DE272339C - - Google Patents
Info
- Publication number
- DE272339C DE272339C DENDAT272339D DE272339DA DE272339C DE 272339 C DE272339 C DE 272339C DE NDAT272339 D DENDAT272339 D DE NDAT272339D DE 272339D A DE272339D A DE 272339DA DE 272339 C DE272339 C DE 272339C
- Authority
- DE
- Germany
- Prior art keywords
- diethyl sulfate
- sodium
- percent
- ethylsulphurate
- vacuo
- 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.)
- Active
Links
- DENRZWYUOJLTMF-UHFFFAOYSA-N Diethyl sulfate Chemical compound CCOS(=O)(=O)OCC DENRZWYUOJLTMF-UHFFFAOYSA-N 0.000 claims description 10
- 239000003085 diluting agent Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000005292 vacuum distillation Methods 0.000 claims description 4
- RRLOOYQHUHGIRJ-UHFFFAOYSA-M sodium;ethyl sulfate Chemical compound [Na+].CCOS([O-])(=O)=O RRLOOYQHUHGIRJ-UHFFFAOYSA-M 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 10
- 229940008406 diethyl sulfate Drugs 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- KIWBPDUYBMNFTB-UHFFFAOYSA-N Ethyl sulfate Chemical compound CCOS(O)(=O)=O KIWBPDUYBMNFTB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- AKEJUJNQAAGONA-UHFFFAOYSA-N Sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L cacl2 Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L na2so4 Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- HHXABRHYMHOZMM-UHFFFAOYSA-N C(C)[ClH]S(=O)(=O)Cl Chemical compound C(C)[ClH]S(=O)(=O)Cl HHXABRHYMHOZMM-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- FUGINSUSTSZAEY-UHFFFAOYSA-M potassium;ethyl sulfate Chemical compound [K+].CCOS([O-])(=O)=O FUGINSUSTSZAEY-UHFFFAOYSA-M 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/24—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfuric acids
Description
KAISERLICHESIMPERIAL
PATENTAMT.PATENT OFFICE.
Die bisher bekannten Verfahren zur Darstellung von Diäthylsulfat (Mischen von Alkohol und Schwefelsäure und nachfolgende Chloroformextraktion, Vakuumdestillation eines Gemisches von absolutem Alkohol und Schwefelsäure, Einleiten von Schwefelsäureanhydrid in Äthyläther, Einwirkung von Alkohol auf Äthylschwefelsäurechlorid, trockene Destillation von äthylschwefelsaurem Kalium u. dgl.) haben insgesamt zu mangelhaften Ausbeuten geführt.The previously known processes for the preparation of diethyl sulfate (mixing alcohol and sulfuric acid and subsequent chloroform extraction, vacuum distillation one Mixture of absolute alcohol and sulfuric acid, introduction of sulfuric anhydride into Ethyl ether, action of alcohol on ethylsulfuric acid chloride, dry distillation of Potassium ethylsulphurate and the like) have resulted in poor overall yields.
Der vorliegenden Erfindung liegt nun die Beobachtung zugrunde, daß es gelingt, Diäthylsulfat mit wesentlich höheren, von der Theorie nicht weit entfernten Ausbeuten technisch darzustellen, wenn man äthylschwefelsaures Natrium für sich oder im Gemisch mit einem geeigneten Verdünnungsmittel, z. B. trockenem Natriumsulfat, im Vakuum destilliert.The present invention is based on the observation that it is possible to use diethyl sulfate to be technically represented with significantly higher yields not far removed from theory, if you have sodium ethylsulphurate by itself or as a mixture with a suitable diluent, e.g. B. dry Sodium sulfate, distilled in vacuo.
Zur Ausführung des Verfahrens wird äthylschwefelsaures Natrium eventuell unter gleichzeitigem Rühren im Vakuum erhitzt und das überdestillierende Diäthylsulfat in üblicher Weise in einer geeigneten Vorlage aufgefangen. Das so erhaltene Diäthylsulfat kann, wenn gewünscht, noch einem bekannten Reinigungsprozeß (ζ. Β. Rektifikation durch nochmalige Vakuumdestillation oder Wasserzusatz und Chloroformausschüttelung mit nachträglichem Verjagen des Chloroforms u. dgl.) unterworfen werden.To carry out the process, ethylsulfuric acid is used Sodium possibly heated in vacuo with simultaneous stirring and the diethyl sulfate distilling over in the usual way Way caught in a suitable template. The diethyl sulfate thus obtained can, if desired, another known cleaning process (ζ. Β. rectification by repeated Vacuum distillation or addition of water and chloroform extraction with subsequent Chasing away chloroform and the like).
Ausführungsbeispiel.Embodiment.
4000 g kristallwasserfreies äthylschwefelsaures Natrium werden im Vakuum destilliert.4000 g of anhydrous sodium ethylsulphurate are distilled in vacuo.
Das übergegangene Diäthylsulfat wird mit kaltem Wasser versetzt und mit Chloroform ausgeschüttelt. Das Chloroform wird abgehoben, mit Chlorcalcium getrocknet, vom Chlorcalcium abfiltriert und verjagt. Der aus reinem Diäthylsulfat bestehende Rückstand wiegt 1720 bis 1870 g. Die Ausbeute an reinem Diäthylsulfat beträgt demnach 83 bis 90 Prozent der Theorie und wird 'wahrscheinlich beim Verarbeiten größerer Quantitäten und mit rationeller Apparatur noch weiter steigen.The transferred diethyl sulfate is mixed with cold water and with chloroform shaken out. The chloroform is lifted off, dried with calcium chloride, calcium chloride filtered off and chased away. The residue, consisting of pure diethyl sulfate, weighs 1720 up to 1870 g. The yield of pure diethyl sulfate is accordingly 83 to 90 percent of the Theory and is likely to be more efficient when processing larger quantities Apparatus continue to rise.
Die Verbrennung eines auf diese Weise dargestellten Diäthylsulfats ergab folgende Zahlen:The combustion of a diethyl sulfate prepared in this way gave the following figures:
0,2420 g Substanz ergaben:0.2420 g of substance resulted in:
a) 0,1479 g H2O = 6,78 Prozent H, a) 0.1479 g H 2 O = 6.78 percent H,
b) 0,2772 g CO2 = 31,23 Prozent C.b) 0.2772 g CO 2 = 31.23 percent C.
Berechnet für Diäthylsulfat:
H = 6,48 Prozent,
C = 31,12 Prozent.Calculated for diethyl sulfate:
H = 6.48 percent,
C = 31.12 percent.
3535
4040
4545
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Will man bei Gegenwart eines Verdünnungsmittels arbeiten, so mischt man das äthylschwefelsaure Natrium mit dem Verdünnungsmittel (z. B. 2 Teile äthylschwefelsaures Natrium und I.Teil Natriumsulfat) innigst zu-If you want to work in the presence of a diluent, the ethylsulfuric acid is mixed Sodium with the diluent (e.g. 2 parts of ethylsulfuric acid and 1 part of sodium sulfate).
sammen und unterwirft die Mischung dann der Vakuumdestillation.together and then subjects the mixture to vacuum distillation.
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE272339C true DE272339C (en) |
Family
ID=528917
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT272339D Active DE272339C (en) |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE272339C (en) |
-
0
- DE DENDAT272339D patent/DE272339C/de active Active
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