Diethylene sulfone type reactive salt-free liquid dye, preparation method and application
A double vinyl sulfone type, liquid dye technology, applied in the direction of reactive dyes, application, dyeing method, etc., can solve the problems of water solubility decline of dyes, unable to obtain vinyl sulfone type structure, etc., and achieve the effect of maintaining pH stability
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Embodiment 1
[0055]
[0056] Step 1: Preparation of vinylsulfone-based reactive sodium salt dye-free color paste
[0057] Add 1,500 parts of water and 366 parts of 4-vinylsulfonylaniline into reaction tank 1, stir evenly, add 608 parts of hydrochloric acid (30%), add 2,000 parts of ice, and cool down to 0°C. Add 400 parts of water to the reaction tank 2, add 141 parts of sodium nitrite, stir until the sodium nitrite is completely dissolved, add the sodium nitrite solution into the reaction tank 1, diazotization reaction for 2 hours, control the reaction temperature 0-5 °C, use starch-KI test paper to detect the presence of nitrous acid. After the reaction, excess nitrous acid was removed with urea. Add 341 parts of H acid monosodium salt into reaction tank 1, and act for 6 hours at 10-15°C and pH≤2. Add 1000 parts of ice into the reaction tank 1, lower the temperature to below 10°C, add sodium carbonate, control the pH to 5.5-6.0, and react for 1 hour. If no diazonium salt is detected...
Embodiment 2
[0082]
[0083] Step 1: Preparation of vinylsulfone-based reactive sodium salt dye-free color paste
[0084] Add 800 parts of water and 183 parts of 4-vinylsulfonylaniline to the reaction tank 1, stir evenly, add 304 parts of hydrochloric acid (30%), add 1000 parts of ice, and cool down to 0°C. Add 200 parts of water to the reaction tank 2, add 70.5 parts of sodium nitrite, stir until the sodium nitrite is completely dissolved, add the sodium nitrite solution into the reaction tank 1, and carry out the diazotization reaction for about 2 hours. Control the reaction temperature 0- At 5°C, use starch-KI test paper to detect the presence of nitrous acid. After the reaction, excess nitrous acid was removed with urea. Add 341 parts of H acid monosodium salt into reaction tank 1, and act for 6 hours at 10-15°C and pH≤2. Add 800 parts of water to reaction tank 3, add 213 parts of 2-methoxy-5-vinylsulfonylaniline, stir evenly, add 304 parts of hydrochloric acid (30%), add 1000 par...
Embodiment 3
[0094]
[0095] Step 1: Preparation of vinylsulfone-based reactive sodium salt dye-free color paste
[0096] Change 183 parts of 4-vinylsulfone anilines in step one in embodiment 2 into 267 parts of 2,5-diacetyl-4-vinylsulfone anilines, and change 213 parts of 2-methoxyl groups-5-vinylsulfone anilines into into 183 parts of 4-vinylsulfone aniline, salting out into 20% sodium chloride, and other conditions unchanged, 1519 parts of filter cakes were obtained, the dye content was 43.78%, the HPLC purity was 92.64%, and the yield was 79.69%; Color paste concentration C of UV intensity meter 2a 18.16%, HPLC purity M 2a 3800 parts of 96.36% (603nm) salt-free color paste, in which Ca 2+ Ion content 105ppm, Mg 2+ Ion 77ppm, Cl -1 Ion content 33ppm, SO 4 2- The ion content is 223ppm.
[0097] Step 2: Preparation of vinylsulfone-based active lithium salt dye salt-free color paste
[0098] In the above synthesis steps, NaOH, sodium nitrite and sodium carbonate are replaced by ...
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