▎ 摘　　要

NOVELTY - Preparation of phthalocyanine/graphene composite sensing material, involves adding concentrated sulfuric acid, graphite powder and sodium nitrate, stirring, adding potassium permanganate, heating, stirring, adding distilled water, heating, diluting with distilled water, adding hydrogen peroxide solution, washing, drying, dispersing graphene oxide in distilled water, ultrasonically dispersing, adding hydrazine hydrate solution, adjusting pH, filtering and washing to obtain graphene, grinding pyromellitic anhydride, urea, chloride salt and ammonium molybdate, heating to obtain black intermediate product, immersing in hydrochloric acid, filtering, adding hot water, washing, adding intermediate product to aqueous solution of sodium hydroxide, heating, stirring, suction filtering, adjusting pH, centrifuging to obtain phthalocyanine derivative, dispersing graphene in organic solvent, adding phthalocyanine derivative to dispersion, ultrasonically dispersing and leaving still the product. USE - Method for preparing phthalocyanine/graphene composite sensing material for cyanide ion recognition (claimed). ADVANTAGE - The method enables simple, rapid and economical preparation of phthalocyanine/graphene composite sensing material with high sensitivity, and detects the cyanide ion of 1-100 mu M. DETAILED DESCRIPTION - Method for preparing phthalocyanine/graphene composite sensing material, involves (1) adding 23-92 ml concentrated sulfuric acid, 1-4 g graphite powder and 0.5-2 g sodium nitrate, stirring at 0-3 degrees C for 10-30 minutes, slowly adding 3-12 g potassium permanganate, heating at less than 20 degrees C, stirring in an ice water bath for 2-4 hours to obtain reaction liquid as ink green suspension, reacting at 35 degrees C for 30-60 minutes, then slowly adding distilled water, heating at not more than 100 degrees C, diluting the reaction with a large amount of distilled water after 15-45 minutes, adding 5-15 ml of 30-50 wt.% hydrogen peroxide solution, gradually changing the reaction liquid to bright yellow suspension, washing with distilled water and dilute hydrochloric acid, detecting with barium chloride solution until the filtrate is free of sulfate ion, drying to obtain graphene oxide, dispersing 100-300 mg graphene oxide in 100-300 ml distilled water, ultrasonically dispersing for 30-60 minutes, forming uniform yellow-brown turbid liquid, adding 85-250 mu L hydrazine hydrate solution, adjusting the pH of the reaction solution with aqueous ammonia at 9-11, reacting for 1-3 hours under oil bath condition of 85-95 degrees C, filtering and washing to obtain graphene, (2) fully grinding pyromellitic anhydride, urea, chloride salt and catalyst ammonium molybdate, heating for 5-10 minutes to obtain black intermediate product, immersing in 2-6 M hydrochloric acid for 12-24 hours, filtering, adding large amount of hot water, washing the filter cake, adding intermediate product to aqueous solution of sodium hydroxide with mass fraction of 5-20 %mass, heating, stirring at 75-95 degrees C for 6-12 hours, suction filtering, adjusting the pH of filtrate at 2-4 with hydrochloric acid, centrifuging to obtain phthalocyanine derivative, (3) dispersing 5-20 mg graphene in 50-150 ml organic solvent, ultrasonically processing for 0.5-2 hours, so that the graphene is uniformly dispersed in the solvent, adding 5-10 mu M phthalocyanine derivative to dispersion, ultrasonically dispersing at room temperature for 0.5-2 hours, and leaving still for 10-40 minutes to obtain final product. The molar ratio of pyromellitic anhydride, urea and chloride is 1:10-20:2-3. An INDEPENDENT CLAIM is included for application of phthalocyanine/graphene composite sensing material, which involves uniformly assembling 5-10 mg phthalocyanine derivative/graphene solution on filter paper and uniformly coating the high-polymer film with film-forming material to obtain test paper.