▎ 摘 要
NOVELTY - Preparing fluorescent coating, involves: (1) reacting sulfuric acid, 5-nitro-pyridine-3, 4-diamine and sodium nitrite, to form 5-nitro-pyridine-3, 4-diamine, reacting 6-cyano-indole -3 -carboxylate methyl ester and sodium hydroxide and methyl 6-cyanindole-3-carboxylate, to form azo compounds; (2) reacting azo compound, 2, 2, 6, 6-tetramethyl piperidine alcohol and tetraisopropyl titanate, to obtain light stable compound (A); (3) reacting benzoin with compound (A), adding petroleum ether, to obtain benzoin condensate; (4) reacting europium chloride, benzoin condensate and 4,7-dihydroxy-1,10-phenanthroline, to form fluorescent powder; (5) forming microcapsules; 6) treating graphene oxide with triethylamine, adding 2 bromoisovaleryl bromide, adding a triazole compound, reacting to obtain modified graphene; (7) reacting modified graphene, azobisisobutyronitrile and microcapsule, adding 1-hydroxyl tetradecane, mixing formed paint precursor with ethyl acetate and resin USE - Method is used for preparing corrosion resistant fluorescent coating. ADVANTAGE - The use of modified graphene, 2 bromoisovaleryl bromide and 5 mercapto -4-p-chlorophenyl-4 hydrogen-3 hydroxy 1,2,4 triazole, in the preparation of corrosion-resistant fluorescent paint, enables to improve the dispersion of graphene oxide. The prepared corrosion-resistant fluorescent paint has enhanced corrosion resistance and long-lasting fluorescence. DETAILED DESCRIPTION - Preparation corrosion resistant fluorescent coating, involves: (1)mixing 98 wt.% concentrated sulfuric acid, deionized water, 5-nitro-pyridine-3, 4-diamine, in mass ratio 1.5: 3.5: 1, cooling to 2 °C, stirring for 26 minutes, at 70 rotations/minute (rpm), adding aqueous sodium nitrite solution which is 1.25 times the amount of 5-nitro-pyridine-3, 4-diamine, the mass ratio of sodium nitrite and deionized water in sodium nitrite aqueous solution is 2: 3, reacting for 61 minutes, to obtain 5-nitro-pyridine-3, 4-diamine solution, mixing deionized water, 6-cyano-indole -3- carboxylate methyl ester and sodium hydroxide in mass ratio 5.5: 1: 1.5, stirring for 50 minutes, at 80 rpm, cooling to 3°C, adding methyl 6-cyanindole-3-carboxylate at rate 0.3ml/minute, the adding amount is 2 times that of 5-nitropyridine-3, 4-diamine solution, after reacting for 3 hours, adding 10 wt.% hydrochloric acid, until the solution pH is 6.5, filtering, washing the filter cake 3 times with deionized water, to obtain azo compounds; (2) mixing azo compound, 2, 2, 6, 6-tetramethyl piperidine alcohol and tetraisopropyl titanate in mass ratio 1: 2: 0.002, reacting for 8 hours at 153 °C, adding xylene the adding amount is 3 times that of azo compound, cooling to 55 °C, adding methanol, the adding amount is 4.5 times of azo compound, cooling to 2°C, filtering, drying at 80°C for 4 hours, to obtain light stable compound; (3) dissolving benzoin in absolute ethanol which is 6 times of benzoin, adding photostable compound which is 2.6 times of benzoin solution, the mass ratio of light-stable compound and dehydrated alcohol in light-stable compound solution, is 1:2.35, reacting for 6 hours, under 80rpm, distilling for 54 minutes, at 57°C, under vacuum 30 kilopacals (kPa), then adding petroleum ether which is 4 times of benzoin, cooling to 3°C, filtering and washing with distilled water, 4 times to obtain benzoin condensate; (4) dissolving europium oxide in 38 wt.% concentrated hydrochloric acid which is 16.5 times of europium oxide, heating to 39°C, heat preserving for 64 minutes, to form europium chloride solution, in water bath at 55°C adding benzoin condensate dissolved in ethanol, adding amount is 5.5 times of anhydrous ethanol, stirring and adding europium chloride solution which is 2 times of benzoin condensate, adding 10 wt.% sodium hydroxide solution until pH of solution, stirring and reacting for 2.5 hours, at 150 rpm, adding 4,7-dihydroxy-1,10-phenanthroline which is 2 times of absolute ethanol, reacting for 2 hours, at 85°C, distilling for 2.7 hours, drying at 75℃, under vacuum degree 20 kPa, for 3.5 hours, to form self-made fluorescent powder; (5) mixing self-made fluorescent powder, polyethylene glycol and deionized water in mass ratio 1:0.1:15, stirring at 1300 rpm, for 25 minutes, ultrasonically treating for 16 minutes, under pressure 30 kilohertz (kHz), then adding acrylic resin which is 0.75 times of self-made fluorescent powder, stirring evenly, adding 10 wt.% hydrochloric acid solution until pH of solution is 3, raising the temperature to 65°C and stirring for 2.5 hours, at same speed, adding 20 wt.% sodium hydroxide solution until the solution pH is 6.5, washing 4 times with deionized water to obtain microcapsules; 6) mixing graphene oxide, triethylamine and N,N-dimethylformamide in mass ratio 1:4:46 and ultrasonically dispersing at 30 kHz, for 36 minutes, in an ice-water bath, adding 2 bromoisovaleryl bromide which is twice of graphene oxide, stirring at speed 250 rpm, for 18 hours, then adding 5-mercapto-4-p-chlorophenyl-4 hydrogen-3-hydroxyl-1,2,4-triazole which is 2 times that of graphene, stirring for 5.5 hours, at same speed, washing with N, N-dimethylformamide and deionized water, 4 times, then centrifuging at 6000 rpm, for 12 minutes, drying at 65℃ for 3 hours and grinding with 500 mesh sieve to obtain modified graphene; (7) mixing modified graphene, azobisisobutyronitrile and methanol in a mass ratio 1:0.006:58.5, adding modified graphene microcapsules which is 3 times that of modified graphene, placing in water bath at 55°C, reacting for 26 hours, adding 1-hydroxyl tetradecane which is 0.55 times that of modified graphene, stirring at room temperature, at speed 80 rpm for 6 hours, washing with methanol and deionized water 4 times, evaporating at 69°C and vacuum drying at 30kPa, distilling for 2 hours, to get the paint precursor, mixing the paint precursor, ethyl acetate and amino resin in a mass ratio 1:1.9:0.4, to obtain corrosion-resistant fluorescent paint.