CH183878A - Process for the preparation of a complexed metal-containing dye. - Google Patents

Process for the preparation of a complexed metal-containing dye.

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Publication number
CH183878A
CH183878A CH183878DA CH183878A CH 183878 A CH183878 A CH 183878A CH 183878D A CH183878D A CH 183878DA CH 183878 A CH183878 A CH 183878A
Authority
CH
Switzerland
Prior art keywords
mole
parts
nitro
phenol
diazotized
Prior art date
Application number
Other languages
German (de)
Inventor
Gesellschaft Fuer Chemis Basel
Original Assignee
Chem Ind Basel
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chem Ind Basel filed Critical Chem Ind Basel
Publication of CH183878A publication Critical patent/CH183878A/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B45/00Complex metal compounds of azo dyes
    • C09B45/02Preparation from dyes containing in o-position a hydroxy group and in o'-position hydroxy, alkoxy, carboxyl, amino or keto groups
    • C09B45/24Disazo or polyazo compounds
    • C09B45/32Disazo or polyazo compounds containing other metals
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B33/00Disazo and polyazo dyes of the types A->K<-B, A->B->K<-C, or the like, prepared by diazotising and coupling
    • C09B33/02Disazo dyes
    • C09B33/06Disazo dyes in which the coupling component is a diamine or polyamine

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Coloring (AREA)

Description

  

      Zusatzpatent    zum Hauptpatent     Nr.182047.       Verfahren zur Herstellung eines komplex gebundenes  Metall enthaltenden     Farbstoffes.       Es wurde gefunden, dass man einen kom  plex gebundenes Metall enthaltenden Farb  stoff herstellen kann, wenn man 1     Mol        diazo-          tiertes        4-Nitro-2-amino-l-phenol,    1     Mol        diazo-          tierte        4-Nitro-2-amino-l-phenol-6-sulfonsäure,

       1     Mol        1.3-Diaminobenzol    und ein Eisen ab  gebendes Mittel aufeinander einwirken lässt.  



  Der erhaltene Farbstoff stellt ein oliv  schwarzes Pulver dar, das sich in Wasser  leicht mit     grünstichig    dunkelbrauner Farbe  löst und chromgegerbtes Leder aus neutralem  Bade in dunklen     olivbraunen    echten Tönen  färbt.  



  <I>Beispiel:</I>  15,4 Teile     4-Nitro-2-amino-l-phenol    wer  den in 40 Teilen Wasser und 20,7 Teilen  30     %iger    Salzsäure gelöst; die Lösung wird  durch Beigabe von Eis abgekühlt und bei  5 bis 10 0 mit 6,9 Teilen     Natriumnitrit        diazo-          tiert.    Die     Diazoverbindung    neutralisiert man  hierauf mit 40     Volumteilen    10,6     0%iger    Soda-         lösung    und gibt sie zu einer mit Eis auf 5 0       gekühlten        und        mit        13,

  3        Teilen        30%iger     Natronlauge versetzten Lösung von 10,9 Tei  len     1.3-Diaminobenzol    in 100 Teilen Wässer.  Man rührt bis zum     Verschwinden    der     Diazo-          reaktion    bei 5 bis 10 0, was etwa 1 Stunde       dauert,        fügt        weitere        13,

  3        Teile        30        %ige        Na-          tronlauge    hinzu und hierauf die in üblicher  Weise hergestellte und mit     Sodalösung    neu  tralisierte     Diazolösung    aus 23,4 Teilen     4-          Nitro-2-amino-l-phenol-6-sulfonsäure.    Man  rührt bei 12 bis 18 0 während 12 bis 15 Stun  den. Nach dieser Zeit ist die Kupplung be  endet.

   Nun erwärmt man das     Reaktions-          gemisch        auf        auf        601,        fügt        11,5        Teile        30        %-          ige    Salzsäure hinzu, kocht auf, versetzt mit  24,3 Teilen     Ferrichlorid    in Form einer etwa  32 0%igen wässerigen Lösung und kocht 1  Stunde unter     Rückflusskühlung.    Hierauf  scheidet man den Farbstoff mit 100 Teilen  Kochsalz ab, filtriert und trocknet bei mässi  ger Temperatur.



      Additional patent to main patent number 182047. Process for the preparation of a complexed metal-containing dye. It has been found that a dye containing complex bonded metal can be produced if 1 mole of diazotized 4-nitro-2-amino-1-phenol, 1 mole of diazotized 4-nitro-2-amino-1 -phenol-6-sulfonic acid,

       1 mole of 1,3-diaminobenzene and an iron releasing agent can act on each other.



  The dye obtained is an olive black powder which dissolves easily in water with a greenish dark brown color and dyes chrome-tanned leather from a neutral bath in dark olive brown real shades.



  <I> Example: </I> 15.4 parts of 4-nitro-2-amino-l-phenol are dissolved in 40 parts of water and 20.7 parts of 30% strength hydrochloric acid; the solution is cooled by adding ice and diazotized at 5 to 10 0 with 6.9 parts of sodium nitrite. The diazo compound is then neutralized with 40 parts by volume of 10.6% strength soda solution and added to a cooled with ice to 50 and with 13,

  3 parts of 30% sodium hydroxide solution of 10.9 parts of 1,3-diaminobenzene in 100 parts of water. The mixture is stirred until the diazo reaction disappears at 5 to 10 0, which takes about 1 hour, then another 13,

  3 parts of 30% strength sodium hydroxide solution are added and then the diazo solution of 23.4 parts of 4-nitro-2-amino-1-phenol-6-sulfonic acid prepared in the customary manner and neutralized with soda solution. The mixture is stirred at 12 to 180 for 12 to 15 hours. After this time, the coupling ends.

   The reaction mixture is now heated to 601, 11.5 parts of 30% strength hydrochloric acid are added, the mixture is boiled, 24.3 parts of ferric chloride in the form of an approximately 320% strength aqueous solution are added and the mixture is refluxed for 1 hour. The dye is then separated off with 100 parts of sodium chloride, filtered and dried at a moderate temperature.

 

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung eines komplex gebundenes Metall enthaltenden Farbstoffes, dadurch gekennzeichnet; dass man 1 Mol diazotiertes 4-Nitro-2-amino-l-phenol, 1 Mol diazotierte 4-Nitro-2-ainino-l-phenol-6-sulfon- säure, 1 Mol 1.3-Diaminobenzol und ein Eisen abgebendes Mittel aufeinander einwir ken lässt. PATENT CLAIM: Process for the production of a complexed metal-containing dye, characterized in that; that 1 mole of diazotized 4-nitro-2-amino-1-phenol, 1 mole of diazotized 4-nitro-2-ainino-1-phenol-6-sulfonic acid, 1 mole of 1,3-diaminobenzene and an iron releasing agent are added to one another ken. Der erhaltene Farbstoff stellt ein oliv schwarzes Pulver dar, das sich in Wasser leicht mit grünstichig dunkelbrauner Farbe löst und chromgegerbtes Leder aus neutralem Bade in dunklen olivbraunen echten Tönen färbt. The dye obtained is an olive black powder which dissolves easily in water with a greenish dark brown color and dyes chrome-tanned leather from a neutral bath in dark olive brown real shades.
CH183878D 1935-01-24 1935-01-24 Process for the preparation of a complexed metal-containing dye. CH183878A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH183878T 1935-01-24
CH182047T 1935-01-24

Publications (1)

Publication Number Publication Date
CH183878A true CH183878A (en) 1936-04-30

Family

ID=25720647

Family Applications (1)

Application Number Title Priority Date Filing Date
CH183878D CH183878A (en) 1935-01-24 1935-01-24 Process for the preparation of a complexed metal-containing dye.

Country Status (1)

Country Link
CH (1) CH183878A (en)

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