• 专利标题:   Preparing synergistic flame retardant graphene polymer material involves taking graphene oxide, adding absolute ethanol, obtaining epoxy solution, adding dodecyl primary amine, adding pentaerythritol, and obtaining anhydride polymer.
  • 专利号:   CN106893274-A, CN106893274-B
  • 发明人:   YANG B, YU F, YANG Z, MA Q
  • 专利权人:   SHANDONG BENYUAN CRYSTAL TECHNOLOGY CO
  • 国际专利分类:   C08F218/08, C08F222/06, C08F008/12, C08G063/183, C08K013/06, C08K003/04, C08K003/36, C08K009/04, C08L031/04, C08L067/02
  • 专利详细信息:   CN106893274-A 27 Jun 2017 C08L-067/02 201765 Pages: 6 Chinese
  • 申请详细信息:   CN106893274-A CN10187796 27 Mar 2017
  • 优先权号:   CN10187796

▎ 摘  要

NOVELTY - Preparing synergistic flame retardant graphene polymer material involves taking graphene oxide, adding 3-10 times absolute ethanol, raising temperature to 40-55 degrees C, adding propylene oxide, and stirring for 20-30 minutes to obtain epoxy solution. The dodecyl primary amine, 3-5 times the weight of pentaerythritol are added and stirred. The epoxy solution is added and reaction is stirred for 10-13 hours. The 4-6 wt.% phosphoric acid aqueous solution is dropped temperature is raised to 90-100 degrees C. The stannous octoate is added. USE - Method for preparing synergistic flame retardant graphene polymer material (claimed). ADVANTAGE - The method enables to prepare synergistic flame retardant graphene polymer material, which has good flame retardant performance. DETAILED DESCRIPTION - Preparing synergistic flame retardant graphene polymer material involves taking graphene oxide, adding 3-10 times absolute ethanol, raising temperature to 40-55 degrees C, adding propylene oxide, and stirring for 20-30 minutes to obtain epoxy solution. The dodecyl primary amine, 3-5 times the weight of pentaerythritol are added and stirred. The epoxy solution is added and reaction is stirred for 10-13 hours. The 4-6 wt.% phosphoric acid aqueous solution is dropped temperature is raised to 90-100 degrees C. The stannous octoate is added. The reaction is carried out for 5-7 hours, filtered, washed with water, vacuumed at 70-90 degrees C for 2-3 hours, and cooled to obtain the esterified graphene. The sorbitan monostearate, 16-18 times the weight of ethyl acetate are added and stirred and dissolved. The phosphorus esterification graphene is added and preheated at 50-60 degrees C for 10-20 minutes to obtain ester dispersion. The maleic anhydride and vinyl acetate are mixed. The mixture is added with 80-100 times the butyl acetate and stirred. The ester dispersion is added and stirred. The catalyst is added and nitrogen is introduced and stirred at 70-76 degrees C for 4-7 hours, filtered. The precipitate is vacuum dried at 50-60 degrees C for 1-2 hours, cooled to room temperature to obtain anhydride polymer. The anhydride polymer is added to the deionized water at its weight of 100-120 times and stirred at 60-70 degrees C for 4-5 hours. The mixture is filtered, washed with water and dried at room temperature to hydrolyze the polymer. The ethyl orthosilicate is taken and added with 400-470 times the weight of deionized water, stirred and 10-12 wt.% ammonia is dropped to adjust the pH to 10-12, and stirred at room temperature for 2-3 hours. The tert-butyl alcohol is added and temperature is raised to 60-70 degrees C. The temperature is kept for 1-2 hours to obtain the hydroxylated silica sol. The molar ratio of 2-3: 1 of ethylene glycol, terephthalic acid are mixed into the reactor. The nitrogen is introduced and temperature is raised to 230-250 degrees C. The reactor pressure is 0.2-0.3MPa. The esterification reaction is performed for 3-5 hours to obtain material, which is dried at 70-80 degrees C to obtain phosphide ester monomer. The hydrolysed polymer, phosphide ester monomer mixture are sent to the reactor and nitrogen is introduced in the reactor exhaust. The temperature is raised to 270-300 degrees C. The stirring blade is opened and stirring reaction is performed for 4-6 hours to obtain the material. The hydroxyl silicon sol is mixed and stirring reaction is performed for 2-3 hours, cooled, dehydrated, vacuumized at 90-100 degrees C for 1-2 hours to obtain synergistic flame retardant graphene polymer material. The graphene oxide, propylene oxide, dodecyl primary amine, phosphoric acid aqueous solution having a concentration of 4-6 wt.%, stannous octoate, sorbitan monostearate, t-butanol, maleic anhydride, vinyl acetate, azobisisobutyronitrile, ethyl orthosilicate and terephthalic acid are added in weight ratio of 20-26: 1-2: 3-5: 130-170: 0.4-1: 3-5: 20-26: 6-10: 37-40: 1.3-2: 20-25: 300-370.