Fiber-reactive azo dyes, their preparation and use
An azo dye, -CH2CH2Z technology, applied in the direction of reactive dyes, azo dyes, organic dyes, etc.
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Embodiment 1
[0090] a) 19 parts of cyanuric chloride are suspended in 200 parts of water and 100 parts of ice in the presence of a wetting agent. Then 32 parts of 2-amino-5-hydroxy-naphthalene-1,7-disulfonic acid were added, followed by stirring at 5°C to 10°C for 3-4 hours until the reaction was complete. During the reaction, the pH was maintained at 1.5 with 20% sodium hydroxide solution.
[0091] b) 35 parts of 4-aminoazobenzene-3,4'-disulfonic acid are first added to 300 parts of water at 15°C. After adding 23 parts by volume of 31% hydrochloric acid, 20.5 parts by volume of 5N sodium nitrite solution were used for a rapid diazotization reaction. After the reaction, excess nitrite was removed.
[0092] c) The diazo compound prepared in step b) is added to the reaction mixture obtained in step a), and the pH is maintained between 4.5 and 5 with 15% sodium carbonate solution.
[0093] d) The reaction mixture prepared in step c) was added in batches to 31 parts of the compound of formu...
Embodiment 2
[0098] a) Similarly, the reaction mixture obtained according to step a) of Example 1 was added in batches to 28 parts of the compound of formula (4a), while maintaining the pH at 4 to 4.5 with 15% sodium carbonate solution. The temperature was raised to 30°C. The mixture was stirred until the reaction was complete.
[0099] b) The diazo compound prepared according to step 1 b) is added to the compound prepared according to step a). During this time the pH was maintained between 4.5 and 5 with 15% sodium carbonate solution. After the coupling reaction, the pH was raised to 5.5.
[0100] The dyestuff of formula (Ia) according to the invention is isolated by sodium chloride salting-out method.
Embodiment 3
[0102] a) 34.4 parts of a compound of formula (8a) (in free acid form) are initially added to 400 parts of water at a pH of 2.8 to 3.2. Then, a suspension obtained by dispersing 43 parts of the compound of formula (9a) (written in free acid form and known from EP568876) in 400 parts of water, adjusted to pH 4-4.5, is added in portions. During the reaction, the pH was adjusted to 2.8 to 3.2 and maintained with 15% sodium carbonate solution. The temperature was increased to 30°C. The mixture was stirred until the reaction was complete.
[0103]
[0104] The dyestuff (λ max =510nm) (in the form of free acid) was isolated by sodium chloride salting-out method.
[0105]
PUM
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