CH209641A - Process for the preparation of a solid diazonium salt. - Google Patents

Process for the preparation of a solid diazonium salt.

Info

Publication number
CH209641A
CH209641A CH209641DA CH209641A CH 209641 A CH209641 A CH 209641A CH 209641D A CH209641D A CH 209641DA CH 209641 A CH209641 A CH 209641A
Authority
CH
Switzerland
Prior art keywords
diazonium
solid
diazonium salt
salt
preparation
Prior art date
Application number
Other languages
German (de)
Inventor
Aktiengesellsc Farbenindustrie
Original Assignee
Ig Farbenindustrie Ag
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 Ig Farbenindustrie Ag filed Critical Ig Farbenindustrie Ag
Publication of CH209641A publication Critical patent/CH209641A/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
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films

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

Description

  

  Verfahren zur Herstellung eines festen     Diazoniumsalzes.       Es wurde gefunden, -dass man aus Lösun  gen von     Diazoniumsalzen    durch     Behandeln     mit     Kobaltchlorür    oder     einem    andern Kobalt  salz in Gegenwart von Chlorionen Kobalt  chlorürdoppelsalze der betreffenden     Diazo-          niumverbindungen    in     fester    Form     gewinnen     kann. Die so erhaltenen festen     Diazonium-          salze    sind gut haltbar und besitzen eine gute  Löslichkeit.  



       Diazoniumdoppelsalze    mit     Kobaltchlorür     sind bisher nicht bekannt     .geworden.        Es    ist  auch durchaus überraschend,     dass        Diazonium-          verbindungen        mittels        Kobaltchlorür    aus  gefällt     werden,    zumal sich     feste        Diazonium-          doppelsalze    mit Hilfe der entsprechenden  Salze des dem Kobalt sehr     nahestehenden     Nickels nicht .gewinnen lassen.

   Die neuen       Kobaltchlorürdoppelsalze    lassen sich, mit den  gebräuchlichen     Verdünnungs-        bezw.-        Einstell-          mitteln,    gemischt, zu wertvollen, haltbaren       Diazosalzen    verarbeiten.  



       Gea        nstand        .des    vorliegenden Patentes     ist       ein Verfahren zur     Herstellung        eines        festen          Diazoniumsalzes,        welches    dadurch gekenn  zeichnet ist,     @dass    man aus     einer    mineral  sauren     Diazolösung    von     1-Amino-2-phenogy-          5-chlorbenzol    mit     Kobaltchlorür    das Kobalt  chlorürdoppelsalz der     Diazoniumverbindung     in fester Form abscheidet.

      <I>Beispiel:</I>    200     Gewiehtsteile        1-Amino-2-phenogy-5-          chlorbenzol    werden in 591,3     Gewichtsteile          Salzsäure    von 22,5     Gewichtsprozent    ein  getragen. Nach der     Chlorhydratbildung    wird  auf 0   C abgekühlt und mit 74     Gewichts-          teilen    Eis versetzt.

   Die     Diazotierung    erfolgt  durch     Zulauf    von 165     Gewichtsteilen    einer  40     gewichtsprozentigen        Natriumnitritlösung     bei<B>10-15'C.</B> Nach     Filtration    der     Diazo-          niumlösung    wird das     KobaItchlorürdoppel-          salz    durch Zulauf einer Lösung von 111,1       Gewichtsteilen        Kobaltchlorür        (CoC12    . 6     H20)     in 100     Gewichtsteiler <     Wasser gefällt.

   Zur      vollständigen     Abseheidung    des     Salzes    wer  den 130     Gewielitsteile        Kochsalz    zugesetzt.  Das erhaltene     Iiobaltchlorürdoppelsalz    wird  abgesaugt und getrocknet.  



  Es     stellt    ein grünes, kristallines Pulver  dar, das     geit    haltbar ist und eine gute Lös  lichkeit besitzt. Durch     Vermischen    mit  den gebräuchlichen     Färbereihilfsmitteln,    wie  wasserfreiem Natriumsulfat oder teilentwäs  sertem Aluminiumsulfat usw., kann es auf       handelsübliehe    Form eingestellt werden.



  Process for the preparation of a solid diazonium salt. It has been found that, from solutions of diazonium salts by treatment with cobalt chloride or another cobalt salt in the presence of chlorine ions, cobalt chlorine double salts of the diazonium compounds in question can be obtained in solid form. The solid diazonium salts obtained in this way have a good shelf life and good solubility.



       Diazonium double salts with cobalt chloride are not yet known. It is also quite surprising that diazonium compounds are precipitated by means of cobalt chloride, especially since solid diazonium double salts cannot be obtained with the aid of the corresponding salts of nickel, which is very close to cobalt.

   The new cobalt chloride double salts can be mixed with the usual thinners or adjusting agents and processed into valuable, durable diazo salts.



       The subject of the present patent is a process for the production of a solid diazonium salt, which is characterized by the fact that from a mineral acidic diazo solution of 1-amino-2-phenogy-5-chlorobenzene with cobalt chlorine the cobalt chlorine double salt of the diazonium compound is in solid form Form separates.

      <I> Example: </I> 200 parts by weight of 1-amino-2-phenogy-5-chlorobenzene are added to 591.3 parts by weight of 22.5 weight percent hydrochloric acid. After the chlorohydrate formation, the mixture is cooled to 0 C and mixed with 74 parts by weight of ice.

   The diazotization takes place by adding 165 parts by weight of a 40 weight percent sodium nitrite solution at <B> 10-15'C. </B> After the diazonium solution has been filtered, the cobalt chloride double salt is converted by adding a solution of 111.1 parts by weight of cobalt chloride (CoC12. 6 H20) precipitated in 100 parts by weight of water.

   To completely separate out the salt, 130 parts by weight of table salt are added. The iobalt chloride double salt obtained is filtered off with suction and dried.



  It is a green, crystalline powder that is stable and has good solubility. By mixing it with the usual dyeing auxiliaries, such as anhydrous sodium sulfate or partially dewatered aluminum sulfate, etc., it can be adjusted to the commercially available form.

 

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung eines festen Diazoniumsa.lzes, dadurch gekennzeichnet, da.ss man aus einer mineralsauren Diazolösung von 1-Amino-9--phenogy-5-ehlorbenzol mit Iioba.ltchlorür das hobaltchloriirdoppelsalz der Diazoniumverbinduug in fester Form ab scheidet. PATENT CLAIM: A process for the production of a solid diazonium salt, characterized in that a mineral acid diazo solution of 1-amino-9-phenogy-5-chlorobenzene with Iioba.ltchlorür separates the double salt of the diazonium compound in solid form. Das so erhaltene Diazoniumsalz stellt ein grünes, kristallines Pulver dar. das gut halt bar ist und eine ;ute Löslichkeit besitzt. Durch Vermischen \mit den gebräuchlichen Färbereihilfsmitteln, wie wasserfreiem Na triumsulfat oder teilentwässertem Alumi niumsulfat usw., kann es auf handelsübliche Form eingestellt werden. The diazonium salt obtained in this way is a green, crystalline powder which is easy to hold and has good solubility. By mixing it with the usual dyeing auxiliaries such as anhydrous sodium sulphate or partially dehydrated aluminum sulphate, etc., it can be adjusted to the commercially available form.
CH209641D 1938-02-01 1939-01-19 Process for the preparation of a solid diazonium salt. CH209641A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE209641X 1938-02-01
CH209641T 1939-01-19

Publications (1)

Publication Number Publication Date
CH209641A true CH209641A (en) 1940-04-30

Family

ID=25724743

Family Applications (2)

Application Number Title Priority Date Filing Date
CH210991D CH210991A (en) 1938-02-01 1939-01-19 Process for the preparation of a solid diazonium salt.
CH209641D CH209641A (en) 1938-02-01 1939-01-19 Process for the preparation of a solid diazonium salt.

Family Applications Before (1)

Application Number Title Priority Date Filing Date
CH210991D CH210991A (en) 1938-02-01 1939-01-19 Process for the preparation of a solid diazonium salt.

Country Status (1)

Country Link
CH (2) CH210991A (en)

Also Published As

Publication number Publication date
CH210991A (en) 1940-08-15

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