▎ 摘 要
NOVELTY - Preparation of graphene-added composite thermal insulation material involves adding a fire-resistant and flame-retardant inorganic material and a flame-retardant component to a binder, adding graphene, a dispersant and a coupling agent, fully stirring, dispersing, mixing with expandable polystyrene particles and molding. The flame-retardant component is prepared by (i-1) mixing carbon tetrachloride, phosphorous acid, tetrahydrofuran, triethylamine and diethanolamine and reacting to obtain an intermediate (a1), (i-2) mixing the intermediate (a1) and tetrahydrofuran, adding p-toluenesulfonyl chloride, dripping potassium hydroxide aqueous solution into the solution and reacting to obtain an intermediate (a2), (i-3) mixing intermediate (a2), triphenylphosphine and acetonitrile to obtain a modifier, and (i-4) mixing sodium montmorillonite and deionized water, stirring, dissolving the modifier in absolute ethanol and adding to the mixed solution, and reacting. USE - Preparation of graphene-added composite thermal insulation material. ADVANTAGE - The method enables preparation of graphene-added composite thermal insulation material having improved flame retardance. The modifier used in the preparation of flame-retardant component is a compound containing nitrogen and phosphorus, which can accelerate the flame-retardant component to form a stable carbon layer, thereby preventing heat diffusion and preventing oxygen from entering unburned portion, and simultaneously releasing incombustible gas and diluting concentration of combustible gas. DETAILED DESCRIPTION - Preparation of graphene-added composite thermal insulation material involves (i) adding a fire-resistant and flame-retardant inorganic material and a flame-retardant component to a binder, adding graphene, a dispersant and a coupling agent, fully stirring and dispersing to obtain a mixture, and (ii) mixing the mixture with expandable polystyrene particles, stirring and dispersing, adding to a molding machine, performing steam heating and performing secondary foaming molding. The flame-retardant component is prepared by (i-1) mixing carbon tetrachloride, phosphorous acid and tetrahydrofuran, reducing the temperature to 0 degrees C, dripping triethylamine and diethanolamine into the obtained solution, reacting by stirring at 20 degrees C for 11 hours and post-processing to obtain an intermediate (a1), (i-2) mixing the intermediate (a1) and tetrahydrofuran, adding p-toluenesulfonyl chloride at a temperature of 0 degrees C, dripping potassium hydroxide aqueous solution into the obtained solution, reacting at 20 degrees C for 7 hours and post-processing to obtain an intermediate (a2), (i-3) mixing the intermediate (a2), triphenylphosphine and acetonitrile, setting the temperature to 80 degrees C under nitrogen protection, refluxing for 72 hours and post-processing to obtain a modifier, and (i-4) mixing sodium montmorillonite and deionized water, stirring at 80 degrees C for 2 hours to obtain a mixed solution, dissolving the modifier in absolute ethanol and adding to the mixed solution, maintaining the temperature at constant, continuously stirring, reacting for 5 hours and post-processing.