• 专利标题:   Cyanation reduction graphene oxide/polyarylether nitrile hybrid material used for manufacture of high temperature-resistant polymer material comprises cyanation reduction graphene oxide and phthalonitrile-terminated polyarylether nitrile.
  • 专利号:   CN110144107-A
  • 发明人:   WEI R, TU L, LIU C, CHENG M, WANG L, YOU Y, ZHAN C, LIU S, LIU X
  • 专利权人:   UNIV CHINA ELECTRONIC SCI TECHNOLOGY
  • 国际专利分类:   C08J005/18, C08J007/00, C08K003/04, C08K009/04, C08L071/10
  • 专利详细信息:   CN110144107-A 20 Aug 2019 C08L-071/10 201977 Pages: 10 Chinese
  • 申请详细信息:   CN110144107-A CN10437503 24 May 2019
  • 优先权号:   CN10437503

▎ 摘  要

NOVELTY - A cyanation reduction graphene oxide/polyarylether nitrile hybrid material comprises cyanation reduction graphene oxide and phthalonitrile-terminated polyarylether nitrile connected together through high-temperature-resistant aromatic ether bond and phthalocyanine ring. The hybrid material is film with glass transition temperature of greater than 360 degrees C, 5% heat decomposition temperature of greater than 500 degrees C, dielectric constant of greater than 15.0 at 1 kHz and dielectric loss of less than 0.030 at 1 kHz. USE - The cyanation reduction graphene oxide/polyarylether nitrile hybrid material is used for manufacture of high temperature-resistant polymer material. ADVANTAGE - The material has good high-temperature resistance, high dielectric property, glass transition temperature of greater than 360 degrees C, 5% heat decomposition temperature of greater than 500 degrees C, dielectric constant of greater than 15.0 at 1kHz and dielectric loss of less than 0.030 at 1 kHz. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is included for preparation of the cyanation reduction graphene oxide/polyarylether nitrile hybrid material comprising: (A) adding phosphorus sheet graphite, concentrated sulfuric acid and concentrated phosphoric acid to flask, mechanically stirring at speed of 100-300 revolutions/minute (rpm), adding potassium permanganate, continuously stirring for 10-30 minutes, reacting and stirring in water bath system at 40-80 degrees C for 8-20 hours at rate of 300-1000 rpm, pouring in deionized water and concentrated sulfuric acid at volume ratio of 1:1, stirring for 3-10 minutes at stirring speed of 30-100 rpm, adding 30% hydrogen peroxide until solution becomes golden yellow, standing for 10-30 hours, pouring upper clear, repeatedly washing and centrifuging turbid liquid with deionized water until pH is 5.5-6.5 and freeze-drying to obtain graphene oxide powder; (B) dispersing graphene oxide into N,N-dimethylformamide to prepare 1.0-5.0 mg/mL dispersion, ultrasonically processing for 0.5-2 hours, adding aminophthalonitrile comprising 4-(4'-aminophenoxy)phthalonitrile, 3-(4'-aminophenoxy)phthalonitrile and/or 4-aminophthalonitriles, passing nitrogen at flow rate of 0.05-1 mL/minute for 5-10 minutes, adding isoamyl nitrite, reacting at 50-100 degrees C for 8-20 hours, filtering, washing filter cake with N,N-dimethylformamide until filtrate is colorless and vacuum-drying at 50-100 degrees C for 20-50 hours to obtain cyano-graphene oxide; (C) dispersing cyano-graphene oxide into N,N-dimethylformamide to prepare 1.0-5.0 mg/mL dispersion, ultrasonically processing for 0.5-2 hours, adding hydrazine hydrate, reacting at 80-120 degrees C for 4-12 hours, filtering, washing filter cake with N,N-dimethylformamide until filtrate is colorless and vacuum-drying at 50-100 degrees C for 20-50 hours to obtain cyano-reduced graphene oxide; (D) adding cyano-reduced graphene oxide into N-methylpyrrolidone, ultrasonically stirring for 0.5-2 hours, pouring mixed system to flat glass plate, drying in blast oven at 100-200 degrees C for 4-8 hours, naturally cooling to room temperature and uncovering film from glass plate; and (E) placing film in high-temperature oven, drying at 280-360 degrees C for 2-10 hours and naturally cooling to room temperature.