▎ 摘　　要

NOVELTY - Preparation of masterbatch involves (A) adding graphene to mixed acid, ultrasonically processing, acidifying to obtain graphene slurry, centrifuging the graphene slurry, recovering the obtained supernatant, separating the bottom black graphene suspension, washing, drying to obtain acidified graphene, preparing solution using methanol and water, heating the solution, adding mixed modifier to the solution, mixing to obtain a mixed hydrolyzate, which is graphene modified solution, adding the acidified graphene to the graphene modified solution, adding graphene to the solution, ultrasonically processing to perform graphene modification, stirring, centrifuging, washing, adding methanol to obtain modified graphene-methanol suspension, (B) preparing unsaturated polyolefin solution, (C) placing the graphene methanol suspension and unsaturated polyolefin solution into two containers, stirring, centrifuging the reaction product to collect the lower sediment and baking. USE - Preparation of masterbatch for preparing polymer composite material. ADVANTAGE - The method produces masterbatch which utilizes graphene having uniform distribution. The masterbatch improves the electrical conductivity and mechanical properties of the polymer composite material. DETAILED DESCRIPTION - Preparation of masterbatch involves (A) adding graphene to mixed acid of concentrated nitric acid and sulfuric acid in a ratio of 1:3, ultrasonically processing at 50-70 degrees C under a frequency of 15-40 kHz for 2-8 hours, acidifying to obtain graphene slurry, centrifuging the graphene slurry at a speed of 4000 rpm for 10 minutes using a centrifuge to separate the mixture, recovering the obtained supernatant, separating the bottom black graphene suspension, washing with clean water, adjusting the pH of the suspension to 6 or more, drying at 60-80 degrees C to a constant weight using a vacuum oven to obtain acidified graphene, preparing solution using 80-95 wt.% methanol and water, heating the solution to 50-80 degrees C, adjusting the pH of the solution to 4-6 using formic acid, adding mixed modifier of aminosilane coupling agent and polyether surfactant to the solution, mixing at a speed of 500-2000 rpm while ultrasonically stirring under a frequency of 10-30 kHz to hydrolyze the aminosilane coupling agent for 2-20 hours to obtain a mixed hydrolyzate, which is graphene modified solution, adding the acidified graphene to the graphene modified solution, adding 0.01-20 wt.% graphene to the solution, adjusting the temperature of the solution to 50-80 degrees C, ultrasonically processing to perform graphene modification for 1-10 hours, stirring at a speed of 500-2000 rpm to ensure that the graphene mixed liquid is flow dynamic, centrifuging the modified graphene slurry at a speed of 4000 rpm for 10 minutes using a centrifuge to separate the graphene suspension at the bottom layer, washing 3 times with methanol, adding methanol to obtain modified graphene-methanol suspension having graphene content of 0.1-10 wt.%, (B) heating cyclohexane to 50-80 degrees C, adding 5-15 wt.% unsaturated polyolefin particles, maintaining the temperature constant, stirring at a speed of 500-2500 rpm until the particles completely disappear and the liquid is transparent to obtain unsaturated polyolefin solution, (C) placing the graphene methanol suspension and unsaturated polyolefin solution into two containers equipped with stirring device and discharge port to stably control the liquid outflow speed, using the stirring device of the container to stir the graphene slurry at a speed of 500-4000 rpm and the unsaturated polyolefin solution at a speed of 300-1000 rpm, closing the discharge port of the two containers, placing the closed container under the discharge port to hold the products, opening the discharge port, setting the outlet flow rates of the two containers, closing the discharge ports, centrifuging the reaction product in the lower container at a speed of 2000 rpm for 5 minutes using a centrifuge to collect the lower sediment, baking at 80-120 degrees C using a vacuum oven to obtain masterbatch and (D) compounding the masterbatch with conductive functional component, polymers and functional components such as reinforcer or flame-retardant by melt blending to prepare a polymer composite material. The masterbatch has graphene content of 0.1-60 wt.%.