PT99612A - PROCESS FOR PREPARING LIQUID COMPOSITIONS ADJUVED DETERGENTS COMPOSING AN AMINE SALT OF AN ANIONIC SURFACTANT ACID CONTAINING ONE OR MORE GROUPS SULFONIC ACID - Google Patents

Description

73 388 CTE / JA / PL60873ΡΤ -2-

The present invention relates to liquid adjuvanted detergent compositions and to their production and use.

In recent times, mainly for reasons of economy of manufacture, liquid adjuvanted detergents of energetic action have penetrated the market for spray-dried powders, with the result that much work has been done in relation to physics, to the chemistry of product formulation. These liquid adjuvanted detergents are often sold in 2 liter plastic bottles. Typical products are those described in GB-B-2123846, GB-B-2153839, EP-B-0086614 and EP-B-0151884.

As a consequence of this commercial development the spray dry market sector has responded by the introduction of detergent concentrates having very low amounts of inert ingredients. This means that without loads and diluents the product can be presented to the public with a connotation designated as environmentally friendly and thus it can be claimed that the use of the product is less polluting. This is because much less product is used per load of washing machine because of its strength. Additionally the associated packaging can be significantly reduced compared to the traditional packaging of the powder with a resulting savings in paper and paperboard. The use of diethanolamine dodecylbenzenesulfonate in an aqueous energetic detergent is mentioned with reference to Table 3 of AU-B-507431.

Another breakthrough in detergent technology occurred when the market for detergent detergents responded to products in concentrated powders. As a result liquid detergent concentrates are available which are typically sold in 1 liter plastic bottles. Taking into account the higher detergent potency of these concentrates the amount of concentrate required for a ¥ machine loading. 73 388 CTE / JA / PL60 8 7 3 3 -3-

& washing is often about half the volume of an energetic, aqueous, adjuvanted detergent used to wash the same laundry load. Accordingly, a 1 liter bottle of concentrate may be used to wash approximately as many laundry loads as a 2 liter bottle of a conventional, energetic, liquid, aqueous detergent. However, to date, this sector has basically been forced to formulate its products as dispersions of inorganic adjuvants in non-aqueous mixtures of nonionic surfactants, as in EP-B-0030096 or in EP-B-0120659, or as formulations of a nonionic surfactant blend in the emulsion state with a saturated solution of one or more adjuvants, using vegetable gums or other emulsifying agents, as stabilizers, as in GB-A-2148926.

A problem arises with conventional, non-aqueous liquid adjuvanted detergent compositions containing nonionic surfactants as the sole class of surfactant, as they tend to gel by dispersion in water.

In GB-A-2148926 the surfactants in the emulsion are nonionic surfactants, whereas in the case of EP-B-0120659, claim 9 mentions the presence of an anionic surfactant in the composition, but the Specification completely omits its use in any of its Examples. This omission occurs because it is difficult to obtain commercially available anionic surfactants, such as sodium dodecylbenzenesulfonate, in the non-pasty solid state (all of which are usually offered in admixture with sodium sulfate to prevent the material from being tacky and forming balls.

Accordingly, the prior art does not use anionic surfactants in adjuvanted, non-aqueous detergent liquids, and this is regrettable because this class of detergents is one of the most cost-effective and most effective of all commercially available surfactants.

In the non-aqueous class of liquid detergents, the

73 388

The water analogue of the adjuvanted system of, for example, GB-B-2153839, is the class of anhydrous solvents known as polyethylene glycols (P.E.G). The liquid members of this class are those with a molecular weight between about 100 and about 600, commonly called peg. 100, PEG. 200, PEG. 300 and so on.

It would be desirable to produce a liquid detergent composition having an energetic action with an anionic surfactant as an integral part of the liquid phase in which the adjuvants are dispersed by mixing in stick apparatus, bead forming apparatus or ball mill (H rod, bead or bali milling "). It would still be desirable to provide a non-aqueous, liquid, non-aqueous, adjuvanted detergent composition which does not gel by dispersion in water. The present invention therefore seeks to provide a substantially anhydrous liquid adjuvanted detergent composition containing an anionic surfactant. It further seeks to provide a liquid, substantially anhydrous adjuvanted detergent composition which shows little or no tendency to gel by dispersion in water.

According to the present invention there is provided a liquid adjuvanted detergent composition comprising a substantially anhydrous liquid organic phase having uniformly distributed therein (i) an amine salt of an anionic surfactant acid containing one or more sulfonic acid groups and (ii) a finely divided particulate adjuvant. The liquid organic phase is substantially anhydrous. In other words, it is preferably devoid of added water and contains only the amount of water which is normally present in the ingredients used in the production of the liquid adjuvanted detergent composition of the invention. Accordingly, a composition according to the invention typically contains less than about 5% w / w water, more preferably less than about 2% w / w water and even more preferably less than

CTE / JA / PL60873EN -5-

about 1% w / w of water, e.g. about 0.5% w / w or less, to about 0.1% or less of water, based on the total weight of the composition. The organic liquid phase may include a water-soluble organic solvent. In this case, a liquid adjuvanted detergent composition comprising a water soluble organic solvent phase is provided uniformly therein (i) an amine salt of an anionic surfactant acid containing one or more sulfonic acid groups and (ii) ) a finely divided particulate adjuvant.

Typically a significant proportion of the amine salt of the anionic surfactant, and preferably all of it, is dissolved in the liquid organic phase, preferably in a form similar to the micelles typically found in the aqueous detergent solutions, whereas the adjuvant is insoluble in the liquid organic phase . The water-soluble organic solvent may comprise an alcohol of lower molecular weight, for example an alkanol containing from 1 to 6, or more preferably from 2 to 4 carbon atoms, such as ethanol, n-propanol, iso-propanol, n-butanol or the like. Another class of water soluble organic solvents are water soluble liquid organic compounds containing two or more hydroxyl groups. Examples of such compounds include ethylene glycol, propylene glycol, 1,4-butylene glycol, 1,5-pentamethylene glycol, glycerol, polyalkylene glycols such as polyethylene glycol, polypropylene glycol and mixed polyalkylene ether glycols such as polyethylene-polyoxypropylene glycols. as well as mixtures of two or more of them.

A preferred type of water-soluble organic solvent are polyethylene glycols, of which those having molecular weights of at least 150, for example molecular weights in the range of about 200 to about 600 are preferred. However, any solvent which is liquid at and below ambient temperature (eg up to about -10 ° C), which is

73 388

Which can be miscible with water and allows dispersion of the amine salt of the anionic surfactant acid and the adjuvant. If desired, water-soluble mixtures of organic solvents may be used. For example, a mixture of an alkanol such as ethanol or iso-propanol and a polyethylene glycol may be used.

It will usually be necessary to incorporate at most a small amount of only an organic solvent soluble in water or a mixture of organic solvents, for example up to about 20% w / w solvent, based on the total weight of the composition. A preferred range is from about 1% w / w to about 15% w / w solvent, based on the total weight of the composition.

One of the purposes for which this solvent, if present, is added may be to adjust the viscosity of the composition to a desired value. A useful degree of control over the viscosity of the composition can be achieved, in particular by the addition of a glycol as a polyethylene glycol (e.g. polyethylene glycol PEG 200).

The amine salts useful in the practice of the present invention may be prepared by reacting an organic amine with an anionic surfactant acid containing one or more sulfonic acid groups.

Particularly preferred amines are alkanolamines, such as monoethanolamine, diethanolamine and triethanolamine, and monocyclic heterocyclic amines, such as morpholine.

In use the liquid adjuvanted detergent compositions of the invention will be diluted with water. This dilution step may occur, for example, in the washing cycle of an automatic washing machine. Since the adjuvant is usually alkaline in nature and can typically contain an alkali metal ion, cation exchange can occur by diluting the liquid adjuvanted detergent composition with water. Thus the quaternary ammonium ion of the salt of the anionic surfactant acid present in the composition may, for example, be exchanged with sodium ions of the adjuvant. Consequently the 73388

CTE / JA / PL60 87 3PT-7-

The anionic surfactant may be associated in the resulting aqueous solution with, for example, sodium ions or the ions of another alkali metal, whereas the quaternary ammonium ion may undergo hydrolysis to provide the free amine. Since some amines have pungent or unpleasant odors, it will generally be preferred to select as the amine salt of the anionic surfactant acid a material which, upon hydrolysis of the quaternary ammonium ion, does not release an amine with an unpleasant odor. For this reason preferred salts of anionic surfactant acids for use in the compositions of the invention contain alkanolammonium or morpholinium ions such as the monoalkanolammonium, dialkanolammonium and trialkanolammonium salts of anionic surfactant acids such as the monoethanolammonium, diethanolammonium and triethanolammonium salts of anionic surfactant acids and morpholinium salts of anionic surfactant acids.

As adjuvant, any of the adjuvants known as sodium metaphosphate, sodium paraphosphate, sodium tri-polyphosphate, sodium silicate, sodium carbonate, a zeolite, a layered silicate, trisodium citrate or a mixture of two or more of these. It is beneficial to include an anhydrous material such as anhydrous sodium carbonate as an ingredient in the formulation of a liquid adjuvanted detergent composition according to the invention because the anhydrous material absorbs water to form a solid sodium carbonate hydrate. In this way, any water present or formed in the composition can be absorbed and the substantially non-aqueous nature of the composition is maintained, in addition to the sodium carbonate being available to act as an alkaline adjuvant.

Examples of surfactant acids include alkyl benzene sulfonic acids in which the alkyl group contains from about 6 to about 20 carbon atoms, for example from 10 to 14 carbon atoms, primary or secondary alkyl sulfonic acids containing from about 10 to about 26 carbon atoms, for example 10 to 14 carbon atoms, and alpha-olefin sulfonic acids obtained by the sulfonation of an alpha-olefin containing, for example, from about 10 to about 22

73 388

Carbon atoms such as a Câ, â, <â, † olefin or a mixture containing the same. In addition to a sulphonic acid group-containing material, a sulfated fatty alcohol may also be used for the production of the salt or amine salts, usually in admixture with a sulfonic acid group-containing material; typical sulfated fatty alcohols include those containing from about 10 to about 26 carbon atoms, for example a mixture of sulfated fatty alcohols containing C 10, C 12, C 16 and C 18 fatty alcohols. Typical of such a mixture of fatty alcohols is one containing alcohols in the following proportions; C10 3.0%, C12 57.0%, 20.0%, 9.0% and 11.0%. The composition of the invention may further comprise one or more nonionic surfactants. Typical nonionic surfactants include fatty acid monoethanolamides such as coconut fatty acid monoethanolamide, for which a typical formulation is a mixture of fatty acid monoethanolamides as follows; Cg 0.5%, Cg 6.5%, C10 6.0%, C12 49.5%, C14 19.5%, C16 8.5%, Clg (stearic) 2.0%, C18 (oleic) 6 , 0% and C18 (linoleic) 1.5%. Other suitable nonionic surfactants include polyoxyalkylene ethers of alkanols, typically alkoxyl polyoxyalkylene ethers typically containing 3 or more ethylene oxide groups, for example from about 6 to about 20 ethylene oxide residues and based on alkanols containing from about 6 to about 26 carbon atoms. Polyoxyethylene oxypropylene ethers of alkanols may also be used; these may also be based on C9 to C20 alkanols and may contain from about 3 to about 20 ethylene oxide residues, i.e. a mixture of ethylene oxide and propylene oxide residue residues. The alkanols and mixtures of alkanols on which these nonionic surfactants are based may be produced by hydrogenation of methyl esters produced by transesterification of naturally occurring vegetable oils such as coconut oil, sunflower oil, palm oil, rapeseed oil and or animal fats such as tallow or lard. A typical polyoxyethylene ether of a alkanol is based on the lauryl alcohol condensed with approximately 8 moles of ethylene oxide. The polyoxyalkylene ethers of alkylphenols are another type of surfactant

CTE / JA / PL60873EN. Mixtures of nonionic surfactants may be used.

The compositions of the present invention may include an amphoteric surfactant or a mixture of amphoteric surfactants. Typical amphoteric surfactants include dicarboxylated derivatives of oleic imidazoline, capryl amphocarboxyglycinate, octyl iminodipropionate, octyldimethyl betaine, coconut complex iminodiglycinates and fatty ampho polycarboxyglycinates. Often, a mixture of amphoteric surfactant and nonionic surfactant are present in the compositions of the invention. The weight ratio of amphoteric surfactant to nonionic surfactant may vary between broad limits, for example in the range of from about 1: 100 to about 100: 1.

Preferably, a liquid adjuvanted detergent composition according to the invention contains at least about 0.1% w / w of an amine salt of an anionic surfactant acid to about 20% w / w or more, eg up to about 25% w / w, even more preferably from about 2% w / w to about 15% w / w, based on the total weight of said composition.

Preferably, a liquid adjuvanted detergent composition according to the invention comprises from about 0.1% w / w to about 20% or more of a nonionic surfactant or surfactants, an amphoteric surfactant or surfactants or a a mixture of nonionic and amphoteric surfactants, even more preferably up to about 35% w / w, or more, eg up to about 50% w / w, most preferably from about 2% to about 35% w / based on the total weight of the composition.

A liquid adjuvanted detergent composition according to the invention may additionally comprise a bleach and, optionally, a bleach activator. Typically such a composition may contain from about 0.1% w / w to about 10% w / w or more, eg up to about 15% w / w of a bleach and optionally from about 0.03% w / w to about 3% w / w, or more,

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E.g. up to about 5% of a bleach activator, based on the total weight of the composition.

Other secondary ingredients which may be included in the composition of the invention include preservatives, optical brighteners, fragrances, foam depressants, foam reinforcers and / or stabilizers, soaps, dyes, pigments, buffers, corrosion inhibitors, sequestering agents, moisturizers, enzymes, enzyme stabilizers, fabric softeners, fabric conditioners and the like. Typical sequestering agents include ethylenediaminetetraacetic acid, nitrilotrioacetic acid and acrylic acid-maleic acid copolymers such as those sold under the trademark Polycarboxylate AMC. One or more of these secondary ingredients may be included in the compositions of the invention as appropriate. These other secondary ingredients typically comprise not more than about 5% w / w each of the compositions of the invention, for example in the range of about 0.001% w / w to about 2% w / w, each one, based on the total weight of the composition.

The compositions of the invention may be formulated so as to have about the same washing power as standard, aqueous, liquid, energetic, adjuvanted detergents. Preferably, however, the compositions of the invention will be formulated as concentrates which have several times, e.g. from about 2 to about 5 times, the washing power of conventional, liquid, energetic, liquid detergent detergents. To this end it is desirable to formulate the compositions as concentrates in which the solid components comprise in total at least about 30% w / w and preferably at least about 45% w / w to about 50% w / w or even more, based on the weight of the composition. The invention further provides a process for the production of a liquid adjuvanted detergent composition comprising the step of reacting in an organic phase an anionic surfactant acid containing one or more free sulfonic acid groups having

73 388

CTE / JA / PL6 Ο 8 7 3 EN an amine. Such an amine may be a primary amine, a secondary amine or a tertiary amine.

In one form of the process the reaction is carried out in an organic phase which includes a water-soluble organic solvent. In this case there is provided in accordance with the invention a process for the production of a liquid adjuvanted detergent composition comprising the step of reacting an anionic surfactant acid containing one or more free sulfonic acid groups in a solvent phase organic solvent comprising a water-soluble solvent, with an amine. The amine may be a primary amine, a secondary amine or a tertiary amine.

Accordingly, the invention contemplates the in situ production of quantities of salts of organic bases of anionic, spurious, sulfonic acids. Highly adjuvant liquids can be produced from solutions of an acid such as dodecylbenzenesulfonic acid in PEG 200 (polyethylene glycol 200), in addition products of ethylene oxide or in a mixture of both. These solutions may additionally contain anionic nonionic surfactants. The organic bases that were used were mono-, di- and triethanolamine and morpholine, but any primary, secondary or tertiary amine could be used without an unpleasant odor. From these materials, very transparent, pale yellow syrups can be produced which are excellent carriers for transporting the silicate, carbonate, phosphate and polyphosphate adjuvants which will be micronised to produce the non-aqueous adjuvant laundry liquid. solution 67.5 g 15.0 g 100.0 g 75.0 g

As an example of this technology the following was prepared: Dodecylbenzenesulfonic acid

Fatty alcohol ethoxylate (4 moles E.O.)

Alkylene oxide addition product (Marlox FK 64) Polyethylene glycol 200 (The word &quot; Marlox &quot; is a registered trademark).

73 388

CTE / JA / PL6 Ο 8 7 3 EN -12-

The above ingredients were simply stirred together in any order to give an amber syrup. This solution was then converted to the quaternary ammonium salt of the sulfonic acid by titration with one of the previously mentioned amines. The resulting syrups had the following viscosity:

Viscosities at 25 ° C (mPa)

Triethanolamine salt 275 Diethanolamine salt 247 Monoethanolamine salt 254 Morpholine salt 261

An additional series of similar syrups may be prepared by default of polyethylene glycol or fatty alcohol ethoxylate.

When any of these syrups were mixed with an adjuvant such as sodium tri-polyphosphate (35%), sodium silicate powder &quot; Soluble &quot; or sodium carbonate (5% each) and micronized by grinding, the result was a fully degreased, liquid, flowable laundry detergent. All other usual secondary ingredients could be added and are compatible, including soaps which can be formed in situ having a fatty acid in solution in the PEG mixture prior to titration with the amine. The invention is further illustrated in the following Examples. Example 1

A liquid adjuvanted detergent concentrate is produced from the following ingredients:

CTE / JA / PL60873-Dodecylbenzenesulfonic acid 11.5

Alkylene oxide addition product (Marlox FK 64) 12.0

Alcohol ethoxylate (4 moles E.O.) 3.0 Coconut fatty acid 5.2

Triethanolamine 8.5

Polyethylene glycol (PEG 200) 12 f0

Sub-total 52.2

Sodium Silicate (Soluble Powder C) 5.0

Anhydrous Sodium Carbonate (Calcined Soda) 5.0

Sodium tri-polyphosphate 35.0 i

Secondary Ingredients 2.8

Sub-total 47.8

Total 100.0 u

% w / w

All organic compounds, with the exception of triethanolamine, are mixed together to give a dark amber syrup. To this is added triethanolamine sufficient for neutralization; the approximate end point corresponds to the color change from syrup to lighter yellow. To this syrup all other ingredients are added and the mixture is then micronised in a drop forming apparatus. In this preparation the presence of sodium carbonate is bifunctional because it acts as an alkaline adjuvant in the product and as a drying agent.

Examples 2 to 5

Further liquid detergent concentrates were produced by mixing the following ingredients and micronising one into a drop forming apparatus:

73 388 CTE / JA / PL6 Ο8 73ΡΤ -14-

Example Ns 2 3 4 5 Diethylamine salt of% w / w% P / W% w / w% dodecylbenzenesulfonic acid Alcohol ethoxylate 13.5 13.5 13.5 12.6 (3 moles of EO) Ethoxylate of alcohol 7.0 7.0 7.0 10.7 (7 moles of EO) Alcohol ethoxylate 8.3 8.3 8.3 (7 moles of AO) 12.6 12.6 12.6 24.2 Polyethylene glycol 5.5 5.5 5.5 - Isopropyl alcohol 2.5 2.5 2.5 2.5 Sub-total 49.4 49.4 49.4 50.0 Sodium tri-polyphosphate 31.3 38.0 38.0 38.0 Sodium silicate 3.0 3.0 3.0 3.0 Calcined soda - 5.0 5.5 5.5 Sodium perborate 10.0 - - - TAED 1.9 - - - Sodium carboxymethylcellulose 1 , 0 1.0 1.0 1.0 EDTA 1.0 0.4 1.0 1.0 Secondary ingredients 2_tA 3.2 2 * 1 2.0 Sub-total 50.6 50.6 50.6 50.0 Total 100.0 100.0 100.0 100 , 0 υ

Notes: 1. Alcohol ethoxylate (3 moles of EO) = polyethylene glycol ether (3 moles of ethylene oxide) of a mixture of C1-2-15 alkanols. 2. Alcohol ethoxylate (7 moles of EO) = polyethylene glycol (7 moles of ethylene oxide) of a mixture of C 12-15 alkanols

Alcohol ethoxylate = polyethylene / propylene glycol ether (7 moles of alkylene oxide: 3

73 388 CTE / JA / PL6 Ο8 7 3GB -15-

12-15 '92% propylene oxide / 8% ethylene oxide) of a mixture of alkanols c-κ κ. 4. TAED = tetraacetylethylenediamine. 5. EDTA = ethylenediaminetetraacetic acid 6. Secondary ingredients = enzymes, fragrance, TIo2,

Bitrex (an anti-ingestion agent) and an optical brightener.

Liquid adjuvant detergents were concentrated successfully. Ethanol can be used in place of iso-propanol with equally good results.

Examples 6 to 9

The diethanolamine salt of dodecylbenzenesulfonic acid is replaced in the formulations of Examples 2 to 5 by an equal weight of the corresponding triethanolamine salt. In each case, liquid adjuvant detergent concentrates of equally good quality were obtained.

Examples 10 to 21

Liquid adjuvanted detergent concentrates were produced by blending the following ingredients and combining all of the liquid ingredients together in each listed formulation, with the exception of the secondary ingredients. The formation of the amine salt from dodecylbenzenesulfonic acid was achieved by stoichiometric addition of the relevant amine. All solid ingredients were then added, with the exception of any thermally labile enzyme present. The resulting mixture was then micronized in a ball mill to produce an easily flowable product which could then be inoculated with the appropriate amount of enzyme or enzymes (if used):

v

CTE / JA / PL60 8 7 3 EN -16-

Example In dodecylbenzenesulfonic acid Alcohol ethoxylate (3 moles of E.O.)

Marlox FK 64 Triethanolamine Diethanolamine Monoethane 1amine Polyethylene glycol (PEG 200) Iso-propanol Sub-total

Zeolite (Wessalith P) Sodium Tri-Polyphosphate Calcined Soda Sodium Silicate Powder (Soluble C)

EDTA

Sodium carboxymethyl cellulose Optical brightening agent (DMS-X)

Optical brightening agent (CBS-X)

Anti-foaming agent (DB-100) thio2

Esters Fragrance: Wait

Termamyl SL Sodium perborate TAED

Subtotal

Total

10 11 12 13% W / W% W / W% W / W% W / D 7.76 10.05 7.23 8.36 11.46 16.35 10.68 10.50 27.45 31.61 25.57 26.00 4.28 - 3.99 - - - - 3.14 2.68 - 2.49 2.50 53.63 60.71 49.96 50.50 7.17 15.44 - - - - 31.18 37.10 26.77 12.14 - 5.00 5.35 3.64 2.99 3.00 3.21 3.64 0.99 0.40 1.07 1.21 0.99 1.00 0.80 0.97 0.90 0 , 90 0.05 - - - 0.14 0.20 0.20 0.20 0.85 0.97 0.83 1.00 0.64 0.72 - 0.60 0.32 0.36 - 0 , 30 - - 9.97 - - - 1.99 - 46.37 39.29 50.04 49.50 100.00 100.00 100.00 100.00

73 388 CTE / JA / PL6 Ο 87 3E Example NB 14 15 16 17.% w / w% w / w% w / w% w / w Dodecylbenzenesulfonic acid Alcohol ethoxylate 8.36 8.36 6.16 7.41 (3 moles of EO) 10.50 10.50 8.73 10.50 Marlox FK 64 26.00 26.00 21.62 26.00 Triethanolamine - - 3.40 4.08 Diethanolamine 3.14 3.14 - - Monoethanolamine - - - - Polyethyleneglycol (PEG 200) - - 10,19 - Iso-propanol 2.50 2.50 - - Sub-total 50.50 50.50 50.29 50.49 Zeolite (Wessalith P) - - - Sodium tri-polyphosphate 38.00 30, 63 30.63 30.64 Calcined Soda Sodium Silicate Powder 4.10 '(Soluble C) 3.00 2.99 2.99 2.99 EDTA 0.40 0.99 0.99 0.99 Sodium Carboxymethylcellulose Optical brightening agent 1.00 1.00 1.00 1.00 (DMS-X) Optical brightening agent 0.90 0.90 0.90 0.90 (CBS-X) - - - Anti-foaming agent (DB -100) - - 0.21 - TI02 0.20 0.20 0.20 0.20 Fragrance 1.00 0.83 0.83 0.83 Esters: Esperase SL 0.60 - - - Termamyl SL 0.30 - - - Sodium perborate - 9.97 9.97 9.97 TAED - 1.99 1.99 1.99 Sub-tota l 49.50 49.50 49.71 49.50 Total 100.00 100.00 100.00 100.00

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CTE / JA / PL6 Ο 8 7 3 18 -18- 18 19 20 21% w / w% w / w% w / w% w / w 6.86 8.85 7.38 8.34 9.73 10.74 10.46 10.45 23.17 26.60 25.90 25.95 3.78 - 4.06 - - 3.21 - 3.13 4.63 12.78 12.45 12.47 2.33 - 2.49 2.50 50.50 61.88 62.74 62.84 38.00 28.19 30.26 30.21 4.10 - 3.00 3.00 3.00 1.55 1.50 1.50 0.40 0.40 0, 20 0.40 1.00 0.50 0.50 0.15 0.90 - 0.40 0.50

Example Ns Dodecylbenzenesulfonic acid Alcohol ethoxylate (3 moles of E.O.)

Marlox FK 64 Triethanolamine Diethanolamine Monoethanolamine Polyethylene glycol (PEG 200) Iso-propanol Sub-total

Zeolite (Wessalith P) Sodium Tri-Polyphosphate Calcined Soda Sodium Silicate Powder (Soluble C)

EDTA

Sodium carboxymethyl cellulose Optical brightening agent (DMS-X)

Optical brightening agent (CBS-X) - 0.26 0.25 0.25 0.20 0.15 0.15 0.15 1.00 0.61 0.60 0.60 0.60 - 0.25 0 , 25 0.30 - 0.15 0.15 - 5.11 - - - 1.35 - - 49.50 38.12 37.26 37.16 100.00 100.00 100.00 100.00

Anti-foam agent (DB-100) TI02

Fragrance Esters: Esperase SL Termamyl SL Sodium perborate TAED

Subtotal

Total

Examples 22 to 26

Further liquid detergent concentrates were prepared

CTE / JA / PL6 Ο 8 7 3 "19-

according to the general procedure of Example 10 to 21 using the following ingredients:

Example NE Dodecylbenzene-22% w / w sulfonic acid Alcohol ethoxylate 8.80 (3 moles EO) Alcohol ethoxylate 7.00 (7 moles EO) 8.30 Marlox FK 64 12.60 Triethanolamine Polyethylene glycol 4.70 ( PEG 200) 6.00 Iso-propanol 2.50 Sub-total 49.90 50 r10 23 24 25 26% P / W% w / w% w / w% 11.10 8.80 11.10 11.10 8, 80 7.00 8.80 8.80 11.50 8.30 11.50 11.50 10.90 8.70 10.90 10.90 5.90 4.70 5.90 5.90 12.50 9 , 90 12.50 12.50 2.10 2.50 2.10 2.10 62.80 49.90 62.80 62.80 22.75 - 15.10 15.10 - 20.00 - - 5.95 26.00 17.80 11.90 4.00 2.00 2.00 2.00 0.80 0.20 0.40 0.40 1.00 0.50 0.50 0.50 0.80 0.40 0.40 0.40 0.20 0.20, 20 0.20 0.80 0.40 0.40 0.40 0.60 0.25 0.25 - 0.30 0.15 0.15 - - - - 5.00 - 1.30 37.20 50.10 37.20 37.20 100.00 100.00 100.00 100.00

Zeolite (Wessalith P)

Sodium tri-polyphosphate 38.00

Calcined Soda 5.00 Sodium Silicate Powder (Soluble C) 3.00 EDTA 0.40

Sodium carboxymethylcellulose 1.00

Optical brightening agent (DMS-X) 0.90 TiO2 0.10

Fragrance 0.80 Esters: Esperase SL 0.60

Termamyl SL 0.30

Sodium perborate TAED -_

Sub-total 100.00

Total

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CTE / JA / PL6 Ο 8 7 3 EN -20-

If desired, a small amount of bitter-tasting material, such as Bitrex, may be added to a concentrate according to any of Examples 10 to 26 in order to discourage ingestion of the concentrate by, for example, children. In the case of Bitrex, amounts as low as 0.005% w / w are sufficient for this purpose. &quot; Termamyl &quot; are trademarks

Reference should be made to Notes of Examples 2 to 5 for further explanation of Examples 10 to 26? The words, Wessalith ,,, &quot; Bitrex &quot;, &quot; and registered.

Claims (21)

73 388 CTE / JA / PL6 Ο87 3P. -21- A liquid adjuvant detergent composition comprising a substantially anhydrous liquid organic phase having uniformly distributed therein (i) an amine salt of an anionic surfactant acid containing one or more sulfonic acid groups and ( ii) a finely divided particulate adjuvant, characterized in that it comprises the step of reacting, in an organic phase, the acid form of an anionic surfactant acid containing one or more free sulfonic acid groups with an amine. A process according to claim 1, characterized in that said liquid organic phase comprises a water-soluble organic solvent. A process according to claim 2, characterized in that said water-soluble organic solvent comprises a hydroxyl solvent selected from glycols and low molecular weight alkanols. A process according to claim 2 or 3, characterized in that said water-soluble organic solvent comprises an alkanol containing from 2 to 4 carbon atoms, a polyethylene glycol having a molecular weight in the range of from about 150 to about 600 or a mixture thereof. Process according to any one of claims 2 to 4, characterized in that the composition prepared comprises from about 1% w / w to about 20% w / w of the said water-soluble organic solvent. A process according to any one of claims 1 to 5, characterized in that said amine salt is a salt derived from a monocyclic alkanolamine or heterocyclic amine. A process according to any one of claims 1 to 7, Characterized in that said amine salt is a salt derived from monoethanolamine, diethanolamine, triethanolamine or morpholine. A process according to any one of claims 1 to 7, wherein said anionic surfactant acid comprises an alkylbenzenesulfonic acid in which the alkyl group contains from about 6 to about 20 carbon atoms, a primary or secondary alkylsulfonic acid containing from 10 to about 26 carbon atoms, an alpha-olefin sulfonic acid obtained by the sulfonation of an alpha-olefin containing from about 10 to 22 carbon atoms or a mixture thereof. A process according to any one of claims 1 to 8, characterized in that the composition prepared comprises from about 0.1% w / w to about 25% w / w of said amine salt. A process according to any one of claims 1 to 9, characterized in that said adjuvant comprises sodium meta phosphate, sodium paraphosphate, sodium tri-polyphosphate, sodium silicate, sodium carbonate, a zeolite, trisodium citrate or a mixture of two or more thereof. A process according to any one of claims 1 to 10, characterized in that the composition prepared comprises from about 15% w / w to about 60% w / w of said adjuvant. A process according to any one of claims 1 to 11, characterized in that the composition prepared further comprises at least one non-ionic surfactant. A process according to claim 12, wherein said nonionic surfactant comprises a fatty acid monoethanolamide, a polyoxyalkylene ether of an alkanol, a polyoxyalkylene ether of an alkylphenol or a mixture thereof. A process according to claim 12 or 13, characterized in that the composition prepared comprises from about 0.1% w / w to about 50% w / w of the said surfactants or nonionic surfactant. A process according to any one of claims 1 to 14, characterized in that an amine salt of a sulphated fatty alcohol containing from about 10 to about 26 carbon atoms is further added. A method according to any one of claims 1 to 15, characterized in that a bleach is further added. A process according to claim 16, characterized in that a bleach activator is further added. The composition of claim 17, wherein the composition prepared comprises from about 0.1% w / w to about 15% w / w of a bleach and from about 0.03% w / w to about 5% w / w. % w / w of a bleach activator. 4 A process according to any one of claims 1 to 18, characterized in that an enzyme is further added. A process according to claim 19 characterized in that an enzyme stabilizer is further added. A process according to any one of claims 1 to 20, characterized in that an amphoteric surfactant is further added. Lisboa 26. m. 1991 By S.B. CHEMICALS LIMITED = 0 OFFICIAL AGENT =