CH151131A - Process for the preparation of a sulfuric acid ester. - Google Patents
Process for the preparation of a sulfuric acid ester.Info
- Publication number
- CH151131A CH151131A CH151131DA CH151131A CH 151131 A CH151131 A CH 151131A CH 151131D A CH151131D A CH 151131DA CH 151131 A CH151131 A CH 151131A
- Authority
- CH
- Switzerland
- Prior art keywords
- sulfuric acid
- acid ester
- preparation
- degree
- sulphonation
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C305/00—Esters of sulfuric acids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Herstellung eines Schwefels:iureesters. Es wurde gefunden, dass man einen wert vollen Schwefelsäureester erhält, wenn man Rizinusölsäure mit den Additionsprodukten, welche Schwefeltrioxyd mit organischen Basen bildet, behandelt.
Der so hergestellte Schwefelsäureester ist in Wasser sehr leicht löslich. Er zeigt einen Sulfierungsgrad von über 85 % und soll als Hilfsmittel in der Textilindustrie verwendet werden. (Bestimmung des Sulfierungsgrades nach Dr.
A. Landolt, Melliands Textil berichte 1928, pag. 759-763 und 1929, pag. ?l.f-?1.5.) <I>Beispiel:</I> Zu ?:00 Teilen wasserfreiem Pyridin lässt man langsam unter Rühren und Kühlen 80 Teile Chlorsulfonsäure zutropfen; dabei scheidet sich das gebildete Pyridinsulfo- trioxyd teilweise kristallin aus.
Man lässt diese dünnbreiige Suspension unter gutem Rühren bei 3,0-35 langsam zu 10.0 gr Rizi- nusölsäure zufliessen, wobei nur mässige Temperaturerhöhung stattfindet, und hält dann während einigen Stunden bei genann tem Temperaturintervall. Die Reaktionsflüs sigkeit wird unter Kühlen mit 30 % iger Na tronlauge neutralisiert, von den zum grossen Teile ausgeschiedenen Mineralsalzen getrennt und das Filtrat vom Pyridin durch Destilla tion im Vakuum bei mässiger Temperatur (zirka 50:') befreit.
Der feste Rückstand wird in möglichst wenig Wasser gelöst, die Lösung zwecks Befreiung von noch vorhan denen Mineralsalzen mit verdünnter Schwe felsäure gerade angesäuert und die saure Salzlösung vom ausgeschiedenen Schwefel säureester der Rizinusölsäure getrennt. Der so erhaltene hochsulfierte Schwefelsäureester der Rizinusölsäure wird zuletzt mit Natron lauge gerade neutralisiert und diese Lösung direkt in Verwendung genommen.
Process for the production of a sulfur: iureester. It has been found that a valuable sulfuric acid ester is obtained when ricinoleic acid is treated with the addition products which sulfur trioxide forms with organic bases.
The sulfuric acid ester produced in this way is very easily soluble in water. It shows a degree of sulphonation of over 85% and is intended to be used as an aid in the textile industry. (Determination of the degree of sulfation according to Dr.
A. Landolt, Melliands Textil reports 1928, pag. 759-763 and 1929, pag.? Lf-? 1.5.) <I> Example: </I> To?: 00 parts of anhydrous pyridine are slowly allowed to 80 with stirring and cooling Add parts of chlorosulfonic acid dropwise; the pyridinesulfotrioxide formed separates out partly in crystalline form.
This thin slurry suspension is allowed to slowly flow in to 10.0 g of castor oleic acid with thorough stirring at 3.0-35, with only a moderate increase in temperature, and then held for a few hours at the temperature range mentioned. The reaction liquid is neutralized with 30% sodium hydroxide solution while cooling, separated from the mineral salts which have largely precipitated out, and the filtrate is freed from pyridine by distillation in vacuo at a moderate temperature (about 50%).
The solid residue is dissolved in as little water as possible, the solution is acidified with dilute sulfuric acid in order to free it from any mineral salts that are still present and the acidic salt solution is separated from the precipitated sulfuric acid ester of castoroleic acid. The highly sulfated sulfuric acid ester of castoroleic acid thus obtained is finally neutralized with sodium hydroxide solution and this solution is used directly.
Claims (1)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CH151131T | 1930-05-28 | ||
CH149091T | 1931-05-29 |
Publications (1)
Publication Number | Publication Date |
---|---|
CH151131A true CH151131A (en) | 1931-11-30 |
Family
ID=25715333
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CH151131D CH151131A (en) | 1930-05-28 | 1930-05-28 | Process for the preparation of a sulfuric acid ester. |
Country Status (1)
Country | Link |
---|---|
CH (1) | CH151131A (en) |
-
1930
- 1930-05-28 CH CH151131D patent/CH151131A/en unknown
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