• 专利标题:   Preparation of hyperbranched poly(cyclophosphazene)-grafted-graphene by microwave-assisted method involves adding gamma-aminopropyltriethoxysilane and graphene oxide in ethanol concentrated mixture and vacuum drying.
  • 专利号:   CN103407999-A, CN103407999-B
  • 发明人:   YAN H, LIU C, LI T, FENG S
  • 专利权人:   UNIV NORTHWESTERN POLYTECHNICAL
  • 国际专利分类:   C01B031/04
  • 专利详细信息:   CN103407999-A 27 Nov 2013 C01B-031/04 201415 Pages: 9 Chinese
  • 申请详细信息:   CN103407999-A CN10307168 21 Jul 2013
  • 优先权号:   CN10307168

▎ 摘  要

NOVELTY - A hyperbranched poly(cyclophosphazene)-grafted-graphene is prepared by microwave-assisted method involves (1) adding gamma -aminopropyltriethoxysilane and graphene oxide in ethanol concentrated mixture; (2) adding sodium citrate and modified graphene oxide in deionized water solution; (3) adding hexachlorocyclotriphosphazene and modified graphene in diethyl ether solution, vacuum drying to obtain hexachlorocyclotriphosphazene-grafted-graphene, adding hexachlorocyclotriphosphazene-grafted-graphene and hexamethylenediamine in toluene solution; (4) and repeating step (3). USE - Preparation of hyperbranched poly(cyclophosphazene)-grafted-graphene (claimed). ADVANTAGE - Preparation of hyperbranched poly(cyclophosphazene)-grafted-graphene has mild reaction, fast reaction speed, and produces high yield. Product has excellent chemical and thermal stability. DETAILED DESCRIPTION - A hyperbranched poly(cyclophosphazene)-grafted-graphene is prepared by microwave-assisted method involves (1) adding gamma -aminopropyltriethoxysilane (silane coupling agent KH-550):graphene oxide with mass ratio of 1:1-10 in 0.01-1 mass% ethanol concentrated mixture, ultrasonically dispersing for 30 minutes, adding nitrogen gas, centrifuging in microwave reactor at 300 rpm in 50-80 V for 0.5-3 hours, successively washing with ethanol and deionized water for 3 times, performing suction filtration to obtain dark gray solid product, vacuum drying at 60 degrees C for 4 hours to obtain modified graphene oxide; (2) adding sodium citrate:modified graphene oxide with mass ratio of 1:0.1-10 in 0.01-1 mass% deionized water solution, ultrasonically dispersing for 30 minutes, adding in microwave reactor, centrifuging at 50-100 degrees C for 10-60 minutes to obtain black solid product, successively washing with ethanol and deionized water for 3 times, vacuum drying at 60 degrees C for 5 hours to obtain modified graphene; (3) adding hexachlorocyclotriphosphazene:modified graphene with mass ratio of 1:0.1-10 in 0.01-1 mass% diethyl ether solution, continuously adding ether solution containing 1-20 vol.% triethylamine, reacting at 10-50 degrees C for 0.5-3 hours, further adding 40-80 vol.% n-heptane solution, reacting for 1-3 hours, filtering to obtain gray-black solid product, washing with ethanol for 3 times, vacuum drying at 60 degrees C for 2 hours to obtain hexachlorocyclotriphosphazene-grafted-graphene, adding hexachlorocyclotriphosphazene-grafted-graphene:hexamethylenediamine with molar ratio 1:5-10 in toluene solution containing 1-20 vol.% triethylamine, reacting at 30-80 degrees C for 5-30 minutes in microwave reactor, centrifuging to obtain gray-black solid product, successively washing with ethanol and deionized water for 3 times, vacuum drying at 60 degrees C for 10 hours; (4) and repeating step (3) for 1-10 times. DESCRIPTION OF DRAWING(S) - The drawing shows a schematic diagram of a hyperbranched poly(cyclophosphazene)-grafted-graphene. (Drawing includes non-English language text).