Solvay Fluor Und Derivate Gmbh

Kali-chemie Aktiengesellschaft

Solvay (societe Anonyme)

Solway Fluor Und Derivate Gmbh

Solvay Fluor and Derivate Gmbh

Johannes Eicher

Werner Rudolph

Hans-Walter Swidersky

Max Josef Braun

Karl-Heinz Fazniewscy

Francine Janssens

Kerstin Eichholz

Carsten Brosch

Thomas Born

Karlheinz Fazniewscy

Pascal Pennetreau

Stefan Palsherm

Matthias Rieland

Matthias Marek

Lore Hirsch

Eckhard Hausmann

Bernhard Schulte

Sulfuryl fluoride, which is useful as a fumigant, may be contaminated with sulfur dioxide and possibly other impurities such as sulfuryl chloride, depending on the way it is produced. According to the invention, sulfur dioxide and, if applicable, sulfuryl chloride fluoride are removed from a contaminated sulfuryl fluoride product by using aluminum oxide as an adsorbing agent. The method of the invention is highly advantageous because it eliminates the need to use activated carbon as an additional adsorbent.

Purification of sulfuryl fluoride

Organic compounds, e.g. fluorinated organic compounds such as fluorinated carboxylic acids or fluorinated carboxylic acid chlorides, may contain small amounts of carboxylic acid fluorides, hydrogen fluoride or hydrolyzable fluoride, which during the preparation of derivatives of the fluorinated organic compounds, for example by esterification, may yield corrosive fluorides or hydrogen fluoride. The invention is a method for the synthesis and/or purification of preferably fluorinated organic compounds such as carboxylic acids, carboxylic acid chlorides and derivatives such as esters thereof, starting from corresponding carboxylic acid chlorides containing acid fluorides or hydrolyzable fluoride, and alcohols under the catalytic action of &ldquo;onium&rdquo; salts of carboxylic acids, to obtain products which have a low fluoride content. Alternatively, an inorganic oxide adsorbent is utilized. The method is especially suitable for the synthesis of esters of trifluoroacetic acid, chlorodifluoroacetic acid, trifluoroacetoacetic acid and/or difluoroacetoacetic acid.

Synthesis of low-fluoride organic compounds

A process for preparing R113a from Rl13, and R123 from R123a or R123b by rearrangement over AlCl.sub.3, in which when the reaction mixture is heated sudden start-up of the reaction, which often causes large amounts of heat to be released and the reaction to run away, is prevented by using a specially activated AlCl.sub.3, which has been activated by means of a metal halide selected from the group consisting of NaF.multidot.nHF with 0&lt;n.ltoreq.2, AgCl and FeCl.sub.3. In addition to it being considerably easier to control the reaction, shorter reaction times for the rearrangement and a decrease in the amount of by-products which are formed, are observed.

Chlorofluoro(hydro)carbon conversion process

A process for preparing ketones, for example CF.sub.3 C(O)CH.sub.3, CF.sub.3 C(O)CH.sub.2 C(O)CF.sub.3 and CF.sub.3 C(O)CF.sub.2 H, in which .beta.-ketoesters are transesterified and decarboxylated using a carboxylic acid, for example trifluoroacetic acid, in the presence of a catalyst, particularly an 'onium' salt of a carboxylic acid or an effective amount of a proton-donating acid, preferably a sulfonic acid such as alkyl- or arylsulfonic acids, or a mineral acid. The process is advantageously carried out in the absence of water, so that no formation of acetals or hydrates occurs, and no dehydrating step is needed. The process is simple to carry out, and if transesterification is carried out with a sufficiently active carboxylic acid, for example with trifluoroacetic acid, the presence of an additional catalyst is unnecessary.

Process for preparation of ketones

A process for preparing R113a from R113, and R123 from R123a or R123b by rearrangement over AlCl.sub.3, in which when the reaction mixture is heated sudden start-up of the reaction, which often causes large amounts of heat to be released and the reaction to run away, is prevented by using a specially activated AlCl.sub.3, which has been activated by means of a metal halide selected from the group consisting of NaF.nHF with 0&lt;n.ltoreq.2, AgCl and FeCl.sub.3. In addition to it being considerably easier to control the reaction, shorter reaction times for the rearrangement and a decrease in the amount of by-products which are formed, are observed.

Chlorofluoro (hydro) carbon conversion process

Process for the preparation of 1,1,1,2-tetrafluoroethane by reaction of hydrogen fluoride with a trihaloethylene according to which trifluoroethylene is chosen as trihaloethylene and the reaction is carried out in the liquid phase.

Process for the preparation of 1,1,1,2-tetrafluoroethane

A method of preparing CH.sub.2 FCF.sub.3 from fluorodichloro-ethylene using a catalytically active niobium, tantalum or molybdenum fluorosulfonate compound or a catalyst mixture which comprises a niobium, tantalum or molybdenum halide and a sulfonic acid derivative.

Method of preparing 1,1,1,2-tetrafluoroethane

A process for working up the hydrogen fluoride phase of reaction mixtures from fluorination reactions comprising contacting the hydrogen fluoride phase with oleum in order to obtain dried hydrogen fluoride, which can be recycled to the fluorination reaction.

Process for working up a hydrogen fluoride phase from a fluorination

A process for preparing fluorine-containing ethane derivatives using hydrogen fluoride and a catalytically active formulation comprising a tantalum fluorosulfonate compound or a niobium fluorosulfonate compound is described. The process is particularly suitable for preparing ethane derivatives which contain a CF.sub.3 group, for example for preparing CF.sub.3 CHCl.sub.2 (R123) from perchloroethylene.

Process for preparing fluorine-containing ethane derivatives

A process for preparing fluorine-containing ethane derivatives using hydrogen fluoride and a catalytically active formulation comprising a tantalum fluorosulfonate compound or a niobium fluorosulfonate compound is described. The process is particularly suitable for preparing ethane derivatives which contain a CF.sub.3 group, for example for preparing C.sub.3 CHCl.sub.2 (R123) from perchloroethylene.

A method of preparing fluorine-containing ethane derivatives using a catalyst mixture which comprises a metal halide and a sulfonic acid derivative is described. The method is particularly well suited for preparing CF.sub.3 CHCl.sub.2 (R123) from perchloroethylene and for preparing CF.sub.3 CH.sub.2 F (R134a) from trifluoroethylene.

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Garbsen, Germany

Johannes Eicher