Polyvinyl amine-co-acrylic acid dye, and preparation method and application thereof
A technology based on polyvinylamine and acrylic acid, which can be used in dyeing methods, azo dyes, organic dyes, etc., and can solve the problems of difficult preparation of carboxyl-containing polymer cross-linked dyes and high reaction conditions
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Embodiment 1
[0093] Add 7.0g of N-vinylformamide (NVF) and 3.0g of acrylic acid (AA) to a four-necked flask equipped with a thermometer, mechanical stirring and reflux condenser, and add 11.3g of DMF and 45.3g of ethyl acetate N 2 Warm up to 50-70°C under protection, then add 0.5-1.0g of dodecyl mercaptan (DDM) chain transfer agent and 0.5-1.0g of AIBN initiator, and polymerize for 2-10 hours. During the reaction, white precipitates gradually precipitate out. Cool to room temperature after completion, filter with suction, wash the filter cake three times with 50 mL of acetone, and dry in vacuum at 50°C. The infrared spectrum of the product obtained is as figure 1 Shown at 1711cm -1 Detect the characteristic peak of C=O in the carboxyl group, at 1673cm -1 The amide C=O absorption peak was detected at 3050cm -1 The absorption peak of the aldehyde group C-H was detected at , indicating that the copolymerization of N-vinyl formamide and acrylic acid occurred, and the corresponding non-hydr...
Embodiment 2～6
[0096] Preparation of 1#~4# and 13# color bodies:
[0097] Add 1.90g of cyanuric chloride (0.0103mol) and 20g of small ice cubes into a 250mL beaker, beat at 0-5°C for 30min until milky. Slowly add the aqueous solution (0.01mol, 85.6%) containing 4.0g H acid into the above-mentioned beating liquid, react at 0-5°C, and use 10% Na 2 CO 3 The solution adjusts the pH value of the reaction at 4 to 5, and detects the end point of the reaction with Ehrlich reagent;
[0098] Weigh 0.93g of aniline (0.01mol, 98%), add 20mL of water and 2.5mL of concentrated hydrochloric acid with a mass fraction of 37%, cool to 0-5°C, add 0.73g of sodium nitrite (0.0105mol), and the The solution should keep the Congo red reagent to be acidic, and the starch potassium iodide test paper to turn blue. After 30 minutes, use Ehrlich reagent to detect the end point of the reaction, and use sulfamic acid to destroy excess nitrous acid;
[0099] Add the above-mentioned diazonium salt dropwise to the conden...
Embodiment 7～15
[0102] Preparation of 5#~12# and 14# color bodies:
[0103] Add 1.90g of cyanuric chloride (0.0103mol) and 20g of small ice cubes into a 250mL beaker, beat at 0-5°C for 30min until milky. Slowly add the aqueous solution (0.01mol, 85.6%) containing 4.0g H acid into the above-mentioned beating liquid, react at 0-5°C, and use 10% Na 2 CO 3 The solution adjusts the pH value of the reaction at 4 to 5, detects the end point of the reaction with Ehrlich reagent, adds 0.93g of aniline (0.01mol, 98%) after the completion of the reaction, raises the temperature to 25 to 30°C, and uses 10% Na 2 CO 3 Solution control pH value is between 2~3, after reacting 3~4h, thin-layer chromatography (TLC) detects the end point of reaction (developing agent is n-butanol: isopropanol: ethyl acetate: water=2:4:1: 3, v / v, R f =0.63);
[0104] Weigh 0.93g of aniline (0.01mol, 98%), add 20mL of water and 2.5mL of concentrated hydrochloric acid with a mass fraction of 37%, cool to 0-5°C, add 0.73g of s...
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