Dye composition, dye, preparation method and raw material composition of dye thereof
A technology of dye composition and raw material composition, which is applied in the direction of azo dyes, organic dyes, monoazo dyes, etc., can solve the problems of insufficient lifting power, dyeing depth and fastness, and achieve bright color, good lifting performance, Good dyeing effect
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Embodiment 1
[0031] Embodiment 1: the preparation method of dye composition
[0032] After 9.16 grams (0.05mol) of 2,4-dinitroaniline and 8.41 grams (0.05mol) of 2-nitro-4-methoxyaniline are mixed, add in 15 grams of 70% sulfuric acid (0.11mol), then in Slowly add 40% sulfuric acid solution of nitrosylsulfuric acid dropwise at 15°C to 25°C to complete the diazotization reaction (detected by TLC), and 16% by mass of N-ethyl-3-cyano -A solution of 4-methyl-6-hydroxyl-2-pyridone (18.20 grams) (add 30.6 grams of 30% sodium hydroxide solution to dissolve), and a coupling reaction occurs at 0-10 ° C, and the end point of the reaction is controlled by the permeation circle method . After the reaction, the temperature of the reaction system was raised to 65°C-75°C for 2 hours, filtered, and the product was washed with water until the pH value of the eluate was 6-7 to obtain a bright orange powder dye composition with a yield of 94.2%. The content is greater than or equal to 98% by HPLC analysis,...
Embodiment 2
[0033] Embodiment 2: the preparation method of dye composition
[0034] After 11.72 grams (0.064mol) of 2,4-dinitroaniline and 6.05 grams (0.036mol) of 2-nitro-4-methoxyaniline are mixed, add in 11 grams of 98% sulfuric acid (0.11mol), then in Slowly add 45% nitrosyl sulfuric acid dropwise at 18~22°C, and after the diazotization reaction is completed by HPLC detection, it will be mixed with N-ethyl-3-cyano-4-methyl-6-hydroxyl with a mass fraction of 12%. - A solution of 2-pyridone (17.80 g) (dissolved in 95 g of 25% sodium carbonate solution) was subjected to a coupling reaction at -5 to 5° C., and the end point of the reaction was detected by the percolation ring method. After the reaction, the temperature of the reaction system was raised to 65°C-75°C for 2 hours, filtered, and the product was washed with water until the pH value of the eluate was 6-7 to obtain a bright orange powder dye composition with a yield of 94.8%. The content is greater than or equal to 98% by HPLC ...
Embodiment 3
[0035] Embodiment 3: the preparation method of dye composition
[0036]After 4.39 grams (0.024mol) of 2,4-dinitroaniline and 12.78 grams (0.076mol) of 2-nitro-4-methoxyaniline are mixed, add in 85 grams of 70% sulfuric acid (0.61mol), then in Slowly add 20% nitrosyl sulfuric acid dropwise at 28~32°C, and after the diazotization reaction is completed by HPLC detection, it will be mixed with N-ethyl-3-cyano-4-methyl-6-hydroxyl with a mass fraction of 16%. - A solution of 2-pyridone (20.50 g) (dissolved with 38.6 g of 50% potassium hydroxide solution) was subjected to a coupling reaction at 8-15° C., and the end point of the reaction was detected by the percolation ring method. After the reaction, the temperature of the reaction system was raised to 65°C-75°C for 2 hours, filtered, and the product was washed with water until the pH value of the eluate was 6-7 to obtain a bright orange powder dye composition with a yield of 95.3%. The content is greater than or equal to 98% by HP...
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