Catalysis in halogen exchange reactions
AssigneeAlbemarle Corporation
InventorsBruce C. Berris, Chi-Hung Cheng
Life of this patent
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Abstract
Impure tetra(dihydrocarbylamino)phosphonium halide is contacted with a liquid cyclic ether to dissolve the phosphonium halide and leave at least a portion of the impurities comprising at least quaternary ammonium halide or an amidophosphoxide remaining in the solid state. The solids and the liquid phase are separated from each other, an anhydrous non-solvent for the tetra(dihydrocarbylamino)phosphonium halide is mixed with the separated liquid phase to precipitate the tetra(dihydrocarbylamino)phosphonium halide, which is then separated from the liquid phase. The so-treated tetra(dihydrocarbylamino)phosphonium halide is more efficient as a catalyst for halogen exchange reactions than the original untreated tetra(dihydrocarbylamino)phosphonium halide.
Claims13
A halogen exchange process which comprises heating a mixture formed from ingredients comprising (i) at least one finely-divided essentially anhydrous alkali metal fluoride, (ii) at least one haloaromatic compound having at least one halogen atom of atomic number greater than 9 on an aromatic ring, and (iii) an aminophosphonium catalyst, at one or more reaction temperatures at which at least one said halogen atom of said haloaromatic compound is replaced by a fluorine atom, wherein said catalyst ingredient is a tetra(dihydrocarbylamino)phosphonium halide which has been subjected to a pretreatment process which comprises:
- a) contacting an impure tetra(dihydrocarbylamino)phosphonium halide with a liquid cyclic ether under conditions effective to dissolve the tetra(dihydrocarbylamino)phosphonium halide and leave at least a portion of said impurities remaining in the solid state;
- b) separating the solids and the liquid phase of a) from each other;
- c) mixing an anhydrous non-solvent for the tetra(dihydrocarbylamino)phosphonium halide with the liquid phase from b) to precipitate the tetra(dihydrocarbylamino)phosphonium halide;
- and
- d) separating the precipitated tetra(dihydrocarbylamino)phosphonium halide solids and the liquid phase of c) from each other.
Dependencies are inferred from the claim text.