• 专利标题:   Preparation of graphene/nano silicon dioxide/polyvinyl chloride resin particles involves forming modified graphene/nano silicon dioxide at preset conditions, followed by aqueous phase micro-suspension polymerization of modified graphene/nano silicon dioxide and vinyl chloride, at preset conditions.
  • 专利号:   CN113788905-A, CN113788905-B
  • 发明人:   WAN B, LOU J, ZHENG Q, CHEN Z, LU K, YE X, GE Q
  • 专利权人:   HANGZHOU ELECTROCHEMICAL GROUP CO LTD
  • 国际专利分类:   C08F114/06, C08F002/20, C08F002/44, C08K003/04, C08K003/36, C08K007/00, C08K009/06
  • 专利详细信息:   CN113788905-A 14 Dec 2021 C08F-114/06 202219 Chinese
  • 申请详细信息:   CN113788905-A CN11187985 23 Apr 2020
  • 优先权号:   CN10326650, CN11187985

▎ 摘  要

NOVELTY - Preparation of graphene/nano silicon dioxide/polyvinyl chloride resin, involves: 1) mixing 1000 parts of deionized water, 2-15 parts of graphene, 1-8 parts of emulsifier, 1-5 parts of silane coupling agent and 15-50 parts of nano silicon dioxide in a container, heating to 55-80degrees Celsius, treating for 3-7 hours at 500-1000 watts (W), again treating for 2-5 hours at 500-1000W to form modified graphene/nano silicon dioxide; 2) adding 10000 parts of deionized water, 6 parts of composite emulsifier, 0.5 part of pH regulator and 0.1-0.3 part of chain extender, followed by adding 1022-1078 parts of modified graphene/nano silicon dioxide, 10-15 parts of initiator, discharging nitrogen for 3 times, vacuumizing to-0.98 MPa, adding 5000 parts of vinyl chloride, stirring at 10-25degrees Celsius for 30 minutes, at preset speed. Further reaction is performed at preset conditions and then adding terminator to form slurry of graphene/nano silicon dioxide/polyvinyl chloride resin. USE - The distribution method is used for preparing graphene/nano silicon dioxide/polyvinyl chloride resin particles. ADVANTAGE - The graphene/nano silicon dioxide/polyvinyl chloride resin particles prepared from modified graphene/silicon dioxide and chloroethylene through aqueous phase micro-suspension polymerization, are fine particles having improved thermal stability and mechanical property. DETAILED DESCRIPTION - A distribution preparation method for graphene/nano silicon dioxide/polyvinyl chloride resin, involves: 1) mixing 1000 parts of deionized water, 2-15 parts of graphene, 1-8 parts of emulsifier, 1-5 parts of silane coupling agent and 15-50 parts of nano silicon dioxide in a container, heating to 55-80degrees Celsius, placing the container in ultrasonic processor, treating for 3-7 hours at 500-1000 watts (W). The container is taken out and liquid is poured into a microwave reactor and treated for 2-5 hours at 500-1000W to form modified graphene/nano silicon dioxide; 2) polymerization step: adding 10000 parts of deionized water, 6 parts of a composite emulsifier, 0.5 part of pH regulator and 0.1-0.3 part of chain extender into a stainless steel polymerization kettle, followed by adding 1022-1078 parts of modified graphene/nano silicon dioxide prepared in step 1, and 10-15 parts of an initiator, closing the kettle, discharging nitrogen for 3 times, vacuumizing to-0.98 MPa, adding 5000 parts of vinyl chloride, stirring at 10-25degrees Celsius for 30 minutes, at speed 300 rotations/minute. The speed is then adjusted to 180 rotations/minute, followed by heating to 57 degrees Celsius, reacting for 2.5-4 hours, adding a terminator after the reaction is finished. The slurry is centrifuged, and the obtained solid is dried to form graphene/nano silicon dioxide/polyvinyl chloride resin. The graphene is physical multilayer graphene. The amount of graphene contained in the resin is 0.5-50, based on the weight of vinyl chloride monomer. The emulsifier used in step 1) is reactive surfactants selected from allyl polyoxyethylene ether and/or 3-allyloxy-1-hydroxy-1-propane sulfonate. The amount of the emulsifier used is 30-10 wt.%, based on the weight of graphene.