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CN-121991443-A - Solvent-resistant flame-retardant fluororubber material and preparation process thereof

CN121991443ACN 121991443 ACN121991443 ACN 121991443ACN-121991443-A

Abstract

The invention relates to the technical field of fluororubber, and discloses a solvent-resistant flame-retardant fluororubber material and a preparation process thereof. The fluororubber material comprises 90-110 parts of fluororubber, 30-40 parts of fluorinated silicone rubber, 20-25 parts of flame-retardant filler, 5-8 parts of plasticizer, 2-3 parts of vulcanizing agent and 1-2 parts of triallyl isocyanurate, wherein the preparation of the plasticizer comprises the steps of adding 2, 2-trifluoroethylamine into epoxy soybean oil, heating to 80-85 ℃ and stirring for reacting for 6-8 hours to obtain the plasticizer, and the preparation of the flame-retardant filler comprises the steps of coating aluminum hydroxide with epoxy silane coupling agent modified silicon dioxide to obtain epoxy modified composite filler, and modifying with 2, 2-trifluoroethylamine to obtain the flame-retardant filler. The prepared fluororubber material has excellent mechanical property and toughness, and has excellent flame retardance.

Inventors

  • WU MINGGANG
  • WU CHAO
  • ZHU MING
  • YANG HU

Assignees

  • 江苏罗孚新材料有限公司

Dates

Publication Date
20260508
Application Date
20260319

Claims (10)

  1. 1. A preparation process of a solvent-resistant flame-retardant fluororubber material is characterized by comprising the following steps: Step 1, methyl vinyl silicone rubber is modified by using 1H, 2H-perfluoro decanethiol to obtain fluorinated silicone rubber; and 2, premixing fluororubber and fluorinated silicone rubber, adding a flame retardant filler, a plasticizer, a vulcanizing agent and triallyl isocyanurate, mixing, vulcanizing, and obtaining the solvent-resistant flame retardant fluororubber material.
  2. 2. The preparation process of the solvent-resistant flame-retardant fluororubber material is characterized by comprising, by mass, 90-110 parts of fluororubber, 30-40 parts of fluorinated silicone rubber, 20-25 parts of flame-retardant filler, 5-8 parts of plasticizer, 2-3 parts of vulcanizing agent and 1-2 parts of triallyl isocyanurate.
  3. 3. The preparation process of the solvent-resistant flame-retardant fluororubber material as claimed in claim 1, wherein the preparation process of the fluorinated silicone rubber comprises the steps of adding methyl vinyl silicone rubber into tetrahydrofuran, adding 1H, 2H-perfluorodecanethiol, stirring uniformly, adding a photoinitiator, irradiating with ultraviolet light, post-treating and drying to obtain the fluorinated silicone rubber.
  4. 4. The preparation process of the solvent-resistant flame-retardant fluororubber material according to claim 3, wherein the fluorinated silicone rubber comprises the following raw materials, by mass, 3-5 parts of methyl vinyl silicone rubber, 30-40 parts of tetrahydrofuran and 0.02-0.03 part of photoinitiator; when the addition amount of the 1H, 2H-perfluoro decanethiol is 6-8 parts, preparing the high-fluorinated silicone rubber; when the addition amount of the 1H, 2H-perfluoro decanethiol is 3-4 parts, the low-fluorinated silicone rubber is prepared.
  5. 5. The process for preparing the solvent-resistant flame-retardant fluororubber material according to claim 4, wherein the fluorinated silicone rubber is composed of high fluorinated silicone rubber and low fluorinated silicone rubber in a mass ratio of (1-2): 1.
  6. 6. The preparation process of the solvent-resistant flame-retardant fluororubber material according to claim 1, wherein the preparation of the plasticizer comprises the following steps of adding 2, 2-trifluoroethylamine into epoxidized soybean oil, heating to 80-85 ℃ and stirring and reacting for 6-8 hours to obtain the plasticizer.
  7. 7. The preparation process of the solvent-resistant flame-retardant fluororubber material according to claim 6 is characterized in that the plasticizer comprises, by mass, 10-15 parts of 2, 2-trifluoroethylamine and 80-100 parts of epoxidized soybean oil.
  8. 8. The preparation process of the solvent-resistant flame-retardant fluororubber material is characterized by comprising the following steps of adding aluminum hydroxide into water, uniformly stirring, adding sodium hexametaphosphate aqueous solution, adjusting pH to 8-9 by sodium hydroxide aqueous solution to obtain mixed solution, adding the mixed solution into a coating tank, stirring and heating to 40-45 ℃, uniformly dripping sodium silicate aqueous solution, simultaneously adding sulfuric acid to keep pH to 8-9, stirring and curing for 20-30 min, filtering, and drying at 160-180 ℃ for 10-12 h to obtain silicon dioxide coated aluminum hydroxide; adding an epoxy silane coupling agent into an ethanol aqueous solution, adjusting the pH to 4-5, stirring for 3-5 min, adding silicon dioxide coated aluminum hydroxide, heating to 40-60 ℃ and stirring for 4-6 h, filtering, washing and drying to obtain an epoxy modified composite filler; Adding the epoxy modified composite filler into N, N-dimethylformamide, uniformly stirring, adding 2, 2-trifluoroethylamine, heating to 80-85 ℃, stirring and reacting for 6-8 hours, filtering, washing and drying to obtain the flame-retardant filler.
  9. 9. The preparation process of the solvent-resistant flame-retardant fluororubber material is characterized in that the silicon dioxide coated aluminum hydroxide comprises, by mass, 8-10 parts of aluminum hydroxide, 0.3-0.5 part of sodium hexametaphosphate aqueous solution with the concentration of 50-70 g/L and 1-3 parts of sodium silicate aqueous solution with the concentration of 80-100 g/L; The epoxy modified composite filler comprises the following raw materials, by mass, 1-2 parts of epoxy silane coupling agent, 100-150 parts of ethanol aqueous solution and 10-15 parts of silicon dioxide coated aluminum hydroxide; The flame-retardant filler comprises, by mass, 10-15 parts of epoxy modified composite filler and 1-2 parts of 2, 2-trifluoroethylamine.
  10. 10. The solvent-resistant flame-retardant fluororubber material prepared by the preparation process of the solvent-resistant flame-retardant fluororubber material according to any one of claims 1-9.

Description

Solvent-resistant flame-retardant fluororubber material and preparation process thereof Technical Field The invention relates to the technical field of fluororubber, and discloses a solvent-resistant flame-retardant fluororubber material and a preparation process thereof. Background The fluororubber is a synthetic polymer elastomer with main chain or side chain containing fluorine atoms, has excellent solvent resistance, high temperature resistance and ageing resistance, and has wide application in the fields of aerospace, electronic and electric, petrochemical industry and the like. However, the fluororubber has the defects that firstly, the tensile strength of the fluororubber can meet the basic use requirement, but the brittleness of the material is high due to the strong rigidity of a molecular chain and weak segment movement capability, and secondly, the flame retardance of the fluororubber needs to be optimized in a targeted manner. In order to improve the performance of fluororubber, the prior art usually introduces modified components such as silicone rubber, plasticizer, inorganic filler and the like for blending, but the uniformity of a mixed system is poor due to the compatibility problem, so that the performance cannot be improved, and the mechanical property of the material is reduced. In summary, research on a solvent-resistant flame-retardant fluororubber material with mechanical properties and toughness and a preparation process thereof has important significance. Disclosure of Invention The invention aims to provide a solvent-resistant flame-retardant fluororubber material and a preparation process thereof, so as to solve the problems in the background technology. In order to solve the technical problems, the invention provides a preparation process of a solvent-resistant flame-retardant fluororubber material, which comprises the following steps: Step 1, methyl vinyl silicone rubber is modified by using 1H, 2H-perfluoro decanethiol to obtain fluorinated silicone rubber; and 2, premixing fluororubber and fluorinated silicone rubber, adding a flame retardant filler, a plasticizer, a vulcanizing agent and triallyl isocyanurate, mixing, vulcanizing, and obtaining the solvent-resistant flame retardant fluororubber material. More optimally, the solvent-resistant flame-retardant fluororubber material comprises, by mass, 90-110 parts of fluororubber, 30-40 parts of fluorinated silicone rubber, 20-25 parts of flame-retardant filler, 5-8 parts of plasticizer, 2-3 parts of vulcanizing agent and 1-2 parts of triallyl isocyanurate. More optimally, the preparation method of the fluorinated silicone rubber comprises the following steps of adding methyl vinyl silicone rubber into tetrahydrofuran, adding 1H, 2H-perfluoro decanethiol, uniformly stirring, adding a photoinitiator, irradiating with ultraviolet light, post-treating and drying to obtain the fluorinated silicone rubber. More preferably, the vulcanizing agent is 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, and the photoinitiator is DMPA (benzoin dimethyl ether). More optimally, the post-treatment steps are that adding absolute ethyl alcohol for flocculation, taking solid, adding tetrahydrofuran for dissolution, removing impurities and removing solvent. More optimally, the fluorinated silicone rubber comprises the following raw materials, by mass, 3-5 parts of methyl vinyl silicone rubber, 30-40 parts of tetrahydrofuran and 0.02-0.03 part of photoinitiator; when the addition amount of the 1H, 2H-perfluoro decanethiol is 6-8 parts, preparing the high-fluorinated silicone rubber; when the addition amount of the 1H, 2H-perfluoro decanethiol is 3-4 parts, the low-fluorinated silicone rubber is prepared. More preferably, the fluorinated silicone rubber is composed of high fluorinated silicone rubber and low fluorinated silicone rubber in a mass ratio of (1-2): 1. More optimally, the preparation of the plasticizer comprises the following steps of adding 2, 2-trifluoroethylamine into epoxidized soybean oil, heating to 80-85 ℃, stirring and reacting for 6-8 hours, and thus obtaining the plasticizer. More optimally, the plasticizer comprises the following raw materials, by mass, 10-15 parts of 2, 2-trifluoroethylamine and 80-100 parts of epoxidized soybean oil. More optimally, the preparation method of the flame-retardant filler comprises the steps of adding an epoxy silane coupling agent into an ethanol water solution, adjusting the pH to 4-5, stirring for 3-5 min, adding silicon dioxide coated aluminum hydroxide, heating to 40-60 ℃, stirring for 4-6 h, filtering, washing and drying to obtain an epoxy modified composite filler, adding the epoxy modified composite filler into N, N-dimethylformamide, stirring uniformly, adding 2, 2-trifluoroethylamine, heating to 80-85 ℃, stirring and reacting for 6-8 h, filtering, washing and drying to obtain the flame-retardant filler. The epoxy modified composite filler comprises, by mass, 1-2 parts of an epoxy silane