DE922771C - Process for purifying pentaerythritol - Google Patents
Process for purifying pentaerythritolInfo
- Publication number
- DE922771C DE922771C DEC4731A DEC0004731A DE922771C DE 922771 C DE922771 C DE 922771C DE C4731 A DEC4731 A DE C4731A DE C0004731 A DEC0004731 A DE C0004731A DE 922771 C DE922771 C DE 922771C
- Authority
- DE
- Germany
- Prior art keywords
- pentaerythritol
- rays
- carbonic acid
- temperature
- irradiation
- 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
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
- C07C31/18—Polyhydroxylic acyclic alcohols
- C07C31/24—Tetrahydroxylic alcohols, e.g. pentaerythritol
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Reinigung von Fentaerythrit Pentaerythrit ist bisher in reiner Form nicht erhalten worden. Abgesehen davon, daß er in der Regel vom Herstellungsausgangsprodukt herrührende Tetranitroderivate enthält, weist er bis zu 30% einen Gehalt von Dipentaerythrit auf.Process for purifying fentaerythritol is pentaerythritol so far has not been obtained in its pure form. Apart from the fact that it is usually derived from the production base product Contains derived tetranitrogen derivatives, it has a dipentaerythritol content of up to 30% on.
Gemäß der vorliegenden Erfindung wird zur reinen Herstellung eine wäßrige Lösung von Pentaerythrit unter gleichzeitiger Einleitung von Kohlensäure mit Rotstrahlen, ultravioletten Strahlen oder Röntgenstrahlen bestrahlt, abfiltriert und umkristallisiert. Die Bestrahlung und Kohlensäureeinleitung nimmt man bei einer Temperatur von 70 bis 75° vor.According to the present invention, for production only, a aqueous solution of pentaerythritol with simultaneous introduction of carbonic acid irradiated with red rays, ultraviolet rays or X-rays, filtered off and recrystallized. The irradiation and the introduction of carbon dioxide are taken from one Temperature from 70 to 75 ° before.
Beispiel i Pentaerythrit wird in Emailleschalen in Wasser gelöst. Es wird z. B. mit Hilfe von Siedetauchern aus Quarzglas auf 70 bis 75° erwärmt. Nach Einstellung der Temperatur wird 5 bis 6 Stunden lang Kohlensäure eingeblasen und während dieser Zeit mit Röntgenstrahlen bestrahlt. Es fällt Pentaerythrit aus, der abfiltriert und gewaschen wird. Es wird sodann etwa nach 5 Stunden mit kochendem Wasser gewaschen und filtriert. Unter Verwendung von reinem Alkohol wird dreimal umkristallisiert. Schließlich wird der Alkohol verdampft, nochmals gewaschen und schließlich bei i2o° im Trockenschrank getrocknet.Example i Pentaerythritol is dissolved in water in enamel dishes. It is z. B. heated to 70 to 75 ° with the help of fused quartz glass. After the temperature has been set, carbonic acid is blown in for 5 to 6 hours and irradiated with X-rays during this time. Pentaerythritol precipitates out and is filtered off and washed. It is then washed with boiling water after about 5 hours and filtered. It is recrystallized three times using pure alcohol. Finally, the alcohol is evaporated, washed again and finally dried in a drying cabinet at 120 °.
Der Schmelzpunkt des so erhaltenen Produktes liegt oberhalb 22o°.The melting point of the product thus obtained is above 220 °.
Das Produkt besitzt vier alkoholische Hydroxylgruppen und fünf Kohlenstoffatome. Es ist eine reinweiße kristallinische Masse und enthält keinen Stickstoff mehr. Das Produkt ist frei von Tetranitroderivaten und vor allen Dingen frei von Dipentaerythrit.The product has four alcoholic hydroxyl groups and five carbon atoms. It is a pure white crystalline mass and no longer contains any nitrogen. The product is free of tetranitro derivatives and above all free from dipentaerythritol.
Beispiel a 3o kg handelsüblicher Pentaerythrit, in denn noch alle Verunreinigungen enthaltene sind, werdeni in. eine Schale geschüttet und mit 5o 1 Wasser vermischt. Alsdann wird der Kohlensäurestrom ein gelassen, gleichzeitig werden Quarztauchsieder eingesetzt, und es wird mit Infrarot bestrahlt. Die Flüssigkeit wird auf 70'°' erhitzt. Dieser Prozeß dauert 5 bis 6 Stunden,. Nach Beendigung läßt man kristallieven. Der entstandene Kristallkuchen wird zerschlagen und sodann mit 7o'°1 heißem Wasser abgespült. Daraufhin wird das Produkt getrocknet und zermahlen. Das Ergebnis ist reinster Pentaerythrit ohne jede Verunreinigung, An Stelle der Rotstrahlen können auch Ultraviolett- oder Röntgenstrahlen verwendet werden. Da Röntgenstrahlen und Ultraviolettstrahlen wirksaurer sind, erfolgt die Umsetzung in reinsten Pentaerythrit in der halben Zeit.Example a 30 kg of commercially available pentaerythritol, then all of them Contains impurities are poured into a bowl and treated with 5o 1 water mixed. Then the carbonic acid stream is let in, at the same time quartz immersion heaters are used and infrared radiation is used. The liquid is heated to 70 '°'. This process takes 5 to 6 hours. After finishing lets one crystallize. The resulting crystal cake is smashed and then with Rinsed 7o '° 1 hot water. The product is then dried and ground. The result is the purest pentaerythritol without any contamination, instead of the Red rays can also use ultraviolet or X-rays. There X-rays and ultraviolet rays are more effectively acidic, the reaction occurs in the purest pentaerythritol in half the time.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEC4731A DE922771C (en) | 1951-09-21 | 1951-09-21 | Process for purifying pentaerythritol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEC4731A DE922771C (en) | 1951-09-21 | 1951-09-21 | Process for purifying pentaerythritol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE922771C true DE922771C (en) | 1955-01-24 |
Family
ID=7013473
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEC4731A Expired DE922771C (en) | 1951-09-21 | 1951-09-21 | Process for purifying pentaerythritol |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE922771C (en) |
-
1951
- 1951-09-21 DE DEC4731A patent/DE922771C/en not_active Expired
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