DE1000354B - Production of salts of fluorosulfinic acid - Google Patents
Production of salts of fluorosulfinic acidInfo
- Publication number
- DE1000354B DE1000354B DES37403A DES0037403A DE1000354B DE 1000354 B DE1000354 B DE 1000354B DE S37403 A DES37403 A DE S37403A DE S0037403 A DES0037403 A DE S0037403A DE 1000354 B DE1000354 B DE 1000354B
- Authority
- DE
- Germany
- Prior art keywords
- sulfur dioxide
- fluoride
- salts
- fluorosulfinate
- production
- 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.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 150000003839 salts Chemical class 0.000 title description 4
- 239000002253 acid Substances 0.000 title description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 5
- HMKJMFKGFGKCPL-UHFFFAOYSA-M fluorosulfite Chemical compound [O-]S(F)=O HMKJMFKGFGKCPL-UHFFFAOYSA-M 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 10
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 description 6
- 235000003270 potassium fluoride Nutrition 0.000 description 5
- 239000011698 potassium fluoride Substances 0.000 description 5
- SGQWCRMKJYYBKC-UHFFFAOYSA-M 14986-57-3 Chemical compound [K+].[O-]S(F)=O SGQWCRMKJYYBKC-UHFFFAOYSA-M 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- RDVCRTKBZOIUNV-UHFFFAOYSA-M [Rb+].[O-]S(F)=O Chemical compound [Rb+].[O-]S(F)=O RDVCRTKBZOIUNV-UHFFFAOYSA-M 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- AHLATJUETSFVIM-UHFFFAOYSA-M rubidium fluoride Chemical compound [F-].[Rb+] AHLATJUETSFVIM-UHFFFAOYSA-M 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- XUIIKFGFIJCVMT-LBPRGKRZSA-N L-thyroxine Chemical compound IC1=CC(C[C@H]([NH3+])C([O-])=O)=CC(I)=C1OC1=CC(I)=C(O)C(I)=C1 XUIIKFGFIJCVMT-LBPRGKRZSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- ZJTRUVGHRKSQBF-UHFFFAOYSA-M [S+](=O)=O.[F-] Chemical compound [S+](=O)=O.[F-] ZJTRUVGHRKSQBF-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012025 fluorinating agent Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- CSABAZBYIWDIDE-UHFFFAOYSA-N sulfino hydrogen sulfite Chemical class OS(=O)OS(O)=O CSABAZBYIWDIDE-UHFFFAOYSA-N 0.000 description 1
- 125000005207 tetraalkylammonium group Chemical group 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/46—Compounds containing sulfur, halogen, hydrogen, and oxygen
- C01B17/463—Fluorosulfonic acid (FSO3H)
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Herstellung von Salzen der Fluorsulfinsäure Salze der Fluorsulfinsäu:re (Fluors.ulfinate) sind in der Literatur noch nicht beschrieben «-orden. Es wurde nun gefunden, daß man in einfacher Weise zu Fluorsulfina:ten der Alkalimetalle und quartärer Stickstoffbasen gelangt, wenn man die entsprechenden Fluori.de genügend lange der Einwirkung von gasförmigem oder flüssigem Schwefeldioxyd aussetzt. Die Reaktion vollzieht sich um so leichter, je größer das Kation des betreffenden Fluorids ist. So sind vor allem Kali,umfluorid, Rubid iumfluorid und Cäsiumfluorid sowie Tetraalkylammoniumfluoride dieser Reaktion zugänglich. Aber auch Natriumfluorid addiert Schwefeldioxyd. in gewissem, wenn auch mäßigem Umfange. Die erhaltenen Verbindungen erweisen sich durch ihr Röntgendiagramm als selbständige chemische Individuen und nicht nur als strukturell durch Einbau von Schwefeldiioxyd leicht modifiziertes Fluorid.Production of salts of fluorosulfinic acid Salts of fluorosulfinic acid (Fluorosulfinate) have not yet been described in the literature. It was now found that one can easily get to fluorosulfine: th of the alkali metals and Quaternary nitrogen bases can be obtained if the appropriate Fluori.de is sufficient long exposure to the action of gaseous or liquid sulfur dioxide. the The larger the cation of the fluoride in question, the easier it is for the reaction to take place is. So are mainly potash, umfluorid, rubid iumfluorid and cesium fluoride as well Tetraalkylammonium fluoride this reaction accessible. But also sodium fluoride adds sulfur dioxide. to a certain extent, if moderately. The compounds obtained turn out to be independent chemical individuals and by their X-ray diagram not only as slightly modified structurally through the incorporation of sulfur dioxide Fluoride.
Die Ausgangsfluoride werden in gut getrocknetem Zustand, frei von Hydrogenfluorid eingesetzt, da nur der als neutrales Fluorid vorhandene Anteil mit dem Schwefeldioxyd zu Fluorsulfinat reagiert. Die Umsetzung mit Schwefeldioxyd vollzieht sich bei mäßigen Temperaturen, vorzugsweise bei Zimmertemperatur, je nach der Vermischungsintensität in längerer oder kürzerer Zeit. Im Falle von Kalium-, Rubidium- und Cäsiumfluorid erreicht man bei Zimmertemperatur in «-eiigen Tagen fast theoretische Ausbeuten. Die so erhaltenen Fluo.rsttlfinate stellen farblose, kristalline Pulver dar, welche an feuchter Luft unter Abspaltung von Schwefeldioxyd in Hydrogettfluoride und Disulfite zerfallen. Sie können als besond-,rs wirksame Fluorierungsmittel Verwendung finden.The starting fluorides are in a well-dried state, free from Hydrogen fluoride is used, since only the proportion present as a neutral fluoride with the sulfur dioxide reacts to form fluorosulfinate. The implementation with sulfur dioxide takes place at moderate temperatures, preferably at room temperature, depending on the mixing intensity in a longer or shorter period of time. In the case of potassium, rubidium and cesium fluoride almost theoretical yields are achieved at room temperature in a few days. The so obtained Fluo.rsttlfinate are colorless, crystalline powders, which in moist air with splitting off of sulfur dioxide into hydrogettfluorides and disulphites disintegrate. They can be used as particularly effective fluorinating agents.
Beispiel i Darstellung von Kaliumfluorsulfinat aus Kaliumfluorid und flüssigem Schwefeldioxyd i kg feinstgepulvertes Kaliumfluorid wird in einem Rührautoklav von etwa .I 1 zusammen mit etwa 2 kg flüssigem Schwefeldioxyd unter langsamem Rühren bei Zimmertemperatur sich selbst überlassen. Nach 5 Tagen wird das überschüssige Schwefeldioxyd bei Zimmertemperatur und Atmosphärendruck abgelassen. Der Rückstand, in einer 'Menge von 2,05 kg gewonnen, stellt ein feines farbloses Pulver dar, das etwa 96Molprozent Kaliumfluorsulfinat enthält.EXAMPLE i Preparation of potassium fluorosulfinate from potassium fluoride and liquid sulfur dioxide 1 kg of finely powdered potassium fluoride is left to itself in a stirred autoclave of about .I 1 together with about 2 kg of liquid sulfur dioxide with slow stirring at room temperature. After 5 days, the excess sulfur dioxide is drained off at room temperature and atmospheric pressure. The residue, obtained in an amount of 2.05 kg, is a fine colorless powder containing about 96 mole percent potassium fluorosulfinate.
Beispiel 2 Darstellung von Kaliumfluorsulfinat aus Kaliumfluorid und gasförmigem Schwefeldioxyd i kg feinstgepulvertes Kaliumfluorid wird in einen eisernen Rührautoklav gefüllt. Nach Verdrängen der Luft wird ein Vorratsgefäß mit flüssigem Schwefeldioxyd von Zimmertemperatur über den Gasraum angeschlossen, so daß der entsprechende Dampfdruck des Schwefeldioxyds sich au-eh auf das Kaliumfluorid auswirkt. Nach Einschalten des Rührwerks beobachtet man eine lebhafte Absorption von Schwefeldioxyd" die bei der Addii,tion von etwa i kg Schwefeldioxyd. abklingt. Man erhält rund 2 kg eines etwa 9o°/oigen Kaliumfluorsulfinates.Example 2 Preparation of potassium fluorosulfinate from potassium fluoride and gaseous sulfur dioxide in kg of finely powdered potassium fluoride is converted into an iron Stirring autoclave filled. After displacing the air there is a storage vessel with liquid Sulfur dioxide from room temperature connected via the gas space, so that the appropriate The vapor pressure of the sulfur dioxide also affects the potassium fluoride. After switching on the agitator one observes a lively absorption of sulfur dioxide "the at the addition of about 1 kg of sulfur dioxide. subsides. You get around 2 kg of one about 90% potassium fluorosulfinate.
Beispiel 3 Darstellung von Rubidi.umfluorsulfinat 5o g Rubi:diumfluorid werden zusammen mit flüssigem Schwefeldioxyd in ein Glasrohr eingeschmolzen und 3 Tage stehengelassen. Nach dem Öffnen des Glasrohres und Abdampfen des überschüssigen Schwefeldioxyds erhält man Rubidiumfluorsulfinat in praktisch quantitativer Ausbeute. In ähnlicher Weise mit demselben günstigen Ergebnis verläuft die Umsetzung zwischen Cäsiumfluorid und Schwefeldioxyd. Beispiel d Darstellung von Tetrame,tthylammon.iu@mfluorsulfinat Auf i8o g scharf getrocknetes Tetramet:hylammoniumfluorid werden bei -8o° und Atmosphärendruck etwa 5oo g Schwefeldioxyd kondensiert. Das Salz löst sich beim Umschwenken des verflü'ss'igten Gases auf. Anschließend dampft man das überschüssige Schwefeldioxyd bei Atmosphärendruck und etwa -6° ab und erhält als Rückstand - einer vollständigen Umsetzung entsprechend - etwa 320 g eines farblosen Kristallisates der Zusammensetzung [N(CH3)4]SOZF.EXAMPLE 3 Preparation of Rubidium Fluorosulfinate 50 g of rubidium fluoride are melted together with liquid sulfur dioxide in a glass tube and left to stand for 3 days. After opening the glass tube and evaporating the excess sulfur dioxide, rubidium fluorosulfinate is obtained in a practically quantitative yield. The reaction between cesium fluoride and sulfur dioxide proceeds in a similar way with the same favorable result. Example d Preparation of tetrame, tthylammon.iu @ mfluorosulfinate. About 500 g of sulfur dioxide are condensed on 180 g of sharply dried tetramet: hylammonium fluoride at -80 ° and atmospheric pressure. The salt dissolves when the liquefied gas is swiveled around. The excess sulfur dioxide is then evaporated at atmospheric pressure and at about -6 ° and as residue - corresponding to a complete conversion - about 320 g of colorless crystals of the composition [N (CH3) 4] SOZF are obtained.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DES37403A DE1000354B (en) | 1954-01-30 | 1954-01-30 | Production of salts of fluorosulfinic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DES37403A DE1000354B (en) | 1954-01-30 | 1954-01-30 | Production of salts of fluorosulfinic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1000354B true DE1000354B (en) | 1957-01-10 |
Family
ID=7482564
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DES37403A Pending DE1000354B (en) | 1954-01-30 | 1954-01-30 | Production of salts of fluorosulfinic acid |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1000354B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1000901A1 (en) * | 1998-11-11 | 2000-05-17 | Solvay Fluor und Derivate GmbH | Method for producing sulfuryl fluoride |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2312413A (en) * | 1939-12-27 | 1943-03-02 | Du Pont | Manufacture of fluosulphonates |
| US2408785A (en) * | 1944-06-28 | 1946-10-08 | Ozark Chemical Company | Method of production of anhydrous monofluorophosphoric acid |
| US2408784A (en) * | 1943-03-11 | 1946-10-08 | Ozark Chemical Company | Anhydrous monofluorophosphoric acid and method of producing it |
| US2430963A (en) * | 1944-11-27 | 1947-11-18 | Gen Chemical Corp | Manufacture of fluosulfonic acid |
| US2481807A (en) * | 1947-11-28 | 1949-09-13 | Ozark Mahoning Co | Method of producing monofluorophosphates |
| US2488298A (en) * | 1946-09-12 | 1949-11-15 | Ozark Mahoning Co | Method of producing hexafluorophosphoric acid |
-
1954
- 1954-01-30 DE DES37403A patent/DE1000354B/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2312413A (en) * | 1939-12-27 | 1943-03-02 | Du Pont | Manufacture of fluosulphonates |
| US2408784A (en) * | 1943-03-11 | 1946-10-08 | Ozark Chemical Company | Anhydrous monofluorophosphoric acid and method of producing it |
| US2408785A (en) * | 1944-06-28 | 1946-10-08 | Ozark Chemical Company | Method of production of anhydrous monofluorophosphoric acid |
| US2430963A (en) * | 1944-11-27 | 1947-11-18 | Gen Chemical Corp | Manufacture of fluosulfonic acid |
| US2488298A (en) * | 1946-09-12 | 1949-11-15 | Ozark Mahoning Co | Method of producing hexafluorophosphoric acid |
| US2481807A (en) * | 1947-11-28 | 1949-09-13 | Ozark Mahoning Co | Method of producing monofluorophosphates |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1000901A1 (en) * | 1998-11-11 | 2000-05-17 | Solvay Fluor und Derivate GmbH | Method for producing sulfuryl fluoride |
| US6238642B1 (en) | 1998-11-11 | 2001-05-29 | Solvay Fluor Und Derivate Gmbh | Process of preparing sulfuryl fluoride |
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