• 专利标题:   Preparation of sol polyaniline composite graphene conductive material, involves mixing tetraethyl orthosilicate and deionized water, dripping aqueous ammonia to adjust pH and mixing with alcohol dispersion containing 2-bromo-4-methylphenol.
  • 专利号:   CN107722264-A
  • 发明人:   LIU M
  • 专利权人:   QINGYUAN CHUQU INTELLIGENT TECHNOLOGY CO
  • 国际专利分类:   C08G073/02, C08K013/06, C08K003/04, C08K003/36, C08K005/20, C08K005/3492, C08K009/04
  • 专利详细信息:   CN107722264-A 23 Feb 2018 C08G-073/02 201819 Pages: 7 Chinese
  • 申请详细信息:   CN107722264-A CN11185452 23 Nov 2017
  • 优先权号:   CN11185452

▎ 摘  要

NOVELTY - Preparation of sol polyaniline composite graphene conductive material, involves (i) adding 2-bromo-4-methylphenol in absolute ethanol, stirring to obtain alcohol dispersion, (ii) adding tetraethyl orthosilicate in deionized water, stirring, dripping aqueous ammonia, adjusting pH, stirring, mixing with alcohol dispersion, increasing temperature, adding sodium myristate soap, heat-preserving while stirring to obtain silica gel dispersion, (iii) adding dimethylamine to silica gel dispersion, heating, distilling off ethanol, filtering, washing precipitate, drying and cooling. USE - Preparation of sol polyaniline composite graphene conductive material. ADVANTAGE - The method improves the dispersion of graphene in the polymer, reduces agglomeration effectively, and improves the stability of finished material. The sol added in the preparation method improves the mechanical property of the composite material, and effectively improves the conductivity of the polymer through acid doping. DETAILED DESCRIPTION - Preparation of sol polyaniline composite graphene conductive material, involves (i) adding 0.6-1 pt. wt. 2-bromo-4-methylphenol to its weight of 20-30 times in absolute ethanol, stirring evenly to obtain alcohol dispersion, (ii) adding tetraethyl orthosilicate to its weight of 40-50 times into deionized water, stirring evenly, dripping aqueous ammonia with concentration of 10-14%, adjusting the pH to 10-12, stirring the reaction for 2-3 hours, mixing with the alcohol dispersion, then increasing the temperature to 60-65 degrees C, adding 1-4 pts. wt. sodium myristate soap, heat-preserving for 40-50 minutes while stirring to obtain silica gel dispersion, (iii) adding 2-3 pts. wt. dimethylamine to the silica gel dispersion, increasing the temperature to 45-50 degrees C, heat-preserving for 1-2 hours while stirring, distilling off ethanol, filtering, washing the precipitate, and drying at 100-110 degrees C for 30-40 minutes, cooling to room temperature to obtain secondary amidated silica sol, (iv) mixing 1-2 pts. wt. acetic acid and 2-4 pts. wt. phosphorus trichloride, adding in deionized water in an amount of 16-20 times the weight of the mixture, stirring evenly to obtain chlorinated mixed solution, (v) mixing 1-3 pts. wt. trichloroisocyanuric acid and 0.5-1 pt. wt. beta -hydroxyalkylamide, adding in deionized water in an amount of 400-500 times the weight of the mixture, stirring, adding 30-40 pts. wt. graphene oxide, ultrasonically processing for 3-5 minutes to obtain acid-doped graphene dispersion, (vi) adding 1-2 pts. wt. methanesulfonyl chloride to 20-30 times its weight in dimethylformamide, stirring evenly, adding to secondary aminated silica sol, increasing the temperature to 65-70 degrees C, stirring for 10-20 minutes, reducing the temperature to room temperature, adding chlorinated mixed solution, ultrasonically processing for 1-2 hours, filtering, precipitating with dimethylformamide, washing with deionized water 3-4 times in sequence, then vacuum drying at 50-60 degrees C for 1-2 hours to obtain amidated silica sol, (vii) adding amidated silica sol to the acid-doped graphene dispersion, stirring evenly to obtain amidated graphene sol dispersion, (viii) adding 150-180 pts. wt. aniline monomer to amidated graphene sol dispersion, stirring evenly, adding with 1-2 pts. wt. dilaurate dibutyltin into the reactor, stirring evenly, purging with nitrogen, increasing temperature to 70-75 degrees C, adding 5-6 pts. wt. initiator, carrying out insulation reaction for 4-6 hours, discharging, filtering, washing the precipitate, vacuum drying at 90-100 degrees C for 2-3 hours, and cooling to room temperature to obtain sol polyaniline composite graphene conductive material.