• 专利标题:   Manufacture of graphene/liquid crystal polymer nano composite material involves reacting alkynyl-modified graphene oxide, non-liquid crystal polymer, liquid crystal polymer, cuprous bromide, and triamine complexing agent.
  • 专利号:   CN102993461-A, CN102993461-B
  • 发明人:   TANG H, WU P, YING Y
  • 专利权人:   UNIV FUDAN
  • 国际专利分类:   C08K003/04, C08K009/04, C08L101/12, C09C001/46, C09C003/10
  • 专利详细信息:   CN102993461-A 27 Mar 2013 C08K-009/04 201401 Pages: 11 Chinese
  • 申请详细信息:   CN102993461-A CN10582859 28 Dec 2012
  • 优先权号:   CN10582859

▎ 摘  要

NOVELTY - Carapace-type liquid crystal polymer having azide group at terminal is prepared by atomic transfer free radical polymerization method. Alkynyl-modified graphene oxide is obtained by Hummers method. Alkynyl-modified graphene oxide, non-liquid crystal polymer, liquid crystal polymer, cuprous bromide catalyst, N,N,N',N",N"-pentamethyl diethylene triamine complexing agent, and dimethylformamide are added in Schlenk flask and reacted. The solid is washed and dried to obtain oxidized graphene/carapace-type liquid crystal polymer nano composite material. USE - Manufacture of oxidized graphene/carapace-type liquid crystal polymer nano composite material used as filler nanocomposite (claimed). ADVANTAGE - The oxidized graphene/carapace-type liquid crystal polymer nano composite material having excellent compatibility is easily and efficiently manufactured. DETAILED DESCRIPTION - 0.4-3 g Carapace-type liquid crystal monomer having azide group at terminal, 0.0115-0.0863 g cuprous bromide low-valent transition metal salt, 0.0136-0.102 g N,N,N',N",N"-pentamethyl diethylene triamine complexing agent, 0.0188-0.141 g 3-azido-ethyl-2-bromo isobutyrate initiator and 2-15 ml chlorobenzene solvent are added to Schlenk flask, flask is sealed, and reacted at 80-90 degrees C for 24-48 hours. Liquid nitrogen is added and polymerization is stopped. Unreacted monomer is removed, and non-liquid crystal polymer having controlled molecular weight is prepared. 0.8-6 g Carapace-type liquid crystal monomer, 0.0019-0.0091 g cuprous bromide, 0.0017-0.0106 g N,N,N',N",N"-pentamethyl diethylene triamine complexing agent, 0.0024-0.0147 g 3-azido-ethyl-2-bromo isobutyrate initiator and 4-25 ml chlorobenzene solvent are added in Schlenk flask, flask is sealed, and reacted at 80-90 degrees C for 24-48 hours. The liquid nitrogen is added to polymerization tube, and unreacted monomer is removed. Carapace-type liquid crystal polymer having azide group at terminal is prepared by atomic transfer free radical polymerization method. 140-500 mg graphene oxide is added to 40-140 ml thionyl chloride, 0.5-1.5 ml dimethylformamide as a catalyst is added and reacted at 60-80 degrees C for 24 hours. Carboxyl acylation reaction of graphene oxide is carried out, unreacted thionyl chloride is rotationally evaporated, solid material is dried at 40-50 degrees C in a vacuum oven for 24 hours and dissolved in dimethylformamide. 0.28-1 g Propargyl alcohol and 8.1-29 ml anhydrous triethylamine are slowly added to the solution and stirred for 1-2 hours in ice water bath, reacted at 60-80 degrees C for 24 hours. The obtained solid is washed, unreacted propargyl alcohol is removed, and solid is dried at 45-50 degrees C in a vacuum oven to obtain alkynyl-modified graphene oxide by Hummers method. 40-80 mg Alkynyl-modified graphene oxide, 0.2-0.6 g non-liquid crystal polymer, 0.5-1.5 g liquid crystal polymer, 0.0024-0.0072 g cuprous bromide catalyst, 0.0028-0.0084 g N,N,N',N",N"-pentamethyl diethylene triamine complexing agent, and 20-50 ml dimethylformamide are added in Schlenk flask and reacted at 25-90 degrees C for 24-48 hours. The solid is washed, unreacted polymer is removed and dried at 60-70 degrees C for 24 hours to obtain oxidized graphene/carapace-type liquid crystal polymer nano composite material.