Patent GB-928594-A (GB)
Title: Manufacture of perfumes
IPC: C11B9/02
Filed: 1959-09-21
Abstract: A method of manufacturing concentrates from perfumery materials (which are chosen from raw naturally occurring organic materials and their concretes and absolutes) comprises treating the perfumery materials with a solvent which consists of at least one fluorinated hydrocarbon propellant, liquefied by the maintenance of sufficient pressure, and separating the resulting liquid solution from that portion of the perfumery material treated which does not dissolve in the solvent.  The concretes referred to are crude extracts of the raw naturally occurring organic materials, while the absolutes are carefully prepared alcoholic extracts of the concretes.  The fluorinated hydrocarbon propellants are fluorinated or chlorofluorinated hydrocarbons which may be used as propellants in aerosol packages, examples being CCl3F, CCl2F2, CHClF2, CCl2F.CClF2, C2ClF5, CH3.CClF2, dichloro-tetrafluoro-ethanes, octafluoro-cyclobutane and materials sold under the trade name "Isotron".  It is stated that the fraction of the perfumery material which remains in solution in the propellant is characterized by the distinctive odour of the perfume oil and by an increased concentration of the active nerve-stimulating ingredient.  The perfumery materials treated may be chosen from plant raw materials and their extracts, animal glands and their extracts and the exudates or resins and their extracts.  The perfumery material may be agitated with the liquid solvent or the liquid solvent may be circulated through the perfumery material; the perfumery material may be given one, two or more extractions.  If desired, a series of fluorinated hydrocarbon solvents may be used successively on any given perfumery material.  Thus, (a) the perfumery material may be extracted with one fluorinated hydrocarbon solvent and then the concentrate from the extract may be treated with another fluorinated hydrocarbon solvent or (b) the perfumery material may be treated with one fluorinated hydrocarbon solvent and the residue treated with another fluorinated hydrocarbon solvent.  The liquid solution obtained by the method of the invention may be cooled to separate wax or other precipitate and then filtered; the cooling may be effected by evaporation of the fluorinated hydrocarbon solvent.  The concentrates obtained may be refined to very pure absolutes by extraction with ethyl alcohol.  If desired the concentrates may be utilized in aerosol packages, either in the same solvent as was used for extraction or in a different propellant.  In the examples, the manufacture of concentrates from flowers (hyacinth, lilac, lily of the valley, gardenia, rose or honeysuckle), leaves (grass or lilac), resins (Peru balsam, resinoid castoreum or styrax), essences (costus) and absolutes (abs. Resinoid Castoreum, abs. Summortelle, abs. Oak Moss, abs. Resin Styrax, abs. Orange Flowers, abs. Jasmin, abs. Civet, abs. Lavender or abs. Resinoid Benzoin) is described.  In a further example, a concentrate is manufactured from a perfume oil made up of resinoid labdanum vetiver Bourbon, sandalwood, patchouly, coumarin, abs. Oak Moss and bergamot.