CH201516A - Process for the preparation of a solid diazonium salt. - Google Patents

Process for the preparation of a solid diazonium salt.

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Publication number
CH201516A
CH201516A CH201516DA CH201516A CH 201516 A CH201516 A CH 201516A CH 201516D A CH201516D A CH 201516DA CH 201516 A CH201516 A CH 201516A
Authority
CH
Switzerland
Prior art keywords
diazonium salt
solid
preparation
methylsulfuric acid
weight
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 CH201516A publication Critical patent/CH201516A/en

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

  

  Verfahren zur Herstellung eines festen     Diazoniumsalzes.       Gegenstand des vorliegenden Zusatz  patentes ist ein Verfahren zur Herstellung  eines festen     Diazoniumsalzes,    welches da  durch     gekennzeichnet    ist,

       dass    man aus einer       mineralsauren        Diazolösung    von     1-Amino-2-          phenoxy-5-chlorbenzol    nach Zusatz von     me-          thylschwefelsaurem    Natrium das     methyl-          schwefelsaure        Diazoniumsalz    in fester     Form     abscheidet.  



  <I>Beispiel:</I>  100 Gewichtsteile     1-Amino-2-phenoxy-5-          chlorbenzol    werden bei 25 bis 30   C     portions-          weise    in 151,9 Gewichtsteile 40%ige     Nitro-          sylschwefelsäure        eingetragen.    Nach beende  tem     Eintragen    wird so lange bei dieser Tem  peratur gerührt, bis     eine    Probe in Wasser  klar löslich ist. Die     Diazotierung    wird nun in  500 Gewichtsteile Wasser und 200 Gewichts  teile     Eis    gegossen und die     Diazolösung    fil  triert.

   Das Filtrat wird dann mit 154,6 Ge  wichtsteilen einer 41,5 gewichtsprozentigen  Lösung von     methylschwefelsaurem    Natrium    versetzt und die alsbald     beginnende        Abschei-          dung    durch Zusatz von 80 Gewichtsteilen  Glaubersalz vervollständigt. Das     methyl-          schwefelsaure        Diazoniumsalz    wird bei niedri  ger     Temperatur    getrocknet.  



  Das erhaltene     Diazoniumsalz    stellt ein       gelblichweisses        kristallines    Pulver dar. Es  besitzt eine gute Haltbarkeit und ist leicht  löslich. Durch Vermischen     mit    den gebräuch  lichen     Färbereihilfsmitteln,    wie wasserfreiem       Natriumsulfat    oder teilentwässertem     Alu-          miniumsulfat    usw., kann es auf handels  übliche Form eingestellt werden.



  Process for the preparation of a solid diazonium salt. The subject of the present additional patent is a process for the production of a solid diazonium salt, which is characterized by

       that one separates the methylsulfuric acid diazonium salt in solid form from a mineral acid diazo solution of 1-amino-2-phenoxy-5-chlorobenzene after addition of methylsulfuric acid.



  <I> Example: </I> 100 parts by weight of 1-amino-2-phenoxy-5-chlorobenzene are introduced in portions at 25 to 30 ° C. into 151.9 parts by weight of 40% strength nitrosylsulfuric acid. After the end of the entry system, the mixture is stirred at this temperature until a sample is clearly soluble in water. The diazotization is then poured into 500 parts by weight of water and 200 parts by weight of ice and the diazo solution is fil trated.

   154.6 parts by weight of a 41.5 percent by weight solution of sodium methylsulfuric acid are then added to the filtrate, and the separation which soon begins is completed by adding 80 parts by weight of Glauber's salt. The methyl sulfuric acid diazonium salt is dried at a lower temperature.



  The diazonium salt obtained is a yellowish-white crystalline powder. It has a good shelf life and is easily soluble. 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.

 

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung eines festen Diazoniumsalzes, welches dadurch gekenn zeichnet ist, dass man aus einer mineralsauren Diazolösung von 1-Amino-2-phenoxy-5-chlor- benzol nach Zusatz von methylschwefel- saurem Natrium das methylschwefelsauie Di- azoniumsalz in fester Form abscheidet. PATENT CLAIM: Process for the production of a solid diazonium salt, which is characterized in that the methylsulfuric acid diazonium salt is obtained in solid form from a mineral acid diazo solution of 1-amino-2-phenoxy-5-chlorobenzene after addition of methylsulfuric acid separates. Das so erhaltene Diazoniumsalz stellt ein gelblichweisses kristallines Pulver dar. Es be sitzt eine gute Haltbarkeit und ist leicht lös lich. Durch Vermischen mit den gebräuch lichen Färbereihilfsmitteln, wie wasserfreiem Natriumsulfat oder teilentwässertem Alu miniumsulfat usw., kann es auf handels übliche Form eingestellt werden. ÜNTERANSPRüCU Verfahren nach Patentanspruch, dadurch gekennzeichnet, dass man die Abscheidung des Diazoniumsalzes durch Aussalzen vervoll ständigt. The diazonium salt obtained in this way is a yellowish-white crystalline powder. It has a good shelf life and is easily soluble. By mixing it with the usual dyeing auxiliaries, such as anhydrous sodium sulfate or partially dehydrated aluminum sulfate, etc., it can be adjusted to the standard form. UNDERCLAIMS Process according to patent claim, characterized in that the deposition of the diazonium salt is completed by salting out.
CH201516D 1936-03-10 1937-03-08 Process for the preparation of a solid diazonium salt. CH201516A (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE201516X 1936-03-10
DE201517X 1936-03-10
DE201514X 1936-03-10
CH199458T 1937-03-08

Publications (1)

Publication Number Publication Date
CH201516A true CH201516A (en) 1938-11-30

Family

ID=27429710

Family Applications (3)

Application Number Title Priority Date Filing Date
CH201517D CH201517A (en) 1936-03-10 1937-03-08 Process for the preparation of a solid diazonium salt.
CH201516D CH201516A (en) 1936-03-10 1937-03-08 Process for the preparation of a solid diazonium salt.
CH201514D CH201514A (en) 1936-03-10 1937-03-08 Process for the preparation of a solid diazonium salt.

Family Applications Before (1)

Application Number Title Priority Date Filing Date
CH201517D CH201517A (en) 1936-03-10 1937-03-08 Process for the preparation of a solid diazonium salt.

Family Applications After (1)

Application Number Title Priority Date Filing Date
CH201514D CH201514A (en) 1936-03-10 1937-03-08 Process for the preparation of a solid diazonium salt.

Country Status (1)

Country Link
CH (3) CH201517A (en)

Also Published As

Publication number Publication date
CH201517A (en) 1938-11-30
CH201514A (en) 1938-11-30

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