• 专利标题:   Preparing modified graphene oxide-silica composite filler by mixing graphene oxide and water, dispersing, adding modifier and aqueous ammonia, freeze-drying, mixing silicon source and modified graphene oxide, adding surfactant, and aging.
  • 专利号:   CN112980217-A
  • 发明人:   DING G, TAI H, HU Y, CHENG G, LU Q, CHEN C, WU M
  • 专利权人:   UNIV ANHUI SCI TECHNOLOGY, JIANGSU XINLU TRANSPORTATION DEV CO LTD
  • 国际专利分类:   C08K013/06, C08K003/04, C08K003/36, C08K009/04, C08L009/06, C08L091/00, C09C001/46, C09C003/06, C09C003/08
  • 专利详细信息:   CN112980217-A 18 Jun 2021 C09C-001/46 202165 Pages: 8 Chinese
  • 申请详细信息:   CN112980217-A CN10194737 21 Feb 2021
  • 优先权号:   CN10194737

▎ 摘  要

NOVELTY - Preparing modified graphene oxide-silica composite filler, involves (a) mixing graphene oxide and water to obtain graphene oxide aqueous solution, and dispersing to obtain graphene oxide aqueous solution, (b) adding modifier and aqueous ammonia to the aqueous solution, (c) adding to a hydrothermal reactor, and cooling, (d) washing with deionized water to remove unreacted modifier, and freeze-drying to obtain modified graphene oxide, (e) mixing the modified graphene oxide and deionized water to obtain modified graphene oxide aqueous solution, and dispersing to obtain modified graphene oxide aqueous solution, (f) mixing silicon source and modified graphene oxide aqueous solution to obtain a mixed solution, adding surfactant, heat-preserving the mixture, adding dilute hydrochloric acid, and forming a gel-like substance to obtain modified graphene oxide-silica gel, (g) leaving the gel still, aging, and washing with deionized water, and (h) drying, and pulverizing the dried powder. USE - The method is useful for preparing modified graphene oxide-silica composite filler used in solution-polymerized styrene butadiene rubber. ADVANTAGE - The method effectively solves the problem of agglomeration of reinforcing fillers, reduces the interaction between fillers, and improves the mechanical properties and anti-aging properties of rubber. DETAILED DESCRIPTION - Preparing modified graphene oxide-silica composite filler, involves (a) mixing graphene oxide and water in a mass ratio of 1:(40-60) to obtain graphene oxide aqueous solution, and ultrasonically dispersing at 25-30 degrees C for 25-35 minutes under an ultrasonic frequency of 35-40 kHz using an ultrasonic cleaning machine to obtain 16-25 mg/ml graphene oxide aqueous solution, (b) adding modifier and aqueous ammonia with a pH of 10-11 to the aqueous solution, where the volume ratio of the modifier, the aqueous ammonia, and aqueous solution is (5-7):(1-3):25, (c) magnetically stirring at 25-30 degrees C for 20 minutes, adding to a hydrothermal reactor, reacting at 170-190 degrees C for 8-12 hours, and cooling, (d) washing with deionized water for 3-5 times to remove unreacted modifier, and freeze-drying for 48 hours to obtain modified graphene oxide, (e) mixing the modified graphene oxide and deionized water in a mass ratio of 1:1200 to obtain modified graphene oxide aqueous solution, and ultrasonically dispersing at 25-30 degrees C for 25-35 minutes under an ultrasonic frequency of 35-40 kHz using the ultrasonic cleaning machine to obtain 0.83 mg/ml modified graphene oxide aqueous solution, (f) mixing the silicon source and modified graphene oxide aqueous solution in a mass ratio of 1:5 to obtain a mixed solution, adding surfactant, where the mass ratio of the surfactant to the modified graphene oxide aqueous solution is 1:500, mixing, pre-stirring for 20-30 minutes, heat-preserving the mixture at 0-5 degrees C, adding 1 mol/l dilute hydrochloric acid, where the mass ratio of silicon source to dilute hydrochloric acid is 1:2.5, stirring while dripping for 4-6 hours, and forming a gel-like substance to obtain modified graphene oxide-silica gel, (g) leaving the gel still, aging for 10-12 hours, filtering under reduced pressure using a suction filter, and washing with deionized water for 5-10 times, and (h) drying in a blast drying oven at 80 degrees C for 5-8 hours, and pulverizing the dried powder to obtain the composite filler. An INDEPENDENT CLAIM is included for use of the composite filler in solution-polymerized styrene butadiene rubber, comprising 100 parts per hundred (phr) solution polymerized styrene butadiene rubber (SLR3402), 6 phr zinc oxide, 1 phr stearic acid, 0.7 phr accelerator CZ, 0.6 phr accelerator DM, phr sulfur 2.5, 5 phr aromatic oil tetrakis(dimethylamino)ethylene, 0.1 phr scorch inhibitor and 30-50 phr composite filler.