Purification of sulfuryl fluoride

Information

  • Patent Grant
  • 6143269
  • Patent Number
    6,143,269
  • Date Filed
    Thursday, July 29, 1999
    24 years ago
  • Date Issued
    Tuesday, November 7, 2000
    23 years ago
Abstract
Sulfuryl fluoride (SO.sub.2 F.sub.2) frequently contains chlorine, sulfur dioxide and other acidic impurities owing to its production. Effective purification is possible if the sulfuryl fluoride is contacted with hydrogen peroxide or a precursor thereof, preferably in an aqueous solution. The purified product is suitable as a pesticidal agent, for example.
Description

BACKGROUND AND OF THE INVENTION
This application claims the priority of German patent application 198 34 882.7, filed on Aug. 1, 1998, the disclosure of which is expressly incorporated by reference herein.
The present invention relates to the purification of sulfuryl fluoride.
Sulfuryl fluoride (SO.sub.2 F.sub.2) can be used as a pesticide (fumigant). It is prepared, for example, by reacting sulfur dioxide, chlorine or sulfuryl chloride and hydrogen fluoride over a catalyst, for example an alkali bifluoride on activated carbon. See DE-B 1 208 296. The crude product, which still contains hydrogen fluoride, hydrogen chloride, sulfur dioxide, chlorine and sulfuryl chlorofluoride, is purified by means of water in two scrubbers connected in series.
It is an object of the present invention to devise a process with which sulfuryl fluoride can be purified more effectively.
SUMMARY OF THE INVENTION
This object is achieved by the process according to the invention, which provides for sulfuryl fluoride to be purified by contacting with hydrogen peroxide or a precursor thereof.
"Precursors of hydrogen peroxide" are understood to be those compounds which release hydrogen peroxide, in particular in the form of an aqueous solution. Precursors that do not react too basically (risk of decomposition of the SO.sub.2 F.sub.2) can also be used, for example perborates or percarbonates, e.g., as sodium salts. Preferably contacting is effected with hydrogen peroxide, which is expediently in the form of an aqueous solution.
DETAILED DESCRIPTION OF THE INVENTION
The concentration of hydrogen peroxide or of the precursor thereof is advantageously in the range of 0.1 to 10% by weight of the aqueous solution.
The contacting of the sulfuryl fluoride to be purified with the purification solution is expediently effected in a temperature range of 0 to 40.degree. C.
The purification process according to the present invention can be performed immediately following the preparation of SO.sub.2 F.sub.2. Alternatively, the purification process according to the present invention can be performed in time-related conjunction with the application or use of SO.sub.2 F.sub.2. For example, SO.sub.2 F.sub.2 which has not yet been purified or has only been partially purified can be purified according to the invention immediately before application, e.g. as a pesticide. Of course, the purification process according to the present invention can also be performed sometime between the preparation and application of the SO.sub.2 F.sub.2.
The process according to the present invention can be used particularly for the purification of sulfuryl fluoride which contains chlorine, fluorine and/or sulfur dioxide. It is also effective if acids such as hydrofluoric acid or hydrochloric acid are additionally contained therein.
The advantage of the process according to the present invention is, inter alia, that the purification can be performed rapidly and effectively. The sulfuryl fluoride is not attacked in so doing.
The sulfuryl fluoride prepared according to the present invention is substantially free of sulfur dioxide and chlorine, and can therefore be used particularly well as a pesticide. No additional purification is necessary before use. Owing to its purity, no harmful effects on sensitive materials need be feared when it is used.
The following example is intended to explain the invention further, without restricting its scope.





EXAMPLE
Purification of SO.sub.2 F.sub.2 with H.sub.2 O.sub.2
Crude SO.sub.2 F.sub.2 gas containing 0.5% SO.sub.2 (percent surface when measured by gas chromatography) was passed at ambient temperature through a scrubber which contained an aqueous H.sub.2 O.sub.2 solution (H.sub.2 O.sub.2 concentration: 8% by weight). The SO.sub.2 F.sub.2 leaving the scrubber contained less than 0.05% SO.sub.2 (measured using gas chromatography).
The foregoing disclosure has been set forth merely to illustrate the invention and is not intended to be limiting. Since modifications of the disclosed embodiments incorporating the spirit and substance of the invention may occur to persons skilled in the art, the invention should be construed to include everything within the scope of the appended claims and equivalents thereof.
Claims
  • 1. A process for the preparation of purified sulfuryl fluoride, comprising contacting impure sulfuryl fluoride with hydrogen peroxide or a precursor thereof, thereby obtaining purified sulfuryl fluoride.
  • 2. A process according to claim 1, wherein said hydrogen peroxide or precursor thereof is in an aqueous solution.
  • 3. A process according to claim 2, wherein said aqueous solution contains said hydrogen peroxide or precursor thereof at a concentration in the range of 0.1 to 10% by weight.
  • 4. A process according to claim 1, wherein said contacting is carried out at a temperature of 0 to +40.degree. C.
  • 5. A process according to claim 1, wherein said impure sulfuryl fluoride contains at least one impurity selected from the group consisting of sulfur dioxide, elemental fluorine, and chlorine.
  • 6. A process according to claim 5, wherein said impure sulfuryl fluoride further contains as additional impurity at least one of HF and HCl.
Priority Claims (1)
Number Date Country Kind
198 34 882 Aug 1998 DEX
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Number Name Date Kind
2875127 Kenaga Feb 1959
3132925 Pacini et al. May 1964
3320030 Bisignani et al. May 1967
3403144 Lam et al. Sep 1968
3850542 Barnard et al. Nov 1974
3996029 Gustafson et al. Dec 1976
4003987 Jones et al. Jan 1977
4082839 Eibeck et al. Apr 1978
4102987 Cook et al. Jul 1978
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Number Date Country
1208296 Jan 1966 DEX
43 43 689 Oct 1994 DEX
44 41 628 May 1996 DEX
196 21 516 Dec 1997 DEX
727062 Mar 1955 GBX
Non-Patent Literature Citations (2)
Entry
CA:122:25907 abs of DE4343689, Oct. 1994.
CA:125: 32850 abs of DE4441628, Nov. 1994.