FI85601C - FLYTANDE OCH BLEKANDE TVAETTMEDELSKOMPOSITION FOER TVAETTINRAETTNINGAR. - Google Patents

Description

1 85601

This invention relates to anhydrous liquid heavy duty laundry detergents for laundries.

According to one embodiment of the present invention, a highly effective and stable anhydrous liquid heavy duty detergent for laundries is prepared by dispersing a solid builder salt, sodium perborate monohydrate and a solid activator to a perborate 10 microns, e.g., an average particle size of 2-10 microns or even smaller, such as 1 micron. It is desirable that the milled product contain less than 20% by weight (more preferably less than 10% by weight) of suspended particles having diameters greater than 10 microns.

It will be appreciated that by reducing the particle size by grinding, the fresh reactive surface will be exposed and the surface area available for the reaction will increase. Also, the energy used in a fine grinding operation necessarily results in local thermal: ·. ·. space rises in the mixture to be ground (despite the fact that the grinding mill has been cooled, e.g. during running during grinding-; rack cold water through the mill casing). Nevertheless, the compositions of the invention are very stable and show little or no reduction in bleaching activity already during Hanna or during storage.

'In a grinding operation, it is desirable that the proportion of solids *: ··: be high enough (e.g., at least about 40% such as about 50%) so that the solid particles are in contact with each other and are not, more specifically, liquid nonionic surfaces. · · • · · 2 85601 protected from each other by the active substance. Mills that use grinding balls (ball mills) or similar moving grinding elements have given very good results. Thus, a laboratory batch chopper equipped with 8 mm diameter steatite grinding balls can be used. For larger scale work, a continuous mill with 1 mm or 1.5 mm diameter grinding balls operating in a very small gap between the body and a relatively high speed rotor (e.g. a CoBall mill) can be used; when using such a mill, it is desirable to first feed a mixture of nonionic surfactant and solids through a mill that does not grind so finely (e.g. a colloid mill) to reduce the particle size to less than 100 microns (e.g. to about 40 microns) before is ground in a continuous ball mill to an average particle size of less than about 10 microns in diameter.

It is desirable that the solid builder salt be an alkali metal polyphosphate such as sodium tripolyphosphate ("TPP"). Other suitable polyphosphates include pyrophosphates such as tetrasodium pyrophosphate and metaphosphates. All or part of the polyphosphate may be replaced by one or more detergent builder salts, such as alkali metal carbonates or bicarbonates, silicates, or organic builders, such as polycarboxylates. Typical suitable excipients are mentioned in U.S. Patents 4,316,812; 4,264,466 and 3,630,929.

The preferred activator is tetraacetylethylenediamine ("TAED"). Another suitable activator is glucose pentaacetate. Other suitable activators are mentioned in U.S. Patents 4,264,466 or paragraph 1 of U.S. Patent 4,430,244. Polyacylated compounds are preferred activators.

. ···. The essential features of the invention are set out in the appended claims.

The following examples are provided to further illustrate this invention in this patent application. All proportions are by weight unless otherwise indicated.

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Example 1

The following compounds A and B were both ground for 30 minutes at room temperature in a Wieneroto W-1.S grinder with 8 mm diameter steatite spheres as a liquid suspension with an average particle size of less than about 10 microns in each case.

Shares A B

Non-ionic surfactant 35 32.57

Acid-treated non-ionic surfactant 16 16 TPP 30 30

Ethylenediamine tetramethylene-phosphoric acid sodium salt (EDITEMPA) 1.5 1.5 Copolymer of methacrylic acid and maleic anhydride fully converted to the sodium salt form (Sokalan CP 5) 4 4

Sodium carbonate 2.5 2.5

Sodium perborate monohydrate (NaB03H2O) 4.5: Sodium perborate tetrahydrate - 6.93 0 .: TAED 5 5: Stilbene 4-type optical brighteners 0.5 0.5. . Enzyme Porridge (Protease Precipitated in Nonionic Surfactant) 1 1 - Each composition contains 0.72% active O 2 and has a non-bound water content of less than 1%. After 48 hours of maturation at 35 ° C, composition A is still liquid, while composition B has become practically solid (its: yield stress has increased to more than 20 Pascals). After 5 days of ripening at 35 ° C,. analysis of useful peracetic acid shows that * * in practice the loss of TAED in grinding and maturation is 7% for composition A and 45% for composition B.

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The nonionic surfactant used in the example is a mixture of equal parts of: (a) a relatively water-soluble nonionic surfactant which forms a gel when mixed with water at 25%, especially a C 1 -C 4 alkanol alkoxylated to give ethylene oxide. and 5 propylene oxide units per alkanol unit and (b) a less water-soluble nonionic surfactant, especially a C 1-3 c 1-5 alkanol alkoxylated to give 4 ethylene oxide and 7 propylene oxide units per alkanol unit.

The acid-treated nonionic surfactant is a half ester of succinic acid and a nonionic surfactant (especially an ethoxylated C12-C15 alkanol having about 5 ethylene oxide units per alkanol molecule). e.g. at 60 ° C) preferably in the presence of a small amount of catalyst such as pyridine.The resulting acid-terminated product acts as an antigenic surfactant in the compositions.It lowers the temperature at which the nonionic surfactant forms a gel with cold water and thus helps disperse the compositions in automatic home washing machines. Other carboxylic acid materials soluble in the non-ionic surfactant can be used for this purpose.

TPP is a mixture of anhydrous TPP and a small amount of TPP hexahydrate so that the content of chemically bound water is about 3%, which corresponds to about one H 2 O per molecule of pentasodium tripolyphosphate. Such TPP can be prepared by treating anhydrous TPP with a limited amount of water. The presence of hexahydrate reduces the rapid dissolution of TPP in the wash bath and prevents deposition. One suitable TPP is sold under the name Thermpho-NW; the particle size of this TPP at acquisition is approximately 400 microns; its phase I content is about 60%.

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When preparing the mixture, it is desirable to add solids to the nonionic surfactant prior to grinding, with TPP added last.

The mixture easily disperses in cold water in automatic washing machines. Its specific gravity is about 1.25. It gives excellent washing results when using doses of about 100 grams per wash load (compared to 170 grams per wash load for standard heavy-duty detergent powders) in conventional European household washing machines (using about 20 liters of water per wash) where the water is heated to about 60 ° C.

Example 2

The powdered composition is prepared according to Example 1 from the following ingredients in said proportions:

Non-ionic surfactant 40.8 TPP 49.8

Ethylenediaminetetraacetic acid 1.2 TAED 4.5

Sodium perborate monohydrate 3.6

Hydroxylamine sulphate 0,1

Hydroxylamine sulfate prevents the unwanted loss of bleaching ability caused by an enzyme in dirty clothing, catalase.

As is known, nonionic synthetic surfactants are identifiable by the organic hydrophobic group and the organic hydrophilic group present in them and are typically prepared by condensing an organic aliphatic or hydrophobic aromatic alkyl compound with ethylene oxide (hydrophilic in nature). Virtually any hydrophobic compound having a carboxy, hydroxy, amido or amino group and free hydrogen attached to nitrogen can be condensed with ethylene oxide or its polyhydration product, poly (ethylene glycol), to form a nonionic detergent.

The length of the hydrophilic or polyoxyethylene chain can be easily adjusted to achieve the desired balance between the hydrophobic and hydrophilic groups. Typical suitable liquid nonionic surfactants are mentioned in U.S. Patents 4,316,812 and 3,630,929, as well as in the review and list of nonionic surfactants in Kirk-Othmer's "Encyclopedia of Chemical Technology", 3rd Edition, Vol. 22 (1983), pages 360-379.

The activator generally acts with the peroxide compound to form a peroxyacid bleach in the wash water. It is desirable to add an insulating agent having a high complexing ability to prevent any undesired reaction between such peroxyacid and hydrogen peroxide in the washing solution in the presence of metal ions. Such an insulator is an organic compound capable of forming a complex with Cu 2+ ions such that the stability constant (pK) for the complex is 6 or greater at 25 ° C in 0.1 mol / liter ionic water, where pK is conventionally determined by the formula: pK = -log K, where K; is the equilibrium constant. Thus, for example, the pK values for the m: complexation of copper ions with NTA and EDTA under said conditions: *** are 12.7 and 18.8, respectively. Suitable insulating agents include nitrilotriacetic acid (NTA); ethylenediaminetetraacetic acid (EDTA); diethylenetriaminepentaacetic acid (DETPA); diethylenetriamine pentamethylene phosphoric acid (ETPMP); and sodium salts of ethylenediaminetetramethylenephosphoric acid (EDITEMPA).

*. Other ingredients that may be added to the compositions include enzymes (e.g., proteases, amylases, or lipases, or mixtures thereof); optical brighteners, anti-depot agents (e.g. sodium carboxymethylcellulose), colorants (e.g. pigments or dyes), etc.

»* · • * · • ·

The composition may also contain an inorganic insoluble thickener or a very large surface area dispersant 7,856,011 or other high pore volume carrier materials mentioned in U.S. Patent 3,630,929 in 0.1-10% proportions, e.g. 1-5%. However, it is desirable that the compositions be substantially free of such compounds and silicates, as it has been found that silica and silicates contribute to the undesired degradation of peroxyacid formed in the wash bath.

Typical proportions of ingredients in the compositions of the invention are as follows:

Suspended detergent base in the range of about 10-60%, such as about 20-50%, e.g. about 25-40%.

A liquid phase containing a nonionic surfactant (and optionally, a dissolved carboxylic acid material) in the range of about 30-70%, such as about 40-60%; this phase may also contain a solvent such as a glycol, e.g. polyethylene glycol (e.g. "PEG 400") or hexylene glycol.

The carboxylic acid anti-gelling agent ranges from 0.01 to 1 part per part of nonionic surfactant, such as about 0.05 to 0.6 parts, e.g., about 0.2 to 0.5 parts.

Sodium perborate monohydrate ranges from about 2-15%, such as about 4-10%.

Activator in the range of 1-8, such as about 3-6%.

The proportion of unbound moisture in the composition should be less than about 2%, preferably less than about 1%, such as about 1/2% or less.

Since it is most convenient and efficient to grind all the solid ingredients together, it is within the broader scope of the invention to grind separate suspensions of individual ingredients or groups of ingredients and combine these after such grinding.

In this patent application, all proportions are by weight unless otherwise indicated. Atmospheric pressure is used in the examples unless otherwise noted.

It is to be understood that the above detailed examples are merely illustrative of the invention and that variations may be made therein without departing from the scope of the invention.

Claims (3)

9 85601 A substantially anhydrous liquid heavy duty laundry detergent composition for laundries, characterized in that it comprises solid sodium perborate monohydrate particles, solid perborate activator particles and solid excipient salt particles co-dispersed in an active ingredient, all dispersed in an active ingredient. less than about 10 microns after milling, said composition being substantially free of silica and silicates, and that all particles are initially at least 40 microns in particle size prior to milling, and that said builder salt comprises 10-60% of the particles, 2-15% of sodium perborate monohydrate and 1-15% of activator. 8%. Composition according to claim 1, characterized in that the amount of said enhancer salt is about 25-40%. Composition according to Claim 1 or 2, characterized in that the activator comprises tetraacetylethylenediamine and the builder salt comprises pentasodium tripolyphosphate. 10 85601