Method of preparing stable liquid perfume material mixtures with

Perfume compositions – Perfume compositions – With preservative – stabilizer – or fixative

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512 17, 512 21, A61K 746

Patent

active

055189970

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BRIEF SUMMARY
This application is a 371 of PCT/EP 93/00014, filed Jan. 7, 1993.
The invention relates to a novel method of preparing homogeneous liquid mixtures of solid perfume materials and the use of these mixtures for preparing solvent-free ready-made perfume formulations.
For application reasons (e.g. stability, odor intensity or substantivity), solids are being increasingly used in the modern perfume industry. These substances are indispensable in particular for perfumes for detergents and softeners, since these products are subjected to considerable stresses during preparation, in the market and subsequently during processing. The fragrance of these products is not only of decisive importance in decisions for or against the purchase of a certain product but also accompanies the product from production through storage to use. In addition, the laundry which has been washed or treated with a softener must have a pleasant odor--even after weeks of storage--in order to meet the high quality expectations of the buyer of a branded article.
The problem of these extreme quality requirements with regard to a modern ready-made perfume is illustrated by the fact that about 99.9% of the industrial perfume used "disappears" in the wastewater in the washing or softening process, while only about 0.1% is absorbed by the washed laundry.
For mixing perfume materials, the chemically stable, liquid components are usually initially introduced, as a rule with the addition of further solvents, such as dipropylene glycol (DPG) and diethyl phthalate (DEP) and the like, and the solid components are added gradually with vigorous stirring, the mixture being heated externally or by means of internal heating coils until the solids melt or go into solution. Since the heating surfaces have to be heated to relatively high temperatures in order to achieve sufficient heat transport, a certain amount of damage occurs at these heating surfaces as a result of overheating, particularly in the case of sensitive substances. Moreover, the vigorous mixing results in greater contact with air, so that it is necessary to work under an expensive inert gas atmosphere in order to avoid damage by oxidation.
After dissolution of the solids, the mixture is cooled. Sensitive, readily volatile or chemically unstable materials are then added with gentle stirring, and stirring is continued until the mixture is homogeneous. This method is considerably time-consuming since a disadvantageous solid/liquid mixing ratio is initially present or a time-consuming heating and cooling process is necessary in between and the use of additional solvents not only incurs costs and unnecessarily increases the processing quantities but also additionally pollutes the environment.
DE-A 39 22 389.2 describes a process in which the introduction of the solid materials into the liquid substances is carried out with simultaneous addition of an inert gas to the stirring zone, with the result that the damage which occurs due to overheating and mechanical stressing of the sensitive materials is completely avoided.
However, it proves to be disadvantageous that the proportion of solid substances in conventional perfume formulations is in fact comparatively high and that such substances may be difficult to meter and convey and furthermore, as powders, occupy large volumes, giving rise to transport and storage problems. As a remedy, such substances are in some cases therefore dissolved in suitable solvents and thus converted into the liquid state, with the result that metering and handling are simplified. However, this has the disadvantage that the total amount is greatly increased due to the amounts of solvent, with the result that transport and storage once again become expensive and in addition solvents are introduced into the formulation, which not only constitute a cost factor themselves but are also to be classified as causing environmental pollution.
The above-mentioned solid contents of 20-60% of the total perfume mixture are composed of, in each case, about 20 different materials, which in

REFERENCES:
patent: 2875131 (1959-02-01), Carpenter et al.
patent: 3548006 (1970-12-01), Siriabine
patent: 4650603 (1987-03-01), Sprecker
Arctander, "Perfume & Flavor Chemicals", (1969) pp. 13, 41, 340, 496, 1654.

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