DK165187B - STABILIZED, WATERABLE, BUILD-SUSTAINABLE, CLEAR, PHASE, FLUID, ENZYMENTIC DETERGENT AGENT AND WASHING PROCEDURE - Google Patents

Description

in

DK 165187 B

The present invention relates to a stabilized, aqueous, builder-containing, clear, single-phase, enzyme-containing liquid detergent comprising one or more detergent compounds, an effective amount of an enzyme or enzyme mixture selected from the group consisting of alkaline protease enzymes and α-amylase enzymes. , from 3 to 15% by weight of an enzyme stabilizing system consisting essentially of glycerol and a boron compound selected from the group consisting of boric acid, boron oxide and alkali metal borates capable of reacting with the glycerol, and 85 weight * water, which detergent is suitable for washing or soaking needles, and a method for washing clothes using the detergent.

The formulation of stabilizing enzyme-containing liquid detergents has been the subject of much attention in the prior art. The desirability of incorporating enzymes into detergent agents is primarily due to the ability of proteolytic and amino-lytic enzymes to degrade proteinaceous and starchy substances found on soiled textile fabrics such that stains, such as dots, bloodstains, chocolates, and the like. easier to remove in wash. However, enzymatic materials suitable for detergents, especially proteolytic enzymes, are relatively expensive. In fact, they are generally the most expensive constituent of a typically liquid detergent agent, even when contained in relatively small amounts. In addition, enzymes are known to be unstable in aqueous compositions. This is why, in liquid detergent formulas, an excess of enzymes is usually required to compensate for the expected loss of enzyme activity upon storage over extended periods. Accordingly, the known technique is overflowing with proposals for stabilizing enzyme-containing liquid detergents and especially non-containing liquid agents using various substances which are incorporated into the agent and serve as enzyme stabilizers.

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DK 165187B

2 In the case of liquid detergents containing a builder, the problem of enzyme stability is particularly acute. This is primarily because detergent builders have a destabilizing effect on enzymes even in agents containing enzyme stabilizers which are otherwise effective in non-builder-containing formulations. Furthermore, the incorporation of a builder into a liquid detergent agent presents a further problem, namely the ability to form a stable single-phase solution, the solubility of sodium tripolyphosphate e.g. are relatively limited in aqueous agents and especially in the presence of anion-active and nonionic detergents. Thus, in GB Patent Application No. 2,079,305 published January 20, 1982, e.g. disclose an aqueous liquid, enzyme-containing liquid detergent which is stabilized by a mixture of a polyol and boric acid. However, the agents described in the Examples, rather than being stable, clear, single-phase solutions, are rather vague suspensions that are prone to product separation upon storage for extended periods. Accordingly, the problems of enzyme stability and physical product stability remain problems to be solved by formulating a commercially acceptable, liquid, enzyme-containing liquid detergent.

The present invention provides a stabilized, aqueous, builder-containing, clear single-phase enzyme-containing liquid detergent of the kind mentioned in the preamble, and is characterized in that it comprises: (a) 3-10% by weight of a surfactant nonionic detergent compound , (b) 3-15 wt.% of a surfactant amphoteric detergent compound, 35 (c) 5-25 wt.% of a water-soluble, non-phosphate containing tergent builder.

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3 and that the ratio of glycerol to (i i) counted as borax is at least 1.

The invention also relates to a method of washing which is characteristic of the characterizing part of claim 10.

Thus, in accordance with the process of the invention, washing of stained and / or soiled substances is effected by contacting such substances with an aqueous solution of the liquid detergent defined above. In contrast to the builder-containing, enzyme-containing detergent agents, the agents of the present invention are characteristically clear, single-phase, homogeneous solutions which are physically stable upon storage for extended periods and within a wide temperature range. They are preferably substantially free of phosphate buffer salts.

From UK Patent Specification No. 146,910, an aqueous, enzyme-containing liquid detergent product having one stabilizing system comprising 4-25 weight * of one or more polyhydroxy compounds and boric acid, boron trioxide or an alkali metal ortho-metha or tetraborate, including borax, where the weight ratio of polyhydroxy compound to boron compound, calculated as borax, is less than 1 and the product has a pH of 7.5-25 11.0. The known product is stated to have special advantages when it does not contain any additives. Thus, from Danish disclosure 146,910 no conclusions can be drawn about how to provide a useful detergent agent of the kind in question with a content of non-phosphate-containing detergent builder salt.

From the aforementioned GB Publication Publication No. 2,079.

305 are known liquid, builder-containing and enzyme-containing detergents containing an enzyme stabilizing system comprising glycerol and a boron compound wherein the ratio of glycerol

DK 165187 B

4 and borax are greater than 1, but this system additionally comprises a polyacrylate polymer. Studies have shown that such detergents are not storage stable, and thus a significant phase shift occurs in Health, from which 30 to 80% of the total volume 5 flocculate as solids after storage at room temperature for only 7 days.

*

The use of a mixture of nonionic and amphoteric surfactant detergent agents of the present invention allows such surfactants and the non-phosphate-containing builder to be sufficiently soluble in an aqueous agent to form a homogeneous single-phase solution. The nonionic detergent compound may comprise from ca. 3-10%, preferably from ca. 4-8% by weight of detergent agents, and the amphoteric detergent compound will generally comprise from about 3-15%, preferably from ca. 4-10% by weight of such an agent.

The relative amounts of each of the aforementioned detergents are generally determined by the amount of builder salt used.

For builder concentrations from approx. 5-15% by weight of detergent agents typically include the amphoteric and the nonionic detergent each in an amount of from approx. 4 to 7% by weight, with the relative ratio of amphoteric detergent to nonionic detergent generally being approx. 1. For builder concentrations within the range of approx. 15-25% by weight, the amphoteric detergent is typically present in an amount of from approx. And the relative ratio of amphoteric detergent to nonionic detergent is preferably above about 1, 1.2 to approx. 1.6 o 0 is particularly favorable as the higher ratios generally correspond to higher builder salt concentrations.

The enzyme stabilizing system according to the invention is a mixture of glycerol and a boron compound selected from boric acid, boron oxide and an alkali metal borate capable of reacting with glycerol. The weight of the stabilizing system in the

DK 165187B

5 builder-containing detergent agents are from approx. 3-15%, preferably 4-10% by weight. Mixtures of glycerol and borax are particularly well suited to provide enzyme stability, the weight ratio of glycerol to borax in such stabilizing mixtures generally being from about 1 to about 5 minutes. 1.2-3, with a ratio of approx. 1.5-2.5 is preferred. Accordingly, the preferred amount of glycerol in agents is from ca. 3-7%, and the preferred amount of borax is from ca. 1-4%, based on the weight of the agent.

1 °

The alkaline proteolytic enzymes suitable for the present compositions comprise the various commercial liquid enzyme preparations which have been adapted for use in detergents, with powder form enzyme preparations also being useful, although generally less suitable for incorporation into the builder-containing agents. , liquid detergents. Suitable liquid enzyme preparations thus include "Alcalase" and "Esperase" sold by Novo Industries, Copenhagen, Denmark, and "Maxatase" and "AZ protease" sold by Gist-Brocades, Delft, The Netherlands.

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Among the suitable liquid α-amylase enzyme preparations are those sold by Novo Industries and Gist-Brocades under the trade names "Thermamyl" and "Maxamyl" respectively.

"Esperase" is particularly preferred for the present agents because of its optimized activity at the higher pH values corresponding to the builder-containing detergent agents.

The synthetic nonionic and amphoteric detergents used in practice in the present invention may be any of a wide variety of such compounds which are well known and are described in detail in Surface Active Agents, Vol. II by Schwartz, Perry and Berch, published in 1958 by Interscience Publishers, content-35.

it should be considered to be incorporated in the present text.

The nonionic detergents are usually poly-lower-alkoxylated lipophiles wherein the desired hydrophilic-lipophilic-like

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6 weight is obtained by adding a hydrophilic poly-lower alkoxy group to a lipophilic moiety. For the present agents, the nonionic detergent used is preferably a poly lower alkoxylated higher alkanol wherein the alkanol has 10 to 18 carbon atoms, and wherein the number of moles of lower alkylene oxide (with 2 or 3 carbon atoms) is from 3 -12. Of such substances it is preferred to use those substances in which the higher alkanol is a higher fatty alcohol having 10 or 12-15 carbon atoms and containing from 5-8 or 5-9 lower alkoxy groups per liter. moth.

The lower alkoxy group is preferably ethoxy, but in some cases it may conveniently be mixed with propoxy, the latter, if included, usually being a constituent (below 50%). Examples of such compounds are those compounds in which the alkanol has 12 to 15 carbon atoms and 15 which contains approx. 7 ethylene oxide groups per moles, e.g. "Neo-dol" ® 25-7 and "Neodol" ® 23-6.5, which are products manufactured by Shell Chemical Company, Inc. The former is a condensation product of a mixture of higher fatty alcohols having an average of approx. 12-15 carbon atoms with approx. 7 moles of ethylene oxide and the latter is a similar mixture in which the carbon atom content of the higher fatty alcohol is 12-13 and the number of ethylene oxide groups per mole on average is approx. 6.5. The higher alcohols are primary alkanols. Other examples of (B) samples of such detergents include "Tergitol" 15-S-7 (<E) and "Tergitol" 15-S-9, both of which are linear secondary alcohol ethoxylates manufactured by Union Carbide Corporation. The former is a mixed ethoxylation product of a C ^-C ^ linear secondary alkanol with 7 moles of ethylene oxide, and the latter is a similar product, but with the reaction of 9 moles of ethylene-30 oxide.

Also useful in the present compositions are high molecular weight, nonionic compounds such as "Neodol" 45-11 which are similar ethylene oxide condensation products of higher fat alcohols where the higher fatty alcohol has 14-15 carbon atoms and the number of ethylene oxide groups per mole is approx. 11. Such products are also manufactured by Shell Chemical Company.

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Other useful nonionic compounds are represented by "Plurafac" B-26 (BASF Chemical Company), the reaction product of a higher linear alcohol and a mixture of ethylene and propylene oxides.

In the preferred poly-lower-alkoxylated higher alkanols, the best equilibrium between hydrophilic and lipophilic moieties is obtained when the number of lower alkoxides is from approx. 40-100% of the number of carbon atoms in the higher alcohol, preferably 40-60% 1 ° thereof. The nonionic detergent preferably consists of at least 50% of the preferred ethoxylated alkanols. High molecular weight alkanols and various other, normally solid, non-ionic detergent compounds and surfactants can contribute to the gelation of the liquid detergent and are thus omitted normally or the amount thereof is limited in the present agents, although smaller amounts thereof may be used due to their purification. properties, etc. With respect to both preferred and less preferred nonionic detergents, the alkyl groups contained therein are preferably linear, although a minor degree of weak branching can be tolerated, such as at a carbon atom adjacent to or two carbon atoms from the terminal carbon atom of the straight chain and away from the ethoxy chain on the condition that the branched alkyl thus has a length of not more than 3 carbon atoms. The amount of carbon atoms 25 in such a branched configuration will usually be less and rarely exceed 20% of the total number of carbon atoms in the alkyl moiety. Although linear eel kills, which are end-linked to ethylene oxide chains, are highly preferred and believed to result in the optimal combination of purification action, biodegradability and non-gelling properties, medial or secondary linkage to the ethylene oxide in the chain may also occur. In such cases, it is usually in only a minor portion of such alkyls, generally below 20%, but as is the case in the aforementioned "Tergitols", it may be larger. When propylene oxide is included in the lower alkylene oxide chain, it will also usually be less than 20% thereof and preferably below 10% thereof.

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Amphoteric detergents include higher fat carboxylates, phosphates, sulfates or sulfonates containing a cationic substituent such as an amino group which may be quaternized, e.g. with a lower alkyl group or a chain which is extended by the amino group by condensation with a lower alkylene oxide, e.g. of ethylene oxide. Examples of proprietary amphoteric detergents include: alkyl β-amino dipropionates, RN (C 2 H 4 COOM) 2, alkyl β-aminopropionates, RN (H) C 2 H 4 COOM, and long chain imidazole derivatives of the general formula:

CEL

/ \ N CH- I i

R - C - N - CH ^ CH-AND-COOM

y 2 2 2

OH CHoC00M

2 wherein R in each of the above formulas is an acyclic, hydrophobic group containing from ca. 8-18 carbon atoms, and M is a cation for neutralizing the anion charge.

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Optionally, an anionic detergent may also be used in smaller amounts to supplement the nonionic and amphoteric detergent compounds in the present liquid detergent agents. The amount of anionic detergent will generally be less than about 25%. 5% by weight and preferably below about 3% by weight of the total agent due to the limiting solubility of such agents in the builder-containing liquid detergent media. Alkylbenzene sulfonate salts, wherein the alkyl group contains 10-18 carbon atoms, have particularly limited solubility in the present agents and it is therefore preferred that the present agents be substantially free of such compounds to avoid the possibility of product separation.

The preferred anionic detergents for use herein are sulfated / ethoxylated, higher fatty alcohols with the formula R0 (C2H40) SO3 M ', wherein R is a fatty alkyl of 10-18 or 20 carbon atoms, m is from 2-6 or 8 (preferably with a value from about 1/5 to 1/2 of the number of carbon atoms in R), and M

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9 is a dissolving salt-forming cation such as an alkali metal, ammonium, lower alkylamino or lower alkanolamino, or a higher alkylbenzenesulfonate wherein higher alkyl has 10-15 carbon atoms.

5

Ethylene oxide is the preferred lower alkylene oxide of the anion-active alkoxylate detergent, and the amount thereof in the polyethoxylated higher alkanol sulfate is preferably 2-5 moles of ethylene oxide groups per liter. moles of anionic detergent, with 3 moles being particularly preferred, especially when the higher alkanol has 11 or 12-15 carbon atoms. In order to maintain the desired hydrophilic-lipo-file equilibrium when the carbon atom content of the alkyl chain is at the lower end of the range of 10-18 carbon atoms, the ethylene oxide content of the detergent can be reduced to approx. 2 moles per

15 moles, whereas when the higher alkanol has 16-18 carbon atoms in the higher range, the number of ethylene oxide groups may be increased to 4 or 5 and in some cases up to 8 or 9. The salt-forming cation may likewise be be modified to obtain the best solubility. It may be any suitable dissolving metal or radical, but will most often be alkali metal, e.g. sodium or ammonium. If lower alkylamine or alkanolamine groups are used, the alkyls and alkanols will usually contain from 1-4 carbon atoms and the amines and alkanolamines may be mono-, di- and trisubstituted as in mono-ethanolamine, diisopropanolamine and trimethylamine. A preferred polyethoxylated alcohol sulfate detergent can be obtained from Shell Chemical Company and marketed as "Neodol" 25-3S.

The non-phosphate detergent builder salts are used in the present compositions in amounts, generally from about 1 5 to 25% and preferably from ca. 10-20% by weight. Specific examples of non-phosphorus-containing, water-soluble, inorganic builders include water-soluble inorganic carbonates, bicarbonates and silicates. Alkali metal (e.g., sodium and potassium β -) carbonates, bicarbonates and silicates are particularly suitable herein.

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Water-soluble organic builders are also suitable and include alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates. Specific examples of polyacetate and polycarb® oxylate builders include sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylenediaminetetraacetic acid, nitrilotriacetic acid, benzene polycarboxylic acids (i.e., penta- and tetra-

The percentage amount of water, the main solvent in the present compositions, will usually be from about 1 30-85%, preferably 45-75%, and particularly advantageous from ca. 60-70% by weight of the liquid.

15 The optical fluorescent bleaches or whitening agents used in the liquid detergents are important constituents of modern detergents which give a fresh look and textile appearance so that the laundry is not only clean but also clean. While it is possible to use a single optical bleach for a particular target in the present liquid detergents, it is generally desirable to use blends of such optical bleaches which will have a good clarifying effect on cotton, nylons, polyethers and blends of such textile fabrics, 25 and which are also pale stable. A good description of such optical bleach types is given in the article "The Requirements of Present Day Detergent Fluorescent Whitening Agents" by A. E. Siegrist, J. Am. Oil Chemists Soc., January 1978 (Vol. 55). This article and U.S. Pat. No. 3,812,041, the contents of which are to be considered for incorporation in the present text, both contain detailed descriptions of a wide variety of suitable optical bleaches.

Among the optical bleaching agents suitable in the present liquid detergents are: "Calcofluor" 5BM (American Cyanamide), "Tinopal" LPW (Ciba), "SOF" A-2001 (Ciba), "CDW" (Hilton-Davis), "Phorwite" RKH, "Phorwite" BBH, and "Phorwite" BHC (Verona), "CSL", Powder, Acid (American Cyanamid), "FB" 766 (Verona), "Blancophor" PD (GAF), "UNPA" (Geigy), "Tinonal" RRS? Nn (Geiovl

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Excipients may be included in the present liquid detergent agents to provide additional properties, either functional or aesthetic. Suitable adjuvants include dirt suspending and antigen precipitating agents such as polyvinyl alcohol, sodium carboxymethyl cellulose, hydroxypropyl methyl cellulose, thickening agents, e.g. gums, alginates, agar agar, foam enhancers, e.g. laurine myristine diethanolamide, foaming agents, e.g. silicones, bactericides, e.g. tribromosalicylanilide, hexachlorophen, 10 dyes, pigments (water dispersible), preservatives, ultraviolet light absorbing agents, textile fabric softeners, haze agents, e.g. polystyrene suspensions, as well as perfumes. Such substances will, of course, be selected having regard to the properties desired in the finished product, their compatibility with other components and their solubility in the liquid agent.

The present liquid agents are effective and easy to use. Compared to powerful detergent washing powders, much smaller volumes of the available fluids are used to achieve a similar cleaning of soiled laundry. Using a typically preferred formulation of the present invention, e.g. only approx. 132g or 1/2 cup of liquid for a 25-liter, automatic top-loading type washing machine with a water volume of 55-75 liters and even less for front-loading washing machines. The concentration of the liquid detergent in the wash water is of the order of approx. 0.2%. The amount of the liquid 30 in the washing solution will usually vary from approx. 0.05 to 0.3% and preferably from 0.15 to 0.25%. The amounts of the various constituents of the liquid agent may vary accordingly. Similar results can be obtained by using larger quantities of a more diluted product, but the larger quantity required will mean greater packaging costs and will usually be less convenient for consumers.

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Example 1

Enzyme-containing builder-containing liquid detergents A-F were formulated, as set out in the following Table 1. Percentages given are% by weight.

TABLE 1

A B C D E F

5 Ethoxylated C12-C15 primary alcohol (7 moles EO / mole alcohol) 5.5% 5.5% 5.5% 5.5% 5.5% 5.5% "Varion" CADG {1) 21 21 21 ' .21 21 21

Optical Bleach 0.2 0.2 0.2 0.2 0.2 0.2 0.2

Sodium nitrilo triacetate 15 15 15 15 15 15 10 PBB1 2 3 111111

Perfume 0.3 0.3 0.3 0.3 0.3 0.3

/ o V

Proteolytic Enzyme 1 1 1 1 1 1 1

Glycerol 5 5 5 5

Borax - 1 2 3 - 3 15 H2O --------------- remainder ------------

Percent of active enzyme 12 62 73 "76 21 28

after 6 days at 110 ° F

A 32% aqueous solution of cocosamido-betaine sold by Sherex Chemical Company 2 20 (2) Polar Brilliant Blue - a 1% active color solution 3 "Esperase" sold by Novo Industries containing 5% enzyme, 75% propylene glycol and the rest ELO with an activity of 8.0 KNPU / g (Kilo Novo Protease Units / g).

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The enzyme activities of the agents AF were examined after 6 days of storage at 110 ° F, the percent activity relative to the initial value being given in Table 1. A, E and F were the only agents that did not contain an enzyme stabilizing system according to the invention and sustained an almost complete loss of enzyme activity after 6 days. Agents B, C and D show the marked improvement in enzyme stability, which results in the inclusion of glycerol and borax in the detergent agent.

The agents A-F were all clear, single-phase, homogeneous solutions, which retained their physical stability and clarity after 6 months of storage at both room temperature and at 110 ° F.

W

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Example 2

Enzyme-containing, builder-containing liquid detergents G and H were formulated essentially in a similar manner to agents A-F, except that sodium citrate was used as the builder salt instead of sodium NTA. Mediums are given in the following Table 2 TABLE 2

G H

Ethoxylated C2 2 ”C15 P3 ^ 111®1 alcohol (7 moles EO / mole alcohol) 5.5% 5.5% 10" Varion "CADG1 2 3 21 21

Optical Bleach 0.2 0.2

Sodium Citrate 13 13 "PBbm (2) 1 i

Parfurne 0.3 0.3 (3) 15 Proteolytic enzyme 1 1

Glycerol - 5.

Borax - 3 H2O ------ residue ------

Percent of active enzyme after 6 days 20 at 110 ° F 26 95

A 32% aqueous solution of cocosamidobetain sold by Sherex Chemical Company.

2

Polar Brillant Blue - a 1% active color solution.

3 "Esperase" is sold by Novo Industries containing 5% enzyme, 25 75% propylene glycol and the residual H 2 O with an activity of 8.0 KNPU / g (kg Novo Protease units / g).

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Agent H of the invention showed an enzyme activity after 6 days of 95% compared to Agent G without enzyme stabilizing system content, which lost almost 1/3 of the enzyme activity.

5

The agents were clear, single-phase solutions that remained physically stable after 6 months of storage at both room temperature and 110 ° F.

Example 3 This example shows a storage experiment with the detergent compositions I-L shown in Table 3 below. The object is to show the effect on physical stability when Carbopol 941, a trademark for a crosslinked acrylate polymer, is added to a liquid detergent agent of the invention as indicated in GB Publication No. 2,079,305.

TABLE 3

20 I J K L

Ethoxylated primary C12 "c15 alcohol (7 mol EO / mol alcohol} 5.5% 5.5% 5.5% 5.5%

Varion CADG * 21 21 21 21

Clarifier 0.2 0.2 0.2 0.2 Sodium Nitrolotriacetate 15 15 13 18 PBB1 1111

Perfume 0.3 0.3 ^ 0.3 0.3

Proteolytic Enzyme3 1111

Glycerol 5 5 5 5 30 Borax 3333

Carbopol 9414 - 0.8 0.8 0.8

Water for 1 100% 1 32% aqueous solution of cocosamidobetain supplied by Sherex 35 Chemical Company.

Polar Billiant Blue - a 1% active color solution.

Claims (10)

A stabilized, aqueous, builder-containing, clear, single-phase enzyme-containing liquid detergent comprising: 25 'one or more detergent compounds (d) an effective amount of an enzyme or enzyme mixture selected from the group consisting of alkaline protease enzymes and α-amylase enzymes, (e) 3-15% by weight of an enzyme stabilizing system consisting essentially of (i) glycerol and (ii) a boron compound selected from the group consisting of boric acid, boron oxide and alkali metal borates capable of reacting with the glycerol , and (f) 30-85 wt.% water. DK 165187B 17 characterized in that it comprises (a) 3-10 wt% of a surfactant nonionic detergent compound, 5 (b) 3-15 wt% of a surfactant amphoteric detergent compound see, (c) 5-25 weight FC of a water-soluble, non-phosphate-containing detergent builder salt, and that the ratio of glycerol to (ii) counted as borax is at least 1; Detergent composition according to claim 1, characterized in that the non-ionic detergent compound is a water-soluble C 2 -C 3 -alkyl xylated C 1 -C 10 -alkanol. Detergent agent according to claim 1, characterized in that the builder salt is sodium citrate or sodium nitrilotriacetate. Detergent composition according to claim 1, characterized in that it contains less than 5% by weight of a surfactant anionic detergent compound. Detergent composition according to claim 1, characterized in that it does not substantially contain a C1-C6-alkylbenzenesulfonate ion-active detergent. 30 5. Crosslinked polyacrylate polymer supplied by B.'F. Goodrich Co. After storing the detergent for 7 days at room temperature, detergent I of the invention remained crystal clear, while the other detergents J-L showed significant 10 phase separation, from which 30 to 80% of the total volume was flocculated as solids. Thus, it follows that by following the teachings of GB Publication No. 2,079,305, the desired stabilized, aqueous, builder-containing, clear, single-phase enzyme-containing liquid detergent agent is not obtained, as disclosed in the present invention. Claims. 20 -------------------- Detergent composition according to claim 1, characterized in that it contains 3-7 wt% glycerol and 1-4 wt% alkali metal borate. Detergent composition according to claim 1, characterized in that it does not contain substantially a phosphate detergent builder salt. 18 DK 165187 B Detergent composition according to claim 1, characterized in that the alkali metal borate is borax. Detergent composition according to claim 1, characterized in that the builder salt is present in an amount of 10-20% by weight. Method of washing, characterized in that the stained and / or soiled fabrics to be washed are contacted with an enzyme-containing, builder-containing 10 clear, single-phase, liquid detergent as defined in claim 1. 15 20 25 30 35