Middle-temperature type disperse dye compound and preparation method and application thereof
A technology of disperse dyes and compounds, applied in chemical instruments and methods, dyeing methods, azo dyes, etc., can solve the problem of few varieties of medium-temperature disperse dyes
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Embodiment 1
[0070] (1) Add 78.8ml of water, 20.3g of aniline, 14.4g of acrylonitrile, 0.3g of hydroquinone and 0.75g of 30% hydrochloric acid into the autoclave. After the addition, close the equipment, start magnetic stirring, and evenly heat up to 100°C , and keep the temperature at 100°C for 20-22 hours, the pressure is 0.25MPa, keep the temperature down to 45-50°C for half an hour, then slowly cool down to below 28°C, filter, recover the mother liquor water, and wash the filter cake with water, After drying, 30 g of intermediate B cyanoethylaniline was obtained.
[0071] Add 22.3ml of water, 21.7g of cyanoethylaniline, 5.6g of magnesium hydroxide, 0.15g of hydroquinone and 12.5g of chloropropene into the autoclave. After the addition, close the equipment, start magnetic stirring, and evenly heat up to 100°C for 12h , the pressure is 0.3MPa, then slowly lower the temperature to below 20°C, filter, wash the filter cake with water and dry to obtain 26g of intermediate A-a, the structural...
Embodiment 2
[0077] (1) Add 110ml of water, 27g of aniline, 17g of acrylonitrile, 0.55g of hydroquinone and 1.3g of 30% hydrochloric acid into the autoclave. After the addition, close the equipment, start magnetic stirring, uniformly heat up to 100°C, and keep The temperature is kept at 100°C for 22 hours, the pressure is 0.25MPa, the temperature is lowered to 45-50°C for half an hour, and then slowly lowered to below 28°C, filtered, and the mother liquor is recovered. The filter cake was washed with water and dried to obtain 40 g of intermediate B cyanoethylaniline.
[0078] Add 63.5g of methyl chloroacetate, 21.7g of cyanoethylaniline, and 13.7g of sodium bicarbonate to the three-necked flask, start stirring, uniformly heat up to 120°C and keep for 12h, then slowly cool down to below 20°C, filter, and the filter cake is washed with water, After drying, 30.7 g of intermediate A-c was obtained, and the structural formula of intermediate A-c was (A-c).
[0079] (A-c)
[0080] (2)...
Embodiment 3
[0083] (1) Add 52.5ml of water, 17.3g of aniline, 11g of acrylonitrile, 0.3g of hydroquinone and 0.8g of 30% hydrochloric acid into the autoclave. After the addition, close the equipment, start magnetic stirring, and evenly heat up to 100°C. And keep the temperature at 100°C for 20-22 hours, the pressure is 0.25MPa, keep the temperature down to 45-50°C for half an hour, then slowly cool down to below 28°C, filter, recover the mother liquor, and wash the filter cake with water and dry Afterwards, 25 g of the intermediate B cyanoethylaniline was obtained.
[0084] Add 30ml of water, 21.7g of cyanoethylaniline, 3.5g of magnesium oxide, 0.15g of hydroquinone, and 15g of propylene chloride into the autoclave. After the addition is complete, seal the equipment, start magnetic stirring, and uniformly heat up to 100°C for 12 hours. The pressure is 0.3MPa, then slowly lower the temperature to below 20°C, filter, wash the filter cake with water, and dry to obtain 26g of intermediate A-a...
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