DE347897C - Process for the production of triacetin - Google Patents
Process for the production of triacetinInfo
- Publication number
- DE347897C DE347897C DE1919347897D DE347897DD DE347897C DE 347897 C DE347897 C DE 347897C DE 1919347897 D DE1919347897 D DE 1919347897D DE 347897D D DE347897D D DE 347897DD DE 347897 C DE347897 C DE 347897C
- Authority
- DE
- Germany
- Prior art keywords
- triacetin
- production
- acetic anhydride
- boiling
- percent
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/02—Esters of acyclic saturated monocarboxylic acids having the carboxyl group bound to an acyclic carbon atom or to hydrogen
- C07C69/12—Acetic acid esters
- C07C69/18—Acetic acid esters of trihydroxylic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Herstellung von Triacetin. Triacetin (Triacetylglycerin) wurde bisher in der Weise gewonnen, daß man aus Glycerin und Eisessig zunächst Diacetin herstellte, indem man beide Körper stundenlang kochte (S e e 1 i g, Berichte aq., 1894 S. 3q.67). Über die weitere Acetylierung zum Triacetin schreibt S e e 1 i g an derselben Stelle: »Die vollständige Überführung des Diacetates in Triacetin gelingt nicht durch einfaches.Kochen mit Eisessig, gelingt auch nicht durch Kochen mit Acetanhydrid, wohl aber durch Kochen mitAcetanhydrid unter Zusatz von wasserfreiem Natriumacetat.« Im Gegensatz ztt diesen Angaben und den bisher in der Technik üblichen Verfahren wurde nun die bemerkenswerte Beobachtung ; gemacht, daß die Acetyh rung des Glycerins ohne Kondensationsmittel in sehr kurzer Zeit gelingt, wenn man Glycerin direkt mit Essigsäurean@hydrid in der Wärme behandelt unter Ausnutzung der bei derUmsetzung entstehenden Wärmemengen. Man erzielt so ein hochprozentiges Triacetin.Process for the production of triacetin. Triacetin (triacetylglycerin) has hitherto been obtained in such a way that diacetin is first made from glycerine and glacial acetic acid made by boiling both bodies for hours (S e e 1 i g, reports aq., 1894 p. 3q.67). S e e 1 i g writes about the further acetylation to triacetin in the same place: “The complete conversion of the diacetate into triacetin succeeds not by simply boiling with glacial acetic acid, not even by boiling with acetic anhydride, but probably by boiling with acetic anhydride with the addition of anhydrous sodium acetate. " In contrast to this information and the procedures customary in technology up to now now became the remarkable observation; made that the Acetyh tion of the glycerine without condensation agent in a very short time, if you use glycerine directly Acetic anhydride treated in the heat using the during the implementation resulting amounts of heat. A high-percentage triacetin is achieved in this way.
Der technische Vorteil des vorliegenden Verfahrens gegenüber den bisher bekannten Herstellungsverfahren besteht, abgesehen von der Ersparnis an. Essigsäureanhydrid, an Natriumacetat oder anderen Kondensationsmitteln sowie an Heizstoffen, in dem äußerst schnellen und glatten Verlauf -der Umsetzung. .-Das Fehlen jeglichen Kondensationsmittels gestattet ferner eine bequeme Reindestillation ohne wesentliche Rückstände.The technical advantage of the present process over the previous known manufacturing process exists, apart from the savings. Acetic anhydride, on sodium acetate or other condensing agents as well as on heating materials in which extremely fast and smooth course of implementation. .-The absence of any condensing agent also allows a convenient purifying distillation without significant residues.
Beispiel. In einem emaillierten, mit Rückflußkühler versehenen Rührkessel itn Ölbade werden 300 bis 33o Gewichtsteile Essigsäureanhydrid (Gehalt 9o bis 97 Prozent) auf ioo° erhitzt, die Heizung sodann abgestellt und unter kräftibmem Rühren 92 Gewichtsteile Glycerin (g8,5 bis 99,5 Prozent) einlaufen gelassen.Example. 300 to 33o parts by weight of acetic anhydride (content 9o to 97 percent) are heated to 100 ° in an enamelled stirred tank equipped with a reflux condenser, the heating is then switched off and 92 parts by weight of glycerol (g8.5 to 99.5 percent) are poured in with vigorous stirring calmly.
Die Temperatur steigt schnell auf 13o bis 135° und bleibt bei genügend flottem. Einleiten auf dieser Höhe.The temperature rises quickly to 13o to 135 ° and remains at sufficient brisk. Initiate at this height.
Sodann wird die gebildete Essigsäure abdestilliert, der Rüokstand im Vakuum destilliert und entsäuert. Die Ausbeute beträgt 195 bis 2o5 Gewichtsteile, gleich go bis 95 Prozent der Theorie. Der Siedepunkt des reinen Triacetins ist 140 bis 15o° bei 1o mm.The acetic acid formed is then distilled off and the residue is removed distilled in vacuo and deacidified. The yield is 195 to 2o5 parts by weight, same go to 95 percent of theory. The boiling point of pure triacetin is 140 up to 15o ° at 1o mm.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE347897T | 1919-12-16 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE347897C true DE347897C (en) | 1922-01-26 |
Family
ID=6256735
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE1919347897D Expired DE347897C (en) | 1919-12-16 | 1919-12-16 | Process for the production of triacetin |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE347897C (en) |
-
1919
- 1919-12-16 DE DE1919347897D patent/DE347897C/en not_active Expired
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