DK173111B1 - Laundry Tablets - Google Patents

Description

in DK 173111 B1

Technical area

The present invention relates to laundry detergent tablets which are advantageous in having a good washing effect while being very storage stable and rapidly soluble in the washing water.

Technical background *

Conventionally used laundry detergents can be divided into two main types, liquid and powdery.

In recent years, however, as an alternative to this, a growing focus has been on laundry tablets that offer the advantage of being easy to handle and dispensing in the correct amount.

However, many tablet technical as well as substantive requirements are made for laundry tablets. These requirements often counteract each other and make it very difficult to formulate laundry tablets that are satisfactory at all points.

Thus, laundry tablets should ideally meet the following requirements: have sufficient tablet strength so that they do not crumble or break during storage, transport or handling, be storage stable and able to withstand storage in various climatic conditions with fluctuating temperatures and humidity, be rapidly soluble in the wash water, so that they can exert their effect.

have a good washing effect, which requires a high content of washing active substances, and could optimally exert this washing effect optimally over a wide range of washing programs at different temperatures and water hardness degrees.

Adequate tablet strength can be obtained by increasing the pressure used to compress the laundry tablets. However, increasing the pressure will adversely affect the solubility of the laundry tablets, which is why these properties are difficult to reconcile.

The requirement for quick dissolution of the laundry tablets in the wash! 10 water is further exacerbated by the tendency for environmental, economic and consumer reasons to use less and less water, lower and lower temperatures, and shorter and shorter washing times when washing in washing machines.

The desire for a good washing effect, as mentioned above, requires a high content of detergent, which tends to prolong the decay time of the laundry detergent tablets and to reduce storage stability.

!

Si JP No. 6279799 (LION CORP.) Discloses detergent tablets based on 1 to 50% by weight of an anionic surfactant in the form of a 20 α-sulfo fatty acid derivative and 5 to 60% by weight of an alkali carbonate, which tablets are stated to be readily soluble in water. The alkali carbonate is potassium carbonate or a mixture of potassium carbonate and sodium carbonate in a weight ratio of 100: 0 to 40:60 and preferably has an average particle size of less than 300 μτη, especially of less than 150 μτπ.

JP No. 6108099 (LION CORP.) Discloses highly soluble detergent high wash power tablets comprising 5 to 50% by weight of one or more surfactants, including nonionic surfactants, 10 to 70% by weight of potassium carbonate and H 30 0, 5 to 5% by weight powdered perfume.

tu ni r! No. 3 DK 173111 B1 JP No. 6017099 (LION CORP.) discloses highly soluble detergent high-wash detergent tablets comprising (A) 1 to 50% by weight of an anionic surfactant, (B) 0.1 to 4% by weight of a nonionic surfactant and (C) potassium carbonate in a weight ratio of (B): (A) up to 0.5 and a weight ratio of (B) :( C) up to 0.25.

JP No. 4239100 (LION CORP.) Discloses easily soluble detergent tablets comprising 5 to 50 wt% of one or more surfactants, including nonionic surfactants 10, and 10 to 70 wt% potassium carbonate. The potassium carbonate used preferably has an average particle size of up to 150 μτη.

However, none of these LION writings discloses detergent tablets based on a surfactant system of a non-ionic surfactant and an amphoteric surfactant, and a zeolite-poor or free builder system of a polyfunctional carboxylic acid or a salt thereof, such as citrate, and layer silicate and / or alkali metal silicate and / or zeolite.

From EP No. 0 482 627 A1 (Kao Corporation), laundry detergent tablets comprising potassium carbonate and a nonionic surfactant having an HLB value of 8.0 to 16.0 in a weight ratio of 5 are known. : 1 to 1: 5.

All of the prescriptions disclosed in the document contain relatively large amounts of zeolite and are based on a nonionic surfactant and optionally an anionic surfactant in contrast to the present laundry tablets which are based on a combination of a nonionic surfactant and an amphoteric surfactant as well as a zeolite poor or free builder system of a polyfunctional carboxylic acid and / or a salt thereof, such as citrate, and layer silicate and / or alkali metal silicate and / or zeolite.

4 DK 173111 B1

These known laundry detergent tablets are said to be rapidly soluble in the wash water.

As can be seen from the subsequent comparison experiment, it was found to be very difficult to prepare these 5 tablets in a conventional manner using a tablet machine. Thus, Example 1 and Example 2 of the specification also describe the preparation of tablets by melting and subsequent molding in pressurized cylinders, and in Example 1 molding is printed under pressure for one minute, where the production rate of conventional tablet preparation for comparison is from 25,000 to 90,000 tablets per hour.

Such a casting process will therefore be very inappropriate and uneconomical in the manufacture of industrial scale tablets.

In the comparison experiment, the laundry tablets according to the invention exhibited a superior decay time compared to the laundry tablets known from EP No. 0 482 627 A1.

Thus, it is the object of the present invention to provide storage-stable and rapidly-soluble laundry detergent tablets with high detergent power.

Brief Description of the Invention

This is surprisingly achieved with the laundry tablets of the invention which are characterized in that they comprise: nonionic surfactant 0.1 to 15% by weight amphoteric surfactant 0.1 to 15% by weight of polyfunctional carboxylic acid and / or salt thereof, calculated as trisodium citrate dihydrate, 20 to 50% by weight of layer silicate and / or alkali = 30 thalysilicate and / or zeolite 1 to 30% by weight of potassium carbonate 5 to 70% by weight in 5 and binder and disintegrant and optionally one or more constituents selected from sodium carbonate / bicarbonate and / or potassium carbonate / bicarbonate, enzymes, antifoaming agents, color transfer inhibitors, antigen scavengers, polymers, complexing agents, anionic surfactants and other common adjuvants and additives.

In a preferred embodiment of the invention, the laundry tablets comprise one or more components selected from sodium carbonate / bicarbonate and / or potassium carbonate / bicarbonate, enzymes, antifoaming agents, color transfer inhibitors, antigen deposition agents such as cellulose colloids, e.g. . carboxymethyl cellulose, polymers, anionic surfactants and complexing agents such as phosphonates.

Thus, in a preferred embodiment, the laundry tablets of the invention comprise, in addition to any usual adjuvants and additives, nonionic surfactant 0.1 to 15% by weight of amphoteric surfactant 0.1 to 15% by weight of polyfunctional carboxylic acid and / or salt thereof, calculated as trisodium citrate dihydrate, 20 to 50% by weight of layer silicate and / or alkali metal silicate and / or zeolite 1 to 30% by weight of potassium carbonate 5 to 70% by weight of disintegrant 0.5 to 5% by weight of binder 1 to 8% by weight of sodium carbonate / bicarbonate and / or potassium carbonate / bicarbonate 0 to 10 wt% 30 enzyme 0 to 10 wt% antifoam 0 to 1 wt% color transfer inhibitor 0 to 3 wt% antigen scavenger 0 to 3 wt% 6 DK 173111 B1 polymer 0 to 10 wt% complex binding agent 0 to 10 weight%

DETAILED DESCRIPTION OF THE INVENTION The laundry tablets of the invention are primarily intended for use in ordinary household washing machines, including both "toploader" type washing machines, where the laundry and detergent are inserted into the top of the washing machines in a vertically arranged drum, and the "frontloader" type, wherein the laundry and detergent are introduced into a horizontally arranged drum via a front door.

The "toploader" type washing machines are preferably used in Asia, Australia and the United States, where traditionally low washing temperatures are often used, ranging from 15 to 20 ° C, which makes special demands on the decay time of the laundry tablets.

Washers of the "frontloader" type are especially applicable in 15 Europe. As mentioned before, the trend is towards the use of less and less water consumption combined with shorter and shorter washing times as well as lower and lower temperatures (on average 30 to 60 ° C against earlier 60 to 90 ° C), which also places great demands on the laundry tablets. fall time.

A particular problem when using the laundry washers in the European "frontloader" washers is that the clothes washers in some machine types may have a tendency! to settle in the front door, so that they do not dissolve '25 and come to their full effect. Therefore, when used in such machines, it is important that the laundry tablets dissolve quickly after insertion into the washing drum.

Laundry detergent tablets according to the invention, intended for use in soft, cold water, such as water having a hardness of 30 ° - 7 ° dH and a temperature of 15 - 20 ° C, advantageously have the following composition: 5 7 DK 173111 B1 nonionic surfactant 0.1 to 6 wt.% amphoteric surfactant 0.1 to 5 wt.% polyfunctional carboxylic acid and / or salt thereof, calculated as 5 trisodium citrate dihydrate, 20 to 50 wt.% layer silicate and / or alkali metal silicate and / or zeolite 1 to 10 wt. % potassium carbonate 20 to 70 wt% explosive 0.5 to 5 wt% 10 binder 1 to 5 wt% enzyme 0.25 to 10 wt antigen scavenger 0.25 to 3 wt% antifoaming agent 0 to 1 wt% color transfer inhibitor 0 to 3 wt% Advantageously, the complexing agent 0 to 10% by weight Laundry tablets according to the invention intended for use in hard hot water, such as water having a hardness of 10-20 ° dH and a temperature of 30-60 ° C, advantageously have the following composition: 20 nonionic surfactant 0.1 to 10 wt.% Amphoteric surfactant 0.1 to 10 wt.% Polyfunctional carboxylic acid and / or salt thereof, calculated as trisodium citrate dihydrate, 20 to 40 wt.% Layer silicate and / or alkali metal.

silicate and / or zeolite 5 to 30 wt

potassium carbonate 15 to 40 wt

antigenic agent 0.25 to 3 wt

polymer 1 to 10 weight 30 explosive 0.5 to 5 wt% = binder 1 to 8 wt% enzyme 0.25 to 10 wt% 8 DK173111 B1 antifoaming agent 0 to 1 wt%! color transfer inhibitor 0 to 3 wt% sodium carbonate / bicarbonate and / or potassium * carbonate / bicarbonate 0 to 10 wt% 5 complex binding agent 0 to 10 wt% The laundry detergent tablets of the invention are based on a bu-; fermentation system of a polyfunctional carboxylic acid and / or a salt thereof and layer silicate and / or alkali metal silicate and / or zeolite. Preferably, the laundry detergent tablets are zeolite or ~ 10 zeolite-free, but may, if desired, contain a minor proportion of zeolite, such as 0.1 to 10% by weight, since zeolite, in addition to acting as a builder, acts as a liquid absorbent and thereby contributes to providing a light-flowing powder. .

Zeolite has been dominating the market as a builder component in compact detergents for a number of years due to its good builders, but in recent years it has sought to reduce or avoid its use due to problems, especially in sewage treatment plants due to sludge accumulation. In addition, high concentrations of zeolite can cause problems with discoloration of 20 e.g. dark clothing where the white zeolite particles can be clearly seen.

The laundry tablets are based on a particular surfactant system comprising both nonionic surfactant and amphoteric surfactant, preferably in a weight ratio of 0.1: 1 - 10: 1, such as 0.2: 1 - 5: 1, e.g. 1: 1 - 2: 1. The use of this particular surfactant system in combination with the zeolite-poor or free builder system surprisingly results in a high washing effect combined with good storage stability and fast solubility. As can be seen from the subsequent comparative experiment, the washing effect of these M 30 laundry tablets is fully equal to and even in some cases higher than that of the best products on the market.

- -Λ 3 9 DK 173111 B1

Advantageously, the nonionic surfactant is present in an amount of from 2.5 to 10.0, such as from 3.5 to 8.0, e.g. of from 4.5 to 6.0% by weight and may in principle be selected from all conventional nonionic surfactants usually prepared by condensing a hydrophilic alkylene oxide with a hydrophobic compound. Examples of alkylene oxides include ethylene oxide, propylene oxide and / or butylene oxide, and examples of hydrophobic compounds include alcohols, thioalcohols, diols, fatty acids, fatty acid amides, alkanesulfonamides, alkylamines and alkylphenols.

Among the nonionic surfactants, ethoxylated compounds of primary and secondary fatty alcohols selected from linear fatty alcohols, oxoalcohols and alcohols prepared by the Ziegler process are particularly preferred. fatty alcohols with an equal number of carbon atoms. Particularly preferred are condensation products having 2 to 40 moles of ethylene oxide (EO), preferably 3 to 16 moles of EO per mole of fatty alcohol selected from linear fatty alcohols, such as e.g. C₂ 2jj coconut alcohols, tallow alcohols, oleyl alcohols or other naturally occurring alcohols and mixtures thereof.

Examples of nonionic surfactants are oleyl monoethanolamide + 4 EO and ethoxylated C12-C14 fatty alcohol + 7 EO as well as the short-chain C8_12 alkyl polyglycosides of the so-called APG types which are of vegetable origin. Such compounds are very skin friendly and also environmentally friendly as they are completely biodegradable.

However, petrochemically based surfactants can be used which have a very favorable price level and are available in many different types and variants.

The amphoteric surfactant used is advantageously present in an amount of from 0.5 to 7.0, such as from 1.5 to 6.0, e.g. of from 2.5 to 5.0% by weight and may in principle be selected from all conventional amphoteric surfactants. Examples include betaine derivatives, imidazoline derivatives, alkyl polyamine carboxylates, alkyliminodipropionates etc. Such specific examples should be mentioned oleoampopolycarboxyglycinate, lauramidopropyl betaine and cocosamidopropyl betaine.

In addition to the nonionic surfactant and the amphoteric surfactant, a smaller proportion of an anionic surfactant may also be included in the laundry tablets of the invention if desired. As an anionic surfactant: any anionic surfactant which is conventionally included in laundry detergents and which does not adversely affect the laundry tablets may be used. Thus, too much anionic surfactant can cause the formation of insoluble compounds at higher water hardness levels, which results in a loss of washability.

The polyfunctional carboxylic acid used and / or the salt thereof are advantageously included in an amount of from 20.0 to 40.0, such as from 21.0 to 37.0, e.g. of from 22.5 to 35.0% by weight. Polyfunctional carboxylic acids can generally be defined as those which, in addition to the one mandatory carboxylic acid group, also contain at least one additional functional group selected from carboxylic and hydroxy. Furthermore, the polyfunctional carboxylic acids may also contain nitrogen. Examples of such polyfunctional carboxylic acids include citric acid, nitrilotriacetic acid (NTA), ethylenediaminetetraacetic acid (EDTA) and isoserinediacetic acid (ISDA), of which citric acid M 25 is preferred. Citric acid can be in the form of trisodium citrate dihydrate, anhydrous trisodium citrate and anhydrous monosodium citrate. Particularly preferred is trisodium citrate dihydrate.

'Ϋ - Layer silicate and / or alkali metal silicate and / or zeolite are further included as a mandatory component of the laundry tablets' 1 according to the invention. Advantageously, layer silicate and / or alkali metal silicate and / or zeolite are present in an amount of from 2.0 to 25.0, such as from 5.0 to 22.5, e.g. of from 10.0 to 20.0% by weight. Preferably, layer silicate or a combination is used in P * 11 DK 173111 B1 of layer silicate and a smaller proportion of alkali metal silicate.

An example of alkali metal silicate may be mentioned sodium silicate, preferably sodium silicate having the composition Na 2 O: SiO 2 in the ratio of 1: 1 - 1: 3.5, preferably 1: 2 - 1: 3.5. Also, mixtures of silicates having different alkali content may be used, such as e.g. a mixture of Na 2 O: SiO 2 = 1: 2.5 and Na 2 O: SiO 2 = 1: 2.

As an example of a commercial product, mention may be made of sodium disilicate with the composition Na 2 O: SiO 2 = 1: 2, e.g. provided by 10 Crossfield Chemie B.V., Eijsden, The Netherlands.

As zeolite (aluminum silicate), all known types of aluminum silicates can in principle be used. Examples of such are cited in DK publication no. 151,231, DK no. 154,827 and in EP publication no.

15 289.767.

Particularly preferred as a zeolite component of the laundry detergent of the invention is zeolite A of the formula Na12 (AlO2) ^ 2- (SiO2) 12) xH2O, wherein x = 20-30, preferably x * 27.

The potassium carbonate used is advantageously in an amount of 20 from 10.0 to 50.0, such as from 15.0 to 40.0, e.g. of from 20.0 to 35.0% by weight.

The laundry detergent tablets of the invention, especially those intended for use in hard and / or hot water, may advantageously include a minor amount of sodium carbonate and / or potassium carbonate or alternatively sodium bicarbonate and / or potassium bicarbonate or a mixture thereof, such as in an amount of from 2.5 to 10.0, e.g. of from 4.0 to 7.0% by weight.

Furthermore, one or more constituents advantageously selected from enzymes, antifoam agents, color transfer inhibitors, antigen deposition agents, polymers and complex binding agents are included in the laundry tablets of the invention. period. Such means are quite conventional.

Explosives swell on contact with water, thereby promoting the decay of the tablets. Examples of disintegrants include starch derivatives, cellulose compounds, polyvinylpyrrolidone compounds, polyvinyl polypyrrolidone compounds, bentonite compounds, alginates, gelatin and pectins.

= The amount of explosive typically ranges from 1.5 - 4.0, such as from 1.8 - 3.2, e.g. of from 2.0 to 3.0% by weight.

In addition, to further improve the dissolution time, a smaller amount of an organic carboxylic acid, preferably a polyhydric organic carboxylic acid such as e.g. maleic and hydroxycarboxylic acids malic, citric and tartaric acid, which together with the carbonate and / or bicarbonate used, give a shower effect when the tablets come into contact with water.

Examples of binders include polyethylene glycol, preferably having a molecular weight in the range of 200 - 10,000, glycerol, natural rubbers, e.g. acacia and tragacanth, as well as 20 sugar compounds such as glucose and sucrose. These compounds are discussed in more detail in "Die Tablette" by Dr. W. A.

'Ί Ritschel, published by Cantor KG / Aulendorf, Wurtt, Germany.

The amount of binder typically ranges from 2.0 - 5.0, such as '1', from 3.0 - 5.0% by weight.

Examples of enzymes include mixtures of specifically acting types such as proteases, carbohydrases, esterases, lipases, oxidoreductases, catalases, peroxydases, ureases, isomerases, lyases, transferases, desmolases and nucleases, which in U.S. Pat.

30 3,519,570 and 3,533,139.

Commercial products of such enzymes are most commonly available as aqueous solutions, powders or granules, together with ϋ

II

n

TEN

13 thinners such as sodium chloride, sodium sulfate or certain phosphates. Particularly preferred for use in the laundry tablets of the invention are dust-free granules such as the T granules supplied by Novo Nordisk A / S, 5 Bagswaard, Denmark.

Among these T granules, proteolytic enzymes supplied under the trade names ESPERASE®, SAVINASE® and ALCALASE® are preferred, amylolytic enzymes supplied under the trade name TERMAMYL®, lipolytic enzymes supplied under the trade names "LIPOLASE" and "LIPOLASE" cellulytic enzymes supplied under the trade name CELLUZYME®, and mixtures thereof.

Further examples include the commercial product Durazym, which is a proteolytic enzyme, and the commercial product Duramyl, which is an amylolytic enzyme. These products are very storage stable and are also sold by Novo Nordisk A / S.

The total amount of enzymes may advantageously be in the range of from 0.5 to 8.0, such as from 1.0 to 6.5% by weight.

Examples of antifoam agents include both silicone-free and silicone-based compounds. Of the silicone-based compounds, organopolysiloxane compounds are preferred. An example of a silicone-based organopolysiloxane product is SP 30, a powdered product supplied by Wacker Chemie GmbH, Germany. Also mentioned is DC2-3485, which is a silicone compound and which is provided by N. V. Dow Corning Europe S.A., Brussels, Belgium. If antifoaming agents are included, the amount thereof may advantageously be in the range of from 0.15 to 0.60, such as from 0.20 to 0.55% by weight.

As an example of color transfer inhibitors may be mentioned polyvinylpyrrolidone (PVP), e.g. in the form of the product SOKALAN® HP 50, supplied by BASF AG, Ludwigshafen, Germany. If 14 color transfer inhibitors are included, the amount thereof can typically be in the range of from 0.01 to 1.5, such as from 0.01 to 1.0, e.g. of from 0.1 to 0.5% by weight.

Antigen-depositing agents are advantageously included in the laundry detergent tablets according to the invention to prevent re-deposition of dirt particles. Examples include cellulose colloids such as carboxymethyl cellulose and methyl hydroxycellulose. The amount of antigen scavenger is typically in the range of from 0.5 to 2.5, such as from 1.0 to 2.0% by weight.

As examples of polymers which are advantageously included in laundry tablets intended for washing in hard and / or hot water, mention may be made of polyanionic polymers such as e.g. those disclosed in U.S. Patent Nos. 3,308,067, 3,723,322, 4,144,226 and 4,146,495, and GB Patent Nos. 1,596,756.

Among these, homo- and / or copolymeric carboxylic acids and their sodium or potassium salts are preferred. The amount of polymer used is typically in the range of from 1.0 to 9.0, such as from 3.0 to 7.0, e.g. of from 4.0 to 6.0% by weight.

Examples include polymerisates of acrylic acid, hydroxyacrylic acid, maleic acid, itaconic acid, mesaconic acid, acotinic acid, methylene malonic acid, citric acid and the like, and copolymerates of the above carboxylic acids mutually or with other ethylenically unsaturated compounds such as ethylene, propylene , isobutylene, vinyl alcohol, vinyl methyl ether, furan, acroline, vinyl acetate, acrylamide, acrylonitrile, methacrylic acid and crotonic acid.

The molecular weight of the homo- and copolymers ranges from approx. 1,000 to 1,000,000, preferably from 2,000 to 250,000 and most preferably from 5,000 to 100,000.

As the polycarboxylate, the sodium salt is particularly preferred by an acrylic / maleic acid copolymer having a molecular weight of approx. 70,000.

~ SOKALAN® CP 5, supplied by BASF AG, Ludwigshafen, Germany 11 15 DK 173111 B1 country, is an example of a commercial product with such a composition. Also mentioned are the Norasol® products supplied by NorsoHaas, France, such as Norasol WL 2B, which is a co-granule of approx. 30% polyacrylate having a molecular weight of 5 4,500 and bicarbonate.

Furthermore, if desired, complexing and precipitating agents such as EDTA (ethylenediaminetetraacetic acid), DETPA (diethylenetriamine pentaacetic acid), HEEDTA (hydroxyethylethylenediaminetriacetic acid), ISDA (iso-serine diacetic acid), and phosphonates may be included. phosphonic acids or salts thereof. In particular, an example of a phosphonate is Dequest 2016 D, which is tetrasodium-1-hydroxyethylene (1,1-diphosphonate) with an active acid content of approx. 60% and delivered by Monsanto S.A., Brussels, Belgium. For further discussion of complex binding agents, reference is made to DK No. 167,363.

Other ingredients which may be included in the laundry tablets of the invention, if desired, are additional conventional tablet adjuvants, optical white, bleach, bleach activators, dirt repellent agents, antifouling agents, fabric softeners, dyes, deodorants and deodorizing agents.

The laundry tablets of the invention are prepared in a very conventional manner.

Thus, e.g. a base powder fraction consisting of polyfunctional carboxylic acid and / or salt thereof, layer silicate and / or alkali metal silicate and / or zeolite, potassium carbonate, binder and, where appropriate, sodium carbonate / bicarbonate and / or potassium carbonate / bicarbonate, color transfer inhibitor inhibitor, color transfer inhibitor, color transfer inhibitor, polymer as well as any other powdered components.

16 DK 173111 B1

Further, a fraction of liquid nonionic surfactant is provided, where, if the surfactant is in solid form, heating to above the melting point, e.g. to approx. 40 - 60 ° C, such as 45 - 55 ° C.

Finally, a residual fraction consisting of amphoteric surfactant in powder form and disintegrant, as well as, where appropriate, enzyme and other ingredients such as antifoam agents, which should be exposed to the least heat and stress during processing, should be mixed for stability.

The surfactant fraction is sprayed onto the ground powder extraction in a suitable mixer with continuous stirring for approx. 5 to 18 minutes depending on the mixer used, after which in the residual fraction is added with stirring for a further approx. 2 - 10 minutes. This results in a lightly flowing, slightly granular powder with a weight of approx. 600 - 900 g / l.

The powder mixture is compressed in a tablet machine, e.g. KORSCH type ΕΚ III, for tablets of the desired weight and size.

The following examples further illustrate the invention.

Example 1 In the manner described above, laundry washes tablets according to the invention were prepared with the compositions CL1 - CL11 listed below. The laundry tablets were compressed on a KORSCH ΕΚ III tablet machine using Z 25 using a pressure of 50 - 60 kN. The tablets had a “! circular cross section with a diameter of 40 mm, a height of 12 - tZ 14 mm and a weight of 25 g.

Tablet strength, decay time, and volume increase during storage were measured for each of the prepared laundry tablets, and are also listed in Table 1 below.

- =

"TSI

T3i

"-" NI -..... vm T = S [_ __ 17 DK 173111 B1

Tablet strength was measured by vertical penetration down the middle of the tablet at a rate of 50 mm / min with a flat 8 mm 0 steel piston using a Holland CT5 tablet strength test apparatus, and both the initial tablet strength and 5 tablet strength after storage under accelerated aging conditions at 35 ° C and 75% RH for 1 week, 2 weeks and 4 weeks were measured.

When curing the laundry tablets within the first 24 hours, a certain increase in pressure is allowed, but the pressure should not then increase substantially further during storage as the dissolution time can thereby be inappropriately increased.

The decay time was measured by placing the tablet in a stainless steel basket of circular cross section with a diameter of 50 mm. The steel basket is placed in a 1000 ml beaker containing 15 900 ml of 20 ° C thermostat water (11 ° dH). Stir at 1000 rpm.

The tablets have decayed when no tablet residue can be observed in the wire basket. Both the initial decay time and the decay time after 1, 2 and 4 weeks of storage under accelerated aging conditions at 35 ° C and 75% RH were measured. The decay time must not be significantly increased during storage.

Finally, the laundry volume tablets' percentage volume increase was measured using a Mitutoyo slider after storage under accelerated aging conditions at 35 ° C and 75% RH for 4 weeks.

25 The percentage increase in the volume of the laundry was to be as small as possible, indicating good storage stability.

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2 n OS «O-ι O fN o <r ^> 21 DK 173111 B1

Footnotes to Table 1:

Citrate ADM fine: trisodium citrate dihydrate, fine granules, supplied by Archer Daniels Midland Company, Kent, UK = 5 Citrate Cadot-fine: trisodium citrate dihydrate, fine granules, supplied by Gadot,

Israel K2CO3. NDH. granules (coarse): potassium carbonate, 99,100 granules, supplied by Des Proanits 10 Chemique, Harbonnieres, France K2CO3. SCPA (fine): potassium carbonate, fine granulate, supplied by SCPA, Paris Cedex, France SKg - $ _ irel; 15 layer silicate in grind form, grinder SKS-6, supplied by Hoechst AG, Frankfurt am Main, Germany SKS-6 powder: layer silicate in powder form, supplied by Hoechst AG, Frankfurt am Main, Germany 20 SKS-6 granulate: layer silicate in granular form, supplied by Hoechst AG, Frankfurt, Germany

Ψ: H

Soap HB 3: -in soap granules HB3, based on vegetable oils, supplied by '25 Hirtler GmbH, Heitersheim, Germany PEG 6000: polyethylene with a molecular weight of 6,000 mwm wm 22 DK 173111 B1

Amfolak X07-SD8Q: oleoampopolycarboxyglycinate, 80% active content, provided by

Akzo Nobel Surface Chemistry AB, Stenungsund, Sweden OMA-4: 5 oleyl monoethanolamide + 4 EO, supplied by Akzo Nobel Surface Chemistry AB, Stenungsund, Sweden

Wessalith CD: 71.0% zeolite A, 20.5% water, 5.4% polycarboxylate and 2.4% non-ionic surfactant (ethoxylated fatty alcohol), provided by Degussa 10 AG, Frankfurt, Germany

Imbentin AG124s / 060: ethoxylated lauryl myristyl alcohol, supplied by Dr. W. Kolb AG, Hedingen, Switzerland

Tinopal CBSX: 15 optical white, supplied by Ciba-Geigy, Basel, Switzerland Alcalase: proteolytic enzyme, supplied by Novo Nordisk A / S, Bagswaard, Denmark

Sokalan CP7: 20 acrylic acid / maleic acid copolymer in the form of the sodium salt having a molecular weight of approx. 50,000, supplied by BASF AG, Ludwigshafen, Germany

Sokalan CP5: acrylic acid / maleic acid copolymer in the form of the sodium salt 25 having a molecular weight of approx. 70,000, provided by BASF AG,

Ludwigshafen, Germany

Norasol WL 2B: co-granulate of 30% active LMW 45 N - polyacrylate with a molecular weight of 4,500 and bicarbonate, supplied by NorsoHaas S.A., 23 DK 173111 B1 j Verneuil-en-Halatte, France

Avicel PH 200:

microcrystalline cellulose, provided by FMC Corp., Philadelphia, USA

5 Collidone: polyvinylpyrrolidone, 80% active content, supplied by BASF AG, Ludwigshafen, Germany i = Pluriol E 1500: polyethylene glycol of molecular weight 1500, supplied by BASF AG, 10 Ludwigshafen, Germany

Thermosyl: amylolytic enzyme, supplied by Novo Nordisk A / S, Bagsvær, Denmark

Lipolasa ·· 15 lipolytic enzyme, supplied by Novo Nordisk A / S, Bagswaard,

Denmark

Lipolase Ultra: lipolytic enzyme, supplied by Novo Nordisk A / S, Bagswaard,

Denmark 20 Savinase S.O Tx ·.

proteolytic enzyme, supplied by Novo Nordisk A / S, Bagswaard, Denmark CMC: carboxymethyl cellulose

M

; 25 DC2-34B5: silicone-based foam damper, supplied by N.V. Dow. Corning Europe S.A., Brussels, Belgium F * 5 m - 24 DK 173111 B1

Anti-foam 5P3Q: silicone-based organopolysiloxane, supplied by Wacker Chemie GmbH, Germany

Example 2 5 This example illustrates an experiment conducted at an independent institute, CTTN-IREN INSTITUTE, Ecully Cedex, France, to compare the washing effect between the laundry detergent tablets and one of the best products on the market, Persil Megaperls Color from Henkel. The latter 10 product is in the form of beads and has a zeolite content of more than 30%, an anionic surfactant content of 5 to 15%, a nonionic surfactant content of 5 to 15% and a polycarboxylate and soap content of less than 5% (according to the labeling on the packaging).

The following test conditions were used:

Washing machine: FOM 71 Washer

Program: Normal wash (without prewash)

Temperature: 40 ° C and 60 ° C

Water Hardness: 28 * F (= 15.7 ° dH) (Ca: Mg = 4: 1) 20 Quantity of clothing: 3.5 kg of normally soiled clothing

Amount of water: 20 1 in the main wash

Number of washes: 3, ie. the numerical values are an average of 24 measurements, with each test cloth measured in 4 x 2 areas. 25 The results are shown in the following table 2. The reflection values given in the table indicate how effective the laundry detergent is in removing the impregnated stains. A high value corresponds to a good efficiency, with the theoretically highest possible value being 100 corresponding to a completely white surface.

DK 173111 B1

In addition, the degree of whiteness was measured spectrophotometrically by repeated washing of a white piece of fabric. The higher the value measured, the higher the degree of whiteness.

; 11 11 ...... Ta ~ * S35 t <9 m

Table 2 26 DK 173111 B1

Dirt Code for Persil CL 9 Persil CL 9 type test cloth Mega- 2x25 g Mega- 2x25 g peris tablet- peris tablet- 80 g ter 80 g ter beads beads

___40 ° C__40 ° C__60 ° C__60 ° C

Pigment Test Stains Fabric * 32.7 37.5 55.6 55.9 on cotton WFK 10 C__32.0 ____ 34 ^ 4 ____ 72.0__76.5 IEC 106__28.1__28.6__41.1__41.2 EMPA 101__22.4__25.8__35.3__32, 8

Average __28.8 31.6__51.0__51.6

Hi <. *?, <>> 1 .., y j .......... A .A ...... "... j r ~,.

Pigment Test Stains Fabric ** 41.0 30.0 59.8 41.1 on Blend WFK 20 C__22,9__29.8__25.1__39.1 flbre EMPA 104__22.1 ___ 27.6__34.2__39.3

Average 28.7 29.1 39.7 39.8 ............. rhl ^ Ax ...........

Protein EMPA 111__65,3__94,1__89,1__99.6 spots EMPA 112__38.3 47.5 52.9__52.5 EMPA 116__49.8__58.6__63.4__67.8 __Average 51.1 66.7 68.5 73.3. ...... FMI. ..i.— - * - - - »* .... 'j_ v .... -v ..? ..'... 1.14 An1

Pale CTTN TYPE

0.0 0.0 0.0 0.0 Good spots EMPA 222__4 / 7__2 ^ 4__16.5__11.6 EMPA 114__20.4__9.0 24.1__9.8 ^^ - 1 '^ Average 8_ 3 ^ 8 1 ^ , 5_7.1 ^

Whiteness_ EMPA 221 5.7 5.5 10.4 10.3 27 DK 173111 B1

Footnote to Table: i

Test cloth Smudstvoe

Test Fabric1 Vegetable and mineral oil, starch, carbon black, oleic acid, cotton morpholine 5 WFK 10 C Standard mud on cotton IEC 106 Mineral oil and carbon black on cotton EMPA 101 Sod / vege tabular oil on cotton I Test Fabric2 Vegetable and mineral oil, starch , carbon black, oleic acid, morpholine on blend fiber WFK 20 C Standard blend on blend fiber EMPA 104 Olive oil and carbon black on blend fiber EMPA 111 Blood EMPA 112 Cocoa 15 EMPA 116 Blood, milk and cocoa on cotton CTTN type The EMPA 222 Untreated bleached) cotton EMPA 114 Wine EMPA 221 White cotton without dirt] 20 As can be seen from the results, the laundry detergent tablets according to the invention exhibit a full wash and even effect: slightly better than Persil Megaperl's Color. This is all the more surprising since a significantly smaller surfactant content is used in the laundry tablets of the invention compared to Persil Megaperl's Color. Thus, a total of 5.0 g of surfactant used in CL9 is used, while in the amount of Persil Megaperls Color used a total of 8 to 24 g of surfactant is included (according to the labeling on the packaging). The degree of whiteness is about the same for both products, with: h 30 as expected, a tendency for higher whiteness is seen by increasing n n 49 2 :: · Ti 28 DK 173111 B1 of the washing temperature.

Example 3 The present example illustrates an experiment that has been made to compare the washing effect between the laundry tablets of the invention and two of the best products on the market, Persil Megaperls Color from Henkel and Ariel Futur Color from Procter & Gamble. Ariel Futur Color, which is a powder product, contains 5 to 15% anionic surfactants, 5 to 15% nonionic surfactants, 5 to 15% polycarboxylates, 15 to 30% 10 zeolites and less than 5% phosphonates (according to packaging labeling) .

The following test conditions were used:

Washing machine: Construction technician Oko-matic WA 1200

Program: Normal wash (without prewash)

Temperature: 40 ° C

Water hardness: 25 ° dH

Quantity of clothes: 3.5 kg clean terry towels

Test cloths: Pre-impregnated clothing pieces 10 x 10 cm, from WFK Krefeld, Germany 20 Number of washes: 6, ie. the numerical values given in the table are an average of 54 measurements, each test cloth being measured in 3 x 3 areas

Spectrophotometer for measuring reflection values: Minolta CR 200

The results are shown in the following Table 3. The reflectance values given in the table are indicative of how effective the laundry tablets are in removing the impregnated stains. A high value corresponds to a good efficiency, with the theoretically highest possible value being 100 corresponding to a completely white surface.

29 DK 173111 B1

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30 DK 173111 B1

As can be seen from the results, the effect of the tea-washing tablets in question is almost equal to the known products for the tested types of dirt. This is a surprisingly good result, since a significantly smaller surfactant content is used in the laundry detergent tablets herein compared to the known products. Thus, CL9 contains 5.0 g surfactant and CLIO 5.1 g surfactant, while Ariel Futur Color contains a total of 8 to 24 g and Persil Megaperls Color from 8.4 g to 25.2 g (i according to the markings on the respective packaging 10).

EksempeJ. The present example and the following Examples 5 and 6 illustrate experiments which have been made to compare the washing effect of the laundry tablets according to the invention and the detergent known from EP No. 0 482 627 (KAO).

In the experiments, the following formulations were used, the recipes being in powder form, since it was difficult to prepare tablets using the ones in EP no.

0 482 627 specified recipes.

DK 173111 B1 31

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The following test conditions were used:

Washing machine: Toploader, Goldstar 7.2 kg WF-1505AHP

Program: Main wash 12 min.

Temperature: 20 ° C

5 Water hardness: 10 ° dH

Quantity of clothing: 1.5 kg of normally soiled clothing

Number of washes: 3, ie. each given numerical value is a mean of 27 measurements, each test cloth being measured on each 3x3 area 10 Spectrophotometer for measuring reflection values: Minolta CR 200

The results are shown in Table 4 below.

Table 4 15 Dirt type Fer wash KAO 1.1 CL 8 ___50 g powder 50 g powder

Standard mud on cotton__38,50__55,89__54.18

Standard dirt on breathable fibers__50,66__70,20__66,81 20 Skin grease on cotton 38,31 61, 57 57,85__ '1 in Blood, milk, ink. In Cotton__12,80__35,38__37.00 1 Blood on Cotton__21,64__66,36 ___ 62.22 in Cocoa on Blend - 25 Fiber__51.8__70,60__68.21

Pigment / Olie__50,51__68,18__66,82

Oil / Pigment / Mælk__50,84__65,63__64,98

Average __39,39__61,73__59.76 1 "a r! I * Ί :: m 34 DK 173111 B1

As can be seen from the above table, the detergent according to EP 0 482 627 (KAO II) showed a slightly better washing effect in the types of dirt examined than the laundry detergent tablets according to the invention. In this connection, it should be mentioned that 5 KAO 1.1 includes a total amount of surfactant of 9.7 g, whereas in CL8 only a total of 5.0 g of surfactant is included.

Bfcsempal · „5, In the same manner as described above in Example 4, another comparative experiment was performed, however, using the following test conditions:

Washing machine: Construction technician Oko-matic WA 1200

Temperature: 40 ° C

Program: Normal wash (without prewash)

Water hardness: 18 ° dH

15 Quantity of clothes: 2 kg of normally soiled clothing + 1.5 kg of clean terry towels

Number of washes: 3, ie. each given numerical value is an average of 27 measurements, each test cloth being measured on each 3x3 area 20 Spectrophotometer for measuring reflection values: Minolta CR 200

The results are shown in Table 5 below.

35 DK 173111 B1

Table 5

Dirt Type Before KAO 1.1 CL 8 wash 50 g powder 2 x 25 g tablets

Standard dirt of 5 cotton__38.50__57, 56__51.70

Standard Mud on Blend Fibers 5 0.66 _66.06__64.73 10 Skin Fat on Cotton__38,31__73,46__62.10

Blood, milk, ink on cotton 12,80__43,71__47,77 15 Blood on cotton 21,64__67,82__72.03

Cocoa on blend fibers 51.88 68.77 ___ 63.52 Pigment /

Oil 50.51__67.01 ____ 65.84

Oil/

Pigment / Milk__50,84__79,75__78.23 Average 39.39__65.52__63.24

As can be seen from the above table, the detergent * according to EP No. 0 482 627 (KAO 1.1) showed a slightly better washing effect I in the soil types examined than the laundry detergent tablets according to the invention. In this connection, it should be mentioned that 30 KAO 1.1 contains a total amount of surfactant of 9.7 g, whereas in CL8 only a total of 5.0 g of surfactant is included.

Example 6 In the same way as described above, another comparative experiment was performed using the following test conditions, however, the washing was carried out at 60 ° C.

-II

«Washing machine: Bauknecht Oko-matic WA 1200 u 36 DK 173111 B1

Temperature: 60 ° C

Program: Normal wash (without prewash)

Water hardness: 18 ° dH

Quantity of clothes: 2 kg of normally soiled clothing + 1.5 kg of clean 5 terry towels

Number of washes: 3, ie. each given numerical value is an average of 27 measurements, each test cloth being measured on each 3x3 area

Spectrophotometer 10 for measuring reflection values: Minolta CR 200

The results are shown in Table 6 below.

37 DK 173111 B1

Table 6

Dirt type Fer wash KAO 1.1 CL 8 _____5 0 g powder 50 g powder

Standard mud 38.50 60.78 62.35 on cotton____ 5 Standard mud 50.66 68.16 65.77 on blend fiber____

Skin fat on body 63.74 moth ____ 38,31__75,75__ 10 Blood, milk, 12.80 47.88 53.68 ink on cotton____

Blood on Cotton 77.96 __21.64__71.13__

Cocoa of 51.88 69.58 64.98 blend fibers Pigment / Oil__50.51__69.69 70.54_

Oil / Pigment / 50.84 80.99 82.30 Milk ______

Average t__39.39 ___ 67.99__67.67_

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"'rvm 38 DK 173111 B1

As can be seen from the results in the above table, the detergent known from EP No. 0 482 627 (KAO 1.1) exhibits a washing effect comparable to that of the laundry detergent tablets of the invention in the types of dirt examined.

5 This is a surprisingly good result, since the total amount of surfactant in KAO 1.1 is significantly higher than the total amount of surfactant in the laundry tablets here.

The present example illustrates an experiment made to compare the dissolution time of the laundry tablets of the invention (CL 8) with the laundry detergent according to EP No. 0 482 627 (KAO 1.1).

In the experiment, 2 x 25 g CL 8 tablets and 2 x 25 g KAO 1.1 tablets were used.

The dissolution time was measured by washing in a Bauknecht Oco-matic WA 1200 washing machine using a normal washing program at 40 ° C, using a water volume of approx. 10 1 in the main sink. The tablets were placed in a large mesh wash bag of 18 x 10 cm during the dissolution test to prevent the tablets from settling in the washing machine door. At the sink, 3.5 kg of clean terry towels were included.

The results are shown in Table 7 below.

Table 7 39 DK 173111 B1

Dissolution time - residual amount of tablet in% as a function of time

Time '; (sdi)' 14 '.! J - A <'<* · - <vt. »>. j, .- '- Λ .....

5 0__100% __ 100% _ _2__90% __ 110% _ _4__54% __ 99% _ _6__12% __ 96% _ _8__0% __ 89% _ 10 10__0% __ 82% _ 12__0% __ 68% _ 14__0% __ 62% _ 16__0% __ 57% __ 18__0% __ 50 % _ 15 20__0% __ 44% _ 22__0% __ 40% _ 24__0% __ 37% __ 26__0% __ 26% _ 28 0% __ 23% _ 20 As shown in the experiment conducted 2 hours after] preparation, the KAO 1.1 tablets were very long about being -j dissolved. At the start of the 1st rinse cycle after 28 minutes, ;; Thus, 1 still had a residual amount of 23% corresponding to a light weight loss of 10.8 g. The laundry tablets according to the invention, on the other hand, were completely dissolved after 8 minutes.

: i. 32 ti? M i. 1} 1i

Claims (8)

40 DK 173111 B1 Laundry tablets, characterized in that they comprise 5 nonionic surfactants 0.1 to 15 wt% amphoteric surfactant 0.1 to 15 wt% polyfunctional carboxylic acid and / or salt thereof, calculated as trisodium citrate dihydrate, 20 to 50 wt% 10 layer silicate and / or alkali metal silicate and / or zeolite 1 to 30 wt% potassium carbonate 5 to 70 wt% and binder and disintegrant and optionally one or more constituents selected from sodium carbonate / bicarbonate and / or potassium carbonate / bicarbonate, enzymes, antifoam agents, color transfer inhibitors, antigen scavengers, polymers, complexing agents, anionic surfactants and other usual adjuvants and additives. Laundry tablets according to claim 1, characterized in that, in addition to any usual adjuvants and additives, they comprise non-ionic surfactant 0.1 to 15% by weight of amphoteric surfactant 0.1 to 15% by weight of polyfunctional carboxylic acid and / or salt thereof, calculated as trisodium citrate dihydrate, 20 to 50 wt. * layer silicate and / or alkali metal silicate and / or zeolite 1 to 30 wt. * potassium carbonate 5 to 70 wt.% explosive 0.5 to 5 wt. * binder 1 to 8 wt.% sodium carbonate / bicarbonate and / or potassium carbonate / bicarbonate 0 to 10 wt% enzyme 0 to 10 wt% 35 antifoaming agent 0 to 1 wt% color transfer inhibitor 0 to 3 wt% 41 to 17 wt% antigen scrubber polymer 0 to 10 wt * complex binding agent 0 to 10 weight * Laundry tablets according to claim 1, characterized in that, in addition to any usual adjuvants and additives, they comprise non-ionic surfactant 0.1 to 6 wt.% Amphoteric surfactant 0.1 to 5 wt. calculated as trisodium citrate dihydrate 20 to 50 wt. * layer silicate and / or alkali metal silicate and / or zeolite 1 to 10 wt. * potassium carbonate 20 to 70 wt.% explosive 0.5 to 5 wt. 0.25 to 10% by weight antigen scavenger 0.25 to 3% * Antifoam 0 to 1% 20 Color Transfer Inhibitor 0 to 3% * Complex Binder 0 to 10% * Laundry tablets according to claim 1, characterized in that, in addition to any usual adjuvants and additives, they comprise non-ionic surfactant 0.1 to 10% by weight of amphoteric surfactant 0.1 to 10% by weight of polyfunctional carboxylic acid and / or γξ salt thereof. , calculated as trisodium citrate dihydrate, 20 to 40% by weight of layer silicate and / or alkali metal silicate and / or zeolite 5 to 30% * potassium carbonate 15 to 40% * «in explosive 0.5 to 5% * in 3. binder 1 to 8 wt * enzyme 0.25 to 10 wt * W1 IS antigen scavenger 0.25 to 3 wt * m m m fm 42 1 to 10 wt polymer * sodium carbonate / bicarbonate and / or potassium carbonate / bicarbonate 0 to 10 weight * antifoam 0 to 1 weight * 5 color transfer inhibitor 0 to 3 weight * complex binding agent 0 to 10 weight * Laundry tablets according to claim 1, characterized in that, in addition to any usual adjuvants and additives, they comprise 10 nonionic surfactants 2.5 to 8 weight * amphoteric surfactant 0.5 to 7 weight * polyfunctional carboxylic acid and / or salt thereof, calculated as trisodium citrate dihydrate, 20 to 40 weight * 15 layer silicate and / or alkali metal silicate and / or zeolite 2 to 25 weight * potassium carbonate 10 to 50 weight * antigen scavenger 0.5 to 2.5 weight * explosive 1.5 to 4 weight * 20 binder 2 to 6 weight * enzyme 0.5 to 7 weight * antifoam 0 to 0.8 weight * color transfer inhibitor 0 to 1.5 weight * sodium carbonate / bicarbonate and / or 25 potassium carbonate / bicarbonate 0 to 9 weight * polymer 0 to 9 weight * complexing agent 0 to 10 weight * Laundry tablets according to claim 1, characterized in that, in addition to any usual adjuvants and additives, they comprise non-ionic surfactant 4.5 to 6.0% by weight amphoteric surfactant 2.5 to 5.0% by weight citrate, calculated as trisodium citrate dihydrate, 22.5 to 35.0 wt * 5 layer silicate and / or alkali metal silicate 10.0 to 20.0 wt% potassium carbonate 20.0 to 32.0 wt * explosive 2.0 to 3.0 wt% binder 3.0 to 5.0 weight * enzyme 1.0 to 6.5 weight * 10 cellulose colloid 1.0 to 2.0 weight * polymer 4.0 to 6.0 weight * complex binding agent 0 to 10 weight * antifoaming agent 0 to 0.55% by weight color transfer inhibitor 0 to 0.5% by weight sodium carbonate / bicarbonate and / or potassium carbonate / bicarbonate 0 to 7.0% by weight : Laundry tablets according to any one of the claims: I - 6, characterized in that the nonionic surfactant is selected from the condensation products of a hydrophilic alkylene oxide with a fatty alcohol, a fatty thio alcohol, a fatty acid, a fatty acid amide, an alkanesulfonamide. , an alkylamine or an alkylphenol and alkyl polyglycosides. IJ Laundry tablets according to any one of claims 1-7, characterized in that the amphoteric surfactant is selected from oleoampopolycarboxyglycinate, lauramidopropyl betaine and cocosamidopropyl betaine. * «..... T * l li m 'IH m F1¾ r" T5 r "-vm