• 专利标题:   Preparing cage-type molecular modified graphene oxide flame retardant useful for e.g. daily life in coating, plastic, comprises taking cage phosphate into three-mouth flask, adding e.g. pentaerythritol, heating, cooling and reacting.
  • 专利号:   CN106432802-A, CN106432802-B
  • 发明人:   FU W, LIU Z, QIAN J, WANG N, WANG S, ZHOU L
  • 专利权人:   UNIV SHENYANG CHEM TECHNOLOGY CO LTD, UNIV SHENYANG CHEM TECHNOLOGY CO LTD
  • 国际专利分类:   C08K003/04, C08K005/527, C08K009/04, C09D163/00, C09D005/18
  • 专利详细信息:   CN106432802-A 22 Feb 2017 C08K-009/04 201733 Pages: 7 Chinese
  • 申请详细信息:   CN106432802-A CN10846413 23 Sep 2016
  • 优先权号:   CN10846413

▎ 摘  要

NOVELTY - Preparing cage-type molecular modified graphene oxide flame retardant comprises (a) taking cage phosphate into three-mouth flask, adding e.g. pentaerythritol into dioxane, stirring, placing into water bath, heating, reacting to obtain white solid, dissolving white solid into absolute ethanol, filtering, cooling and re-crystallizing and vacuum drying, (b) taking acyl chloride-activated pentaerythritol phosphate of dioxane into a three-neck flask, steaming, reacting to obtain acyl chloride activated PEPA intermediates, (c) taking acyl chloride PEPA with graphene oxide, rotating and reacting. USE - The flame retardant is useful for daily life in coating, plastic, rubber and other polymer materials. ADVANTAGE - The flame retardant has no halogen, no toxicity and is environment-friendly. DETAILED DESCRIPTION - Preparing cage-type molecular modified graphene oxide flame retardant comprises (a) taking cage phosphate into 500 ml three-mouth flask, adding 0.2-1 mol pentaerythritol and 0.2-1 mol phosphorus oxychloride, pouring 150-300 ml dioxane as solvent, under stirring at 80-220 revolutions/minute, placing into water bath at 80-90 degrees C for 1-3 hours, continuously heating at 90-100 degrees C, refluxing and reacting for 2-4 hours, finally the temperature is fixed at 95 degrees C, slowly evaporating solvent while stirring and reacting to obtain white solid, dissolving white solid into 200-400 ml absolute ethanol, stirring to completely for dissolving, placing in water bath, stirring at 80-180 revolutions/minute at 70-85 degrees C, filtering at 15-30 degrees C, cooling and re-crystallizing, vacuum drying at 60-120 degrees C for 10-24 hours, (b) taking 100-300 ml acyl chloride-activated pentaerythritol phosphate (PEPA) of dioxane into a three-neck flask, steaming adding 0.2-1 mol diacid chloride, poured into flask containing solvent, under the protection of nitrogen, rotating at 80-220 revolutions/minute, electromagnetic stirring for 3-15 minutes, taking 0.2-1 mol PEPA, adding 5-30 times PEPA into the three-mouth bottle, speed of each time interval is 3-30 minutes and slowly adding into the reaction bottle, adding acid-binding agent to adjust the solution pH value to 7-10,reating at 50-80 degrees C for 4-6 hours to obtain acyl chloride activated PEPA intermediates, (c) reacting acyl chloride PEPA with graphene oxide forming covalent bonding and weight is 50-100 g of graphene oxide, dispersing into 100-400 ml dioxane solvent, 20-40Khz lower frequency ultrasound for 2-5 hours, pouring activated PEPA into intermediate prepared acyl chloride solution, rotating at 80-220 revolutions/minute at 50-80 degrees C and continuously reacting for 5-8 hours.