• 专利标题:   Preparing polyisoprene functionalized graphene by adding graphene oxide to anhydrous tetrahydrofuran, ultrasonically treating, bubbling nitrogen, adding isopropylmagnesium chloride, vacuum filtering and removing excess reagents.
  • 专利号:   CN111087559-A
  • 发明人:   INVENTOR U
  • 专利权人:   HAIMEN YUANMEI ART DESIGN CO LTD
  • 国际专利分类:   C08F236/08, C08F292/00
  • 专利详细信息:   CN111087559-A 01 May 2020 C08F-292/00 202044 Pages: 5 Chinese
  • 申请详细信息:   CN111087559-A CN11232704 23 Oct 2018
  • 优先权号:   CN11232704

▎ 摘  要

NOVELTY - Method for preparing polyisoprene functionalized graphene involves (i) adding graphene oxide to anhydrous tetrahydrofuran, ultrasonically treating, bubbling nitrogen to replace air in flask, adding isopropylmagnesium chloride to anhydrous tetrahydrofuran solution, refluxing, vacuum filtering reaction product, washing with anhydrous tetrahydrofuran and n-hexane, removing excess Grignard reagents and reaction by-products, and drying under vacuum to obtain graphene oxide-magnesium, and (ii) adding graphene oxide-magnesium and titanium (IV) chloride to flask under nitrogen protection, reacting, slowly pouring mixture in flask into glacial ethanol and continuously stirring, dissolving, and performing vacuum suction filtration, and washing the product with hot n-hexane to obtain graphene oxide-titanium, mixing graphene oxide-titanium, triisobutylaluminum and isoprene, polymerizing, adding methanol to terminate the reaction, washing the product, and vacuum-drying. USE - Method for preparing polyisoprene functionalized graphene. ADVANTAGE - The method is simple and successfully prepared polyisoprene functionalized graphene with excellent dispersibility. DETAILED DESCRIPTION - Method for preparing polyisoprene functionalized graphene involves (i) adding 10-20 pts. wt. graphene oxide to flask containing 60-70 pts. wt. anhydrous tetrahydrofuran, ultrasonically treating for 40-50 minutes, bubbling nitrogen to replace the air in the flask several times, adding 20-30 pts. wt. 1.5 mol/l isopropylmagnesium chloride to anhydrous tetrahydrofuran solution, increasing the temperature at 65-75 degrees C and refluxing for 27-29 hours, vacuum filtering the reaction product, washing the product with anhydrous tetrahydrofuran and n-hexane, removing excess Grignard reagents and reaction by-products, and drying under vacuum at 65-75 degrees C for 47-49 hours to obtain graphene oxide-magnesium, and (ii) adding 7-9 pts. wt. graphene oxide-magnesium and 30-40 pts. wt. titanium (IV) chloride (TiCl4) to the flask under nitrogen protection, reacting at 100-105 degrees C for 5-6 hours, after the reaction is completed, slowly pouring the mixture in the flask into glacial ethanol and continuously stirring, dissolving the TiCl4 that did not participate in the reaction in ethanol, and performing vacuum suction filtration, and washing the product with hot n-hexane to obtain graphene oxide-titanium under the condition of 34-36 degrees C, mixing 10-20 pts. wt. graphene oxide-titanium, 8-12 pts. wt. triisobutylaluminum and 30-40 pts. wt. isoprene, polymerizing for 3-5 hours, adding methanol to terminate the reaction, washing the product with ethanol and n-hexane, and vacuum-drying at 45-55 degrees C for 25-27 hours to obtain the product.