• 专利标题:   New hydrophobic graphene modified fluorosilicon compound useful as resin material.
  • 专利号:   CN104774296-A
  • 发明人:   LUO Z, WANG H, ZHU J
  • 专利权人:   TIANCHANG KAILIN CHEM CO LTD
  • 国际专利分类:   C08F230/08, C08F292/00, C08F293/00, C09D153/00, C09D005/16
  • 专利详细信息:   CN104774296-A 15 Jul 2015 C08F-293/00 201582 Pages: 11 Chinese
  • 申请详细信息:   CN104774296-A CN10133667 25 Mar 2015
  • 优先权号:   CN10133667

▎ 摘  要

NOVELTY - A hydrophobic graphene modified fluorosilicon compound (I) is new. USE - Compound (I) useful as resin material (claimed). ADVANTAGE - The compound (I) has high performance. DETAILED DESCRIPTION - A hydrophobic graphene modified fluorosilicon compound of formula (I) is new. C60=single layer graphene; m=degree of polymerization of methyl propylene acyloxy propyl group trimethoxysilane; and n=degree of polymerization of methacrylic acid heptafluorobutyl ester. An INDEPENDENT CLAIM is included for the preparation of hydrophobic graphene modified fluorosilicon resin material comprising: (A) preparing silane coupling agent modified graphene strip in the container, adding graphene, toluene and silane coupling agent 3-aminopropyl trimethoxysilane, vacuumizing-charging inert gas to remove the air in the system, refluxing the reaction in an oil bath, centrifuging, decanting the solvent and the upper layer, adsorbing the upper layer, removing silane coupling agent, and drying to obtain the silane coupling agent modified graphene; (B) preparing single layer graphene atom transfer radical surface initiator in a baking container and adding silane coupling agent, modified graphene and toluene, vacuum sealing with inert gas, adding triethylamine and 2-bromine or butyl acyl bromine, centrifugal separation after completion of the reaction, decanting the organic solution, removing quaternary ammonium salt by-product, and drying to obtain black single layer graphite atom transfer radical surface initiator; (C) preparing C60-poly methacryloyloxy trimethoxysilane macroinitiators in baking container, adding graphene, a surface atom transfer radical initiator, cuprous halide as catalyst, and a compound containing a pyridine ring or a pyridine ring derivative containing compound as a catalyst ligand, to methacryloxy propyl trimethoxysilane and an inert solvent, evacuation-nitrogen cycles after greater than or equal to 3 times, placing the vessel in a constant temperature oil bath and stirring the reaction, then cooling to room temperature to terminate the reaction, and then dissolving in tetrahydrofuran, centrifuging, charging graphene hybrid material precipitates with tetrahydrofuran, washing with acetone and ultrasound to remove adsorbed free polymer, and drying to obtain C60-polymethacryloxy propyl trimethoxysilane macroinitiator; and (D) preparing monolayer graphite tape, adding hybrid performance superhydrophobic material monomer, butyl methacrylate heptafluoroatom, carrying out transfer radical polymerization under an inert atmosphere protection, in the baked vessel adding C60-polymethacryloyloxy trimethoxysilane macromolecules initiator, cuprous halide as catalyst, pyridine ring-containing compound or its derivative as catalyst ligand, atom transfer radical polymerization in an inert solvent, after vacuumizing at least three times with nitrogen cycles, heating the reaction, cooling at room temperature to terminate the reaction, and then dissolving in tetrahydrofuran, centrifuging, collecting the precipitate C60 nano-hybrid material, dissolving in tetrahydrofuran, washing with acetone to remove free polymer adsorbed, and drying under vacuum to obtain C60-polymethacryloxy trimethoxysilane-b-polymethylmethacrylate heptafluorobutyl ester nanohybrid material or fluoropolymer/single-layer graphene hybrid high-performance super-hydrophobic material.