororubber (FKM) has excellent high temperature resistance, oil resistance, chemical resistance and ageing resistance, and is widely applied to the fields of aerospace, automobiles, petrochemical industry and the like. Along with the improvement of miniaturization, intellectualization and electromagnetic compatibility (EMC) requirements of electronic equipment, development of fluororubber composite materials with high strength and high conductivity is an urgent need. The current primary approach to improving the conductivity of fluororubbers is the addition of carbon materials, such as carbon nanotubes or carbon black. However, the use of carbon materials is difficult to meet the requirements of light-colored or colored products, and is accompanied by problems of high cost and poor dispersibility in fluororubbers. In order to solve a series of problems existing in the carbon material as the conductive filler, researchers have proposed using conductive polymers, metal materials, ionic liquids, and the like as the conductive filler of rubber. T. samtretch et al synthesized Polyaniline (PANI)/metal doped TiO 2 nano-conductive composites using cerium doped titanium dioxide (Ce-TiO 2) nanoparticles based on in situ polymerization. Wang et al prepared an aluminum doped zinc oxide (AZO) using aluminum nitrate and zinc chloride and blended the aluminum doped zinc oxide as a filler with polypropylene to produce a composite. Although the above method can produce the conductive filler to some extent, there are still problems of poor dispersibility and poor interface bonding. Disclosure of Invention The invention aims to overcome the defects and shortcomings in the prior art and provide an ionic liquid modified aluminum-doped zinc oxide filler and modified fluororubber. The technical scheme adopted by the invention is as follows: The invention provides an ionic liquid modified aluminum-doped zinc oxide filler, which comprises the following steps: s1, dissolving soluble zinc salt and soluble aluminum salt in a solvent, and continuously adding 1-ethyl-3-methylimidazolium chloride to obtain solution A; S2, dissolving a precipitator in a solvent, and performing ultrasonic treatment to obtain a solution B; and S3, adding the solution B into the solution A, regulating the pH to 7-8, performing coprecipitation reaction to obtain a precipitate, separating, washing and drying the precipitate, and calcining the precipitate in a protective atmosphere to obtain the ionic liquid modified aluminum-doped zinc oxide filler. Preferably, in step S1, the soluble zinc salt is at least one of zinc acetate, zinc chloride, zinc sulfate, and zinc nitrate, and the soluble aluminum salt is at least one of aluminum nitrate, aluminum chloride, aluminum sulfate, and aluminum acetate. Preferably, in the step S1, the mole ratio of the soluble zinc salt, the soluble aluminum salt and the 1-ethyl-3-methylimidazolium chloride is (25-35): 1 (8-12). Preferably, in step S2, the precipitating agent includes at least one of sodium hydroxide, sodium carbonate, and ammonia water. Preferably, in step S2, the precipitant is a combination of sodium hydroxide and sodium carbonate, and the PH of the solution is better regulated while using carbonate buffering. Preferably, in step S2, the precipitant comprises sodium hydroxide and sodium carbonate, and the molar ratio of the sodium hydroxide to the sodium carbonate is (1-3): 1. Preferably, the calcination conditions are elevated to 800-1000 ℃ and incubated for 1-3 hours. The second aspect of the invention provides modified fluororubber, which is obtained by compounding the ionic liquid modified aluminum-doped zinc oxide filler serving as a filler in fluororubber. Preferably, the ratio of the ionic liquid modified aluminum-doped zinc oxide filler to the fluororubber is (1-20): 100. Preferably, the preparation method comprises the following steps: (A) Fully mixing fluororubber and ionic liquid modified aluminum-doped zinc oxide filler at 40-50 ℃, sequentially adding TAIC and Bifide and fifthly, uniformly mixing, and vulcanizing for 5-15min at 8-12Mpa and 150-190 ℃ to obtain a vulcanized fluororubber; (B) Vulcanizing a section of vulcanized fluororubber at 180-220 ℃ to obtain modified fluororubber, wherein the vulcanized fluororubber is vulcanized at 22-26 h; wherein the parts ratio of the fluororubber to the ionic liquid modified aluminum-doped zinc oxide filler to the TAIC to the Bifide is 100 (1-20): 1-3): 0.5-2. The beneficial effects of the invention are as follows: 1. The invention innovatively synthesizes the novel core-shell structure composite filler AZO@ILs by adopting ionic liquid to assist coprecipitation. In the coprecipitation process,