DE475270C - Process for the purification of the calcium salts of the sulfonic acids obtained by direct sulfonation of cresols - Google Patents

Process for the purification of the calcium salts of the sulfonic acids obtained by direct sulfonation of cresols

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Publication number
DE475270C
DE475270C DEF52216D DEF0052216D DE475270C DE 475270 C DE475270 C DE 475270C DE F52216 D DEF52216 D DE F52216D DE F0052216 D DEF0052216 D DE F0052216D DE 475270 C DE475270 C DE 475270C
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DE
Germany
Prior art keywords
cresols
sulfonic acids
calcium salts
purification
acids obtained
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.)
Expired
Application number
DEF52216D
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German (de)
Inventor
Dr Siegfried Jaeger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
IG Farbenindustrie AG
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IG Farbenindustrie AG
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Filing date
Publication date
Application filed by IG Farbenindustrie AG filed Critical IG Farbenindustrie AG
Priority to DEF52216D priority Critical patent/DE475270C/en
Application granted granted Critical
Publication of DE475270C publication Critical patent/DE475270C/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/42Separation; Purification; Stabilisation; Use of additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Description

Verfahren zur Reinigung der Calciumsalze^.der durch unmittelbare Sulfonierung von Kresolen gewonnenen Sulfosäuren Die Alkali- und Erdalkalisalze von Alkoxysubstitutionsprodukten der Phenolsulfosäuren, wie der Kreosot- und Guajacolsulfosäuren, finden bei Erkrankungen der Atmungsorgane und der Lunge therapeutische Anwendung.Process for the purification of calcium salts by direct sulfonation Sulphonic Acids Obtained from Cresols The alkali and alkaline earth salts of alkoxy substitution products the phenol sulfonic acids, such as creosote and guaiacol sulfonic acids, are found in diseases the respiratory organs and the lungs therapeutic application.

Wie überraschenderweise gefunden wurde, haben Calciumsalze von Sulfosäuren der Kresole eine besonders günstige Wirkung in dieser Richtung. Entgegen der bisherigen Ansicht ist nämlich die dem Kreosot eigentümliche therapeutische Wirkung in der Hauptsache den in ihm in überwiegender Menge enthaltenen Kresolen zuzuschreiben. Für die therapeutische Anwendung der Calciumsalze der !<resolsulfosäuren ist es aber erforderlich und wichtig, daß sie frei von jeder Spur von Kresolen und frei von jedem Geruch sind.As has been surprisingly found, calcium salts of sulfonic acids have the cresols have a particularly beneficial effect in this direction. Contrary to the previous one The view is namely the therapeutic effect peculiar to creosote in the Mainly to be ascribed to the cresols contained in it in predominant quantities. For the therapeutic application of the calcium salts of the resolsulfonic acids But it is necessary and important that they are free of any trace of cresols and free of any smell are.

Es wurde nun die Beobachtung gemacht, daß man dieses Ziel am einfachsten und billigsten durch Ausblasen von wäßrigen Lösungen der Calciumsalze der durch unmittelbare Sulfonierung von Kresolen- erhältlichen Sulfosäuren mit Wasserdampf erreichen kann. Die Wasserdampfdestillation dient nicht nur zur Entfernung aller flüchtigen Bestandteile, sondern auch zur Spaltung der sich bei der Sulfonierung und nachfolgenden Absättigung der Sulfosäuren mit Calciumhydroxyd oder -carbonat stets bildenden Kresolate. Auf diese Weise werden auch die letzten Spuren der Kresole entfernt.It has now been observed that this goal is easiest to achieve and cheapest by blowing out aqueous solutions of the calcium salts through immediate sulfonation of cresol-available sulfonic acids with steam can reach. The steam distillation is not only used to remove everything volatile constituents, but also to the cleavage of the sulfonation and subsequent saturation of the sulfonic acids with calcium hydroxide or carbonate always forming cresolates. In this way the last traces of the cresols are also made removed.

Es ist bemerkenswert, daß der Wasserdampf die bisher unbekannten Calciumsalze der erwähnten Sulfosäuren nicht ebenfalls spaltet, und zwar zu Calciumsulfat und Kresol. So zersetzen sich das m-kresolsulfosaure Barium und das entsprechende Bleisalz schon durch Erwärmen auf Temperaturen unter ioo° (vgl. Ber. XX [z887], S. 3o89). Beispiel Rohkresol wird mit der dreifachen Menge Schwefelsäure von 66° B6 bei Wasserbadtemperatur sulfoniert und das erhaltene Gemisch von Rohkresolsulfosäure und überschüssiger Schwefelsäure zur Entfernung der letzteren mit Barythydrat behandelt, vom Bariumsulfat abfiltriert und die Lösung mit Calciumcarbonat versetzt, bis die gesamte Sulfosäure in ihr Calciumsalz übergeführt ist. Die Lösung wird alsdann im. Vakuum eingedampft, bis sie etwa 3oprozentig ist, und dann mehrere Stunden Wasserdampf durchgeleitet. Darauf dampft man im Vakuum vollkommen ein und trocknet das noch etwas feuchte Calciumsalz im Dampftrockenschrank. Man erhält so ein vollkommen von Kresol freies Calciumsalz der kohkresolsulfosäure.It is noteworthy that the water vapor contains the previously unknown calcium salts of the sulfonic acids mentioned does not also cleave, namely to calcium sulfate and Cresol. The m-cresol sulfonic acid barium and the corresponding lead salt decompose even by heating to temperatures below 100 ° (cf. Ber. XX [z887], p. 3o89). Example Raw cresol is made with three times the amount of sulfuric acid of 66 ° B6 at water bath temperature sulfonated and the resulting mixture of raw cresol sulfonic acid and excess Sulfuric acid treated with barium hydrate to remove the latter, from barium sulfate filtered off and the solution mixed with calcium carbonate, until all the sulfonic acid is converted into its calcium salt. The solution is then im. Vacuum evaporated, until it is about 3%, and then passed through water vapor for several hours. Thereon it is completely evaporated in a vacuum and the still slightly moist calcium salt is dried in the steam drying cabinet. A calcium salt completely free of cresol is obtained in this way of the cresol sulfonic acid.

Claims (1)

PATENTANSPRUCH Verfahren zur Reinigung der Calciumsalze der durch unmittelbare Sulfonierung von Kresolen gewonnenen Sulfosäuren, darin bestehend, daß, man die wäßrigen Lösungen dieser Salze mit Wasserdampf behandelt.PATENT CLAIM Process for the purification of the calcium salts by direct sulfonation of sulfonic acids obtained from cresols, consisting of that the aqueous solutions of these salts are treated with steam.
DEF52216D 1922-07-09 1922-07-09 Process for the purification of the calcium salts of the sulfonic acids obtained by direct sulfonation of cresols Expired DE475270C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEF52216D DE475270C (en) 1922-07-09 1922-07-09 Process for the purification of the calcium salts of the sulfonic acids obtained by direct sulfonation of cresols

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEF52216D DE475270C (en) 1922-07-09 1922-07-09 Process for the purification of the calcium salts of the sulfonic acids obtained by direct sulfonation of cresols

Publications (1)

Publication Number Publication Date
DE475270C true DE475270C (en) 1929-04-22

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Family Applications (1)

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DEF52216D Expired DE475270C (en) 1922-07-09 1922-07-09 Process for the purification of the calcium salts of the sulfonic acids obtained by direct sulfonation of cresols

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