DE84951C - - Google Patents

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Publication number
DE84951C
DE84951C DENDAT84951D DE84951DA DE84951C DE 84951 C DE84951 C DE 84951C DE NDAT84951 D DENDAT84951 D DE NDAT84951D DE 84951D A DE84951D A DE 84951DA DE 84951 C DE84951 C DE 84951C
Authority
DE
Germany
Prior art keywords
acid
chalk
amidonaphthol
monosulfonic acid
monosulfonic
Prior art date
Legal status (The legal status 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 status listed.)
Active
Application number
DENDAT84951D
Other languages
German (de)
Publication of DE84951C publication Critical patent/DE84951C/de
Active legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C309/00Sulfonic acids; Halides, esters, or anhydrides thereof
    • C07C309/01Sulfonic acids
    • C07C309/28Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
    • C07C309/45Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton
    • C07C309/49Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton the carbon skeleton being further substituted by singly-bound oxygen atoms
    • C07C309/50Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton the carbon skeleton being further substituted by singly-bound oxygen atoms having at least one of the sulfo groups bound to a carbon atom of a six-membered aromatic ring being part of a condensed ring system

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Description

KAISERLICHESIMPERIAL

PATENTAMT.PATENT OFFICE.

In der Patentschrift Nr. 82900 ist ein Verfahren zur Darstellung der Cn1 a4-Amidonaphtolß4 - monosulfosäure beschrieben, welches darin besteht, dafs Ct1 a4-Amidonaphtol mit einer etwa 75proc. Schwefelsäure auf 130 bis i6o° erhitzt wird. Es hat sich gezeigt, dafs man dieselbe Säure als Nebenproduct bei der nach dem Verfahren des Patentes Nr. 77937 stattfindenden Reinigung des Rohproductes der Amidonaphtolmonosulfosäure des Patentes Nr. 62289 mittelst Kreide gewinnen kann. Da die neue Säure beim Kochen mit Kreide ein nahezu unlösliches Kalksalz bildet, während die O1 a4-Amidonaphtol-e!3-monosulfosäure hierbei in ein leicht lösliches Kalksalz übergeht, ist die Trennung der beiden Säuren und die Gewinnung der Ci1 a4-Amidonaphtol-ß4-monosulfosäure nach diesem Verfahren äufserst leicht ausführbar. Die Anwendung von Aetzkalk an Stelle des kohlensauren Kalks führt dabei nicht zu dem gewünschten Ziel, da Aetzkalk mit beiden Säuren leicht lösliche Salze bildet und die O1 ct4-Amidonaphtol-ß4-monosulfosä'ure überdies in der alkalischen Lösung durch Oxydation schnell zerstört wird.In the patent specification No. 82900 a process for the preparation of the Cn 1 a 4 -amidonaphtholß 4 -monosulfonic acid is described, which consists in the fact that Ct 1 a 4 -amidonaphtol with about 75 perc. Sulfuric acid is heated to 130 to 160 °. It has been shown that the same acid can be obtained as a by-product in the purification of the crude product of amidonaphthol monosulfonic acid of Patent No. 62289 by means of chalk by the process of Patent No. 77937. Since the new acid forms an almost insoluble lime salt when boiled with chalk, while the O 1 a 4 -Amidonaphtol-e! 3 -monosulfonic acid turns into a readily soluble lime salt, the separation of the two acids and the recovery of the Ci 1 a 4 -amidonaphthol-β 4 -monosulfonic acid can be carried out extremely easily by this process. The use of caustic lime instead of carbonate does not lead to the desired goal, since caustic lime forms easily soluble salts with both acids and the O 1 ct 4 -amidonaphthol-β 4 -monosulfonic acid moreover quickly destroys in the alkaline solution by oxidation will.

Beispiel für die^Trennung der beidenExample of the ^ separation of the two

Säuren.Acids.

Das nach dem Verfahren des Patentes Nr. 62289 aus 10 kg Ct1 Ct4-Amidonaphtolsulfat erhaltene Rohproduct der Monosulfosäure wird mit 200 1 Wasser aufgekocht und unter Kochen so lange mit Kreide versetzt, als noch Schäumen eintritt. Aus" dem vom Filtrat befreiten Rückstande wird die neue Säure durch Salzsäure abgeschieden. The crude product of monosulfonic acid obtained from 10 kg of Ct 1 Ct 4 amidonaphthol sulfate by the process of patent no. 62289 is boiled with 200 l of water and chalk is added while boiling until foaming occurs. The new acid is separated from the residue freed from the filtrate by means of hydrochloric acid.

Claims (1)

Pa tent-Anspruch:Patent claim: Verfahren zur Darstellung der Ct1 ^-Amidonaphtol i-monosulfosäure, darin bestehend, dafs man das nach dem Verfahren des Patentes Nr. 62289 entstehende Rohproduct nach dem im Patent Nr. 77937 geschützten Verfahren durch Kochen mit Kreide und Wasser neutralisirt und den hierbei erhaltenen Rückstand nach dem Entfernen der Mutterlauge mit Salzsäure übersättigt.Process for the preparation of Ct 1 ^ -amidonaphtol- β i - monosulfonic acid, consisting in neutralizing the crude product obtained by the process of patent no. 62289 by boiling with chalk and water according to the process protected in patent no residue obtained after removal of the mother liquor is supersaturated with hydrochloric acid.
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