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
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
- C09B67/00—Influencing 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
Landscapes
- 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)
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) |
-
1939
- 1939-01-19 CH CH210991D patent/CH210991A/en unknown
- 1939-01-19 CH CH209641D patent/CH209641A/en unknown
Also Published As
Publication number | Publication date |
---|---|
CH210991A (en) | 1940-08-15 |
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