Cleaning compositions for solid surfaces – auxiliary compositions – Cleaning compositions or processes of preparing
Reexamination Certificate
1999-03-22
2002-04-30
Naff, David M. (Department: 1651)
Cleaning compositions for solid surfaces, auxiliary compositions
Cleaning compositions or processes of preparing
C435S176000, C435S177000, C435S178000, C435S179000, C435S180000, C435S187000, C435S188000, C510S392000, C510S530000
Reexamination Certificate
active
06380140
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, more particularly particulate detergents.
2. Discussion of Related Art
Enzymes, particularly proteases, are widely used in detergents, laundry aids and cleaning products. In general, the enzymes are used not 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 or aqueous solutions of cellulose ethers in accordance with DE-OS 17 67 568 does produce 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 them 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.
Another disadvantage of the preparation mentioned above is that the enzymes can only be processed in the form of dry powders. The fermenter broths typically formed in the production of the enzyme preparations cannot be used in this form, but instead have to be freed from water beforehand. The same is also a precondition in processes where only readily soluble carrier materials, such as sugars, starch and cellulose ethers, are used as binders in the production of enzyme preparations.
EP 168 526 describes enzyme granules containing starch swellable in water, zeolite and water-soluble granulation aids. 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 and granulating the resulting mixture. 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 are highly soluble and disintegrate rapidly under washing conditions so that the granules disintegrate relatively quickly, to some extent even in storage, and the enzymes are deactivated.
European patent EP 0 564 476 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. The storage stability of the enzymes in the granules is also satisfactory. It is also known from this document that sodium carboxymethyl cellulose reduces the disintegration and dispersion rate of the granules in cold wash liquors whereas the addition of relatively high molecular weight polyethylene glycol can vary this effect by increasing the dissolving rate. However, the enzyme granules described in the document in question do not always have such a high disintegration rate that, where they are used in detergents, enough enzyme is present in the wash liquor to eliminate enzymatically removable soils even in the initial phase of machine washing. The use of a special granulation auxiliary system containing alkali metal carboxymethyl cellulose with degrees of substitution of 0.5 to 1 and polyethylene glycol and/or alkyl or alkenyl polyethoxylate in certain quantities was proposed in German patent application DE 43 10 506 as the starting point for a further improvement in solubility. Enzyme granules produced using this granulation auxiliary system do not provide an entirely satisfactory solution to the problem of dispensing behavior in domestic washing machines where the dispensing compartment is not optimally shaped or positioned.
The problem addressed by the present invention was further to develop the attempt to solve these problems through the granulation aid and further to improve the powder properties, more particularly the solubility and dispensing behavior of known products, further to increase the stability in storage both of the enzymes and of the granules containing them and further to reduce losses of activity during processing of the enzymes. According to the invention, this problem has largely been solved by a special granulation auxiliary system.
SUMMARY OF THE INVENTION
The present invention relates to enzyme granules suitable for incorporation in detergents, particularly particulate detergents, containing enzyme and inorganic and/or organic carrier material and granulation auxiliary, characterized in that they contain a phosphated, optionally partly hydrolyzed starch as the granulation auxiliary. In the context of the invention, phosphated starch is understood to be a starch derivative in which the hydroxyl groups of the starch anhydroglucose units are replaced by the group —O—P(O)(OH)
2
or water-soluble salts thereof, more particularly alkali metal salts, such as sodium and/or potassium salts.
In the context of the invention, the mean degree of phosphation of the starch is understood to be the number of esterified oxygen atoms bearing a phosphate group per saccharide monomer of the starch averaged over all the saccharide units. The mean degree of phosphation of the phosphated starches preferably used is in the range from 1.5 to 2.5 because, where these starches are used, much smaller quantities are required to achieve a certain granule strength than where carboxymethyl cellulose is used. Partly hydrolyzed starches in the context of the present invention are understood to be oligomers or polymers of carbohydrates which may be obtained by partial hydrolysis of starch using conventional methods, for example acid- or enzyme-catalyzed methods. They are preferably hydrolysis products with average molecular weights of 440 to 500,000. Polysaccharides having a dextrose equivalent (DE) of 0.5 to 40 and, more particularly, in the range from 2 to 30 are preferred. The dextrose equivalent (DE) is a standard measure of the reducing effect of a polysaccharide by comparison with dextrose which has a DE of 100. Both maltodextrins (DE 3-20) and dry glucose sirups (DE 20-37) and so-called yellow dextrins and white dextrins with relatively high average molecular weights of about 2,000 to 30,000 are also suitable after phosphation.
DETAILED DESCRIPTION OF THE INVENTION
In one preferred embodiment, the enzyme granules contain 0.01% by weight to 25% by weight and, more particularly, 4% by weight to 20% by weight, expressed as dry matter, of enzyme, more particularly protease, lipase, amylase and/or cellulase, 50% by weight to 90% by weight of inorganic and/or organic carrier material and 1% by weight to 50% by weight of granulation auxiliary system containing the phosphated starch, the balance to 100% by weight being water.
Enzyme granules according to the invention preferably contain a m
Paatz Kathleen
Pichler Werner
Raehse Wilfried
Upadek Horst
Henkel Komm.nditgesellschaft Auf Aktien
Murphy Glenn E. J.
Naff David M.
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