CH287090A - Process for the preparation of a chromium-containing azo dye. - Google Patents
Process for the preparation of a chromium-containing azo dye.Info
- Publication number
- CH287090A CH287090A CH287090DA CH287090A CH 287090 A CH287090 A CH 287090A CH 287090D A CH287090D A CH 287090DA CH 287090 A CH287090 A CH 287090A
- Authority
- CH
- Switzerland
- Prior art keywords
- chromium
- dye
- acid
- containing azo
- azo dye
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B45/00—Complex metal compounds of azo dyes
- C09B45/02—Preparation from dyes containing in o-position a hydroxy group and in o'-position hydroxy, alkoxy, carboxyl, amino or keto groups
- C09B45/14—Monoazo compounds
- C09B45/16—Monoazo compounds containing chromium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
- Paper (AREA)
- Coloring (AREA)
Description
<B>Zusatzpatent</B> zum Hauptpatent Nr. 284075. Verfahren zur Herstellung eines chromhaltigen Azofarbstoffes. Es wurde gefunden, dass man zu einem wertvollen, neuen chromhaltigen Azofarbstoff gelangt, wenn man auf den Monoazofarbstoff der Formel
EMI0001.0004
chromabgebende Mittel derart einwirken lässt, dass ein chromhaltiger Azofarbstoff entsteht, der zwei hlonoazofarbstoffmoleküle an ein Chromatom komplex gebunden enthält.
Der neue chromhaltige Farbstoff bildet ein graublaues Pulver, das sich in Wasser mit blauer, in konzentrierter Schwefelsäure mit roter Farbe löst und Wolle aus neutralem oder essigsaurem Bade in graublauen Tönen färbt.
Cber die verwendeten chromabgebenden Mittel sowie über die Reaktionsbedingungen gibt das Hauptpatent Auskunft.
<I>Beispiel:</I> 21,8 Teile 2-Ainino-1.-oxybenzol-4-sulfon- säure-N-dimetlly lamid werden in 200 Teilen Wasser und 15 Voluinteilen 10-n-Salzsäure aufgeschlämmt und bei 5 bis 10 mit 25 Vo- lumteilen 4-n-Natriumnitritlösung diazotiert. Die durch Zugabe von Natriumcarbonat neu tralisierte Diazoverbindung lässt man einlau fen in eine mit Eis auf 0 abgekühlte Lösung von 20,
5 Teilen 1.-Acetylamino-7-oxynaphtha- lin in 52 Volumteilen 2-n-Natriumhydroxyd- lösung und 50 Volumteilen 2-n-Natriumcarbo- natlösung. Nach beendeter Kupplung wird der abgeschiedene Farbstoff filtriert und mit ver dünnter Natriumchloridlösung gewaschen. Ge trocknet stellt er ein schwarzes Pulver dar, (las sich in heissem Wasser mit violetter und in konzentrierter Schwefelsäure mit roter Farbe löst.
Der nach obigen Angaben erhaltene Filter kuchen des Farbstoffes wird in 1500 Teilen Wasser aufgeschlämmt und mit 200 Teilen einer Lösung von chromsalicylsaiirem Kalium- Natrium mit einem Chromgehalt von 1,85% versetzt.
Die Lösung von chromsalicylsauren i Kalium-Natrium erhält man zum Beispiel durch Aufkochen von 100 Teilen einer Chrom sulfatlösung (Cr-SO.i0I1) mit einem Chrom- gehalt von 3,7% mit 19,6 Teilen Salicylsäure,
Lösen des entstandenen Niederschlages durch Zugabe von 15 Volumteilen 10-n-Natrium- hydroxy dlösung und 15 Volumteilen 10-n-Ka- liumhydroxydlösung und Einstellenmit Was ser auf 200 Teile. Das Chromiergemisch wird während etwa 5 Stunden bei Siedetemperatur gehalten und die so erhaltene Chromverbin dung des Farbstoffes durch Natriumchlorid- zugabe abgeschieden und abfiltriert.
<B> Additional patent </B> to main patent no. 284075. Process for the production of a chromium-containing azo dye. It has been found that a valuable, new chromium-containing azo dye is obtained by using the monoazo dye of the formula
EMI0001.0004
lets chromium-donating agents act in such a way that a chromium-containing azo dye is formed which contains two hlonoazo dye molecules bound to a chromium atom in a complex.
The new chromium-containing dye forms a gray-blue powder that dissolves in water with blue, in concentrated sulfuric acid with red color and colors wool from neutral or acetic acid baths in gray-blue tones.
The main patent provides information on the chromium-releasing agents used and the reaction conditions.
<I> Example: </I> 21.8 parts of 2-amino-1.-oxybenzene-4-sulfonic acid-N-dimetlly lamide are suspended in 200 parts of water and 15 parts by volume of 10N hydrochloric acid and at 5 to 10 diazotized with 25 parts by volume of 4N sodium nitrite solution. The diazo compound neutralized by adding sodium carbonate is allowed to run into a solution of 20, which has been cooled to 0 with ice.
5 parts of 1.-acetylamino-7-oxynaphthalene in 52 parts by volume of 2-n sodium hydroxide solution and 50 parts by volume of 2-n sodium carbonate solution. After the coupling has ended, the deposited dye is filtered and washed with dilute sodium chloride solution. When dried it is a black powder (it dissolves in hot water with violet color and in concentrated sulfuric acid with red color.
The filter cake of the dye obtained according to the above information is slurried in 1500 parts of water and treated with 200 parts of a solution of chromsalicylsaiirem potassium-sodium with a chromium content of 1.85%.
The solution of chromium salicylic acid and potassium sodium is obtained, for example, by boiling 100 parts of a chromium sulfate solution (Cr-SO.i0I1) with a chromium content of 3.7% with 19.6 parts of salicylic acid,
Dissolve the resulting precipitate by adding 15 parts by volume of 10-n-sodium hydroxide solution and 15 parts by volume of 10-n-potassium hydroxide solution and adjusting with water to 200 parts. The chromating mixture is kept at the boiling point for about 5 hours and the chromium compound of the dye thus obtained is deposited by adding sodium chloride and is filtered off.
Claims (1)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CH284075T | 1949-11-18 | ||
CH287090T | 1949-11-18 |
Publications (1)
Publication Number | Publication Date |
---|---|
CH287090A true CH287090A (en) | 1952-11-15 |
Family
ID=25732339
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CH287090D CH287090A (en) | 1949-11-18 | 1949-11-18 | Process for the preparation of a chromium-containing azo dye. |
Country Status (1)
Country | Link |
---|---|
CH (1) | CH287090A (en) |
-
1949
- 1949-11-18 CH CH287090D patent/CH287090A/en unknown
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