AT48340B - Process for the preparation of concentrated formic acid from formates. - Google Patents
Process for the preparation of concentrated formic acid from formates.Info
- Publication number
- AT48340B AT48340B AT48340DA AT48340B AT 48340 B AT48340 B AT 48340B AT 48340D A AT48340D A AT 48340DA AT 48340 B AT48340 B AT 48340B
- Authority
- AT
- Austria
- Prior art keywords
- formic acid
- formates
- preparation
- concentrated formic
- sulfuric acid
- Prior art date
Links
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 title claims description 14
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 title claims description 7
- 235000019253 formic acid Nutrition 0.000 title claims description 7
- 238000000034 method Methods 0.000 title claims description 5
- 150000004675 formic acid derivatives Chemical class 0.000 title claims 2
- 238000002360 preparation method Methods 0.000 title claims 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 5
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 239000004280 Sodium formate Substances 0.000 description 3
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 3
- 235000019254 sodium formate Nutrition 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Description
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konzentrierte Sch wefelsäure eingetragen wird. Ein weiterer technischer Vorteil des vorliegenden Verfahrens liegt darin, dass bei diesem Prozess weniger Material zur Anwendung kommt. Denn in einem Fall sind auf 136 Teile Natriumformiat 240 kg Natriumbisulfat zur Umsetzung erforderlich, während man nach dem vorliegenden Verfahren für die gleiche Menge Natriumformiat nur 98 kg Schwefelsäure (rein) braucht, was durch folgende Formeln zum Ausdruck kommt :
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fahren eine erhebliche technische Verbesserung dar.
Beispiel : Zur Darstellung einer 81prozentigen Ameisensäure verfährt man beispielsweise wie folgt : In einen mit kräftigem Rührwerk, Kühl- und Heizvorrichtung versehenen Kessel. der für die Destillation mit Kühler, kühlbarer Vorlage und Vakuumpumpe verbunden ist, gibt man 300 Teile Schwefelsäure von 63, 20 Be und trägt unter Einhaltung einer Temperatur von 10-150 C trockenes Natriumformiat, entsprechend einer Menge von 340 Teilen Reinformiat, ein. Gegen Ende des Eintragens wird die Masse dicker, jedoch macht die Durchführung keine Schwierigkeiten. Nachdem die Einfüllöffnnung verschlossen worden ist, lässt man die Temperatur langsam auf 300 C steigen. Es beginnt dann die Hauptumsetzung, wobei es zu einer Temperatursteigerung bis 90"C kommen kann.
Eine Zersetzung von Ameisensäure findet jedoch nicht statt.
Die Masse wird bei dieser Reaktion wieder völlig dünnflüssig. Man rührt den Kesselinhalt noch etwa 1/2 Stunde bei 750 C durch, stellt das Rührwerk ab und destilliert im Vakuum unter guter Kühlung des Destillates ab. Es werden so etwa 280 Teile Destillat von 81% Ameisensäuregehalt erhalten, was einer Ausbeute von 98% der theoretischen entspricht.
In der gleichen Weise lässt sich die Umsetzung des Formiates mit 66grädiger Schwefelsäure durchführen, nur ist es hierbei besser. die Temperatur während des Eintragens nicht über 10"C steigen zu lassen und besonders gegen Ende des Eintragens gut zu kühlen. Die Selbsterhitzung zum Schluss hat auch hierbei keine Zersetzung zur Folge, denn es konnten aus der gleichen Menge Natriumformiat 249 Teile Ameisensäure von 90, 3% erhalten werden, was einer Ausbeute von über 97% der theoretischen entspricht. In dem Kessel hinterbleibt neutrales Natriumsulfat.
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concentrated sulfuric acid is entered. Another technical advantage of the present method is that less material is used in this process. In one case, 240 kg of sodium bisulphate per 136 parts of sodium formate are required for the conversion, while according to the present process only 98 kg of sulfuric acid (pure) are required for the same amount of sodium formate, which is expressed by the following formulas:
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represent a significant technical improvement.
Example: To prepare an 81% formic acid, proceed as follows: In a kettle equipped with a powerful stirrer, cooling and heating device. which is connected to the cooler, coolable receiver and vacuum pump for the distillation, 300 parts of sulfuric acid of 63.20 Be are added and, while maintaining a temperature of 10-150 C, dry sodium formate, corresponding to an amount of 340 parts of pure formate, is entered. Towards the end of the entry the mass becomes thicker, but the implementation does not present any difficulties. After the filling opening has been closed, the temperature is allowed to rise slowly to 300 ° C. The main conversion then begins, which can lead to a temperature increase of up to 90 "C.
However, formic acid does not decompose.
During this reaction, the mass becomes completely thin again. The kettle contents are stirred for about 1/2 hour at 750 ° C., the stirrer is switched off and the distillate is distilled off in vacuo with good cooling. About 280 parts of distillate with 81% formic acid content are obtained, which corresponds to a yield of 98% of the theoretical.
The conversion of the formate with 66 degree sulfuric acid can be carried out in the same way, but it is better here. not to let the temperature rise above 10 "C during the entry and to cool it well, especially towards the end of the entry. The self-heating at the end does not result in any decomposition either, because 249 parts of formic acid of 90.3 % can be obtained, which corresponds to a yield of over 97% of the theoretical. Neutral sodium sulfate remains in the kettle.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE48340X | 1908-10-15 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| AT48340B true AT48340B (en) | 1911-06-10 |
Family
ID=5625947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AT48340D AT48340B (en) | 1908-10-15 | 1909-03-13 | Process for the preparation of concentrated formic acid from formates. |
Country Status (1)
| Country | Link |
|---|---|
| AT (1) | AT48340B (en) |
-
1909
- 1909-03-13 AT AT48340D patent/AT48340B/en active
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