• 专利标题:   Complex flame retardant useful for rubber, prepared by carrying out cross-linking reaction of modified graphene with cyanuric chloride and dipiperazine phenylphosphine chloride to obtain graphene flame retardant, and loading on nitrate mixed solution and reacting with e.g. trimethoxysilane.
  • 专利号:   CN115746403-A
  • 发明人:   YAN H, SUN W, HAN C, CHENG M, WANG X, WU T
  • 专利权人:   TAIAN YARONG BIOTECHNOLOGY CO LTD
  • 国际专利分类:   C08K003/04, C08K003/28, C08K009/04, C08K009/12, C08L007/00, C08L083/07
  • 专利详细信息:   CN115746403-A 07 Mar 2023 C08K-009/04 202323 Chinese
  • 申请详细信息:   CN115746403-A CN11506856 29 Nov 2022
  • 优先权号:   CN11506856

▎ 摘  要

NOVELTY - Complex flame retardant, which is a graphene flame retardant obtained after cross-linking reaction of modified graphene, cyanuric chloride, and dipiperazinyl phenylphosphine, loading the nitrate mixture with graphene flame retardant and reacting with trimethoxysilane and vinyl hyperbranched polysiloxane in sequence. USE - The flame retardant is useful for rubber (claimed). ADVANTAGE - The flame retardant rubber has excellent flame retardant property and anti-fracture performance. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is also included for reparing the complex flame retardant comprising (1) preparation of modified graphene: uniformly mixing dipiperazinyl phenylphosphine, triethylamine and trichloromethane in mass ratio of 1:0.3:15-1:0.4:20 stirring at 0-5℃ and 300-500 revolutions/minute for 3-5 minutes, continuously stirring, adding acylated graphene with 1.4-1.6 times the mass of dipiperazinylphenylphosphine, continuing to stir and react for 1-2 hours, filtering and washing with chloroform for 3-5 times, drying for 3-4 hours at 20-30℃ and 10-50 Pascal, preparing modified graphene, (2) crosslinking: uniformly mixing the modified graphene cyanuric chloride and trichloromethane in mass ratio of 1:1:15-1:1:20, stirring and reacting at 0-5℃ and 300-500 revolutions/minute for 30-40 minutes, adding dipiperazinyl phenylphosphine (0.2-0.3 times), continuing to stir and react for 5-6 hours, raising the temperature to 50℃, adding modified graphene dipiperazinyl phenyl phosphine (0.2-0.3 times), continuing to stir for 3-4 hours, heating up to 90℃, adding modified graphene dipiperazinyl phenyl phosphine (0.2-0.3 times), continuing to stir and react for 8-10 hours, keeping pH control throughout the reaction process, filtering and washing with chloroform for 3-5 times, drying at 20-30℃ and 10-50 Pa for 3-4 hours, grinding until the grain diameter is less than 0.05 mm, obtaining the graphene flame retardant, (3) loading: uniformly mixing graphene flame retardant and nitrate mixture in a mass ratio of 1:20-1:30, ultrasonic reaction at 90-100℃ and 30-40 kHz for 20-24 hours, filtering and using pure water to wash for 3-5 times, drying at 60-70℃ for 10-12 hours to obtain flame retardant and (4) surface grafting: uniformly mixing the trimethoxy silane, anhydrous ethanol pure water in ratio of 1:140:20-1:180:30, stirring at 10-30℃ and 200-400 revolutions/minute for 40-50 minutes, adding trimethoxy silane (4-5 times), continuously stirring for 80-100 minutes, filtering and using pure water to wash for 3-5 times, drying for 10-12 hours at 60-70℃, uniformly mixing vinyl hyper-branched polysiloxane, chloroplatinic acid and n-hexane in mass ratio of 1:0.3:0.03:8-1:0.5:0.05:12, stirring and reacting at 70-80℃, 400-800 revolutions/minute for 4-6 hours, filtering and washing for 3-5 times with anhydrous ethanol at 20-30℃ and drying at 10-50 Pa for 3-4 hours to obtain the complex flame retardant.