Method for producing aromatic beads

Cleaning compositions for solid surfaces – auxiliary compositions – With oxygen – halogen – sulfur – or nitrogen containing or...

Reexamination Certificate

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C510S446000

Reexamination Certificate

active

06562769

ABSTRACT:

FIELD OF THE INVENTION
This invention relates to the production of perfume shaped bodies, more particularly perfume beads, which may be incorporated in detergents and laundry treatment and aftertreatment compositions and which provide the treated laundry with a perfume-enhancing effect. The present invention also relates to detergents containing the shaped bodies produced in accordance with the invention and to the use of the shaped bodies produced in accordance with the invention for perfuming wash liquors.
BACKGROUND OF THE INVENTION
In the washing, treatment and aftertreatment of laundry, it is now common practice to add small quantities of perfume to the detergents and aftertreatment compositions in order to provide the wash liquor itself and also the laundry treated with the wash liquor with a pleasant fragrance. In addition, besides color and appearance, the perfuming of detergents and aftertreatment compositions is an important aspect of the aesthetic product impression and an important factor in the consumer deciding for or against a certain product. For perfuming, the perfume may, either be directly incorporated in the detergent/composition or may be added to the wash liquor in an additional step. The first method determines a certain product characteristic whereas, in the second method, the consumer is able individually to chose his/her perfume from the various perfume variants on offer—comparable with the choice of an eau-de-toilette or an aftershave lotion.
Accordingly, perfume shaped bodies and processes for perfuming wash liquors are widely described in the prior art. Thus, DE 41 33 862 (Henkel) discloses tablets containing carrier materials, perfumes and optionally other typical detergent ingredients, sorbitol and in addition 20 to 70% by weight of an effervescent system of carbonate and acid being used as the carrier material. These tablets, which may be added for example in the after-rinse cycle or fabric softening cycle of a domestic washing machine, contain about 3 to 15% by weight and preferably 5. to 10% by weight of perfume. In view of their high disintegrator content, the tablets in question are sensitive to atmospheric moisture and have to be stored in a suitably protected form.
DE 39 11 363 (Baron Freytag von Loringhoven) describes a process for the production of a perfume-enriched wash liquor and a perfume addition medium suitable for this purpose. The addition medium present in the form of capsules or tablets contains the perfume together with an emulsifier in liquid form (capsules) or fixed to fillers and carriers (tablets), sodium aluminium silicates and cyclodextrins being mentioned as carriers. The perfume content of the capsules or tablets is at least 1 g for a capsule or tablet volume of more than 1 cm
3
. Tablets or capsules containing more than 2.5 g of perfume for a volume of at least 5 cm
3
are preferred. For storage, tablets or capsules of the type in question have to be provided with a gas- and water-tight covering layer to protect the ingredients. The document in question does not provide any further particulars of the production of physical properties of suitable tablets.
International patent application WO 94/25563 (Henkel-Ecolab) describes a process for the production of detersive shaped bodies using the microwave technique which does not involve any high-pressure tabletting. The tablets produced by this process are distinguished by an extremely dissolving rate or disintegration rate coupled with fracture resistance without any need for a disintegrator. At the same time, they are stable in storage and can be stored without any additional precautions. Tablets with a perfume oil content of 1 to 3% by weight typical of detergents can also be produced by this process. In general, perfume oils are readily volatile and, accordingly, could even evaporate on exposure to microwave radiation. If, therefore, relatively high levels of readily volatile liquid substances are to be used, a two-component system consisting of a component produced by the microwave technique and a component containing the sensitive liquid substances is described.
Particulate additives for perfuming wash liquors and for use in detergents and processes for their production are described in International patent applications WO 97/29176 and WO 97/29177 (Procter & Gamble). According to the teaching of these documents, perfume is added to porous carrier materials (for example sucrose in admixture with zeolite X) and, finally, a coating material (carbohydrates) is applied and the required particle size distribution is established.
Earlier German patent application 197 35 783.0 (Henkel) describes highly concentrated perfume shaped bodies containing carrier material(s), 20 to 50% by weight of perfume(s) and optionally other auxiliaries and additives typical of detergents, at least 50% by weight of the shaped bodies—after subtracting the quantity of perfume—consisting of fatty acids and fatty acid salts. These perfume shaped bodies are suitable both for perfuming detergents and for perfuming laundry in a washing machine.
A process for applying perfumes to laundry in a washing machine is described in DE 195 30 999 (Henkel). In this process, a perfume-containing shaped body produced by exposure to microwave radiation is used in the final rinse cycle of a washing machine. According to the teaching of this document, the preferably spherical shaped bodies with diameters above 3 mm and bulk densities of up to 1100 g/l are produced by introducing a mixture of predominantly water-soluble carrier materials, hydrated substances, optionally surfactants and perfume into suitable molds and sintering the mixture by exposure to microwave radiation. The perfume contents of the shaped bodies are between 8 and 40% by weight and the carrier materials used include starches, silicas, silicates and disilicates, phosphates, zeolites, alkali metal salts of polycarboxylic acids, oxidation products of polyglucosans and polyaspartic acids. A crucial pre-condition of the process described in this document for producing shaped bodies is that at least partly bound water should be present in the mixture sintered by microwaving to form shaped bodies, i.e. the starting materials should be at least partly present in hydrated form.
The solutions proposed in the cited prior art require either additional barrier layers or coating layers to fix the perfume to the carrier or are not equally suitable for perfuming detergents and for direct use solely as a detergent, for example in the final rinse cycle of a washing machine. In addition, there is no reference in the cited prior art to perfume-enhancing effects on the treated laundry.
BRIEF DESCRIPTION OF THE INVENTION
The problem addressed by the present invention was to provide a process for the production of perfume shaped bodies, more particularly perfume beads, which would contain up to 15% by weight of perfume, but which nevertheless would not have to be provided with a gas-tight and water-tight coating layer or pack for storage in order to protect the ingredients or to prevent losses of perfume in storage. Another problem addressed by the present invention was to provide a perfume supply form which could both be incorporated as a compound in standard detergents and also directly used for individually choosing perfume in domestic washing processes and which would create a perfume-enhancing impression on the treated laundry.
Accordingly, the present invention relates to a process for the production of perfume shaped bodies, more particularly perfume beads, with bulk densities above 700 g/l, characterized in that a solid and substantially water-free premix of
a) 65 to 95% by weight of carrier(s),
b) 0 to 10% by weight of auxiliary(ies) and
c) 5 to 25% by weight of perfume
is subjected to granulation or press agglomeration.
DETAILED DESCRIPTION OF THE INVENTION
In the context of the present invention, the expression “substantially water-free” is understood to apply to a state in which the content of liquid water, i.e. water which is not present as water of hydration

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