• 专利标题:   Preparing phosphate-polyaniline-silicon dioxide graft modified graphene/aqueous-based epoxy-containing silicone resin composite coating comprises dispersing phosphate-polyaniline- silicon dioxide graft modified graphene in aqueous epoxy-containing epoxy resin, coating on metal, heating and curing.
  • 专利号:   CN113604151-A, CN113604151-B
  • 发明人:   ZHAO Y, ZHAO T, LI Y, GAO X
  • 专利权人:   UNIV QIQIHAR
  • 国际专利分类:   C09D183/06, C09D005/08, C09D007/62, C09D007/65
  • 专利详细信息:   CN113604151-A 05 Nov 2021 C09D-183/06 202221 Chinese
  • 申请详细信息:   CN113604151-A CN10996062 27 Aug 2021
  • 优先权号:   CN10996062

▎ 摘  要

NOVELTY - Preparing phosphate-polyaniline-silicon dioxide graft modified graphene/aqueous-based epoxy-containing silicone resin composite coating comprises adding graphene oxide into deionized water, dispersing to obtain graphene oxide dispersion liquid, adding aqueous ammonia, stirring to obtain dispersion liquid, adding e.g. ethyl orthosilicate, reacting, filtering, washing, obtaining graphene oxide-silicon dioxide composite material, adding graphene oxide-silicon dioxide composite material into water, stirring, adding phytic acid, stirring, refluxing, cooling, adding aniline, stirring, dropping ammonium persulfate aqueous solution, stirring, filtering, washing, freeze-drying to obtain phosphate-polyaniline- silicon dioxide graft modified graphene composite material, ultrasonically dispersing phosphate-polyaniline- silicon dioxide graft modified graphene composite material in the aqueous epoxy-containing epoxy resin, coating on metal and/or alloy surface, heating, curing to obtain product. USE - The method is useful for preparing phosphate-polyaniline-silicon dioxide graft modified graphene/aqueous-based epoxy-containing silicone resin composite coating. ADVANTAGE - The method improves the dispersibility of graphene and polyaniline; improves the hydrophobicity of the composite coating; has obvious synergistic effect of graphene and polyaniline and improves anti-corrosion performance of the aqueous-based coating. DETAILED DESCRIPTION - Preparing phosphate-polyaniline-silicon dioxide graft modified graphene/aqueous-based epoxy-containing silicone resin composite coating comprises (a) adding graphene oxide into deionized water, ultrasonically dispersing for 3-4 hours to obtain graphene oxide dispersion liquid, adding aqueous ammonia, magnetic stirring for 15 minutes to obtain alkaline graphene oxide dispersion liquid, adding anhydrous ethanol, deionized water and ethyl orthosilicate, stirring, reacting at 60degrees Celsius for 6 hours, filtering, washing until the solid product becomes neutral, obtaining graphene oxide-silicon dioxide composite material, where the concentration of the graphene oxide dispersion liquid is 1-1.5 mg/ml, the ratio of the volume of the ethyl orthosilicate to the graphene oxide is 50 ml: 1 mg, the amount of aqueous ammonia is 25 wt.%, the ratio of the aqueous ammonia and the ethyl orthosilicate is 1: 1, the ratio of the absolute ethyl alcohol, deionized water and ethyl orthosilicate is 80: 15: 5, (b) adding graphene oxide-silicon dioxide composite material obtained in the step (a) into 100 ml deionized water, stirring for 30 minutes to form dispersion, adding phytic acid, stirring, refluxing at 100degrees Celsius for 10-12 hours, cooling, placing a reflux reaction device in the ice water bath at 3-5degrees Celsius, using phytic acid to adjust the pH value of the reaction liquid to 1, adding aniline, magnetically stirring for 30 minutes, dropping ammonium persulfate aqueous solution as initiator, magnetic stirring for 6-8 hours, filtering, washing the solid product to neutral by deionized water, freeze-drying the solid product for 48 hours to obtain phosphate-polyaniline- silicon dioxide graft modified graphene composite material, where in step (a) the ratio of the phytic acid to the graphene oxide is 50 ml:1 mg, the ratio of aniline to graphene oxide is 3:1, the ratio of ammonium persulfate to aniline in the ammonium persulfate aqueous solution is 3:1, (c) adding deionized water and absolute ethyl alcohol into a reagent bottle, adding citric acid, ultrasonically processing until the citric acid is completely dissolved, continuously adding ethyl orthosilicate, gamma-(2,3-epoxypropoxy)propyltrimethoxysilane and dimethyldiethoxysilane into the reagent bottle, stirring, reacting at 40degrees Celsius for 8 hours to obtain an aqueous epoxy-containing silicone resin, where the ratio of the deionized water to the absolute ethyl alcohol is 2: 1, the amount of citric acid, deionized water, absolute ethyl alcohol, ethyl orthosilicate, gamma- (2, 3-epoxy propoxy) propyl trimethoxy silane and dimethyl diethoxy silane is 1-1.5%, the ratio of ethyl orthosilicate, gamma- (2, 3-epoxy propoxy) propyl trimethoxy silane and dimethyldiethoxysilane is 5:12:4, the ratio of the deionized water and absolute ethanol to the ethyl orthosilicate, gamma- (2, 3-epoxy propoxy) propyl trimethoxy silane and dimethyldiethoxysilane is 1:1 and (d) ultrasonically dispersing phosphate-polyaniline- silicon dioxide graft modified graphene composite material obtained in the step (b) in the aqueous epoxy-containing epoxy resin obtained in step (c), coating on the metal and/or alloy surface, heating, curing at 50degrees Celsius to obtain phosphate-polyaniline-silicon dioxide graft modified graphene/aqueous-based epoxy-containing silicone resin composite coating, where the adding amount of the phosphate polyaniline-silicon dioxide graft modified graphene composite material in the aqueous silicon resin is 1.5-3.5wt.%.