JP2002517559A - Detergent tablet - Google Patents

Abstract

  (57) [Summary] The present invention is a compressed granular detergent detergent tablet comprising a surfactant and / or a builder and / or a bleach and optionally other detergent components, said detergent tablet comprising potassium carbonate hemihydrate and Disclosed are tablets characterized by comprising sodium sesquicarbonate.

Description

DETAILED DESCRIPTION OF THE INVENTION

TECHNICAL FIELD [0001] The present invention generally relates to a compression molded article having cleaning properties. Washing molded articles include, for example, laundry detergent tablets, dishwasher tablets, tablets for cleaning hard surfaces,
Bleach tablets, water softener tablets or dyeing tablets for washing machines or dishwashers are included. In particular, the present invention relates to a laundry detergent tablet (hereinafter simply referred to as a detergent tablet) used for washing in a home washing machine.

[0002] Detergent tablets are widely described in the prior art literature and are becoming more and more popular with consumers because of their ease of introduction. Tablet detergents have several advantages over powder detergents. Tablet detergents are easy to put and handle, and have a compact structure, which is advantageous for storage and transportation. As a result, detergent moldings are also extensively described in the patent literature. One problem that often arises when using detergent tablets is the inadequate rate of tablet disintegration and dissolution under the conditions of use. Because sufficiently stable (ie, dimensionally stable and puncture resistant) tablets cannot be manufactured without relatively high pressure, the tablet components are significantly compressed, thus delaying tablet disintegration in the wash liquor,
As a result, the release of the active substance in the cleaning process is excessively slow. The delay in tablet disintegration has the further disadvantage that regular detergent tablets cannot be poured into the washing process from the detergent chamber of a home washing machine. This is because the tablets do not disintegrate fast enough into secondary particles that are small enough to be poured into the washing tub of the washing machine from the detergent input chamber. Also, manufacturing tablets on an industrial scale is complicated. This is because the mixture to be tableted must be accurately measured in volume and then compressed. As the volumetric dose fluctuates, the tablets are compressed to a constant outer size, so that tablets with less premix are softer than average hardness and tablets with more premix are harder. As a result, variations in tablet hardness can result in mechanically unstable tablets at one extreme, and completely insoluble tablets at the other extreme.
The extent of this variation is also affected by the premix. When the tableting pressure of the tableting machine on the premix is plotted against the dissolution rate of the obtained tablet, a curve containing more or less steep straight lines depending on the granular premix according to the above-described conflicting properties is obtained. ,can get. For very steep curves, negligible changes in tableting pressure result in large fluctuations in disintegration time which have a very detrimental effect on mass production of tablets. Therefore, the curve of "tablet pressure-disintegration time" should be flat so that a tablet can be obtained that is stable to an acceptable degree and rapidly dissolves despite the fluctuation of the tablet pressure. It is desirable to produce or improve the premix in an efficient manner.

[0003] Many solutions have been developed in the prior art to overcome the conflicting properties between tablet hardness (ie transport and handling stability) and easy disintegration. One solution, which has become particularly known from the pharmaceutical arts and has been extended to detergent tablets, is that certain disintegrants that facilitate access to water and swell and disintegrate or otherwise disintegrate on contact with water It is to incorporate. Other solutions proposed in the patent literature include tableting premixes with a particular particle size, separating one component from another, and binding individual components or the entire tablet with a binder. Based on coating.

The use of potassium carbonate in combination with other substances to improve the solubility of detergent tablets or compacted detergents or laundry / washing aid moldings,
Are known. For example, European Patent Application EP 482 627 (Kao Corporation) discloses a detergent tablet having improved solubility because it contains a special nonionic surfactant and potassium carbonate in a predetermined weight ratio. It has been described.

[0005] European patent application EP 799 886 (Cleantabs A / S) contains 0.1 to 15% by weight of a nonionic surfactant and the same amount of an amphoteric surfactant, 20 to 50% by weight of a polybasic carboxylic acid or Containing its salt, 1-30% by weight of builder and 5-70% by weight of potassium carbonate,
Detergent tablets that are hard, puncture resistant, but dissolve quickly are described.

The use of potassium carbonate in detergent tablets is described in Japanese Patent Application JP 6279799,
It is also described in JP 6108099, JP 6017099 and JP 4239100 (all Lion Corporation). The tablets disclosed in these documents contain high amounts of potassium carbonate.

The above references only mention the use of the commercially available anhydrous form of potassium carbonate. That is, both of the above documents disclose the use of a composition having a hydrate, such as potassium carbonate 1.5 hydrate, to resolve the conflicting properties between tablet hardness and dissolution rate. Absent. Furthermore, no prior art discloses the use of sodium carbonate sesquihydrate.

[0008] The problem to be solved by the present invention is to provide a detergent tablet having the desired properties of having a high tablet hardness and mechanical stability while having a favorable disintegration rate. . In particular, the physical properties of the premix to be compressed must be such that the "tablet pressure-disintegration time" curve is flat, i.e., slight variations in the tablet pressure are significant changes in the solubility of the tablet. Should be positively influenced to the extent that they do not

[0009] The above-mentioned problem is solved by adding potassium carbonate 1.5 hydrate and / or
Alternatively, it can be solved by adding sodium sesquicarbonate.

The present invention is a compressed granular detergent detergent tablet comprising a surfactant and / or a builder and / or a bleaching agent and optionally other detergent components, said detergent tablet comprising potassium carbonate 1.5 water. A tablet is provided, which comprises a hydrate and / or sodium sesquicarbonate.

According to the invention, potassium carbonate 1.5 hydrate and / or sodium sesquicarbonate maintain the properties of the premix to be tableted, while the solubility of the resulting tablets remains substantially constant and It has been found that it can be improved to be always within acceptable limits over a wide range of tableting pressures. This effect occurs independently of the rest of the composition of the detergent tablet. By using the above compounds in premixes of different composition, from simple water softener or bleach tablets to complex composition tablets or laundry detergent tablets for machine dishwashing, washing with the above mentioned advantages Tablets can be manufactured.

Potassium carbonate hemihydrate Potassium carbonate hemihydrate ("potash hydrate") has a temperature between 0 ° C and about 11 ° C.
A stable phase of potassium carbonate in contact with a saturated solution in the range of 0 ° C., which can be recovered by crystallization from a potassium carbonate supersaturated solution. Potassium carbonate 1.
The pentahydrate crystallizes in the form of a glassy, sparkling, substantially dust-free crystal, has a density of 2.155 gcm ^-3 and completely loses water of crystallization at temperatures of 130-160 ° C. Most industrial potassium carbonate production methods involve first obtaining potassium carbonate hemihydrate and firing the potassium carbonate hemihydrate in a rotary tube furnace at 200-350 ° C.
% Potassium carbonate is formed. Crystallized potassium carbonate hemihydrate is dried at 110-120 ° C without this calcination step and sold as potassium hydrate. The standard industrial process for the above products is, for example, the continuous crystallization process (starting material: KOH
And CO ₂ ), fluidized bed method (starting materials: KOH and CO ₂ ), amine method (KOH / CO _{2 in} the presence of isopropylamine (Mines de Pottasse d'Alsace) or KOH / CO ₂ (in the presence of triethylamine) Kali-Chemie AG), or nepheline cooking (mainly former USSR). Ion-exchanger methods (starting materials; KCl and (NH ₄ ) ₂ CO ₃ ), magnesia methods (Engel-Precht method, Neustrassfurter method) as production methods of minor importance or merely of historical interest ; Starting materials: KCl, MgCO ₃ · 3H ₂ O
And CO _2), formic acid - potassium (formate-potash) method (starting material: potassium sulfate, calcium hydroxide and carbon monoxide), Piesteritz method (starting material: potassium sulfate and calcium cyanamide) and Le Blanc method (starting material: Potassium sulfate, calcium carbonate and carbon).

Sodium sesquicarbonate Sodium sesquicarbonate exists in nature as a mineral (trona) and is represented by the formula: Na ₂ CO ₃ .NaHCO ₃ .2H ₂ O. Tronas are abundant in, for example, the United States (Green River, Wyoming), Kenya (Lake Magadi), and the Republic of Sudan (Dongora). African products can be extracted by open-pit quarrying, while US products are mined. The trona has a density of 2.17 gcm ^-3 and a Mohs hardness of 2.5. Usually, trona is used in the production of pure soda. However, it is also possible to obtain pure Na ₂ CO ₃ .NaHCO ₃ .2H ₂ O using the sodium sesquicarbonate method, which is commercially available. Pure sodium sesquicarbonate can also be obtained by leaving sodium bicarbonate in humid air to remove carbon dioxide, or by introducing carbon dioxide into a sodium carbonate solution.

A preferred detergent tablet of the present invention has a weight of 0.5 to 15%, preferably 1.0 to 12.5%, more preferably 1.5 to 10%, most preferably 2.0%, based on the weight of the tablet.
From 1.5 to 7.5% by weight of potassium carbonate 1.5 hydrate and / or sodium sesquicarbonate.

[0015] In addition to potassium carbonate hemihydrate and / or sodium sesquicarbonate used to improve solubility and disintegration time, the detergent tablets described above are representative of detergent components, especially surfactants and / or Contains components selected from the group of builders and / or bleaches. Other ingredients that can be used in the detergent tablets of the present invention are, for example, bleach activators, enzymes, dyes and fragrances, optical brighteners, polymers, antifoams and the like.

[0016] The detergent tablet of the present invention contains a surfactant selected from the group of anionic, nonionic, zwitterionic or cationic surfactants to exhibit cleaning performance,
From the viewpoint of economy and performance, anionic surfactants are particularly preferred.

Anionic surfactants Suitable anionic surfactants are, for example, the anionic surfactants of the sulfonate and sulfate types. Suitable surfactants of the sulfonate type are preferably
C _9-13 alkyl benzene sulphonate, olefin sulphonate, i.e. a mixture of alkenes and hydroxy alkene sulphonates and, for example, sulfonation with sulfur trioxide gas, followed by an alkaline or acidic hydrolysis of the resulting sulphonation reaction product Or a disulfonate obtained from a _C12-18 monoolefin having a terminal double bond. Another suitable surfactant of the sulfonate type is, for example, alkane sulfonates obtained from C _12-18 alkanes by carrying out hydrolysis or neutralization after sulfochlorination or sulfoxidation. Further, esters of α-sulfofatty acids (ester sulfonates) such as hydrogenated coconut oil, palm kernel oil or α-sulfonated methyl ester of tallow fatty acid are also suitable.

[0018] Another suitable anionic surfactant is a sulfonated fatty acid glycerol ester. Fatty acid glycerol esters in the present invention are monoesters, diesters and triesters produced by esterifying monoglycerol with 1-3 moles of fatty acids or transesterifying triglycerides with 0.3-2 moles of glycerol and A mixture of them. Suitable sulphonated fatty acid glycerol esters are C ₆ -C ₂₂ saturated fatty acids, for example sulphonation reaction products such as caproic acid, caprylic acid, capric acid, myristic acid, lauric acid, palmitic acid, stearic acid or behenic acid. is there.

Suitable alkyl (or alkenyl) sulfates are C _12-18 fatty alcohols such as coconut fatty alcohol, tallow fatty alcohol, lauryl, myristyl,
Cetyl or stearyl alcohol) or the sulfuric acid _{semiesters of C10-20} oxoalcohols and the alkali metal salts of the corresponding semiesters of secondary alcohols of the same chain length, especially the sodium salt. Another suitable alkyl (or alkenyl) sulfonate is an alkyl (or alkenyl) of the above-described chain length, comprising a synthetic linear alkyl chain based on petrochemicals and having similar degradability to similar compounds based on oleochemical raw materials. It is sulfate. C _12-16 alkyl sulfates and C _12-15 alkyl sulfates and C _14-15 alkyl sulfates are preferred from the viewpoint of washing technology. Another suitable anionic surfactant is, for example, US 3,234,258 or US
5,075,041 and can be manufactured by Shell Oil Company as DAN (
It is a 2,3-alkyl sulphate which is commercially available under the name ®.

Linear or branched C _7-21 alcohol ethoxylated with 1 to 6 moles of ethylene oxide (eg, 2-methyl branched C _9-11 alcohol containing an average of 3.5 moles of ethylene oxide (EO)) Also suitable are sulfuric acid monoesters of C _12-18 fatty alcohols containing 1-4 EO). These are used in dishwashing detergents in relatively small amounts, for example in amounts of 1 to 5% by weight, in view of their high foaming properties.

Another suitable anionic surfactant, also called sulfosuccinate or sulfosuccinate, is a monoester and / or diester of a sulfosuccinic acid with an alcohol, preferably a fatty alcohol, especially an ethoxylated fatty alcohol. Which is a salt of alkylsulfosuccinic acid. Suitable sulfosuccinates contain _C8-18 fatty alcohol residues or mixtures thereof. Particularly preferred sulfosuccinates comprise fatty alcohol residues derived from ethoxylated fatty alcohols, which by themselves correspond to nonionic surfactants (see description below).
. Of the above-mentioned sulfosuccinates, sulfosuccinates having fatty alcohol residues derived from narrow-range ethoxylated fatty alcohols are particularly preferred. Alkyl (or alkenyl) chains containing preferably 8 to 18 carbon atoms in the alkyl (or alkenyl) chain
Alternatively, alkenyl) succinic acid or a salt thereof can be used.

Another suitable anionic surfactant is in particular soap. A suitable soap is
Saturated fatty acid soaps, such as salts of lauric acid, myristic acid, palmitic acid, stearic acid, hydrogenated erucic acid and behenic acid, and especially soap mixtures derived from natural fatty acids such as coconut oil, palm kernel oil or tallow fatty acid. is there.

Anionic surfactants can be present in the form of sodium, potassium or ammonium salts, including soaps, and as soluble salts of organic bases (eg, mono-, di- or tri-ethanolamine). be able to. The anionic surfactant is preferably present in the form of a sodium or potassium salt, in particular in the form of a sodium salt.

According to the present invention, suitable detergent tablets are 5 to 5 based on the weight of the tablet.
It contains 0% by weight, preferably 7.5 to 40% by weight, particularly preferably 10 to 20% by weight, of anionic surfactant.

The anionic surfactant used in the detergent tablet of the present invention relates to its choice,
There are no fundamental requirements that limit prescribing freedom. However, suitable detergent tablets are:
It has a soap content of more than 0.2% by weight, based on the total weight of the detergent tablet. Suitable anionic surfactants are alkyl benzene sulfonates and fatty alcohol sulfates, and suitable detergent tablets are 2-20% by weight, preferably 2.5-15% by weight, based on the weight of the detergent composition. It preferably contains 5 to 10% by weight of fatty alcohol sulfate.

Nonionic surfactants Suitable nonionic surfactants are alkoxylated (preferably ethoxylated), especially primary alcohols, preferably 8 to 18 carbon atoms and alcohol. It has an average of 1 to 12 moles of ethylene oxide (EO) per mole, and the alcohol component in the nonionic surfactant is linear or preferably has a methyl branch at the 2-position Or it may comprise straight and methyl branched residues in the form of a mixture normally present in oxo alcohol residues. However, alcohol ethoxylates containing straight-chain residues of C ₁₂ -C ₁₈ natural alcohols (eg coconut oil, palm oil, tallow fat or oleyl alcohol) and an average of 2 to 8 EO per mole of alcohol are particularly preferred. Suitable ethoxylated alcohols include, for example, 3EO or 4
C _12-14 alcohol with EO, C _9-11 alcohol with 7EO, 3EO, 5EO, 7EO or 8
C _13-15 alcohols containing EO, 3EO, C _12-18 alcohols, and mixtures thereof including 5EO or 7 EO, such as mixtures, such as the inclusion of the C _12-18 alcohols containing C _12-14 alcohol with 5EO containing 3EO Is done. The above degree of ethoxylation represents a statistical average,
It can be an integer or a fraction for a particular product. Preferred alcohol ethoxylates have a narrow homolog distribution (narrow range ethoxylates, NRE). In addition to the above nonionic surfactants, fatty alcohols containing more than 12 EO, such as 14EO, 25EO,
Tallow fatty alcohols containing 30EO or 40EO can also be used.

Another type of suitable nonionic surfactant, which can be used as the sole nonionic surfactant or in combination with other nonionic surfactants, is alkoxylation ( Preferably ethoxylated or ethoxylated and propoxylated) fatty acid alkyl esters, preferably containing from 1 to 4 carbon atoms in the alkyl chain, in particular, for example, Japanese Patent Application JP 58/217598 Or a fatty acid methyl ester preferably produced by the production method described in WO-A-90 / 13533.

Another type of nonionic surfactant that can be used to advantage is an alkyl polyglycoside (APG). Suitable alkyl polyglycosides have the formula: RO (G) _z . In the above formula, R is a C ₈ -C ₂₂ (preferably C ₁₂ -C ₁₈ ) linear or branched (particularly 2-
(Methyl branched chain) a saturated or unsaturated aliphatic residue, G means a glucose unit having 5 to 6 carbon atoms (preferably glucose). The degree of glycosylation z is 1.0 to 4.0, preferably 1.0 to 2.0, more preferably 1.1 to 1.4.

[0029] Linear alkyl polyglucosides, ie, alkyl polyglycosides in which the polyglycosyl component is a glucose unit and the alkyl component is an n-alkyl group, are preferably used.

The detergent tablets of the present invention can advantageously contain an alkyl polyglycoside, with an APG content of more than 0.2% by weight, based on the total amount of the tablet, being preferred. Particularly preferred detergent tablets comprise APG in an amount of 0.2-10% by weight, preferably 0.2-5% by weight, more preferably 0.5-3% by weight.

Amine oxide type nonionic surfactants (eg N-cocoalkyl-N, N-dimethylamine oxide and N-tallowalkyl-N, N-dihydroxyethylamine oxide) and fatty acid alkanolamide type nonionic surfactants Agents are also suitable.
The dose of these nonionic surfactants is preferably less than the dose of ethoxylated fatty alcohol, in particular less than half the dose of ethoxylated fatty alcohol.

Another suitable surfactant is of formula (II):

Embedded image Wherein RCO is a C ₆ -C ₂₂ aliphatic acyl group, R ¹ is hydrogen or a C ₁ -C ₄ alkyl or hydroxyalkyl group, and [Z] is 3-10 carbon atoms and 3 ~Ten
Linear or branched polyhydroxyalkyl group having one hydroxyl group. ] It is a polyhydroxy fatty acid amide shown by these. The polyhydroxyfatty acid amide is a known substance which can be obtained usually by reductive amination of a reducing sugar with ammonia, an alkylamine or an alkanolamine, followed by acylation with a fatty acid, a fatty acid alkyl ester or a fatty acid chloride. is there.

The group of polyhydroxy fatty acid amides comprises the formula (III):

Embedded image Wherein R is a C ₇ -C ₁₂ linear or branched alkyl or alkenyl group, R ¹ is a C ₂ -C ₈ linear, branched or cyclic alkyl or aryl group, R ² linear C ₁ -C ₈ may branched or cyclic alkyl group or an aryl group or oxyalkyl group (C ₁ -C ₄ alkyl group or phenyl group is preferred), and [Z] is an alkyl chain Is a linear polyhydroxyalkyl group substituted with at least two hydroxyl groups or an alkoxylated (preferably ethoxylated or propoxylated) derivative of the above groups. ] The compound shown by these is also included.

[Z] is preferably a reducing sugar (eg, glucose, fructose, maltose,
Obtained by reductive amination of lactose, galactose, mannose or xylose). The N-alkoxy-substituted or N-aryloxy-substituted compound is then reacted with a fatty acid methyl ester in the presence of a catalyst alkoxide, for example, as taught in WO-A-95 / 07331, It can be converted to polyhydroxy fatty acid amide.

Builders Builders are the most important detergent components, after cleansing substances. The detergent tablets of the present invention may be any of the builders commonly used in detergents, in particular, zeolites, silicates, carboxylates, organic co-builders and (unless environmentally friendly to the use of phosphates). B) a phosphate can be included. Since the above-mentioned builders can also be used on tablets which do not contain surfactants, it is possible according to the invention to produce tablets which can be used for softening soft water.

A preferred crystalline layered sodium silicate has the formula NaMSi _x O _{2x + 1} .yH ₂ O. In the above formula, M is sodium or hydrogen, x is a number from 1.9 to 4, and y is a number from 0 to 20,
Preferred values for x are 2, 3 or 4. Crystalline layered silicates as described above are described, for example, in European Patent Application EP-A-0 164 514. Preferred crystalline phyllosilicates of the above formula are those in which M has a value of sodium and x has a value of 2 or 3. Both β- and δ-sodium disilicate (Na ₂ Si ₂ O ₅ .yH ₂ O) are particularly suitable, and sodium β-disilicate can be prepared, for example, by the process described in WO-A-91 / 08171. Can be obtained by

Another useful builder dissolves with a delay and exhibits multiple wash cycle properties, having a coefficient (modulus, Na ₂ O: SiO ₂ ratio) of 1: 2 to 1: 3.3, preferably 1: 1.21. ~ 1: 2.8, more preferably 1: 2 to 1: 2.6 amorphous sodium silicate. In the case of conventional amorphous silicates, delayed dissolution can be obtained by various methods such as, for example, surface treatment, compounding, compaction or overdrying. In the context of the present invention, the term amorphous silicate is understood to include X-ray amorphous silicate. In other words, in X-ray diffraction experiments, the X-ray diffraction shows a sharp X-ray characteristic of crystalline materials, except for a maximum of one or more scattered X-rays having a diffraction angle width of several degrees. Do not give an image. However, particularly good builder properties can be achieved if the silicate particles give a distorted or sharp diffraction maximum in electron diffraction experiments. This can be taken to mean that the product has microcrystalline regions of a size of 10 to several hundreds of nm (values below 50 nm, especially values below 20 nm are preferred). So-called X that dissolves with a delay compared to ordinary water glass
Linear amorphous silicates are described, for example, in German Patent Application DE-A-44 00 024.
Compressed amorphous silicates, compounded amorphous silicates and overdried X-ray amorphous silicates are particularly preferred.

The synthetic microcrystalline zeolite containing bound water used in the present invention is preferably a zeolite.
And A and / or Zeolite P. Zeolite MAP (registered trademark: Crosfield)
Is a particularly preferred P-type zeolite. However, zeolites X and A, X and / or
Or mixtures of P are also suitable. In the present invention, for example, CONDEA Augusta S.p.A.
It is sold under the name VEGOBOND AX® and has the formula: nNa_TwoO ・ (1-n) K_TwoO ・ Al_TwoO _Three ・ (2 ~ 2.5) SiO_Two・ (3.5-5.5) H_TwoZeolites X and Zeola that can be denoted by O
A co-crystallized product of zeolite A (zeolite X about 80% by weight) can also be used. Above
Olite is suitable as a builder in granular compounds and throughout the tableted mixture.
It can also be used as a type of "powder" used. Suitable
Zeolite has an average particle size of less than 10 μm (measured by a Coulter counter method)
Volume distribution), preferably 18 to 22% by weight, more preferably 20 to 22% by weight.
Contains bound water.

Of course, the commonly known phosphates can also be used if the use of these phosphates is not to be avoided environmentally. The sodium salts of orthophosphoric acid, pyrophosphoric acid and especially tripolyphosphoric acid are particularly preferred.

Useful organic builders are, for example, polycarboxylic acids which can be used in the form of sodium, provided that they are not environmentally hazardous, such as citric, adipic, succinic, glutaric, tartaric, sugar acids , Aminocarboxylic acid, nitrilotriacetic acid (
NTA). Suitable salts are salts of polycarboxylic acids, such as salts of citric acid, adipic acid, succinic acid, glutaric acid, tartaric acid, sugar acids and mixtures thereof.

[0041] To facilitate the disintegration of disintegrating agents strongly compressed tablet, disintegrants, a so-called tablet disintegrators were mixed in the tablet, can it be to shorten the disintegration time of the tablet. Roempp (9th edition, volume 6, page 4440) and Voigt "L
ehrbuch der pharmazeutischen Technologie "(6th edition, 1997, pp. 182-184)
According to the disintegrant or disintegrant is an auxiliary agent which promotes the rapid disintegration of the tablet in water or gastric juice and the release of the medicament in a resorbable form.

[0042] Based on the effects they have, also referred to as "disintegrants", these substances can cause an increase in volume on contact with water, thus increasing their own volume (swelling) on the one hand and on the other hand The release of gas can create a pressure that breaks the tablet into relatively small particles. Well-known disintegrants are for example carbonate / citric acid systems, but other organic acids can be used. Swellable disintegrants are, for example, synthetic polymers such as polyvinylpyrrolidone (PVP), natural polymers and modified natural substances, for example cellulose and starch and their derivatives, alginate or casein derivatives.

Suitable detergent tablets contain from 0.5 to 10% by weight, preferably from 1 to 5% by weight, more preferably from 2 to 4% by weight, based on the weight of the tablet.

According to the present invention, preferred disintegrants are cellulosic disintegrants, so suitable detergent tablets are 0.5 to 10% by weight, preferably 1 to 5% by weight, more preferably 2 to 4% by weight.
It contains a cellulosic disintegrant in an amount by weight. Pure cellulose has the empirical formula (C ₆ H ₁₀ O ₅ ) _{n and} is formally a cellobiose β-1,4-polyacetal, and cellobiose consists of two molecules of glucose. Preferred celluloses consist of about 500-5000 glucose units and thus have an average molecular weight of 50,000-500,000. In the present invention, a cellulose derivative that can be obtained from cellulose by a polymer-analogous reaction can also be used as a cellulosic disintegrant. The above-mentioned chemically modified cellulose includes, for example, a product of an esterification or etherification reaction in which a hydroxy hydrogen atom is substituted. However, a substituted cellulose in which a hydroxyl group is substituted by a functional group which does not bind via an oxygen atom can also be used as a cellulose derivative. The group of cellulose derivatives includes, for example, alkali metal cellulose, carboxymethyl cellulose (CMC), cellulose esters, cellulose ethers and aminocellulose.

The above-mentioned cellulose derivatives are preferably used as a cellulosic disintegrant not alone but in the form of a mixture with cellulose. The content of the cellulose derivative in the mixture as described above is preferably less than 50% by weight, more preferably less than 20% by weight, based on the cellulosic disintegrant. In one particularly preferred embodiment, pure cellulose without cellulose derivatives is used as the cellulosic disintegrant.

[0046] Microcrystalline cellulose can be used as another cellulosic disintegrant or as part of the components described above. This microcrystalline cellulose attacks only the amorphous region of cellulose (about 30% of the total amount of cellulose) and completely dissolves it, but under the condition that the crystalline part (about 70%) is not damaged. Obtained by partial hydrolysis of cellulose. Next, deagglomeration of the microfine cellulose produced by the hydrolysis occurs, resulting in microcrystalline cellulose that has a primary particle size of about 5 μm and can be compressed into granules with an average particle size of, for example, 200 μm. .

Method of Making Tablets General Detergent tablets are made by pressing the mixture to be tableted into the cavity of a press. Simplest tablet manufacturing (hereinafter simply called tableting)
In the method, the mixture to be compressed is compressed directly, ie, without prior granulation. The advantage of this so-called direct compression is that it is simple and inexpensive to apply since there are no other steps and therefore no other equipment is required. But these advantages are offset by disadvantages. For example, the powder mixture to be pressed directly must have sufficient plastic deformability and good flowability, and must not show a tendency to separate during storage, transport and filling of the die. Unfortunately, meeting the above three requirements is extremely difficult for many mixtures, so direct compression is less applicable, especially in the manufacture of detergent tablets. Thus, in a typical detergent tablet manufacturing process, starting from the powdered component ("primary particles"), the powdered component is agglomerated or granulated in a suitable manner into secondary particles having a larger particle size. Next, these granules or a mixture of different granules is mixed with the individual powdery additives and the resulting mixture is compressed.

According to the present invention, suitable detergent tablets are obtained by tableting a granular premix of at least one batch of surfactant-containing granules and at least one subsequently mixed powdered component. The surfactant-containing granules are compressed, extruded, mixer granulated,
It can be manufactured by a usual granulation method such as pelletization or fluidized bed granulation. As far as the following detergent tablets are concerned, it is advantageous that the bulk density of the premix to be compressed is close to that of a standard compact detergent. In one particularly preferred embodiment, the premix to be compressed has a bulk density of at least 500 g / l, preferably at least 600 g / l, more preferably greater than about 700 g / l.

Potassium carbonate hemihydrate and / or sodium sesquicarbonate The potassium carbonate hemihydrate and / or sodium sesquicarbonate used to improve the solubility of the tablets may be added to the premix just prior to tableting. It only needs to be added, but it may be part of a granule or compound, and the effect of potassium carbonate 1.5 hydrate and / or sodium sesquicarbonate is not impaired even as part of the granule or compound. In a preferred detergent tablet, potassium carbonate hemihydrate and / or sodium sesquicarbonate is a component of the premix or a component of the premix that is subsequently mixed.

In order to compress the granular premix to form a detergent tablet, the granular premix may be powdered with a particulate surface treatment. This is a premix (storage,
It is advantageous for the quality and physical properties of both the tableting) and the final wash tablet. Particulate powders are conventionally known in the art, and zeolites, silicates and other inorganic salts are commonly used. Preferably, however, the premix is pulverized with zeolite particles. Further, faujasite-type zeolites are preferred. In the context of the present invention, the expression “faujasite-type zeolite” refers to a zeolite structure group
Encompasses all three zeolites that make up the four faujasite subgroups (Donald W
See Breck "Zeolite Molecular Sieves" John Wiley & Sons, New York / London / Sydney / Toronto, 1974, p. 92). Therefore zeolite X
In addition, zeolites Y and faujasite and mixtures of said compounds can also be used, pure zeolites X being preferred.

Mixtures or co-crystals of faujasite type zeolites with other zeolites (which need not belong to zeolite structure group 4) can also be used for powdering,
If so, advantageously at least 50% by weight of the pulverized material comprises zeolite of the faujasite type.

According to the present invention, a preferred detergent tablet consists of a granular premix comprising a granular component and a subsequently mixed powdery component, wherein said finely divided component or one of said finely divided components is subsequently mixed. , Having a particle size of less than 100 μm, preferably less than 10 μm and more preferably less than 5 μm, at least 0.2% by weight of the premix to be compressed
Preferably, it is a faujasite-type zeolite which accounts for at least 0.5% by weight, more preferably more than 1% by weight.

Other Ingredients In addition to or instead of the above ingredients, surfactants, builders and disintegrants, the cleaning tablets of the present invention may comprise bleaching agents, bleaching activators, enzymes, fragrances, fragrance carriers, It may contain other representative detergent components selected from the group of fluorescent agents, dyes, foam control agents, silicone oils, anti-redeposition agents, optical brighteners, anti-fading agents, dye transfer inhibitors and preservatives. be able to.

[0054] Among the compounds which form H ₂ O ₂ which serve as bleaching agents the bleaching agent in water, sodium perborate tetrahydrate and sodium perborate monohydrate are particularly important. Other useful bleaching agents are, for example, sodium percarbonate, peroxypyrophosphate, citrate perhydrate-forming or hydrogen peroxide-forming persalts or peracids, perbenzoates, peroxophthalates Acid salts, diperazelinic acid, phthalimido peracid or diperdodecane diacid. If bleaches are used, surfactants and / or builders can be omitted so that pure bleach tablets can be produced. If such a bleaching agent is to be used for washing, a combination of sodium percarbonate and sodium sesquicarbonate is preferably used, regardless of what other ingredients the tablet contains. When preparing detergents or bleach tablets for dishwashers, bleaching agents selected from the group of organic bleaches can also be used. Representative organic bleaches are diacyl peroxides, such as, for example, dibenzoyl peroxide. Another typical organic bleach is a peroxy acid, of which alkyl peroxy acids and aryl peroxy acids are specifically mentioned as examples. Preferred representatives include (a) peroxybenzoic acid and ring-substituted derivatives thereof,
(B) aliphatic or substituted aliphatic peroxy acids such as, for example, alkyl peroxybenzoic acid, but also peroxy-α-naphthoic acid and magnesium monoperphthalate, such as peroxylauric acid, peroxystearic acid, ε-phthalimidoperoxycaproic acid Acid [phthaloiminoperoxyhexanoic acid (PAP)], o
-Carboxybenzamide peroxycaproic acid, N-nonenylamide peradipic acid and N-nonenylamide persuccinate, and (c) aliphatic and aryl fatty acid peroxydicarboxylic acids such as 1,12-diperoxycarboxylic acid, 1,9-
With diperoxyazelaic acid, diperoxysebacic acid, diperoxybrasilic acid, diperoxyphthalic acid, 2-decyldiperoxybutane-1,4-diacid, N, N-terephthaloyl-di (6-aminopercaproic acid) is there.

Other suitable bleaching agents in dishwasher tablets are chlorine and bromine releasing substances. Suitable chlorine or bromine releasing substances are, for example, heterocyclic N-bromoamides and N-
Chloramides such as isocyanuric acid and / or dichloroisocyanuric acid (
DICA) and / or their salts with cations such as potassium and sodium. Hydantoin compounds such as 1,3-dichloro-5,5-dimethylhydantoin are also suitable.

[0056] To improve the bleaching effect when subjected to washing with bleach activators 60 ° C. or lower temperatures,
The bleach activators can also be mixed as such or as part of component b). The bleach activator is preferably C ₁ -C ₁₀ under perhydrolysis conditions.
It may be a compound that produces (more preferably C ₂ -C ₄ ) aliphatic peroxocarboxylic acids and / or optionally substituted perbenzoic acids. Substances that carry an O-acyl and / or N-acyl group and / or an optionally substituted benzoyl group having the number of carbon atoms described above are preferred. Suitable bleach activators are polyacylated alkylenediamines, especially tetraacetylethylenediamine (TAED), acylated triazine derivatives, especially 1,5-diacetyl-2,4-dioxohexahydro-1,3,5-triazine (
DADHT), acylated glycoluril, especially tetraacetylglycoluril (T
AGU), N-acylimides, especially N-nonanoylsuccinimide (NOSI), acylated phenolsulfonates, especially n-nonanoyl or isononanoyloxybenzenesulfonates (n- or iso-NOBS), carboxylic anhydrides, especially phthalic anhydride And acylated polyhydric alcohols, especially triacetin, ethylene glycol diacetate and 2,5-diacetoxy-2,5-dihydrofuran.

Bleaching Catalysts In addition to, or instead of, the conventional bleach activators described above, so-called bleach catalysts can also be compounded in the tablets. The bleaching catalyst is a bleach-enhancing transition metal salt or complex such as, for example, manganese, iron, cobalt, ruthenium or molybdenum-salen or carbonyl complexes. Complexes of manganese, iron, cobalt, ruthenium, molybdenum, titanium, vanadium and copper with nitrogen-containing tripod ligands and cobalt, iron and ruthenium-amine complexes can also be used as bleach catalysts.

Enzymes Suitable enzymes are enzymes selected from proteases, lipases, amylases, cellulases or mixtures thereof. Bacillus subtilis, Bacillus licheniformis and Streptomyces griseus ( Stre
Enzymes obtained from bacterial strains such as ptomyces griseus ) or fungi are particularly preferred. Subtilisin-type proteases are preferred and Bacillus lentus (Baci
llus lentus) are particularly preferred. Of particular interest are, for example, protease and amylase or protease and lipase or protease and cellulase mixtures, or cellulose and lipase mixtures, or proteases, amylase and lipase mixtures, or protease, lipase and cellulase mixtures, and especially cellulase-containing mixtures. Peroxidase or oxidase has also been found to be suitable in some cases.
Enzymes can be adsorbed on a carrier and / or encapsulated in a membrane material to prevent premature degradation of the enzymes. Enzymes in the detergent of the present invention,
The content of enzyme mixture or enzyme granules can be, for example, about 0.1-5% by weight,
Preferably it is 0.1 to about 2% by weight.

Antifouling agent Further, the detergent tablet of the present invention may contain a component (so-called antifouling agent) having a good effect on the removal of oils and fats from the cloth by washing. The above-mentioned effects become particularly apparent when a cloth which has been repeatedly washed with the detergent of the present invention containing the above-mentioned oil-and-fat-soluble component is soiled. Suitable fat-soluble ingredients include, for example, non-ionic cellulose ethers such as methyl cellulose, and 15% based on the non-ionic cellulose ether.
Such as methylhydroxypropylcellulose containing -30% by weight of methoxyl groups and 1-15% by weight of hydroxypropyl groups, and polymers of phthalic acid and / or terephthalic acid known from the prior art or derivatives thereof, in particular ethylene terephthalate and And / or polyethylene glycol terephthalate or derivatives thereof modified to be anionic and / or nonionic. Among the above fat-soluble components, phthalic acid and sulfonated derivatives of terephthalic acid polymer are particularly preferred.

Fluorescent Whitening Agent The above-mentioned detergent tablet may contain a derivative of diaminostilbene disulfonic acid or an alkali metal salt thereof as a fluorescent whitening agent. Suitable optical brighteners are, for example, 4,4'-bis (2-anilino-4-morpholino-1,3,5-triazinyl-6-amino) stilbene-2,2'-disulfonic acid or morpholino groups Is a salt of a compound of similar composition containing a diethanolamino group, a methylamino group, an anilino group or a 2-methoxyethylamino group. Brighteners of the substituted diphenylstyryl type, for example 4,4 '
Alkali metal of -bis (2-sulfostyryl) biphenyl, 4,4'-bis (4-chloro-3-sulfostyryl) biphenyl or 4- (4-chlorostyryl) -4 '-(2-sulfostyryl) biphenyl Salts may be included. Mixtures of the above optical brighteners can also be used.

To improve the aesthetic impression produced by perfume and dye products and to provide consumers with a visually and sensorially "typical and error free" product as well as the required cleaning performance, dyes And flavoring agents are added to the detergent tablets of the present invention. Suitable balms or perfumes include
Individual aroma compounds, such as esters, ethers, aldehydes, ketones, alcohols and synthetic products of the hydrocarbon type are included. The ester type aromatic compound is
For example, benzyl acetate, phenoxyethyl isobutyrate, p-tert-butylcyclohexyl acetate, linalyl acetate, dimethylbenzylcarbinyl acetate, phenylethyl acetate, linalyl benzoate, benzyl formate, ethyl methyl phenyl glycinate, allyl cyclohexyl propionate, propion Styralyl acid and benzyl salicylate. Ethers include, for example, benzyl ethyl ether. Aldehydes include, for example, C ₈ -C ₁₈ linear alkanals, citrals,
Includes citronellal, citronellyl oxyacetaldehyde, cyclamenaldehyde, hydroxycitronellal, linal and burgeonal.
Ketones include, for example, ionone, α-isomethylionone, and methylseryl ketone. Alcohols include anethole, citronellol, eugenol, geraniol, linalool, phenylethyl alcohol and terpineol. Hydrocarbons include in particular terpenes such as limonene and pinene. However, mixtures of various fragrances which give an overall attractive aroma are preferably used. Perfume oils as described above may include natural perfume mixtures obtainable from vegetable sources, such as pine, citrus, jasmine, patchouli, rose or ylang-ylang oil. Salvia oil, chamomile oil, clove oil, melissa oil, mint oil, laurel oil, lime flower oil, juniper oil, vetiver oil, olivenam oil, galvanum oil and labdanum oil and orange flower oil, neroli oil, orange peel oil and Sandalwood oil is also suitable.

The detergent tablets of the invention usually contain less than 0.01% by weight of a dye while
The fragrance can make up as much as 2% by weight of the total composition.

The perfume can be mixed directly with the detergents of the present invention, but may be added to a carrier that enhances the adhesion of the perfume to the laundry and gives the fabric a longer lasting fragrance by releasing the perfume more slowly. It is also advantageous to attach A suitable carrier material is, for example, cyclodextrin, and the cyclodextrin / perfume complex is optionally coated with other auxiliaries.

In order to improve the aesthetic impression of the detergent according to the invention, the detergent according to the invention can be colored with a suitable dye. The choice of a suitable dye is not difficult for the expert, but a suitable dye has a high storage stability, is not affected by other components of the detergent or by light, and is woven so as not to color the textile fibers. It has no noticeable directness to the fiber.

Method for Producing Tablets The tablet of the present invention is prepared by first dry-mixing the components (which may be completely or partially pre-granulated) and then mixing the obtained premix by a conventional method. Molding
/ Shaped, especially manufactured by tableting. To manufacture the tablet of the present invention, the premix is sandwiched between two punches in a die and compressed to obtain a dense compressed body.
This process, hereinafter abbreviated as tableting, consists of four steps: metering, compression (elastic deformation), plastic deformation and ejection.

The premix is first put into a die. The level of filling, and thus the weight and shape of the resulting tablet, depends on the position of the lower punch (lower punch) and the shape of the die. Uniform metering even at high tablet throughput is preferably achieved by volumetric measurement of the premix. As the tableting process progresses, the upper punch (upper punch)
Makes contact with the premix and continues descending towards the lower punch. During this compression stage, the particles of the premix are compacted to one another and the void volume of the filling between the punches continues to decrease. The plastic deformation phase, in which the particles coalesce to form a tablet, begins when the upper punch is at a certain location (and thus at a certain pressure on the premix). Depending on the physical properties of the premix, partial crushing of the constituent particles of the premix also occurs, and the premix sinters at higher pressures. As the tableting speed increases, i.e., at higher throughputs, the formed tablet can have more or less large voids, as the elastic deformation stage becomes progressively shorter. In the final stage of the tableting process, the tablet is extruded from the die by a lower punch and conveyed along a conveyor. At this stage, only the weight of the tablet is crucially established. Because tablets can still change shape and size as a result of physical processes (reexpansion, crystallographic effects, cooling, etc.).

The above tableting process is performed in principle on a commercially available tableting machine equipped with one or two punches. When a tableting machine is equipped with two punches, not only the upper punch is used to apply pressure, but also the lower punch moves while pressing the lower punch during tableting. . When the production volume is small, it is preferable to use an eccentric tableting machine in which a punch is fixed to an eccentric plate, and the eccentric plate is mounted on a shaft rotating at a constant speed. The movement of these punches is similar to the operation of a normal four-stroke engine. Tableting can be performed with one upper punch and one lower punch, but it is also possible to fix several punches to one eccentric plate, in which case the number of holes in the die should be increased accordingly . The throughput of the eccentric press varies from several hundred to up to 3000 tablets / hour depending on the type.

For larger throughputs, rotary tablet presses are generally used. In a rotary tableting machine, a relatively large number of dies are arranged in a circle on a so-called die table.
The number of dies varies from 6 to 55 depending on the model, but more dies are commercially available. The upper and lower punches are associated with each die on the die table, where again the tablet forming pressure is not only actively applied by the upper or lower punches, but also by both punches. The die table and punch move about a common vertical axis,
The punch is guided to the filling, compression, plastic deformation and unloading positions by curved guide rails. In areas where the punches need to be raised and lowered to a particularly large extent (filling, compressing, unloading), the curved guide rail is supported by additional depressing members, pull-down rails and unloading channels. The die is filled from a fixed arrangement supply unit, the so-called filling shoe, connected to the storage container of the compound. The pressure on the premix can be adjusted individually with tools for the upper and lower punches, and the pressure is increased by rolling the punch shaft head through adjustable pressure rolls.

To increase throughput, the rotary press can be equipped with two filling shoes so that tablets can be manufactured by passing only half way around the circumference. To produce a two-layer or multilayer tablet, several filling shoes are placed one after the other without removing the lightly compressed first layer before further filling. With proper process control, shells and bullseye tablets (having a structure similar to onion skin) can also be manufactured in the manner described above. In the case of a bullseye tablet, the upper surface of the core or, to be precise, the upper surface of the core layer is not covered and is therefore visible. A rotary tableting machine may be fitted with one or more punches so that, for example, an outer circle with 50 holes and an inner circle with 35 holes can be used simultaneously for tableting. it can. Modern rotary tablet presses have a throughput of over one million tablets per hour.

Tablet presses suitable for the purposes of the present invention can be obtained, for example, from the following companies:
Apparatebau Holzwarth GbR (Asperg), Wilhelm Fette GmbH (Schwarchenbeck), Hofer GmbH (Vail), KILIAN (Cologne), KOMAGE (Ker Amsee), KORSCH Pressen GmbH (Berlin), Mapag Maschinenbau AG (Berne, Switzerland) and Courtoy NV (Belgium / Luxembourg Halle). One example of a particularly suitable tablet press is the model HPF630 hydraulic double pressure press from LAEIS, D.

Tablets can be manufactured in certain shapes and sizes. Suitable shapes are virtually any convenient shape, such as slabs, bars, cubes,
Squares, and corresponding shapes with flat sides, and especially cylinders with circular or elliptical cross sections. This cylindrical embodiment encompasses shapes ranging from tablets to compact cylinders having a height diameter ratio of greater than one.

The split compacts can be formed as independent individual elements corresponding to a predetermined dose of detergent. However, it is also possible to form a compression molded body having several of the above units in one compression molded body. The smaller the division unit, the easier it is to disintegrate, especially by providing a predetermined weak portion. Laundry detergent for standard European type washing machines with machinery arranged horizontally,
It is advantageous to produce the split compacts as cylindrical or square tablets, preferably having a diameter height ratio of about 0.5: 2 to 2: 0.5. Commercially available hydraulic press,
Eccentric presses and rotary presses are particularly suitable for producing such compacts.

The three-dimensional shape of another embodiment of the tablet of the present invention is such that the tablet is directly placed in the detergent introduction chamber (
It is dimensioned to fit directly into the detergent chamber of a commercial home washing machine so that it can be inserted directly (without using the dosing aid) and dissolve the tablet in the detergent chamber when it comes into contact with water. However, it is of course easy to use a detergent tablet together with the dosing aid, which is preferred in the present invention.

Another suitable tablet that can be manufactured has alternating thick and long sections and thin and short sections, and separates individual sections from this “bar” at predetermined weaknesses corresponding to the short and thin sections described above. It has a plate-like or plate-like (slab) -like structure that can be put into a washing machine. The principle of this "bar" can also be embodied in other geometric shapes, for example in a vertical triangle which is only connected to one of the longitudinal sides.

However, in another possible embodiment, rather than compressing the various components into one tablet, the resulting tablet comprises several layers, ie at least two layers. These various layers can have different dissolution rates. This results in a tablet with favorable performance characteristics. For example, if the tablet contains components that adversely affect each other, incorporate one component into the fast-dissolving layer and incorporate the other component into the slow-dissolving layer, until the second component dissolves. Can be such that the first component has already disappeared. The various layers of the tablet can be arranged in a stack, in which the inner layer dissolves at the edge of the tablet before the outer layer has completely dissolved. However, as another option, the inner layer can be completely covered with a further outer layer to prevent the components of the inner layer from prematurely dissolving.

In another preferred embodiment of the present invention, the tablet comprises at least three layers (ie two outer layers and at least one inner layer), wherein at least one of the inner layers contains a peroxy bleach, whereas a stacked tablet In the case of the above two coating layers,
In the case of an envelope type tablet, the outermost layer does not contain a peroxy bleach. In another possible embodiment, the peroxy bleach and the respective bleach activator or bleach catalyst and / or enzyme present are spatially separated from one another in one and the same tablet. In a multilayer tablet as described above, not only can the tablet be used by a detergent charging chamber or a detergent charging unit added to the cleaning liquid, but in the case of the tablet as described above, the tablet is brought into direct contact with the fabric. There is an advantage that there is no danger of causing stains due to a bleaching agent even when put in a washing machine.

A similar effect can be obtained by coating the individual components of the detergent composition to be compacted or the whole tablet. To achieve this goal,
The tablets to be coated can be sprayed, for example, with aqueous solutions or emulsions, or they can be coated in a manner called melt coating.

After compression, the detergent tablets have a high stability. The fracture resistance of a cylindrical tablet can be determined by the diametral fracture stress. And its diameter fracture stress can be determined according to the following equation: Φ = 2P / BDt. In the above equation,
Φ is the diameter breaking stress (DFS) (Pa), P is the force that exerts pressure on the tablet to cause tablet disintegration (N), D is the tablet diameter (m) and t is the tablet height It is.

In another aspect of the present invention, the present invention provides the use of potassium carbonate hemihydrate and / or sodium sesquicarbonate to increase the breaking hardness of detergent tablets while reducing the dissolution rate. I do. The effect of potassium carbonate hemihydrate and / or sodium sesquicarbonate used according to the invention is that the detergent dissolves at a rate not significantly different from the average value, despite the fluctuations in the tableting pressure for the premix to be tableted. What you get is a tablet. In this way a higher security in the manufacture of the tablet is guaranteed.

[0080]

【Example】

Preparation of Detergent Tablets A premix was prepared by mixing the surfactant-containing granules with the powdered compounding ingredients, and the resulting premix was converted to detergent tablets on a Korsch tablet press. The tableting pressure was adjusted to obtain three series of tablets with different hardness. The premix that provides the tablets E1 and E2 of the invention contains 4% by weight of potassium carbonate 1.5 hydrate or sodium sesquicarbonate. In contrast, Tablet C
Comparative premixes providing 1 and C2 each contain anhydrous potassium carbonate,
Or none of the above substances. Tables 1 and 2 show the composition of the surfactant granules and the composition of the premix to be compressed (and therefore the composition of the tablet).
Shown in

TABLE 1 Composition of surfactant granules (% by weight)

[0081]

Table 2: Premix composition (% by weight)

The use of anhydrous potassium carbonate (C1) results in a tablet characterized by minimal variation in dissolution rate despite variations in tableting pressure. Also not shown. The advantage of the present invention that tablet C2 softens during storage (in some cases considerably) and eliminates process uncertainties due to fluctuations in tableting pressure is not observed here. This is because the manufacturing uncertainty simply shifted to the storage stage.

After storage for 2 days, tablet hardness was measured by deforming the tablet until the tablet broke. The force was applied to the side of the tablet and the maximum force the tablet could withstand was measured.

To examine the disintegration of the tablet, a glass beaker filled with water (600 ml of water)
At a temperature of 30 ° C.) and the time required for the tablet to completely disintegrate was measured.

The experimental data is shown in Table 3.

[0086]

[Table 3] Detergent tablets (physical data)

────────────────────────────────────────────────── ─── Continuing the front page (72) Inventor Zantra Witt-Newsline Federal Republic of Germany-40,664 Langenfeld, Ludwig-Wolker-Strasse 25 (72) Inventor Monica Becker Federal Republic of Germany-42799 Reichlin Gen. Im Rotfeld 14 (72) Inventor Michael Feist D-40667 Meerbusch, Bruhler Wech 58a (72) Inventor Fret Shamville D-DE 40789 Monheim, Niederstrasse No. 96 (72) Inventor Bernhard Müller Federal Republic of Germany Day-56332 Alken, Kertenstrasse No. 2 F-term (reference) 4H003 AB03 AB19 AC08 BA17 DA01 DA05 DA19 EA28 EB12 EB15 EB16 EB22 EB24 EB30 EB32 EB42 ED02 FA32 FA43

Claims (9)

[Claims] 1. A compressed granular detergent detergent tablet comprising a surfactant and / or a builder and / or a bleach and optionally other detergent components, said detergent tablet comprising potassium carbonate hemihydrate. And / or a tablet comprising sodium sesquicarbonate. 2. The detergent tablet according to claim 1, wherein the weight of the tablet is 0.5 to 1%.
Claims comprising potassium carbonate hemihydrate and / or sodium sesquicarbonate in an amount of 5% by weight, preferably 1.0-12.5% by weight, more preferably 1.5-10% by weight, most preferably 2.0-7.5% by weight. The tablet according to item 1. 3. The tablet according to claim 1, wherein the tablet further contains a cellulosic disintegrant. 4. The detergent tablet according to claim 1, wherein said detergent tablet is obtained by tableting a granular premix of at least one surfactant-containing granule and at least one powdered component to be subsequently mixed. Tablet according to any of the above. 5. Tablet according to claim 4, wherein the premix to be compressed has a bulk density of at least 500 g / l, preferably at least 600 g / l, more preferably more than 700 g / l. 6. The component to be mixed later is potassium carbonate 1.5 hydrate and / or
6. The tablet according to claim 4, which is sodium sesquicarbonate. 7. The component to be subsequently admixed is a faujasite-type zeolite having a particle size of less than 100 μm, preferably less than 10 μm, more preferably less than 5 μm, said component being tableted. A tablet according to any of claims 4 to 6, comprising at least 0.2%, preferably at least 0.5%, more preferably more than 1% by weight of the premix. 8. A bleach activator, an enzyme, a pH regulator, a fragrance, a fragrance carrier,
2. The method according to claim 1, further comprising one or more substances selected from the group consisting of a fluorescent agent, a dye, an antifoaming agent, a silicone oil, an anti-redeposition agent, an optical brightener, an anti-fading agent, a dye transfer inhibitor and a preservative. A tablet according to any one of claims 1 to 7. 9. Use of potassium carbonate 1.5 hydrate and / or sodium sesquicarbonate to increase the breaking hardness of detergent tablets and at the same time reduce the dissolution rate.