▎ 摘 要
NOVELTY - Preparing highly stable ceramic-based subnanoporous graphene composite film comprises (1) preparing inorganic transition layer on the ceramic carrier by impregnation-pulling and high-temperature sintering, and drying successfully impregnated carrier and sintering at high temperature, (2) adding graphite oxide powder into deionized water, peeling off the graphite powder by ultrasonic instrument for 2-3 hours to obtain graphene oxide nanosheet dispersion, (3) configuring crosslinking agent solution with mass fraction of 0.1-1 wt.%, and mixing and stirring the graphene oxide suspension and the crosslinking agent solution for more than 16 hours to obtain the graphene oxide-crosslinking agent suspension, and (4) preparing by vacuum filtration method and gas atmosphere reduction method, connecting the ceramic support with inorganic transition layer on the suction filtration device, and raising the temperature to 300-1000℃ at a rate of 1-5℃/minute. USE - The composite film is useful for removing boron in water during the pervaporation process, removing antibiotic pollutants in water during the pervaporation process, and low-concentration volatile organic pollutant wastewater in water during the pervaporation process (all claimed). ADVANTAGE - The composite film: can realize high-efficiency precision separation applications through pervaporation process, e.g. seawater desalination, high-salt wastewater desalination, seawater and geothermal wastewater deboronation and other wastewater (e.g. antibiotic wastewater and low-concentration volatile organic pollutant wastewater); and has excellent separation performance and extreme environmental stability. DETAILED DESCRIPTION - Preparing highly stable ceramic-based subnanoporous graphene composite film comprises (1) preparing inorganic transition layer on the ceramic carrier by impregnation-pulling and high-temperature sintering, configuring the inorganic transition layer sol with concentration of 0.01-0.5 wt.%, dipping and pulling the ceramic carrier in the inorganic transition layer sol, where the dipping time is 5-10 seconds, controlling the pulling speed at 0.5-1.5 cm/second, drying successfully impregnated carrier and sintering at high temperature to obtain inorganic transition layer with thickness of 1-10, (2) adding graphite oxide powder into deionized water, peeling off the graphite powder by ultrasonic instrument for 2-3 hours to obtain graphene oxide nanosheet dispersion, and removing the lower sediment by centrifugation to obtain completely dispersed graphene oxide suspension, where the ratio of described graphite oxide powder to deionized water is 5-50 mg:100 ml, (3) configuring crosslinking agent solution with mass fraction of 0.1-1 wt.%, and mixing and stirring the graphene oxide suspension and the crosslinking agent solution for more than 16 hours to obtain the graphene oxide-crosslinking agent suspension, where the volume ratio of the graphene oxide suspension to the crosslinking agent solution is (1-10):(10-1), and (4) preparing by vacuum filtration method and gas atmosphere reduction method, connecting the ceramic support with inorganic transition layer on the suction filtration device, placing into the graphene oxide-crosslinking agent suspension and suction filtration 10-60 minutes, forming stacked continuous film layer on the surface of the carrier, drying in oven at 40-100℃ for 6-12 hours, placing the dried composite membrane into tube furnace and introducing with gas with flow rate of 10-100 ml/minutes, raising the temperature to 300-1000°C at a rate of 1-5℃/minute, and obtaining highly stable ceramic-based subnanoporous graphene composite film after high-temperature carbonization and reduction for 0.5-10 hours. The composite film is based on ceramics, low-roughness fine-pore inorganic transition layer is introduced on the surface of the carrier, and complete sub-nanometer porous graphene separation layer is introduced, the thickness of the sub-nanoporous graphene separation layer is between 10-500 nm, and the pure water flux in the pervaporation process is 10-300 l/m2/hour at 20-70℃.