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Process for the preparation of a new disazo dye.
CH257017A
Switzerland
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German - Inventor
Aktiengesellschaft Ciba
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Description
translated from German
Zusatzpatent zum Hauptpaten Nr. 229184. Verfahren zur Herstellung eines neuen Disazofarbstoffes. Es wurde gefunden, dass man einen neuen Disazofarbstoff erhält, wenn man tetrazo- tiertes 3,3'-Dioxy-4;4'-diaminodiphenyl in Ge genwart von anorganischen nicht reduzierend wirkenden Atzlaugen mit 2 Hol 2-Athylaini- no-5-oxynaphthaIin-7-.sulfonsKure vereinigt.
Als anorganische nicht reduzierend wir kende Ätzlaugen sind sowohl Ätzalkalien und Ammoniak als auch Lösungen bzw. Auf- sehlämmungen von Hydroxyden der Erd.- alkahmetalle zu verstehen.
Der neue Farbstoff stellt ein schwarzes. broncierendes Pulver dar, das sich in Wasser und in 10%iger Natronlauge mit violetter, in 10%iger Sololösung mit blauer und in konzentrierter Schwefelsäure mit blaugrüner Färbe löst. Er erzeugt auf Baumwolle im Ein- oder Zweibadverfahren mit Kupfersal zen nachbehandelt echte blaue Töne.
Beispiel: 21,6 Teile 3,3'-Dioxy-4,4'-diaminodiphe- nyl, in Form des Chlorhydrates:, werden in 100 Teilen Wasser und 12 Teilen konzen trierter Salzsäure verrührt und bei 5-8 C finit einer wässerigen Lösung von 18,8 Teilen Natriumnitrit tetrazotiert. Nach beendeter Reaktion kühlt man auf 3 C ab, neutralisiert durch Zugabe von 6,4 Teilen Soda und fil triert die ausgefallene Tetrazoverbindung ab.
Man trägt die ausgeschiedene Tetrazo- verbindung in eine auf 5 C abgekühlte Auf schlemmung von 56 Teilen 2-Äthylamino-5- oxynaphthalin-7-sulfonsäure und 29,6 Teilen Caleiumhydroxyd in 200 Teilen Wasser und 11,2 Volumteilen 50%iger Kalilauge- ein. Man kuppelt während 3 Stunden bei 5-8 C und beendet die Reaktion durch mehrstün diges Rühren, bei 10-20 C.
Hierauf ver dünnt man mit 1600 Teilen Wasser von 50 C, setzt 60 Teile Soda zu und filtriert vom Cal- ciumcarbonat ab. Das Filtrat wird mit 140 Teilen 10 % iger Salzsäure versetzt und der Farbstoff durch Aussalzen gewonnen.
Additional patent to main patent no. 229184. Process for the production of a new disazo dye. It has been found that a new disazo dye is obtained if tetrazo- tated 3,3'-dioxy-4; 4'-diaminodiphenyl in the presence of inorganic non-reducing caustic liquors with 2 hol of 2-ethylainino-5-oxynaphthaIin -7-.sulfonsKure united.
Inorganic, non-reducing caustic solutions are both caustic alkalis and ammonia as well as solutions or slurry insulations of hydroxides of the alkaline earth metals.
The new dye represents a black one. bronzing powder that dissolves in water and in 10% sodium hydroxide solution with violet, in 10% solo solution with blue and in concentrated sulfuric acid with blue-green color. It produces real blue tones on cotton in a one or two bath process, post-treated with copper salts.
Example: 21.6 parts of 3,3'-dioxy-4,4'-diaminodiphenyl, in the form of the chlorohydrate: are stirred into 100 parts of water and 12 parts of concentrated hydrochloric acid and an aqueous solution at 5-8 ° C. is finite tetrazotized by 18.8 parts of sodium nitrite. When the reaction has ended, the mixture is cooled to 3 ° C., neutralized by adding 6.4 parts of soda and the precipitated tetrazo compound is filtered off.
The precipitated tetrazo compound is added to a suspension, cooled to 5 ° C., of 56 parts of 2-ethylamino-5-oxynaphthalene-7-sulfonic acid and 29.6 parts of potassium hydroxide in 200 parts of water and 11.2 parts by volume of 50% strength potassium hydroxide solution . The coupling is carried out for 3 hours at 5-8 ° C. and the reaction is ended by stirring for several hours at 10-20 ° C.
It is then diluted with 1600 parts of water at 50 ° C., 60 parts of soda are added and the calcium carbonate is filtered off. 140 parts of 10% hydrochloric acid are added to the filtrate and the dye is obtained by salting out.