Cleaning compositions for solid surfaces – auxiliary compositions – Cleaning compositions or processes of preparing – Enzyme component of specific activity or source
Reexamination Certificate
1999-06-10
2002-02-26
Kopec, Mark (Department: 1751)
Cleaning compositions for solid surfaces, auxiliary compositions
Cleaning compositions or processes of preparing
Enzyme component of specific activity or source
C510S226000, C510S300000, C510S320000, C510S348000, C510S349000, C510S441000, C510S474000, C510S530000
Reexamination Certificate
active
06350728
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to enzyme granules, to a process for their production and to the use of the granules in solid detergents.
2. Discussion of Related Art
Enzymes, particularly proteases, are widely used in detergents, laundry aids and cleaning products. Normally, the enzymes are not used in the form of concentrates, but in the form of mixtures with a diluent and carrier material. If enzyme preparations such as these are mixed with standard detergents, a considerable reduction in enzyme activity can occur during storage, particularly if bleaching-active compounds are present. Application of the enzymes to carrier salts accompanied by granulation in accordance with DE-OS 16 17 190 or by bonding with nonionic surfactants in accordance with DE-OS 16 17 188 does not product a significant improvement in storage life because the sensitive enzymes in mixtures such as these are generally present on the surface of the carrier. Although the stability of the enzymes in storage can be significantly increased by encapsulating the enzymes with or embedding in the carrier material and subsequently converting them into the desired particle form by extrusion, pressing and marumerizing as described, for example, in DE-PS 16 17 232, in DE-OS 20 32 768 and in DE-ASS 21 37 042 and 21 37 043, enzyme preparations of this type show unsatisfactory solubility properties. The undissolved particles can become caught up in the washing and can soil it or can be discharged into the wastewater without being used. Although the encapsulating agents known from DE-OS 18 03 099, which consist of a mixture of solid acids or acidic salts and carbonates or bicarbonates and which disintegrate on addition of water, improve the solubility of enzyme preparations, they are extremely sensitive to moisture and, accordingly, require additional protective measures.
EP 168 526 describes enzyme granules containing starch swellable in water, zeolite and a water-soluble granulation aid. This document discloses a process for the production of such formulations which essentially comprises concentrating a fermenter solution freed from insoluble constituents, introducing the additives mentioned, granulating the resulting mixture and optionally coating the granules with film-forming polymers and dyes. The process with the proposed additive mixture is advantageously carried out with fermentation solutions which have been concentrated to a relatively high dry matter content, for example of 55% by weight. In addition, the granules thus produced have such a high dissolving or disintegration rate under washing conditions that they disintegrate relatively quickly, to some extent even in storage, and the enzymes are deactivated.
International patent application WO 92/11347 describes enzyme granules for use in granular detergents which contain 2% by weight to 20% by weight of enzyme, 10% by weight to 50% by weight of swellable starch, 5% by weight to 50% by weight of water-soluble organic polymer as granulation aid, 10% by weight to 35% by weight of cereal flour and 3% by weight to 12% by weight of water. Additives such as these enable the enzymes to be processed without significant losses of activity.
International patent application WO 93/07263 relates to enzyme-containing granules consisting of a water-soluble or water-dispersible core coated with a vinyl polymer to which a layer of enzyme and vinyl polymer has been applied, the granules having an outer coating of vinyl polymer. The outer coating may also contain pigments. However, the multilayer structure of these enzyme granules makes them relatively difficult to produce.
International patent application WO 95/02031 describes coated enzyme granules of which the coating layer consists of a coating system containing 30% by weight to 50% by weight of fine-particle inorganic pigment, 45% by weight to 60% by weight of an alcohol solid at room temperature with a melting point of 45° C. to 65° C., up to 15% by weight of emulsifier for the alcohol, up to 5% by weight of dispersant for the pigment and up to 3% by weight of water. In view of the presence of relatively large quantities of water-insoluble fatty alcohol, enzyme granules of this type can lead to residue problems when dissolved in water because the presence of the emulsifier is often not sufficient to dissolve the organic components of the coating system.
International patent application WO 93/07260 discloses a process for the production of dust-free enzyme granules which comprises spraying a fermentation broth onto a hydratable carrier material, spraying on a solution of certain coating materials, including fatty acid esters, alkoxylated in alcohols, polyvinyl alcohol, polyethylene glycol, sugar and starch, and evaporating the solvent.
The coating materials used in the documents cited above for the outermost coating layer are normally applied to the enzyme granules in the form of an aqueous dispersion in a fluidized bed dryer. On the one hand, this involves the danger of destruction of at least the surface of the granules by dust abrasion in the fluidized bed which leads to an increased percentage of extremely fine-particle material in the enzyme granules which cannot be used for incorporation in normal particulate detergents because they are not uniformly distributed in the mixture formed and, in addition, enzyme-containing fine dust can lead to allergic reactions in consumers. Accordingly, it is desirable to keep the percentage of fine particles in the enzyme granules as small as possible so that very few have to be removed by sieving or air separation. On the other hand, the use of the coating material in dissolved form is a disadvantage because the solvent applied to the enzyme granules has to be removed again in a separate step.
Accordingly, the problem addressed by the present invention was to develop a coating system which, when uniformly applied to enzyme-containing granules, would counteract surface destruction of the granules, would increase the storage stability of the enzyme by protective coating of the granules as a whole, would enable any color inherent in the uncoated enzyme granules to be covered and would eliminate any potentially troublesome odor of the uncoated granules, probably by reducing the diffusion of the components responsible to the surface of the enzyme granules.
According to the invention, the problem stated above has been solved by enzyme granules suitable for incorporation in detergents, especially particulate detergents, containing enzyme and organic and/or inorganic Garner material and a uniform outer pigment-containing coating layer, characterized in that the outer coating layer consists of a coating system containing 5% by weight to 70% by weight and, more particularly, 10% by weight to 50% by weight of fine-particle inorganic water-insoluble pigment, 45% by weight to 90% by weight and, more particularly, 50% by weight to 85% by weight of a water-soluble organic substance solid at room temperature with a melting point in the range from 40° C. to 70° C. and up to 20% by weight, preferably up to 10% by weight and more preferably from 1% by weight to 5% by weight of flow improvers.
The present invention also relates to a process for the production of enzyme granules suitable for incorporation in particulate detergents with a mean particle size of 0.8 mm to 1.4 mm by extruding an enzyme compound formed by mixing an aqueous enzyme liquid, which may be a concentrated fermentation broth optionally freed from insoluble constituents by microfiltration, with an inorganic and/or organic carrier material as additive, spheronizing the extrudate in a spheronizer, optionally drying and applying an outer coating layer, characterized in that an outer coating layer of a coating system containing 5% by weight to 70% by weight and, more particularly, 10% by weight to 50% by weight of fine-particle inorganic water-insoluble pigment, 45% by weight to 90% by weight and, more particularly, 50% by weight to 85% by weight of a water-soluble organic substance solid at
Kottwitz Beatrix
Paatz Kathleen
Pichler Werner
Raehse Wilfried
Henkel Kommanditgesellschaft Auf Aktien (KGaA)
Jaeschke Wayne C.
Kopec Mark
Mruk Brian P.
Murphy Glenn E. J.
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