• 专利标题:   Preparing phosphorus-containing silicon functionalized graphene oxide, comprises e.g. reacting P-H bond on 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with amino group on gamma-aminopropyltriethoxysilane under action of first solvent.
  • 专利号:   CN108440788-A, CN108440788-B
  • 发明人:   DAI L, WU W, XU Y, WANG X, CHEN G, YUAN C, ZENG B, LUO W, WANG R, HE K
  • 专利权人:   UNIV XIAMEN
  • 国际专利分类:   C08K003/04, C08K009/06, C08L063/00
  • 专利详细信息:   CN108440788-A 24 Aug 2018 C08K-009/06 201866 Pages: 10 Chinese
  • 申请详细信息:   CN108440788-A CN10213585 15 Mar 2018
  • 优先权号:   CN10213585

▎ 摘  要

NOVELTY - Preparing phosphorus-containing silicon functionalized graphene oxide (II), comprises e.g. (i) reacting P-H bond on 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with amino group on gamma-aminopropyltriethoxysilane under action of first solvent and paraformaldehyde, under protection of nitrogen and then precipitating, purifying and drying to obtain phosphorus-containing silicon compound i.e. 9-((((9-oxo-8-oxa-9(5)-phosphatricyclo(8.4.0.0(2,7))tetradeca-1(14),2(7),3,5,10,12-hexaen-9-yl)methyl)(3-(triethoxysilyl)propyl)amino)methyl)-8-oxa-9(5)-phosphatricyclo(8.4.0.0(2,7))tetradeca-1(14),2(7),3,5,10,12-hexaen-9-one (I), and (ii) sonicating graphene oxide is in the second solvent, then adding (I) diluted with third solvent and carrying out hydrolysis reaction at 75-100 degrees C, then purifying by centrifugation and freeze-drying. USE - The method is useful for preparing phosphorus-containing silicon functionalized graphene oxide compound. ADVANTAGE - The method: has mild reaction conditions; and does not contain halogen elements, and is environmentally friendly; and (I): improves the thermal stability of epoxy resin; and exhibits synergistic effect. DETAILED DESCRIPTION - Preparing phosphorus-containing silicon functionalized graphene oxide of formula (II), comprises (i) reacting P-H bond on 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with amino group on gamma-aminopropyltriethoxysilane under the action of the first solvent and paraformaldehyde, under protection of nitrogen at 50-80 degrees C, and then precipitating, purifying the reaction product by vacuum filtration and drying to obtain phosphorus-containing silicon compound i.e. 9-((((9-oxo-8-oxa-9(5)-phosphatricyclo(8.4.0.0(2,7))tetradeca-1(14),2(7),3,5,10,12-hexaen-9-yl)methyl)(3-(triethoxysilyl)propyl)amino)methyl)-8-oxa-9(5)-phosphatricyclo(8.4.0.0(2,7))tetradeca-1(14),2(7),3,5,10,12-hexaen-9-one of formula (I), where the amount of first solvent is in 5-30 times total mass of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, gamma-aminopropyltriethoxysilane and paraformaldehyde; and the molar ratio between gamma-aminopropyltriethoxysilane, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and paraformaldehyde is 1:2-20:2-10, and (ii) sonicating graphene oxide is in the second solvent, then adding (I) diluted with third solvent and carrying out hydrolysis reaction at 75-100 degrees C, then purifying by centrifugation and freeze-drying to obtain final product, where the mass ratio between above graphene oxide and (I) is 1:10-50. A1 = graphene.