• 专利标题:   Preparation of thermosensitive controllable graphene composite material used e.g. for preparing high pressure liquid phase chromatography filler, includes mixing N-isopropyl acrylamide monomer, dithiobenzoate benzyl, and initiator.
  • 专利号:   CN104479058-A, CN104479058-B
  • 发明人:   LIU J, XIAO Y, HUANG R, OU B, WANG C
  • 专利权人:   UNIV HUNAN SCI TECHNOLOGY
  • 国际专利分类:   C08F120/54, C08F008/00, C08F008/34
  • 专利详细信息:   CN104479058-A 01 Apr 2015 C08F-120/54 201540 Pages: 8 Chinese
  • 申请详细信息:   CN104479058-A CN10748760 10 Dec 2014
  • 优先权号:   CN10748760

▎ 摘  要

NOVELTY - Preparation of thermosensitive controllable graphene composite material includes adding N-isopropyl acrylamide monomer, dithiobenzoate benzyl, and initiator in round bottom flask, adding tetrahydrofuran solution, completely dissolving, precipitating polymer, removing tetrahydrofuran and remaining chain transfer agent to obtain pure poly N-isopropyl acrylamide product; placing N-isopropyl acrylamide into flask, adding tetrahydrofuran solution and reducing agent, shaking; adding dried crystalline flake graphite to mixture of potassium nitrate and concentrated acid, and ultrasonically mixing. USE - Method for preparing thermosensitive controllable graphene composite material (claimed) used for temperature control of gel permeation chromatography, analog synthesis of bioactive collagen fibers, and removing skin adhesive tape, and for preparing temperature sensitive film material, high pressure liquid phase chromatography filler and temperature sensitive thickeners. ADVANTAGE - The method is simple, and has short reaction time. DETAILED DESCRIPTION - Preparation of thermosensitive controllable graphene composite material comprises adding N-isopropyl acrylamide monomer, dithiobenzoate benzyl, and initiator in 50 ml round bottom flask, adding 20 ml tetrahydrofuran solution, completely dissolving at 70 degrees C in oil bath nitrogen protecting device for 24 hours, precipitating polymer, removing tetrahydrofuran and remaining chain transfer agent to obtain pure poly N-isopropyl acrylamide product; placing N-isopropyl acrylamide into 100 ml flask, adding tetrahydrofuran solution and reducing agent, shaking at room temperature under anaerobic condition for 48 hours to obtain mercapto poly N-isopropyl acrylamide; adding dried crystalline flake graphite to mixture of potassium nitrate and concentrated acid, ultrasonically mixing, putting in ice water bath, stirring and slowly adding oxidant, heating to 35-45 degrees C, high-speed stirring for 6 hours, slowly adding distilled water, heating to 60-80 degrees C for half an hour, adding distilled water and hydrogen peroxide solution, reacting for 5 minutes, centrifugally washing with distilled water to a pH of 6-8 to obtain purified of graphene oxide, adding dispersant, ultrasonically mixing to obtain graphene oxide gel; weighing oxide graphene and taking 2,4-toluene diisocyanate dispersed in anhydrous toluene, ultrasonically mixing for 30 minutes, reacting for 12 hours under anhydrous oxygen free nitrogen protection at 90 degrees C in oil bath, washing reaction crude product with solvent, centrifugally separating isocyanated graphene oxide, vacuum drying for 24 hours; dissolving triethylamine in anhydrous tetrahydrofuran, mixing with isocyanate functionalized graphene oxide, and mercapto poly N-isopropyl acrylamide for 20 minutes, reacting at room temperature under anaerobic condition for 18 hours, washing crude product with anhydrous tetrahydrofuran, centrifuging, and vacuum drying.