DE724899C - Process for the purification of phosphoric acid esters, such as tricresyl phosphate - Google Patents
Process for the purification of phosphoric acid esters, such as tricresyl phosphateInfo
- Publication number
- DE724899C DE724899C DEB188177D DEB0188177D DE724899C DE 724899 C DE724899 C DE 724899C DE B188177 D DEB188177 D DE B188177D DE B0188177 D DEB0188177 D DE B0188177D DE 724899 C DE724899 C DE 724899C
- Authority
- DE
- Germany
- Prior art keywords
- tricresyl phosphate
- purification
- phosphoric acid
- acid esters
- solvent
- 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
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 title claims description 7
- 238000000034 method Methods 0.000 title claims description 6
- 238000000746 purification Methods 0.000 title claims description 5
- 150000003014 phosphoric acid esters Chemical class 0.000 title claims description 4
- 239000002904 solvent Substances 0.000 claims description 6
- 239000002956 ash Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- 235000002918 Fraxinus excelsior Nutrition 0.000 claims description 2
- 239000011449 brick Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000004576 sand Substances 0.000 claims description 2
- -1 tricresyl phosphate Chemical class 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- 150000002148 esters Chemical class 0.000 description 5
- 239000003077 lignite Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/025—Purification; Separation; Stabilisation; Desodorisation of organo-phosphorus compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/12—Esters of phosphoric acids with hydroxyaryl compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Extraction Or Liquid Replacement (AREA)
Description
Verfahren zur Reinigung von Phosphorsäureestern, wie Trikresylphosphat Gegenstand dos Hauptpatents 723 1-53 ist ein Verfahren zur Reinigung vorn Phosphorsäureestern, wie Trikresylphosphat, die z. B. bei der Reinigung von phenolhaltigen Abwässern verschmutzt worden sind, welches darin besteht, daß die verschmutzten Ester mit Körpern mit großer innerer Oberfläche, wie Kieselgur, Bleicherde, Braunkohlenkoks o. dgl., gemischt und aus der erhaltenen Mischung die Ester mit einem Lösungsmittel, z. B. flüssigem -Butan, extrahiert werden, worauf das Lösungsmittel vom Ester getrennt wird.Process for the purification of phosphoric acid esters, such as tricresyl phosphate The subject of the main patent 723 1-53 is a process for the purification of phosphoric acid esters, such as tricresyl phosphate, which z. B. have been contaminated in the purification of phenol-containing wastewater, which consists in that the contaminated esters with bodies with a large internal surface, such as diatomaceous earth, lignite coke o. z. B. liquid butane, are extracted, whereupon the solvent is separated from the ester.
Bei der Weiterentwicklung dieses Verfahrens wurde nun gefunden, daß ges häufig nicht unbedingt notwendig ist, die verschmutzten Ester vor der Extraktion mit einem Lösungsmittel mit Körpern großer innerer Oberfläche zu vermischen, sondern daß auch Körper, die keine inneren Oberflächen aufweisen, sondern nur äußere Oberflächen, also mehroder weniger feine Pulver von indifferenten. Stoffen, mit Vorteil benutzt werden können. Es eignen sich insbesondere feiner Sand, gemahlene Ziegelsteine, Glaspulver oder sonstiges fein zerkleinertes Material. Sehr vorteilhaft lassen sich ferner Aschen jeder Art, insbesondere Braunkohlenaschen, verwenden, vor allem solche, die gut ausgebrannt sind und die infolgedessen keinen Kohlenstoff mehr enthalten, sondern nur noch aus anorganischen Bestandteilen bestehen. Der Vorteil der Verwendung von solchen indifferenten Stoffen in fein zerkleinerter Form gegenüber den bei dem Verfahren des Hauptpatents benutzten Stoffen mit großer ,innerer Oberfläche besteht darin, daß jene häufig billiger sind als diese und auch die Extraktion rascher und vollständiger durchzuführen gestatten; von den Körpern mit großer innerer Oberfläche wird nämlich häufig ein Teil der Ester sehr fest gebunden, so daß eine vollständige Wiedergewinnung der Ester zeitraubend ist und große Lösungsmittelmengen erfordert. Beispiel Ein aus einer Entphenolungsanlage zur Entphenolung von Hydrierabwässern stammendes verunreinigtes Trikresylph.osphat mit einem Gehalt von etwa 1q.0/0 an nicht mit Wasserdampf flüchtigenVerunreinigumgen wird mit der vierfachen Giewichtsmenge einer vollständig ausgebrannten, aus einer Braunkohlenkess.elfeuerung stammenden Braunkohlenasche vermischt. Die dateientstehende feste Masse ,vird mit einem Kohlenwasserstoffgemisch vom Siedepunkt von 35 bis 6o°, das im wesentlichen aus paraffinischen Kohlenwasserstofffen mit 5 bis 9 C-Atomen besteht, bei gewöhnlicher Temperatur extrahiert. Dabei wird das gesamte Trikresylphosphat praktisch rzstlos wiedergewonnen. Das nach dem Abdampfen des Lösungsmittels erhaltene reine Trikresylphosphat ist völlig frei von nicht flüchtigen Verunreinigungen.In the further development of this process it has now been found that Often it is not absolutely necessary to remove the contaminated ester prior to extraction to mix with a solvent with bodies with a large internal surface, but rather that even bodies that have no internal surfaces, but only external surfaces, thus more or less fine powders of indifferent ones. Fabrics, used with advantage can be. Fine sand, ground bricks, Glass powder or other finely crushed material. Can be very beneficial also use ashes of any kind, in particular lignite ash, especially those that are well burned out and that as a result no longer contain carbon, but only consist of inorganic components. The advantage opposed to the use of such indifferent substances in finely crushed form the substances used in the process of the main patent with a large, inner surface is that these are often cheaper than these and the extraction is also faster and allow it to be carried out more fully; of bodies with a large internal surface namely, a part of the ester is often bound very tightly, so that a complete Recovery of the esters is time consuming and requires large amounts of solvent. Example One from a dephenolation plant for dephenolation of hydrogenation wastewater originating contaminated tricresyl phosphate with a content of about 1q.0 / 0 Contaminants that are not volatile with water vapor are four times the weight a completely burnt out one from a lignite boiler Brown coal ash mixed. The solid mass that arises from the file is mixed with a hydrocarbon mixture from the boiling point of 35 to 60 °, which consists essentially of paraffinic hydrocarbons with 5 to 9 carbon atoms, extracted at ordinary temperature. It will all of the tricresyl phosphate was recovered practically without damage. That after the evaporation The pure tricresyl phosphate obtained from the solvent is completely free of non-volatile substances Impurities.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEB188177D DE724899C (en) | 1939-07-28 | 1939-07-28 | Process for the purification of phosphoric acid esters, such as tricresyl phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEB188177D DE724899C (en) | 1939-07-28 | 1939-07-28 | Process for the purification of phosphoric acid esters, such as tricresyl phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE724899C true DE724899C (en) | 1942-09-09 |
Family
ID=7010611
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEB188177D Expired DE724899C (en) | 1939-07-28 | 1939-07-28 | Process for the purification of phosphoric acid esters, such as tricresyl phosphate |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE724899C (en) |
-
1939
- 1939-07-28 DE DEB188177D patent/DE724899C/en not_active Expired
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